A thin film getter for absorbing alkane gases and a method for producing the same

Abstract

The present application relates to the technical field of thin film getter, especially to IPC C23C14, more particularly to a thin film getter for absorbing alkane gas and a preparation method thereof. The present application provides a thin film getter for absorbing alkane gas, which is composed of a main element A, a necessary element and an optional element; the content of the main element A is 50wt%-95wt%, the content of the necessary element is 0.3-30wt%, and the content of the optional element is 0-20wt%; the necessary element includes one or both of Re and Ir. The thin film getter in the present application has high absorption capacity for methane gas, high bonding strength with the substrate, and improved service life and application range of the thin film getter.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of thin film getter, in particular to IPC C23C14, more particularly to a thin film getter for absorbing alkane gas and a preparation method thereof. BACKGROUND

[0002] In recent years, micro-electro-mechanical system (MEMS) technology makes traditional vacuum sensors more miniaturized and has significant advantages, such as smaller size, lower power consumption, higher sensitivity, better dynamic range, and lower production cost. Thin film getters have key applications in different instruments due to their large room temperature gettering rate and amount, high deposition precision, small space occupancy, and compatibility with activation process and packaging bonding process, which significantly improve their reliability, stability, and service life.

[0003] The existing patent CN201910983447.8 discloses a preparation method of a getter material with a surface high-flux gas distribution system. The raw materials in the getter alloy are prepared into an alloy by melting, and the getter alloy powder is uniformly mixed with stearic acid to form an alloy mixture after crushing and ball milling. The compact is pressed and vacuum sintered to obtain a bulk getter. Compared with traditional flaky getter materials, the bulk getter not only allows gas to flow through a certain channel, but also removes impurity gases in the main flow of gas during the flow of gas, achieving the effect of gas-gas separation. However, the bulk getter has weak bonding ability with the substrate, and has weak and slow absorption capacity for methane gas.

[0004] The existing patent CN202310088961.1 discloses a getter film for improving the gettering capacity of carbon-containing gas. A 0.1-15 μm getter film is deposited on the surface of a stainless steel, Kovar, silicon, germanium, or ceramic substrate by PVD method. The getter film contains one or both of titanium and zirconium, and also contains tungsten, molybdenum, or any combination thereof in a weight percentage of 0.5-20% of the total weight of the getter film, and optionally vanadium, manganese, cobalt, yttrium, and aluminum. The getter film has a certain effect on improving the gettering capacity of CO, CO2, CH4, and other carbon-containing gases, but there is no specific data to verify the gettering effect and load strength for alkane gases. SUMMARY

[0005] To solve the problems in the prior art, the present application provides a thin film getter for absorbing alkane gas in the first aspect, which comprises a main element A, a mandatory element, and an optional element. The content of the main element A is 50wt%-95wt%, the content of the mandatory element is 0.3-30wt%, and the content of the optional element is 0-20wt%. The mandatory element includes one or both of Re and Ir.

[0006] Preferably, the main element A comprises one or more of Ti, Zr, Ta, Nb.

[0007] Preferably, the optional element comprises one or more of V, Co, Fe, Mn, Cr, Al, Sm, Nd, Y.

[0008] Preferably, the main element A content is 60wt% to 94wt%; the essential element content is 0.3 to 28wt%; the optional element M content is 0 to 19wt%.

[0009] Further preferably, the main element content is 65wt% to 93wt%; exemplary are 80wt%, 81wt%, 82wt%, 83wt%, 84wt%, 85wt%, 86wt%, 87wt%, 88wt%, 89wt%, 90wt%, 91wt%, 92wt%, 93wt%.

[0010] Further preferably, the essential element content is 0.3 to 25wt%; exemplary are 0.3wt%, 0.5wt%, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt%, 20wt%, 21wt%, 22wt%, 23wt%, 24wt%, 25wt%.

[0011] Further preferably, the optional element M content is 0 to 15wt%; exemplary are 0wt%, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%.

[0012] Preferably, the thin film getter has a thickness of 0.5 to 20μm.

[0013] In the present application, by adding the essential element Ir, Re, the thin film getter has the ability to absorb alkane gas, especially to effectively absorb methane gas, and has high absorption performance. Among all methane gas, the methane molecule structure has high symmetry, so the van der Waals radius of CH group is the largest, such as -CH3 is about 200pm, and the van der Waals of hydrogen is 120pm. The van der Waals radius of methane is larger than that of all other chemical gases. At the same time, the bond energy of C-H of methane is also the largest, which is: 416.2(kJ*mol -1 ). Each C and 4H are connected, that is, there are four C-H bonds, and the total bond energy is 1652kJ*mol -1Methane gas is difficult to dissociate and absorb because it has greater bond energy than other kinds of gas. For CH4 absorption, the adsorption process is sequentially divided into physical adsorption, chemical adsorption and diffusion. Chemical adsorption is important, and chemical adsorption occurs under the condition that exchange and transfer of electrons between gas molecules and gas adsorbing material occurs, gas molecules are dissociated into atoms by the gas adsorbing material, and the atoms diffuse to the inside of the gas adsorbing cell or the defect of the gas adsorbing material. The gas adsorbing material first breaks the C-H bond in the CH4 gas molecule by using the valence electron in its own compound, and then absorbs the C and H atoms in the chemical adsorption mode into the crystal cell position or defect position of the gas adsorbing compound. Because the bond energy of CH4 is large, the energy required for the gas adsorbing material to break the C-H bond and dissociate into C and H atoms is large, which is the reason why it is more difficult to absorb methane gas than other kinds of gas.

[0014] The present inventors have found that a rhenium atom has 75 electrons, and its valence electron configuration is [Xe]4f 14 5d 5 6s 2 The number of outer valence electrons is 7, and the 2 electrons in the 5s electron structure belong to the Fermi level. The valence electron configuration of iridium is [Xe]4f 14 5d 7 6s 2 The number of valence electrons is 7+2=9, and there are many valence electrons. Due to the special properties of the valence layer configuration of rhenium atoms and iridium atoms, the ability of electron exchange and transfer between the gas adsorbing material and the gas is improved, and the interaction ability with the gas is increased. The C-H bond of methane is easily dissociated, and the gas adsorbing material has strong absorption ability for methane which is difficult to absorb. In the present application, the absorption ability of the thin film gas adsorbing material for methane gas is improved by using different elements to form the thin film gas adsorbing material, and the absorption rate of methane can be as high as 38-69 mL / s·cm 2 The absorption ability of the thin film gas adsorbing material for methane gas is improved by 60%, which is at the top level in the industry.

[0015] In the present application, by adding one or more of the optional elements V, Co, Fe, Mn, Cr, Al, Sm, Nd and Y, the absorption rate of alkanes, especially methane, is further improved. The present inventors have found that in the 3d electron orbital structure of V, Co, Fe, Mn and Cr, the 3P electron region of Al, and the 4f electron orbital structure of Sm, Nd and Y, there are many unpaired electrons, which play a role in conducting electrons, increase the interaction between the atoms of the main element A and the optional elements in the formation process, and enhance the chemical bond ability, thereby increasing the chemical ability, improving the surface tension of the defects of the thin film gas adsorbing material, and further increasing the van der Waals rate of interaction with the gas, which is helpful to the absorption rate of methane gas.

[0016] The second aspect of the present application provides a method for preparing an alkane gas absorbing thin film getter, comprising the following steps:

[0017] The multi-element alloy target material (in the application of target material, the target material is not excluded as the cathode material of ion pump) is sputtered onto a substrate sample by a sputtering process (the physical evaporation method is not excluded to form a thin film getter), thereby forming an alkane gas absorbing thin film getter.

[0018] Preferably, the sputtering process is as follows: in an inert gas atmosphere, the sputtering power is set to 80-3200W, the sputtering time is 10-80min, and the sputtering gas flow is 40-180mL / min.

[0019] Preferably, the inert gas includes one or more of krypton, nitrogen, and argon.

[0020] Preferably, the substrate sample includes one or more of a wafer, a germanium (Ge) metal substrate, a metal substrate, an alloy substrate, silicon carbide, and an inorganic non-metal substrate.

[0021] Preferably, the method for preparing the multi-element alloy target material is as follows: combining the electric arc smelting technology and the hot-pressing sintering technology.

[0022] Preferably, when the alkane gas absorbing thin film getter contains optional elements Nd, Sm, or Y, the specific method for preparing the multi-element alloy target material comprises the following steps:

[0023] P1: proportionally mix the main element A and optional element raw materials: one or more of Nd, Sm, or Y elements, and load them into a vacuum smelting furnace, and extract the vacuum degree in the furnace to 3.5x10 -4 Pa, then fill 0.01-0.1MPa of argon, and smelt the alloy under the protection of high-purity argon to form a master alloy button ingot containing the main element A and optional element M: one or more of Nd, Sm, or Y elements; the master alloys are respectively: A-Nd, A-Sm, A-Y, or A-Nd-Sm, A-Nd-Y, A-Sm-Y, A-Nd-Sm-Y;

[0024] P2: crush the master alloy button ingot under a nitrogen gas flow protective atmosphere, and set the gas flow to 15-50mL / min; and crush the master alloy into a 0.5-12mm block;

[0025] P3: put the 0.5-12mm master alloy block into a ball mill for wet ball milling, and set the ball milling time to 1-22h; and ball mill the master alloy into a fine powder with a powder particle size of 2-25μm;

[0026] P4: mixing the master alloy fine powder with a particle size of 2-25 μm, and 5-30 nm nano-powder of the essential element Re, Ir, one or both of them; and 8-250 nm nano-powder of one or more of the optional elements V, Co, Fe, Mn, Cr, in proportion, and batching; and pressing the batched product into a circular compact with a diameter of 1.5-16 inches and a thickness of 55-100 mm;

[0027] P5: densifying the circular compact by hot-pressing high-temperature sintering technology to obtain a relative density ≥98.

[0028] 5% of the densified plate compact;

[0029] P6: machining the densified plate compact to form a target material of 1-12 inches for preparing a thin film getter.

[0030] Preferably, the specific steps of the P1 melting alloy include: turning on the power of the electric arc melting, then striking an arc on the titanium ingot, starting to melt the raw materials of the main element A and the optional elements Sm, Nd, Y mixed in proportion to form an alloy after the titanium ingot is completely melted, repeating the above steps 4-6 times after the first melting, and applying magnetic stirring in the last two times, with a magnetic stirring time of 2-3 min; after the melting is completed, the alloy sample is completely cooled, argon is filled, the furnace door is opened, and the master alloy button ingot is taken out. The purpose of striking an arc on the titanium ingot is to allow titanium to absorb impurity gases in the melting chamber during the melting process, thereby purifying the melting environment.

[0031] Preferably, the current used during melting is in the range of 150-300 A.

[0032] Preferably, the powder particle size of the essential elements and optional elements in P4 is 5-30 nm and 8-250 nm.

[0033] Preferably, the densification process in P5 by hot-pressing high-temperature sintering technology is as follows: setting the high-temperature temperature to 1500-2000 ℃, the pressure to 500-1200 T, and the holding time to 3 min-6 h, to obtain a densified plate compact with a relative density ≥98.8%.

[0034] Preferably, in the thin film getter for absorbing alkane gas, the alloy does not contain the optional elements Nd, Sm or Y, contains only the optional elements V, Co, Fe, Mn, Cr, or does not contain optional elements, and the multi-element alloy target material is placed in a specific preparation method, which includes the following steps:

[0035] Q1: Mix and batch the main body element A powder; one or more of Ti, Zr, Ta, Nb, with a powder particle size of 2-25 μm, with the optional element Re, Ir, one or both of which is a nano-sized powder, and 0 or more of the optional elements V, Co, Fe, Mn, Cr, in the nano-sized powder, in proportion;

[0036] Q2: Use hot-pressing high-temperature sintering technology to densify the circular compact, to obtain a dense slab with a relative density of ≥98.5%;

[0037] Q3: Machine the dense slab to form a 1-12 inch multi-element alloy target material for preparing a thin film getter.

[0038] Advantages

[0039] 1. In the present application, by adding the optional element E, the thin film getter has high absorption performance while absorbing alkane gas.

[0040] 2. In the present application, by adding the optional element, the rate of absorbing alkane gas, especially methane gas, is further improved.

[0041] 3. In the present application, by one or more of the main body elements Zr, Ti, Ta, Nb, one or both of the optional elements Ir, Re, one or more of the optional elements V, Co, Fe, Mn, Cr, Al, Sm, Nd, Y, the thin film getter prepared has high methane gas absorption capacity and high substrate bonding strength.

[0042] 4. In the present application, the multi-element alloy target material is first prepared by combining arc melting technology and hot-pressing sintering technology, and then the thin film getter is prepared by using a sputtering process, to obtain a thin film getter with excellent substrate bonding strength.

[0043] 5. The thin film getter in the present application has high methane gas absorption capacity and high substrate bonding strength, which improves the service life and application range of the thin film getter. DETAILED DESCRIPTION

[0044] Example 1

[0045] The first aspect of the present embodiment provides a thin film getter for absorbing alkane gas, which has a composition of Zr 42 Ti 21 Ta 21 Nb 0.7 Ir 0.3 Co 15 (wt%).

[0046] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0047] ①Ingredients: According to Zr 42 Ti 21 Ta 21 Nb 0.7 Ir 0.3 Co 15 The alloy formulation (wt%) was prepared by weighing and mixing 42 wt% Zr, 21 wt% Ti, 21 wt% Ta, 0.7 wt% Nb, 0.3 wt% Ir, and 15 wt% Co. All metal raw materials used in the formulation were powders, with a purity ≥ 99.99%.

[0048] ② The metal raw materials used in the formulation, Zr, Ti, Ta, and Nb powders, have a particle size of 3μm; the required element Ir powder has a particle size of 7nm; and the optional element Co powder has a particle size of 100nm. All powders are prepared according to Zr... 42 Ti 21 Ta 21 Nb 0.7 Ir 0.3 Co 15 After being mixed and batched according to the (wt%) ratio, a batch powder containing nanoparticles was formed. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa and a holding time of 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0049] ③ The process of densifying a circular blank with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1720℃, the pressure is 1000T, and the holding time is 2hh, to obtain a dense slab blank with a relative density ≥98.8%.

[0050] ④ The dense slab is machined to form an 8-inch multi-element alloy target.

[0051] ⑤ The alloy composition is Zr 42 Ti 21 Ta 21 Nb 0.7 Ir 0.3 Co 15 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system, with a silicon single-crystal wafer as the sputtering substrate. The sputtering power was 2800W, the sputtering time was 30 min, and the gas flow rate was 60 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0052] The thickness of the thin-film getter is 1.98 μm.

[0053] Example 2

[0054] The embodiment 2 is the same as the embodiment 1 except that the composition of the thin film getter for absorbing alkyl gas is Zr 40 Ti 20 Nb 14 Ta 0.7 Ir 25 Re 0.3 (wt%).

[0055] The embodiment 2 provides a preparation method of the thin film getter for absorbing alkyl gas, comprising the following steps:

[0056] ①Material preparation: according to the Zr 40 Ti 20 Nb 14 Ta 0.7 Ir 25 Re 0.3 (wt%) alloy formula, the content of the optional element is 0wt%. The Zr of 40wt%, the Ti of 20wt%, the Nb of 14wt%, the Ta of 0.7wt%, the Ir of 25wt% and the Re of 0.3wt% are weighed respectively for material preparation. The metal raw materials used for material preparation are powders, and the purity of the powders is ≥99.99%.

[0057] ②The particle size of the metal raw materials Zr, Ti, Ta and Nb used for material preparation is 24μm, the particle size of the Ir powder of the essential element is 28nm, and the particle size of the Re powder of the essential element is 6nm. After the powders are mixed according to the Zr 40 Ti 20 Nb 14 Ta 0.7 Ir 25 Re 0.3 (wt%) ratio, the particle size mixed powder containing nano powder is formed. The particle size mixed powder containing nano powder is pressed, the pressing pressure is 155MPa, the pressure holding time is 1.5min, the circular compact with a diameter of 250mm and a thickness of 18mm is formed;

[0058] ③The circular compact with a diameter of 250mm and a thickness of 18mm is densified by the hot pressing high-temperature sintering technology, the process is as follows: the high-temperature temperature is 1750℃, the pressure is 1000T, the holding time is 2hh, and the dense blank with a relative density of ≥98.8% is prepared.

[0059] ④The dense blank is machined to form an 8-inch multi-element alloy target material.

[0060] ⑤The alloy composition is Zr 40 Ti 20 Nb14 Ta 0.7 Ir 25 Re 0.3 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus, with a germanium metal substrate as the sputtering substrate. The sputtering power was 3000W, the sputtering time was 30min, and the gas flow rate was 60mL / min, resulting in a thin film getter that absorbs alkane gases.

[0061] The thickness of the thin-film getter is 2.00 μm.

[0062] Example 3

[0063] The specific implementation of Example 3 is the same as that of Example 1, except that the component of the thin-film getter for absorbing alkane gases is Zr. 30 Ti 15 Ta 15 Nb5Re 25 V 10 (wt%).

[0064] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0065] ①Ingredients: According to Zr 30 Ti 15 Ta 15 Nb5Re 25 V 10 (wt%) Alloy formulation, with optional element content of 0wt%. 30wt% Zr, 15wt% Ti, 15wt% Ta, 5wt% Nb, 25wt% Re, and 10% V were weighed and mixed separately. The metal raw materials used in the mixing were powders, and the purity of all powders was ≥99.99%.

[0066] ② The metal raw materials used in the formulation, Zr, Ti, Ta, and Nb powders, have a particle size of 10 μm; the required element Re powder has a particle size of 28 nm; and the optional element V powder has a particle size of 10 nm. All powders are prepared according to Zr... 30 Ti 15 Ta 15 Nb5Re 25 V 10 After being mixed and batched according to the (wt%) ratio, a batch powder containing nanoparticles was formed. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa and a holding time of 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0067] The process for densifying the circular compact with a diameter of 250 mm and a thickness of 18 mm by hot pressing and high-temperature sintering technology is as follows: setting the high-temperature temperature to 1730 °C, the pressure to 1000 T, and the holding time to 2 h, to obtain a dense slab with a relative density of ≥98.8%.

[0068] The dense slab is machined to form an 8-inch multi-element alloy target.

[0069] The alloy composition of the target is Zr 30 Ti 15 Ta 15 Nb5Re 25 V 10 (wt%) is placed in a JW-8 type magnetron sputtering device for sputtering, and the sputtering substrate is a stainless steel substrate. The sputtering power is 2800 W, the sputtering time is 30 min, and the gas flow is 60 mL / min, to obtain an alkane gas absorbing thin film getter.

[0070] The thickness of the thin film getter is 2.02 μm.

[0071] Comparative Example 1

[0072] The specific implementation of Comparative Example 1 is the same as that of Example 1, except that the composition of the alkane gas absorbing thin film getter is Zr 37 Ti 21 Ta 21 Nb 21 (wt%)。

[0073] The second aspect of the present embodiment provides a preparation method of an alkane gas absorbing thin film getter, comprising the following steps:

[0074] ①Batching: according to the Zr 37 Ti 21 Ta 21 Nb 21 (wt%) alloy formula, the content of optional elements is 0 wt%. 37 wt% of Zr, 21 wt% of Ti, 21 wt% of Ta, and 21 wt% of Nb are weighed respectively. The alloy composition does not contain the mandatory elements Ir and Re, nor the optional elements V, Co, Fe, Mn, Cr, Al, Sm, Nd, and Y. The metal raw materials used for batching are powders, and the purity of the powders is all ≥99.99%.

[0075] ②The particle size of the metal raw materials Zr, Ti, Ta, and Nb powders used for batching is 20 μm, and all the powders are according to Zr 37 Ti 21 Ta 21 Nb 21After mixing and batching according to the (wt%) ratio, the batch of powder containing nanoparticles is pressed at a pressure of 155 MPa and a holding time of 1.5 min to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0076] ③ The process of densifying a circular blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1600℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0077] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0078] ⑤ The alloy composition is Zr 37 Ti 21 Ta 21 Nb 21 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1000W, the sputtering time was 30 min, and the gas flow rate was 60 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0079] The thickness of the thin-film getter is 1.99 μm.

[0080] Example 4

[0081] The specific implementation of Example 4 is the same as that of Example 1, except that the component of the thin-film getter for absorbing alkane gases is Zr. 50 Ti 20 Nb5Ir 10 V 11 Y4 (wt%).

[0082] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0083] ①Ingredients: According to Zr 50 Ti 20 Nb5Ir 10 V 11 The Y4 (wt%) alloy formula is prepared by first melting a Zr-Y alloy, and then weighing out 50 wt% Zr and 4 wt% Y for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0084] ② Smelting: The prepared Zr... 50Y4 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 280A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Y alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Y alloy button ingot was removed.

[0085] ③ Under the protective atmosphere of argon gas flow, Zr-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0086] ④Zr powder with a particle size of 10μm 50 Y4 alloy fine powder was mixed with 20 wt% Ti, 5 wt% Nb, 10 wt% Ir, and 11 wt% V in batches. The particle sizes of Zr, Ti, and Nb were 20 μm, while the particle sizes of the mandatory element Ir and the optional element V were 20 and 10 nm, respectively. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0087] ⑤ The process of densifying a circular blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1580℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0088] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0089] ⑦ The alloy composition is Zr 50 Ti 20 Nb5Ir 10 V 11 A Y4 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0090] The thickness of the thin-film getter is 1.98 μm.

[0091] Example 5

[0092] The specific implementation of Example 5 is the same as that of Example 1, except that the component of the thin-film getter for absorbing alkane gases is Zr. 45 Ti 30 Re 15 Mn6Fe4 (wt%).

[0093] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0094] ①Ingredients: According to Zr 45 Ti 30 Re 15 The Mn6Fe4 (wt%) alloy formulation has an optional element content of 0 wt%. Zr, Ti, Re, Mn, and Fe are weighed and mixed in weight percentages of 45 wt%, 30 wt%, 15 wt%, 6 wt%, and 4 wt%, respectively. The metal raw materials used in the mixing are powders, and the purity of all powders is ≥99.99%.

[0095] ② The metal raw materials used in the formulation, Zr and Ti powders, have a particle size of 20 μm; the required element Re powder has a particle size of 20 nm; and the optional elements Fe and V powders have a particle size of 200 nm. All powders are prepared according to Zr... 45 Ti 30 Re 15 Mn6Fe4 (wt%) was mixed and batched to form a batched powder containing nanoparticles. The batched powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0096] ③ The process of densifying a circular blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1580℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0097] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0098] ⑤ The alloy composition is Zr 45 Ti 30 Re 15 A Mn6Fe4 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1000 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0099] The thickness of the thin-film getter is 1.96 μm.

[0100] Example 6

[0101] The specific implementation of Example 6 is the same as that of Example 1, except that the component of the thin-film getter for absorbing alkane gases is Zr. 70 Nb 10 Re 10 Nd4Al3V3 (wt%).

[0102] ①Ingredients: According to Zr 70 Nb 10 Re 10 The Nd4Al3V3 (wt%) alloy formula is prepared by first melting a Zr-Nd alloy, and then weighing out 70wt% Zr and 4wt% Nd by mass for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0103] ② Smelting: The prepared Zr... 70 Nd4 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 160A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Nd alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Nd alloy button ingot was removed.

[0104] ③ Under the protective atmosphere of argon gas flow, Zr-Nd alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0105] ④Zr powder with a particle size of 10μm 70 Fine Nd4 alloy powder was mixed with 10 wt% Nb, 10 wt% Re, 3 wt% Al, and 3 wt% V in a batch. The Nb powder had a particle size of 20 μm, while the required element Ir and the optional element V had particle sizes of 20 nm and 240 nm, respectively. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0106] ⑤ The process of densifying a circular compact with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1510℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0107] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0108] ⑦ The alloy composition is Zr 70 Nb 10 Re 10 A Nd4Al3V3 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0109] The thickness of the thin-film getter is 1.90 μm.

[0110] Example 7

[0111] The specific implementation of Example 7 is the same as that of Example 1, except that the component of the thin-film getter for absorbing alkane gases is Zr. 70 Ta 18 Ir2Cr8Sm2 (wt%).

[0112] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0113] ①Ingredients: According to Zr 70 Ta 18 The Ir2Cr8Sm2 (wt%) alloy formula is prepared by first melting a Zr-Sm alloy, and then weighing out 70wt% Zr and 2wt% Sm by mass for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0114] ② Smelting: The prepared Zr... 70 Sm2 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 210A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Sm alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Sm alloy button ingot was removed.

[0115] ③ Under the protective atmosphere of argon gas flow, Zr-Sm alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0116] ④Zr powder with a particle size of 10μm 70 Sm2 alloy fine powder was mixed with 18 wt% Ta, 2 wt% Ir, and 8 wt% Cr in a batch. The Ta powder had a particle size of 10 μm, while the required element Ir and the optional element Cr each had a particle size of 20 nm. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0117] ⑤ The process of densifying a circular compact with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1520℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0118] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0119] ⑦ The alloy composition is Zr 70 Ta 18 An Ir2Cr8Sm2 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1400W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0120] The thickness of the thin-film getter is 1.89 μm.

[0121] Example 8

[0122] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, the composition of which is Ti. 70 Zr 18 Re2Co5Y5 (wt%).

[0123] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0124] ① Ingredients: According to Ti 70 Zr 18The Re2Co5Y5 (wt%) alloy formula is prepared by first melting a Zr-Y alloy, and then weighing out Zr (18wt%) and Y (5wt%) for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0125] ② Smelting: The prepared Zr... 18 Y5 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 280A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Y alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Y alloy button ingot was removed.

[0126] ③ Under the protective atmosphere of argon gas flow, Zr-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0127] ④Zr powder with a particle size of 10μm 18 Y5 alloy fine powder was mixed with 70 wt% Ti, 2 wt% Re, and 5 wt% Co in batches. The Ti powder had a particle size of 10 μm, while the required element Re and the optional element Co each had a particle size of 20 nm. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0128] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0129] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0130] ⑦ The alloy composition is Ti 70 Zr 18A Re2Co5Y5 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0131] The thickness of the thin-film getter is 1.99 μm.

[0132] Example 9

[0133] The specific implementation of Example 9 is the same as that of Example 8, except that the component of the thin-film getter for absorbing alkane gases is Zr. 71 Ir 10 Re 10 Co5Y4 (wt%).

[0134] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0135] ①Ingredients: According to Zr 71 Ir 10 Re 10 The Co5Y4 (wt%) alloy formula is prepared by first melting a Zr-Y alloy, and then weighing out Zr (71 wt%) and Y (4 wt%) for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0136] ② Smelting: The prepared Zr... 71 Y4 metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 280A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Nd alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and this process was repeated four times. Magnetic stirring was applied for the last two cycles, lasting 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Nd alloy button ingot was removed.

[0137] ③ Under the protective atmosphere of argon gas flow, Zr-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0138] ④Zr powder with a particle size of 10μm 71Y4 alloy fine powder was mixed with 10 wt% Re, 10 wt% Ir, and 5 wt% Co in batches. The required elements Re and Ir had a powder particle size of 20 μm, while the optional element Co had a powder particle size of 200 nm. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0139] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1550℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0140] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0141] ⑦ The alloy composition is Zr 71 Ir 10 Re 10 A Co5Y4 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0142] The thickness of the thin-film getter is 1.91 μm.

[0143] Example 10

[0144] The specific implementation of Example 10 is the same as that of Example 9, except that the composition of the thin-film getter for absorbing alkane gases is Ti. 71 Ir 10 Re 10 Co5Y4 (wt%).

[0145] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0146] ① Ingredients: According to Ti 71 Ir 10 Re 10 The Co5Y4 (wt%) alloy formula is prepared by first melting a Ti-Y alloy, and then weighing out 71 wt% Ti and 4 wt% Y for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0147] ② Smelting: The prepared Ti... 71Y4 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 180A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Ti-Y alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with each stirring lasting 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Ti-Y alloy button ingots were removed.

[0148] ③ Under the protective atmosphere of argon gas flow, Ti-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0149] ④ Ti powder with a particle size of 10μm 71 Y4 alloy fine powder was mixed with 10 wt% Re, 10 wt% Ir, and 5 wt% Co in batches. The required elements Re and Ir had a powder particle size of 20 μm, while the optional element Co had a powder particle size of 100 nm. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0150] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0151] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0152] ⑦ The alloy composition is Ti 71 Ir 10 Re 10 A Co5Y4 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1600 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0153] The thickness of the thin-film getter is 1.92 μm.

[0154] Example 11

[0155] The specific implementation of Example 11 is the same as that of Example 8, except that the component of the thin-film getter for absorbing alkane gases is Zr. 75 Re 16 V5Y4.

[0156] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0157] ①Ingredients: According to Zr 75 Re 16 The V5Y4 (wt%) alloy formula is prepared by first melting a Zr-Y alloy, and then weighing out 75wt% Zr and 4wt% Y by mass for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0158] ② Smelting: The prepared Zr... 75 Y4 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 280A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Y alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Y alloy button ingot was removed.

[0159] ③ Under the protective atmosphere of argon gas flow, Zr-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0160] ④Zr powder with a particle size of 10μm 75 Y4 alloy fine powder was mixed with 16 wt% Re and 5 wt% V, wherein the required element Re and the optional element V had powder particle sizes of 20 and 200 nm, respectively. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0161] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1550℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0162] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0163] ⑦ The alloy composition is Zr 75 Re 16 A V5Y4 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0164] The thickness of the thin-film getter is 1.96 μm.

[0165] Example 12

[0166] The specific implementation of Example 12 is the same as that of Example 1, except that the component of the thin-film getter for absorbing alkane gases is Zr. 80 Ir6Co5V5Y4 (wt%).

[0167] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0168] ①Ingredients: According to Zr 80 The Ir6Co5V5Y4 (wt%) alloy formula is prepared by first melting a Zr-Y alloy, and then weighing out 80wt% Zr and 4wt% Y for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0169] ② Smelting: The prepared Zr... 80 Y4 (wt%) metal raw material was loaded into an electric arc melting furnace, and the melting current was set to 280A. First, pure titanium nails in the furnace were melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Zr-Y alloy was melted. After one melting cycle, the alloy sample was allowed to completely cool and solidify. The sample was then flipped using a robotic arm, and the above steps were repeated four times. Magnetic stirring was applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample was allowed to completely cool, argon gas was introduced, the furnace door was opened, and the Zr-Y alloy button ingot was removed.

[0170] ③ Under the protective atmosphere of argon gas flow, Zr-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0171] ④Zr powder with a particle size of 10μm 80Y4 alloy fine powder was mixed with 6 wt% Ir, 5 wt% Co, and 5 wt% V in batches, wherein the required element Ir and the optional element Co had powder particle sizes of 20 and 100 nm, respectively. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0172] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1550℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0173] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0174] ⑦ The alloy composition is Zr 80 An Ir6Co5V5Y4 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 60 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0175] The thickness of the thin-film getter is 1.92 μm.

[0176] Example 13

[0177] The thin-film getter for absorbing alkane gases described in Example 13 is composed of Ti. 80 Re 15 V5 (wt%).

[0178] ① Ingredients: According to Ti 80 Re 15 The V5 (wt%) alloy formula was prepared by weighing and mixing 80 wt% Ti, 15 wt% Re, and 5 wt% V. All metal raw materials used in the mixing were powders, with a purity ≥ 99.99%.

[0179] ② The metal raw materials Ti, Re, and V powders used in the formulation have particle sizes of 10μm, 20nm, and 100nm, respectively. All powders are prepared according to the order of Ti... 80 Re 15 After mixing and batching at a V5 (wt%) ratio, a batch powder containing nanoparticles is formed. The batch powder containing nanoparticles is then pressed at a pressure of 155 MPa and a holding time of 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0180] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0181] ④ The dense slab is machined to form an 8-inch multi-element alloy target.

[0182] ⑤ The alloy composition is Ti 80 Re 15 A V5 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1600 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0183] The thickness of the thin-film getter is 2.01 μm.

[0184] Example 14

[0185] The thin-film getter for absorbing alkane gases described in Example 14 is composed of Ti. 75 Re 15 V9Y1 (wt%).

[0186] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0187] ① Ingredients: According to Ti 75 Re 15 The V9Y1 (wt%) alloy formula is prepared by first melting a Ti-Y alloy, and then weighing out 75wt% Ti and 1wt% Y by mass for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0188] ② Smelting: The prepared Ti... 75 Y1 metal raw material is loaded into an electric arc melting furnace, and the melting current is set to 180A. First, pure titanium nails in the furnace are melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Ti-Y alloy is melted. After one melting cycle, the alloy sample is allowed to completely cool and solidify. The sample is then flipped using a robotic arm, and the above steps are repeated four times. Magnetic stirring is applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample is allowed to completely cool, argon gas is introduced, the furnace door is opened, and the resulting Ti-Y alloy button ingot is removed.

[0189] ③ Under the protective atmosphere of argon gas flow, Ti-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0190] ④ Ti powder with a particle size of 10μm 75 Y1 alloy fine powder was mixed with 15 wt% Re and 9 wt% V, wherein the required element Re and the optional element V had particle sizes of 10 and 50 nm, respectively. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0191] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1550℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0192] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0193] ⑦ The alloy composition is Ti 75 Re 15 A V9Y1 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 60 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0194] The thickness of the thin-film getter is 1.94 μm.

[0195] Example 15

[0196] The thin-film getter for absorbing alkane gases described in Example 15 is composed of Ti. 80 Re 10 Y 10 (wt%).

[0197] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0198] ① Ingredients: According to Ti 80 Re 10 Y 10The alloy formulation (wt%) involves first melting a Ti-Y alloy, then weighing out 80wt% Ti and 10wt% Y for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0199] ② Smelting: The prepared Ti... 80 Y 10 (wt%) Metal raw materials are loaded into an electric arc melting furnace, and the melting current is set to 180A. First, pure titanium nails in the furnace are melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Ti-Y alloy is melted. After one melting cycle, the alloy sample is allowed to completely cool and solidify. The sample is then flipped using a robotic arm, and the above steps are repeated four times. Magnetic stirring is applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample is allowed to completely cool, argon gas is introduced, the furnace door is opened, and the Ti-Y alloy button ingot is removed.

[0200] ③ Under the protective atmosphere of argon gas flow, Ti-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0201] ④ Ti powder with a particle size of 10μm 80 Y 10 Fine alloy powder was mixed with 10 wt% of the essential element Re, wherein the Re powder particle size was 20 μm. This resulted in a powder containing nanoparticles. The powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0202] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0203] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0204] ⑦ The alloy composition is Ti 80 Re 10 Y 10 A (wt%) alloy target was placed in a JW-8 magnetron sputtering apparatus for sputtering, with a stainless steel substrate as the sputtering substrate. The sputtering power was 1600W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0205] The thickness of the thin-film getter is 1.91 μm.

[0206] Example 16

[0207] The thin-film getter for absorbing alkane gases described in Example 16 is composed of Ti. 79 Re 20 Y1 (wt%).

[0208] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0209] ① Ingredients: According to Ti 79 Re 20 The Y1 (wt%) alloy formula is prepared by first melting a Ti-Y alloy, and then weighing out 79 wt% Ti and 1 wt% Y for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0210] ② Smelting: The prepared Ti... 79 Y1 (wt%) metal raw material is loaded into an electric arc melting furnace, and the melting current is set to 180A. First, pure titanium nails in the furnace are melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Ti-Y alloy is melted. After one melting cycle, the alloy sample is allowed to completely cool and solidify. The sample is then flipped using a robotic arm, and the above steps are repeated four times. Magnetic stirring is applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample is allowed to completely cool, argon gas is introduced, the furnace door is opened, and the Ti-Y alloy button ingot is removed.

[0211] ③ Under the protective atmosphere of argon gas flow, Ti-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0212] ④ Ti powder with a particle size of 10μm 79 Y1 alloy fine powder was mixed with 20 wt% of the essential element Re, wherein the Re powder particle size was 20 μm. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0213] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0214] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0215] ⑦ The alloy composition is Ti 79 Re 20 A Y1 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1600 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0216] The thickness of the thin-film getter is 1.91 μm.

[0217] Example 17

[0218] The specific implementation of Example 17 is the same as that of Example 5, except that the composition of the thin-film getter for absorbing alkane gases is Ti. 80 Re 15 Co 55 (wt%).

[0219] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0220] ① Ingredients: According to Ti 80 Re 15 The Co5 (wt%) alloy formulation was prepared by weighing 80 wt% Ti, 15 wt% Re, and 5 wt% Co to form the formulation of Example 17. The metal raw materials used in the formulation were powders, and the purity of the powders was ≥99.99%.

[0221] ② The Ti powder used in the batching has a particle size of 10μm, and the Re powder, an essential element, has a particle size of 20nm. These are prepared separately, mixed separately, and then batched to form a batch powder containing nanoparticles. This batch powder containing nanoparticles is then pressed at a pressure of 155MPa for 1.5 minutes to form a circular compact with a diameter of 250mm and a thickness of 18mm.

[0222] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0223] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0224] ⑤ The alloy composition Ti 80 Re 15 A Co5 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1600 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0225] The thickness of the thin-film getter is 1.92 μm.

[0226] Example 18

[0227] The thin-film getter for absorbing alkane gases described in Example 18 is composed of Ti. 80 Re 18 Co1Y1 (wt%).

[0228] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0229] ① Ingredients: According to Ti 80 Re 18 The Co1Y1 (wt%) alloy formula is prepared by first melting a Ti-Y alloy. 80 wt% Ti and 1 wt% Y are weighed separately for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0230] ② Smelting: The prepared Ti... 80 Y1 (wt%) metal raw material is loaded into an electric arc melting furnace, and the melting current is set to 180A. First, pure titanium nails in the furnace are melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Ti-Y alloy is melted. After one melting cycle, the alloy sample is allowed to completely cool and solidify. The sample is then flipped using a robotic arm, and the above steps are repeated four times. Magnetic stirring is applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample is allowed to completely cool, argon gas is introduced, the furnace door is opened, and the Ti-Y alloy button ingot is removed.

[0231] ③ Under the protective atmosphere of argon gas flow, Ti-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0232] ④ Ti powder with a particle size of 10μm 80Y1 alloy fine powder was mixed with 18 wt% Re and 1 wt% Co, with the Re and Co powders having a particle size of 20 nm. This resulted in a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 60 MPa for 2 minutes to form a circular compact with a diameter of 80 mm and a thickness of 18 mm.

[0233] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0234] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0235] ⑦ The alloy composition is Ti 80 Re 18 A Co1Y1 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0236] The thickness of the thin-film getter is 1.98 μm.

[0237] Example 19

[0238] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 80 Re3V 17 (wt%).

[0239] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0240] ① Ingredients: According to Ti 80 Re3V 17 (wt%) Alloy formulation. 80 wt% Ti, 3 wt% Re, and 17 wt% V were weighed separately; the metal raw materials used in the formulation were powders, and the purity of the powders was ≥99.99%.

[0241] ② The main element Ti powder used in the formulation has a particle size of 10 μm, the required element Re powder has a particle size of 20 nm, and the optional element V powder has a particle size of 20 nm. All powders are prepared according to the Ti... 80 Re3V 17After being formulated (wt%), a batch of powder containing nanoparticles was formed. The batch of powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0242] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0243] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0244] ⑤ The alloy composition is Ti 80 Re3V 17 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0245] The thickness of the thin-film getter is 2.01 μm.

[0246] Example 20

[0247] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 75 Re7Co 18 (wt%).

[0248] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0249] ① Ingredients: According to Ti 75 Re7Co 18 (wt%) Alloy formulation. 75wt% Ti, 7wt% Re, and 18wt% Co were weighed separately. The metal raw materials used in the formulation were powders, and the purity of each powder was ≥99.99%.

[0250] ② The main element Ti powder used in the formulation has a particle size of 10 μm, the required element Re powder has a particle size of 20 nm, and the optional element Co powder has a particle size of [missing information]. All powders are prepared according to Ti [missing information]. 75 Re7Co 18After being formulated (wt%), a batch of powder containing nanoparticles was formed. The batch of powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0251] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0252] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0253] ⑤ The alloy composition is Ti 75 Re7Co 18 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0254] The thickness of the thin-film getter is 2.05 μm.

[0255] Example 21

[0256] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 83 Ir7Co 10 (wt%).

[0257] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0258] ① Ingredients: According to Ti 83 Ir7Co 10 (wt%) Alloy formulation. 83 wt% Ti, 7 wt% Ir, and 10 wt% Co were weighed separately; the metal raw materials used in the formulation were powders, and the purity of the powders was ≥99.99%.

[0259] ② The main element Ti powder used in the formulation has a particle size of 10 μm, the element Ir powder has a particle size of 20 nm, and the optional element Co powder has a particle size of 10 nm. All powders are prepared according to the Ti... 83 Ir7Co 10After being formulated (wt%), a batch of powder containing nanoparticles was formed. The batch of powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0260] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0261] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0262] ⑤ The alloy composition is Ti 83 Ir7Co 10 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0263] The thickness of the thin-film getter is 1.93 μm.

[0264] Example 22

[0265] The specific implementation of Example 22 is the same as that of Example 5, except that the component of the thin-film getter for absorbing alkane gases is Zr. 65 Ti 30 Re5 (wt%).

[0266] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0267] ①Ingredients: According to Zr 65 Ti 30 Re5 (wt%) alloy formulation. Zr, Ti, and Re were weighed in weight percentages of 65 wt%, 30 wt%, and 5 wt%, respectively, to form the formulation of Example 22; the metal raw materials used in the formulation were powders, and the purity of the powders was ≥99.99%.

[0268] ② The Zr and Ti powders used in the formulation have a particle size of 10 μm, and the Re powder, a mandatory element, has a particle size of 20 nm. All powders are prepared according to Zr... 65 Ti 30Re5 (wt%) was separately proportioned and then mixed and batched to form a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0269] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0270] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0271] ⑤ The alloy composition is Zr 65 Ti 30 A Re5 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1600 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0272] The thickness of the thin-film getter is 2.02 μm.

[0273] Example 23

[0274] The specific implementation of Example 23 is the same as that of Example 2, except that the component of the thin-film getter for absorbing alkane gases is Zr. 65 Ti 22 Re8Ir5 (wt%).

[0275] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0276] ①Ingredients: According to Zr 65 Ti 22 Re8Ir5 (wt%) alloy formulation. Zr, Ti, Re, and Ir were weighed out in the following weight percentages: 65 wt%, 22 wt%, 8 wt%, and 5 wt%. All metal raw materials used in the formulation were powders, with a purity ≥ 99.99%.

[0277] ② The Zr and Ti powders used in the formulation have a particle size of 10 μm, and the Re and Ir powders, which are essential elements, have a particle size of 20 nm. All powders are prepared according to Zr... 65 Ti 22Re8Ir5 (wt%) was separately proportioned and then mixed in batches to form a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0278] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0279] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0280] ⑤ The alloy composition is Zr 65 Ti 22 A Re8Ir5 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1500W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0281] The thickness of the getter film is 1.97 μm.

[0282] Example 24

[0283] The specific implementation of Example 24 is the same as that of Example 2, except that the component of the thin-film getter for absorbing alkane gases is Zr. 65 Ti 30 Ir5 (wt%)

[0284] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0285] ①Ingredients: According to Zr 65 Ti 30 Ir5 (wt%) alloy formulation. Zr, Ti, and Ir were weighed out at mass percentages of 65 wt%, 30 wt%, and 5 wt%, respectively. All metal raw materials used in the formulation were powders with a purity ≥ 99.99%.

[0286] ② The Zr and Ti powders used in the formulation have a particle size of 10 μm, and the Ir powder, a mandatory element, has a particle size of 20 nm. All powders are prepared according to Zr... 65 Ti 30Ir5 (wt%) was separately proportioned and then mixed and batched to form a batch powder containing nanoparticles. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0287] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0288] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0289] ⑤ The alloy composition is Zr 65 Ti 30 An Ir5 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0290] The thickness of the thin-film getter is 2.1 μm.

[0291] Example 25

[0292] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the component of the thin-film getter for absorbing alkane gases is Zr. 93 Re7 (wt%).

[0293] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0294] ① Ingredients: Weigh 93 wt% Zr and 7 wt% Re respectively; the metal raw materials used in the preparation are powders, and the purity of the powders is ≥99.99%.

[0295] ② The main element Zr powder used in the formulation has a particle size of 10μm, and the essential element Re powder has a particle size of 20nm. After mixing, a batch of powder containing nanoparticles is formed. The batch of powder containing nanoparticles is pressed at a pressure of 155MPa and a holding time of 1.5min to form a circular compact with a diameter of 250mm and a thickness of 18mm.

[0296] ③ The process of densifying a circular blank with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1545℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0297] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0298] ⑤ The alloy composition is Zr 93 A Re7 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0299] The thickness of the thin-film getter is 1.98 μm.

[0300] Example 26

[0301] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Zr. 77 Re 23 (wt%).

[0302] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0303] ① Ingredients: Weigh 77 wt% Zr and 23 wt% Re respectively; the metal raw materials used in the ingredients are powders, and the purity of the powders is ≥99.99%.

[0304] ② The main element Zr powder used in the formulation has a particle size of 10 μm, and the essential element Re powder has a particle size of 20 nm. All powders are prepared according to Zr... 77 Re 23 After being formulated (wt%), a batch of powder containing nanoparticles was formed. The batch of powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0305] ③ The process of densifying a circular blank with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1545℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0306] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0307] ⑤ The alloy composition is Zr 77 Re 23 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0308] The thickness of the thin-film getter is 1.93 μm.

[0309] Example 27

[0310] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the component of the thin-film getter for absorbing alkane gases is Zr. 93 Ir7 (wt%)

[0311] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0312] ① Ingredients: Weigh 93 wt% Zr and 7 wt% Ir respectively; the metal raw materials used in the ingredients are powders, and the purity of the powders is ≥99.99%.

[0313] ② The main element Zr powder used in the formulation has a particle size of 10 μm, and the essential element Ir powder has a particle size of 20 nm. All powders are prepared according to Zr... 93 After Ir7 (wt%) is added, a batch powder containing nanoparticles is formed. The batch powder containing nanoparticles is pressed at a pressure of 155 MPa and a holding time of 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0314] ③ The process of densifying a circular blank with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1545℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0315] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0316] ⑤ The alloy composition is Zr 93 An Ir7 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0317] The thickness of the thin-film getter is 1.95 μm.

[0318] Example 28

[0319] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the component of the thin-film getter for absorbing alkane gases is Zr. 77 Ir 23 (wt%).

[0320] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0321] ① Ingredients: Weigh 77 wt% Zr and 23 wt% Ir respectively; the metal raw materials used in the ingredients are powders, and the purity of the powders is ≥99.99%.

[0322] ② The main element Zr powder used in the formulation has a particle size of 10 μm, and the essential element Ir powder has a particle size of 20 nm. All powders are prepared according to Zr... 77 Ir 23 After being formulated (wt%), a batch of powder containing nanoparticles was formed. The batch of powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0323] ③ The process of densifying a circular blank with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1545℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0324] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0325] ⑤ The alloy composition is Zr 77 Ir 23 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0326] The thickness of the thin-film getter is 1.92 μm.

[0327] Example 29

[0328] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 93 Re7 (wt%).

[0329] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0330] ①Ingredients: Weigh 93 wt% Ti and 7 wt% Re respectively; the metal raw materials used for ingredient preparation are powders, and the purity of the powders is ≥99.99%.

[0331] ② The main element Ti powder used in the formulation has a particle size of 10μm, and the essential element Re powder has a particle size of 20nm. After formulation, a batch of powder containing nanoparticles is formed. The batch of powder containing nanoparticles is pressed at a pressure of 155MPa and a holding time of 1.5min to form a circular compact with a diameter of 250mm and a thickness of 18mm.

[0332] ③ The process of densifying a circular blank with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1515℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0333] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0334] ⑤ The alloy composition is Ti 93 A Re7 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1700 W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0335] The thickness of the thin-film getter is 1.95 μm.

[0336] Example 30

[0337] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 77 Re 23 (wt%).

[0338] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0339] ①Ingredients: Weigh 77 wt% Ti and 23 wt% Re by mass respectively; the metal raw materials used for ingredient preparation are powders, and the purity of the powders is ≥99.99%.

[0340] ② The main element Ti powder used in the formulation has a particle size of 10μm, and the essential element Re powder has a particle size of 20nm. After formulation, a batch of powder containing nanoparticles is formed. The batch of powder containing nanoparticles is pressed at a pressure of 155MPa and a holding time of 1.5min to form a circular compact with a diameter of 250mm and a thickness of 18mm.

[0341] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0342] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0343] ⑤ The alloy composition is Ti 77 Re 23 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0344] The thickness of the thin-film getter is 1.91 μm.

[0345] Example 31

[0346] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 93 Ir7 (wt%)

[0347] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0348] ①Ingredients: Weigh 93 wt% Ti and 7 wt% Ir respectively; the metal raw materials used for ingredient preparation are powders, and the purity of the powders is ≥99.99%.

[0349] ② The main element Ti powder used in the formulation has a particle size of 10 μm, and the essential element Ir powder has a particle size of 20 nm. All powders are prepared according to the Ti... 93 After Ir7 (wt%) is added, a batch powder containing nanoparticles is formed. The batch powder containing nanoparticles is pressed at a pressure of 155 MPa and a holding time of 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0350] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1525℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0351] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0352] ⑤ The alloy composition is Ti 93 An Ir7 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0353] The thickness of the thin-film getter is 1.93 μm.

[0354] Example 32

[0355] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 77 Ir 23 .

[0356] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0357] ①Ingredients: Weigh 77 wt% Ti and 23 wt% Ir respectively; the metal raw materials used for ingredient preparation are powders, and the purity of the powders is ≥99.99%.

[0358] ② The main element Ti powder used in the formulation has a particle size of 10 μm, and the essential element Ir powder has a particle size of 20 nm. All powders are prepared according to the Ti... 77 Ir 23 After being formulated (wt%), a batch of powder containing nanoparticles was formed. The batch of powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0359] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0360] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0361] ⑤ The alloy composition is Ti 77 Ir 23 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0362] The thickness of the thin-film getter is 1.90 μm.

[0363] Example 33

[0364] The first aspect of this embodiment provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 84 Ir 13 Re3 (wt%).

[0365] The second aspect of this embodiment provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0366] ① Ingredients: According to Ti 84 Ir 13 The Re3 (wt%) alloy formula was prepared by weighing 84 wt% Ti, 13 wt% Ir, and 3 wt% Re by mass. All metal raw materials used in the formulation were powders, with a purity ≥ 99.99%.

[0367] ② The main element Ti powder used in the formulation has a particle size of 10 μm, and the essential elements Re and Ir powder have a particle size of 20 nm. All powders are prepared according to the Ti... 84 Ir 13 After adjusting the Re3 (wt%) ratio, a batch powder containing nanoparticles was formed. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0368] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0369] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0370] ⑤ The alloy composition is Ti 84 Ir 13A Re3 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 1800W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0371] The thickness of the thin-film getter is 1.98 μm.

[0372] Comparative Example 2

[0373] Comparative Example 2 provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 80 V 10 Y 10 (wt%). The alloy formulation does not contain the essential elements Ir and Re.

[0374] The second aspect of this comparative example provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0375] ① Ingredients: According to Ti 80 V 10 Y 10 The alloy formulation (wt%) involves first melting a Ti-Y alloy. 80 wt% Ti and 10 wt% Y are weighed separately for batching. The purity of all metal raw materials used in the batching is ≥99.99%.

[0376] ② Smelting: The prepared Ti... 80 Y 10 (wt%) Metal raw materials are loaded into an electric arc melting furnace, and the melting current is set to 180A. First, pure titanium nails in the furnace are melted to purify the furnace, as the pure titanium nails absorb impurity gases (O, Co, etc.) during the melting process. After melting the pure titanium nails, the Ti-Y alloy is melted. After one melting cycle, the alloy sample is allowed to completely cool and solidify. The sample is then flipped using a robotic arm, and the above steps are repeated four times. Magnetic stirring is applied for the last two cycles, with a stirring time of 3 minutes. After melting, the alloy sample is allowed to completely cool, argon gas is introduced, the furnace door is opened, and the Ti-Y alloy button ingot is removed.

[0377] ③ Under the protective atmosphere of argon gas flow, Ti-Y alloy button ingots were crushed with a gas flow rate of 25 mL / min; the ingots were crushed into 5 mm blocks; the 5 mm blocks were then placed in a ball mill for wet ball milling for 1.5 h to produce intermediate alloy fine powder with a particle size of 10 μm.

[0378] ④ Ti powder with a particle size of 10μm 80 Y 10(wt%) alloy fine powder, and 10wt% V, wherein the particle size of the optional element V is 10nm. A batch powder containing nanoparticles is formed. The batch powder containing nanoparticles is pressed at a pressure of 60MPa for 2min to form a circular compact with a diameter of 80mm and a thickness of 18mm.

[0379] ⑤ The process of densifying a circular pressed blank with a diameter of 80mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1505℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab blank with a relative density ≥98.8%.

[0380] ⑥ The dense slab is machined to form a 2-inch multi-element alloy target.

[0381] ⑦ The alloy composition is Ti 80 V 10 Y 10 A (wt%) alloy target was sputtered in a JW-8 magnetron sputtering apparatus with a stainless steel substrate. The sputtering power was 1500W, the sputtering time was 30 min, and the gas flow rate was 75 mL / min, resulting in a thin-film getter that absorbs alkane gases.

[0382] The thickness of the thin-film getter is 1.99 μm.

[0383] Comparative Example 3

[0384] Comparative Example 3 provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 84 Ir 13 Re3 (wt%).

[0385] The second aspect of this comparative example provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0386] ① Ingredients: According to Ti 84 Ir 13 The Re3 (wt%) alloy formula was prepared by weighing 84 wt% Ti, 13 wt% Ir, and 3 wt% Re by mass. All metal raw materials used in the formulation were powders, with a purity ≥ 99.99%.

[0387] ② The main element Ti powder used in the formulation has a particle size of 10 μm, and the essential elements Re and Ir powder have a particle size of 20 nm. All powders are prepared according to the Ti... 84 Ir 13After adjusting the Re3 (wt%) ratio, a batch powder containing nanoparticles was formed. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0388] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0389] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0390] ⑤ The alloy composition is Ti 84 Ir 13 A Re3 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system with a stainless steel substrate. The sputtering power was 3200W, the sputtering time was 30 min, and the gas flow rate was 50 mL / min.

[0391] The thickness of the thin-film getter is 1.98 μm.

[0392] Comparative Example 4

[0393] Comparative Example 4 provides a thin-film getter for absorbing alkane gases, wherein the thin-film getter for absorbing alkane gases is composed of Ti. 84 Ir 13 Re3 (wt%).

[0394] The second aspect of this comparative example provides a method for preparing a thin-film getter for absorbing alkane gases, comprising the following steps:

[0395] ① Ingredients: According to Ti 84 Ir 13 The Re3 (wt%) alloy formula was prepared by weighing 84 wt% Ti, 13 wt% Ir, and 3 wt% Re by mass. All metal raw materials used in the formulation were powders, with a purity ≥ 99.99%.

[0396] ② The main element Ti powder used in the formulation has a particle size of 10 μm, and the essential elements Re and Ir powder have a particle size of 20 nm. All powders are prepared according to the Ti... 84 Ir 13 After adjusting the Re3 (wt%) ratio, a batch powder containing nanoparticles was formed. The batch powder containing nanoparticles was then pressed at a pressure of 155 MPa for 1.5 min to form a circular compact with a diameter of 250 mm and a thickness of 18 mm.

[0397] ③ The process of densifying a circular compact with a diameter of 250mm and a thickness of 18mm by hot pressing and high-temperature sintering is as follows: the high temperature is set at 1530℃, the pressure is 1000T, and the holding time is 2h, to obtain a dense slab with a relative density ≥98.8%.

[0398] ④ The dense slab is machined to form a 2-inch multi-element alloy target.

[0399] ⑤ The alloy composition is Ti 84 Ir 13 A Re3 (wt%) alloy target was sputtered in a JW-8 magnetron sputtering system. The sputtering substrate was a stainless steel substrate. The sputtering power was 3000W, the sputtering time was 30 min, and the gas flow rate was 30 mL / min.

[0400] The thickness of the thin-film getter is 2.2 μm.

[0401] Performance testing

[0402] 1. The activation conditions, absorption rate of alkane gases (absorption rate of methane gas), and specific surface area of ​​the thin-film getters prepared in Examples 1 to 33 and Comparative Examples 1 to 4 were determined. The results are shown in Table 1.

[0403] The inhalation rate test method is the dynamic constant pressure method. The basic principle is that gas passes through a capillary with known conductance and is absorbed by the getter material, creating a pressure difference across the capillary. This pressure difference is recorded, and the inhalation rate and volume of the getter membrane can be calculated as: S = F(p_m - p_g) / p_g, where S is the inhalation rate of the sample, p_m is the pressure at the end of the capillary furthest from the getter, and p_g is the pressure at the end of the capillary closest to the getter. The pressure of the gas being tested is fixed at 4 × 10⁻⁶. -4 Pa ensures that the sample's inhalation rate does not change due to pressure variations during the test. The testing instrument model is JW-T01, software copyright number: 2020SR1040904. It conforms to the national standard GB / T 25497-2010 and the American Society for Testing and Materials (ASTM) standard F798-97(2002).

[0404] 2. Determine the bonding strength between the thin film getter and the matrix prepared in Examples 1-33 and Comparative Examples 1-4. The results are recorded in Table 1.

[0405] The equipment used to measure the adhesion strength between the film and the substrate was an automatic scratch tester, model WS-2005. This method was recognized as a mechanical industry standard by the Ministry of Machinery Industry of the People's Republic of China in 1997 (JB / T8554—1997). Its principle is "acoustic emission detection technology." When the scratching needle scratches or peels off the film layer of the sample, it emits a weak acoustic signal; the load value at this point is the adhesion strength between the film layer and the substrate (also called the critical load strength). This method is mainly applicable to testing the adhesion strength between films with thicknesses of 0.5-50 μm and the substrate. The results are shown in Tables 1 and 6.

[0406]

[0407]

[0408] 1. As can be seen from Examples 1-3, the four main elements range from 74.5% to 84.7%, and the optional elements Re and Ir are added individually or in combination, with the composition ranging from 0.3% to 25%. Examples 1 and 3 have optional elements Co and V, with optional elements ranging from 0% to 15%. No optional elements were added in Example 2. The gas-absorbing membranes in Examples 1-3 all have good methane absorption rate and load strength.

[0409] 2. Comparative Example 1: No required elements Re and Ir or optional elements were added. Even though the specific surface area of ​​the Comparative Example 1 sample was higher than that of Example 1, the absorption rate of CH4 gas in Comparative Example 1 was zero.

[0410] 3. Comparison of Examples 1-3 with Comparative Example 1 revealed that the addition of essential elements Re and Ir, either alone or in combination, helps to improve the proximity load strength between the sample and the substrate. This indicates that essential elements Re and Ir not only improve the bonding strength between the getter film and the substrate, but also help to increase the rate at which the sample absorbs CH4.

[0411] Table 2

[0412]

[0413] 4. As can be seen from Examples 4-8, the combination of three main elements or two main elements with the mandatory elements Re and Ir, and the composite addition of optional elements between 0-15%, yields excellent CH4 adsorption rate and load strength.

[0414] Table 3

[0415]

[0416]

[0417] 5. As can be seen from Examples 9-12, the combination of one of the main elements (Ti or Zr) with the required elements Re and Ir, as well as the combination of optional elements, can also yield excellent CH4 adsorption rates and loading strength. Examples 9 and 10 show that Zr has a better methane adsorption capacity than Ti.

[0418] Table 4

[0419]

[0420] 6. As can be seen from Examples 9-21, the combination of the main element Ti with the required element Re and the optional elements results in a high CH4 adsorption rate and load strength.

[0421] 7. Examples 17-18 demonstrate that the combination of the main element Ti with the mandatory element Re, and the optional element combination, results in higher methane adsorption performance than in Example 22. This illustrates that the alloy combination of the main element + selected element + optional element is beneficial for improving methane adsorption performance.

[0422] 8. Examples 19-21 demonstrate a combination of the subject element Ti with different amounts of the essential elements Re and Ir, as well as optional element combinations, which results in better methane adsorption performance than Examples 25-33.

[0423] 9. Example 22 expresses the main element Ti, combined with the mandatory element Re, without adding any optional elements. Its methane adsorption performance is lower than that of Examples 9-16. Compared with Examples 5 and 8, Example 22 also contains the main elements Ti and Zr and the mandatory element Re, without adding any optional elements, and its methane adsorption performance is lower.

[0424] 10. As can be seen from Examples 23-24, when the two main elements Ti and Zr are combined with the essential element Re, and the optional elements are zero, the methane adsorption performance is lower than that of Examples 17-18. This further illustrates that having zero optional elements is not conducive to improving methane adsorption performance.

[0425] 11. As can be seen from implementations 22 and 24, Ir has a stronger methane adsorption effect than Re.

[0426] Table 5

[0427]

[0428] 12. Examples 29-33 show a combination of the main element Ti with different amounts of the essential elements Re and Ir, with zero optional elements, and the methane adsorption performance is lower than that of Examples 17-18.

[0429] Table 6

[0430]

[0431]

[0432] 13. As can be seen from Examples 13-32, the addition of optional elements is beneficial to increasing the CH4 absorption rate. The alloy formed by the main Ti element and the mandatory and optional elements has a higher load strength than that of Zr; if the mandatory element is zero, the alloy formed by the main element and the optional elements has a zero CH4 absorption rate; the addition of optional elements is beneficial to improving the methane absorption performance.

[0433] 14. Comparative Example 2, lacking the essential elements Ir and Re, exhibits zero methane adsorption performance. Comparative Example 3, with a sputtering power exceeding the range at 3200 W, shows a sharp decrease in methane adsorption performance to 1.5 mL / s.cm. 2 The specific surface area also decreased sharply to 13m². 2 / g.

[0434] 15. In Comparative Example 4, the sputtered gas flow rate exceeded the range at 30 mL / min, resulting in a sharp decrease in methane adsorption performance to 8.5 mL / s·cm², and a sharp decrease in specific surface area to 15 m². 2 / g.

[0435] In this invention, a multi-element alloy target is prepared using 50wt%–95wt% of a main element A, 1–30wt% of a mandatory element E, and 0–20wt% of an optional element M. A thin-film getter is then prepared by sputtering, resulting in a high methane gas absorption capacity and a fast methane gas absorption rate. Using elements other than those described in this invention cannot achieve the high methane gas absorption rate described in this application. When no mandatory element is used in Comparative Examples 1 and 2, the performance of the thin-film getter at a vacuum degree of 1×10⁻⁶ is [performance value missing]. -4 At Pa, after incubation at 550℃ for 30 minutes, the initial alkyl uptake rate reached 0 mL / s. 2 The near-field load strength reaches 20N; the specific surface area reaches 19m². 2 / g and under a vacuum of 1×10 -4 At Pa, after incubation at 550℃ for 30 minutes, the initial alkyl uptake rate reached 0 mL / s. 2 The near-field load strength reaches 26N; the specific surface area reaches 18m². 2 / g, after removing the required element, it can no longer absorb methane gas, and the loading rate and specific surface area also decrease significantly.

Claims

1. A thin-film getter for absorbing alkane gases, characterized in that, Its components include a main element A, essential elements, and optional elements; the content of the main element A is 60wt% to 94wt%; the content of the essential elements is 0.3% to 28wt%; the content of the optional elements is 0% to 19wt%; the main element A includes one or more of Ti, Zr, Ta, and Nb; the essential elements include one or two of rhenium and iridium; the optional elements include one or more of V, Co, Fe, Mn, Cr, Sm, Nd, and Y. The method for preparing the thin-film getter for absorbing alkane gases includes the following steps: sputtering a multi-element alloy target onto a substrate sample by a sputtering process to form a thin-film getter for absorbing alkane gases; The sputtering process is as follows: in an inert krypton atmosphere, the sputtering power is set to 80-3200 W, the sputtering time is 10-80 min, and the sputtering gas flow rate is 40-180 mL / min; The preparation method of the multi-element alloy target is: a combination of electric arc melting technology and hot pressing high-temperature sintering technology; When the thin-film getter for absorbing alkane gases contains optional elements Nd, Sm, or Y, the specific preparation method of the multi-element alloy target material includes the following steps: P1: Mix the main element A and one or more optional elemental raw materials (Nd, Sm, or Y) in a certain proportion, and load them into a vacuum melting furnace. Evacuate the furnace to a vacuum level of 3.5 × 10⁻⁶. -4 Pa, then argon gas at 0.01 to 0.1 MPa is introduced, and the alloy is smelted under the protection of high-purity argon gas to form a master alloy button ingot containing the main element A and one or more optional elements: Nd, Sm or Y; the master alloys are respectively: A-Nd, A-Sm, AY or A-Nd-Sm, A-Nd-Y, A-Sm-Y, A-Nd-Sm-Y; P2: Under a nitrogen gas flow protective atmosphere, the master alloy button ingot is crushed, with the gas flow rate set at 15-50 mL / min; it is crushed into master alloy blocks of 0.5-12 mm. P3: Place the 0.5-12 mm master alloy block into a ball mill for wet ball milling. Set the ball milling time to 1-22 h to ball mill the master alloy into fine powder with a particle size of 2-25 μm. P4: Mix fine powder of master alloy with a particle size of 2-25μm with one or two of the essential elements rhenium and iridium in 5-30nm nanoscale powder; and one or more of the optional elements V, Co, Fe, Mn and Cr in 8-250nm nanoscale powder in a certain proportion; press the mixed powder into a circular blank with a diameter of 80mm and a thickness of 18mm; P5: The round pressed blank is densified by hot pressing and high temperature sintering technology to prepare a dense slab blank with a relative density of ≥98.5%; P6: The dense slab is machined to form a 2-inch target for preparing thin-film getters; When the thin-film getter for absorbing alkane gases does not contain optional elements Nd, Sm, or Y, or only contains optional elements V, Co, Fe, Mn, or Cr, or contains no optional elements, the specific preparation method of the multi-element alloy target material includes the following steps: Q1: Mix one or more of the main element A powder (Ti, Zr, Ta, Nb) with a particle size of 2-25 μm, with one or two of the essential elements Re and Ir of the nano-scale powder and one or more of the optional elements V, Co, Fe, Mn, and Cr of the nano-scale powder in a certain proportion; press the mixed powder into a circular compact with a diameter of 250 mm and a thickness of 18 mm. Q2: The round pressed billet is densified by hot pressing and high temperature sintering technology to prepare a dense slab with a relative density of ≥98.5%; Q3: Machining the dense slab to form a 2 or 8-inch target for preparing thin-film getters.

2. The thin-film getter for absorbing alkane gases according to claim 1, characterized in that, The content of the main element is 65wt% to 93wt%; the content of the essential element is 0.3wt% to 25wt%; and the content of the optional element is 0wt% to 15wt%.

3. The thin-film getter for absorbing alkane gases according to claim 1, characterized in that, The specific steps for smelting the alloy in P1 include: turning on the power supply for arc melting, then igniting an arc on the titanium ingot. After the titanium ingot is completely melted, the alloy is formed by mixing the main element A and optional elements Nd, Sm, or Y in proportion. After one melting cycle, the alloy sample is allowed to cool and solidify completely. The sample is then flipped over using a robotic arm. The above steps are repeated 4 to 6 times. Magnetic stirring is applied during the last two cycles for 2-3 minutes. After the melting is completed, argon gas is introduced after the alloy sample has cooled completely. The furnace door is then opened, and the master alloy button ingot is removed.

4. The thin-film getter for absorbing alkane gases according to claim 1, characterized in that, The current used during the smelting process is in the range of 150–300 A.

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