Titanium-aluminum alloy target as well as preparation method and application thereof

Abstract

The invention discloses a titanium-aluminum alloy target as well as a preparation method and application thereof, and belongs to the technical field of alloy targets. According to the titanium-aluminum alloy target material, a titanium-aluminum alloy residual target is placed on a mixed powder layer formed by pre-mixed titanium powder and pre-mixed aluminum powder, then the pre-mixed titanium powder and pre-mixed aluminum powder are laid on a sheath, then sheath welding and degassing are carried out, and hot isostatic pressing treatment is carried out under the specific temperature and pressure range; the waste titanium-aluminum alloy residual target can be fully utilized, the preparation cost of the titanium-aluminum alloy residual target is reduced, and the resource utilization rate is increased; in addition, the titanium-aluminum alloy target material prepared by adopting the technical scheme is high in purity, high in density, high in target material flatness and uniform and fine in grain structure.

Description

Technical Field

[0001] The invention belongs to the technical field of alloy target materials, and in particular relates to a titanium-aluminum alloy target material and a preparation method and application thereof. Background Art

[0002] Titanium-aluminum alloy is an alloy sputtering target for vacuum coating. Titanium-aluminum alloy targets with different characteristics can be obtained by adjusting the content of titanium and aluminum in the alloy. Titanium-aluminum intermetallic compounds are hard and brittle materials with good wear resistance. A layer of titanium-aluminum intermetallic compounds on the surface of ordinary tools can effectively extend the service life of the tools. If sputtering is carried out in conjunction with nitrogen discharge arcing, a high-hardness and low-friction coefficient surface film can be obtained, which is particularly suitable for the surface coating of various tools, molds and other vulnerable parts, so it has good application prospects in the mechanical processing industry.

[0003] Patent CN116121542A pre-treats, pickles, washes with water, and cleans with organic solvents the titanium-aluminum alloy residual target, and obtains a target block after drying; and then obtains a titanium-aluminum alloy target by electromagnetic induction melting, ultrasonic treatment, and cooling the melt. However, this technical solution has many steps, which leads to increased costs. Therefore, how to prepare high-purity, high-performance titanium-aluminum alloy targets at low cost has become a research hotspot in the target field. Summary of the invention

[0004] The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a titanium-aluminum alloy target material with high purity, high density, high target flatness, uniform and fine grain structure, and its preparation method and application, which uses titanium-aluminum alloy residual target as raw material.

[0005] To achieve the above object, in a first aspect of the present invention, the present invention provides a method for preparing a titanium aluminum alloy target, the preparation method comprising the following steps:

[0006] (1) placing graphite paper and a separator in the bottom of the bag in sequence, then spreading the premixed titanium powder and aluminum powder on the separator to obtain a mixed powder layer, then placing the pretreated titanium-aluminum alloy residual target on the mixed powder layer, then spreading the premixed titanium powder and aluminum powder on the titanium-aluminum alloy residual target, and finally placing the graphite paper and the separator in sequence and welding;

[0007] (2) Degassing the welded sheath, and after degassing, hot isostatic pressing at 400-600° C. and 80-140 MPa, and then removing the sheath to obtain a titanium aluminum alloy target.

[0008] The titanium-aluminum alloy target material provided by the present invention is prepared by placing a titanium-aluminum alloy residual target on a mixed powder layer formed by premixed titanium powder and aluminum powder, then covering a sheath with the premixed titanium powder and aluminum powder, and then performing sheath welding, degassing, and hot isostatic pressing under a specific temperature and pressure range; the waste titanium-aluminum alloy residual target can be fully utilized, the preparation cost of the titanium-aluminum alloy residual target can be reduced, and the resource utilization rate can be improved; and the titanium-aluminum alloy target material prepared by the technical solution of the present invention has high purity, high density, high target flatness, and uniform and fine grain structure.

[0009] As a preferred embodiment of the preparation method of the present invention, the temperature of the hot isostatic pressing is 450-550° C. and the pressure is 100-120 MPa.

[0010] Exemplarily, the temperature of the hot isostatic pressing may be any point value or any two point range value between 450-550°C, such as 450°C, 460°C, 470°C, 480°C, 490°C, 500°C, 510°C, 520°C, 530°C, 540°C, 550°C, etc. The pressure of the hot isostatic pressing is 100-120MPa, such as 100MPa, 102MPa, 104MPa, 106MPa, 108MPa, 110MPa, 112MPa, 114MPa, 116MPa, 118MPa, 120MPa, etc.

[0011] The present invention has been found that the selection of temperature and pressure during the hot isostatic pressing process will affect the uniformity of the temperature field, thereby affecting the density of the formed target material and the fine uniformity of the grains; wherein, the pressurization method during the hot isostatic pressing process is pressurization in all directions, which is conducive to the close bonding of the titanium-aluminum alloy residual target and the powder, and the appropriate temperature range and all-round pressurization method can improve the density of the titanium-aluminum alloy target material while refining and homogenizing the grain structure of the titanium-aluminum alloy target material; especially when the temperature and pressure of the hot isostatic pressing are further selected within the above range, the comprehensive performance of the obtained titanium-aluminum alloy target material is better.

[0012] As a preferred embodiment of the preparation method of the present invention, the hot isostatic pressing time is 3-8 hours.

[0013] Exemplarily, the hot isostatic pressing time may be any point value or any two point range values ​​between 3-8 hours, for example, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, etc.

[0014] The present invention has found that the time of hot isostatic pressing treatment will also affect the comprehensive performance of the titanium aluminum alloy target. When the time of hot isostatic pressing treatment is further selected to be 3-8h, the obtained titanium aluminum alloy target has a higher density and better grain uniformity.

[0015] As a preferred embodiment of the preparation method of the present invention, the mass percentage of the premixed titanium powder and aluminum powder is 40-60% based on the mass of the titanium-aluminum alloy residual target.

[0016] As a preferred embodiment of the preparation method of the present invention, the mass ratio of the titanium powder to the aluminum powder is (3-6): (4-7).

[0017] Exemplarily, the mass ratio of the titanium powder to the aluminum powder may be 3:4, 3:5, 3:6, 3:7, 4:4, 4:5, 4:6, 4:7, 5:4, 5:5, 5:6, 5:7, 6:4, 6:5, 6:6, 6:7, etc.

[0018] As a preferred embodiment of the preparation method of the present invention, the purity of the titanium powder is greater than 99.9%, and the median particle size of the titanium powder is 30-50 μm.

[0019] As a preferred embodiment of the preparation method of the present invention, the purity of the aluminum powder is greater than 99.9%, and the median particle size of the aluminum powder is 30-50 μm.

[0020] The present invention has found that the purity of titanium powder and aluminum powder and the median particle size of the two will affect the mixing effect of the two and the adhesion effect on the surface of the titanium-aluminum alloy residual target; at the same time, the mass ratio of titanium powder and aluminum powder will also affect the subsequent sintering effect on the surface of the titanium-aluminum alloy residual target; when the mass ratio range of titanium powder and aluminum powder and the purity and median particle size of titanium powder and aluminum powder are further selected within the above range, the obtained titanium-aluminum alloy target material has a higher density, a higher surface smoothness of the target material, and a more uniform and fine grain structure.

[0021] As a preferred embodiment of the preparation method of the present invention, the premixing method of titanium powder and aluminum powder is: adding titanium powder and aluminum powder into a mixer, and mixing the powders at a speed of 6-12 r / min for 5-10 hours.

[0022] Preferably, the mixer is a V-shaped powder mixer.

[0023] Preferably, the powder mixing barrel in the V-shaped powder mixer is a polyurethane lined powder mixing barrel.

[0024] Preferably, in the mixer, the ratio of powder to ball material is 1:2.

[0025] Preferably, after adding titanium powder and aluminum powder into the mixer, argon gas is filled in for 10-40 minutes before the powder mixing operation is performed.

[0026] The present invention has found that when the above-mentioned pre-mixing method of titanium powder and aluminum powder is adopted, the introduction of other impurities can be avoided while ensuring that the titanium powder and aluminum powder are fully mixed, thereby effectively improving the density and particle size uniformity of the titanium aluminum alloy target.

[0027] As a preferred embodiment of the preparation method of the present invention, the pressure in the package after degassing is ≤5×10 - 4 Pa.

[0028] As a preferred embodiment of the preparation method of the present invention, the pretreatment method of the titanium-aluminum alloy residual target is: machining the titanium-aluminum alloy residual target, followed by alkali washing, water washing, organic solvent washing, and drying in sequence to obtain the pretreated titanium-aluminum alloy residual target.

[0029] The above-mentioned pretreatment method is used to treat the titanium-aluminum alloy residual target, which can effectively remove the oxide layer on the surface of the residual target back plate and the sputtering layer, thereby facilitating the subsequent close bonding of titanium powder and aluminum powder with the residual target, thereby improving the density of the prepared titanium-aluminum alloy target material.

[0030] Preferably, the alkaline washing is washing with a NaOH aqueous solution, and the organic solvent washing is washing with ethanol and / or acetone.

[0031] Preferably, in the preparation method provided by the present invention, two titanium-aluminum alloy target materials can be prepared simultaneously in one package.

[0032] In a second aspect of the present invention, the present invention provides a titanium-aluminum alloy target material, and the titanium-aluminum alloy target material is prepared by the preparation method of the present invention.

[0033] The titanium-aluminum alloy target material provided by the present invention has excellent comprehensive performance, specifically, has good density, surface flatness and fine and uniform grain structure, and can be effectively used in subsequent sputtering.

[0034] In the third aspect of the present invention, the present invention provides the use of the titanium aluminum alloy target in vacuum coating.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] The titanium-aluminum alloy target material provided by the present invention is prepared by placing a titanium-aluminum alloy residual target on a mixed powder layer formed by premixed titanium powder and aluminum powder, then covering a sheath with the premixed titanium powder and aluminum powder, and then performing sheath welding, degassing, and hot isostatic pressing under a specific temperature and pressure range; the waste titanium-aluminum alloy residual target can be fully utilized, the preparation cost of the titanium-aluminum alloy residual target can be reduced, and the resource utilization rate can be improved; and the titanium-aluminum alloy target material prepared by the technical solution of the present invention has high purity, high density, high target flatness, and uniform and fine grain structure. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 This is a schematic diagram of the package structure in Example 1;

[0038] Figure 2 This is a microscopic morphology of the titanium aluminum alloy target prepared in Example 1. DETAILED DESCRIPTION

[0039] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0040] Unless otherwise specified, the reagents, methods and equipment used in the present invention are all conventional reagents, methods and equipment in the art; and unless otherwise specified, the raw materials used in parallel experiments are from the same batch of raw materials.

[0041] Example 1

[0042] An embodiment of the present invention provides a titanium aluminum alloy target material, and a method for preparing the titanium aluminum alloy target material comprises the following steps:

[0043] (1) removing the oxide layer on the surface of the back plate and the sputtering layer of the one-piece titanium-aluminum alloy residual target by lathe processing, and then washing the residual target with alkali (NaOH aqueous solution), water and organic solvent (ethanol and acetone in sequence), and drying after washing to obtain a pretreated titanium-aluminum alloy residual target;

[0044] (2) Pour titanium powder (purity>99.9%, median particle size of 40 μm) and aluminum powder (purity>99.9%, median particle size of 40 μm) in a mass ratio of 4:6 into a 20L polyurethane-lined powder mixing barrel, then place them into a V-type powder mixer at a ball-to-material ratio of 1:2, introduce argon for 20 minutes, and mix at a speed of 10 r / min for 8 hours to obtain pre-mixed titanium powder and aluminum powder;

[0045] (3) Using a stainless steel sheath of appropriate size, cutting graphite paper and a low-carbon steel partition of corresponding size, placing the graphite paper and the partition in turn at the bottom of the sheath, then spreading the premixed titanium powder and aluminum powder on the partition to obtain a mixed powder layer, then placing the pretreated titanium-aluminum alloy residual target on the mixed powder layer, then spreading the premixed titanium powder and aluminum powder in the sheath containing the titanium-aluminum alloy residual target (the mass percentage of the premixed titanium powder and aluminum powder is 40% based on the mass of the titanium-aluminum alloy residual target), and then placing the graphite paper and the partition in turn; finally, welding the cover plate to the sheath and the degassing pipe by argon arc welding;

[0046] (4) The welded sheath is subjected to helium mass spectrometry leak detection and vacuum degassing, and the air is sealed until the pressure inside the sheath is ≤5×10 - 4 Pa; then the degassed package is placed in a hot isostatic pressing environment at a temperature of 500°C and a pressure of 110MPa for 6 hours;

[0047] (5) After hot isostatic pressing, the jacket is removed and the target is formed by lathe to obtain a titanium aluminum alloy target.

[0048] Example 2

[0049] An embodiment of the present invention provides a titanium aluminum alloy target material, and a method for preparing the titanium aluminum alloy target material comprises the following steps:

[0050] (1) removing the oxide layer on the surface of the back plate and the sputtering layer of the one-piece titanium-aluminum alloy residual target by lathe processing, and then washing the residual target with alkali (NaOH aqueous solution), water and organic solvent (ethanol and acetone in sequence), and drying after washing to obtain a pretreated titanium-aluminum alloy residual target;

[0051] (2) Pour titanium powder (purity>99.9%, median particle size of 30 μm) and aluminum powder (purity>99.9%, median particle size of 50 μm) in a mass ratio of 6:4 into a 20L polyurethane-lined powder mixing barrel, and then put them into a V-type powder mixer at a ball-to-material ratio of 1:2, introduce argon for 40 minutes, and mix at a speed of 6 r / min for 10 hours to obtain pre-mixed titanium powder and aluminum powder;

[0052] (3) Using a stainless steel sheath of appropriate size, cutting graphite paper and a low-carbon steel partition of corresponding size, placing the graphite paper and the partition in turn at the bottom of the sheath, then spreading the premixed titanium powder and aluminum powder on the partition to obtain a mixed powder layer, then placing the pretreated titanium-aluminum alloy residual target on the mixed powder layer, then spreading the premixed titanium powder and aluminum powder in the sheath containing the titanium-aluminum alloy residual target (the mass percentage of the premixed titanium powder and aluminum powder is 50% based on the mass of the titanium-aluminum alloy residual target), and then placing the graphite paper and the partition in turn; finally, welding the cover plate to the sheath and the degassing pipe by argon arc welding;

[0053] (4) The welded sheath is subjected to helium mass spectrometry leak detection and vacuum degassing, and the air is sealed until the pressure inside the sheath is ≤5×10 - 4 Pa; then the degassed package is placed in a hot isostatic pressing environment at a temperature of 450°C and a pressure of 120MPa for 8h;

[0054] (5) After hot isostatic pressing, the jacket is removed and the target is formed by lathe to obtain a titanium aluminum alloy target.

[0055] Example 3

[0056] An embodiment of the present invention provides a titanium aluminum alloy target material, and a method for preparing the titanium aluminum alloy target material comprises the following steps:

[0057] (1) removing the oxide layer on the surface of the back plate and the sputtering layer of the one-piece titanium-aluminum alloy residual target by lathe processing, and then washing the residual target with alkali (NaOH aqueous solution), water and organic solvent (ethanol and acetone in sequence), and drying after washing to obtain a pretreated titanium-aluminum alloy residual target;

[0058] (2) Pour titanium powder (purity>99.9%, median particle size of 50 μm) and aluminum powder (purity>99.9%, median particle size of 30 μm) in a mass ratio of 3:7 into a 20 L polyurethane-lined powder mixing barrel, then place them in a V-type powder mixer at a ball-to-material ratio of 1:2, introduce argon for 10 minutes, and mix at a speed of 12 r / min for 5 hours to obtain pre-mixed titanium powder and aluminum powder;

[0059] (3) Using a stainless steel sheath of appropriate size, cutting graphite paper and a low-carbon steel partition of corresponding size, placing the graphite paper and the partition in turn at the bottom of the sheath, then spreading the premixed titanium powder and aluminum powder on the partition to obtain a mixed powder layer, then placing the pretreated titanium-aluminum alloy residual target on the mixed powder layer, then spreading the premixed titanium powder and aluminum powder in the sheath containing the titanium-aluminum alloy residual target (the mass percentage of the premixed titanium powder and aluminum powder is 60% based on the mass of the titanium-aluminum alloy residual target), and then placing the graphite paper and the partition in turn; finally, welding the cover plate to the sheath and the degassing pipe by argon arc welding;

[0060] (4) The welded sheath is subjected to helium mass spectrometry leak detection and vacuum degassing, and the air is sealed until the pressure inside the sheath is ≤5×10 - 4 Pa; then the degassed package is placed in a hot isostatic pressing environment at a temperature of 550°C and a pressure of 100 MPa for 3 hours;

[0061] (5) After hot isostatic pressing, the jacket is removed and the target is formed by lathe to obtain a titanium aluminum alloy target.

[0062] Example 4

[0063] The embodiment of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of embodiment 1 is that in step (4), hot isostatic pressing is performed at a temperature of 400° C. and a pressure of 140 MPa.

[0064] Example 5

[0065] The embodiment of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of embodiment 1 is that in step (4), hot isostatic pressing is performed at a temperature of 600° C. and a pressure of 80 MPa.

[0066] Example 6

[0067] The embodiment of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of Example 1 is that in step (4), the hot isostatic pressing treatment time is 2 hours.

[0068] Example 7

[0069] The embodiment of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of Example 1 is that in step (4), the hot isostatic pressing treatment time is 10 hours.

[0070] Example 8

[0071] The embodiment of the present invention provides a titanium-aluminum alloy target material. The only difference between the preparation method of the titanium-aluminum alloy target material and that of embodiment 1 is that in step (3), the mass percentage of the premixed titanium powder and aluminum powder is 30% by mass.

[0072] Example 9

[0073] The embodiment of the present invention provides a titanium-aluminum alloy target material. The only difference between the preparation method of the titanium-aluminum alloy target material and that of embodiment 1 is that in step (3), the mass percentage of the premixed titanium powder and aluminum powder is 70% by mass.

[0074] Example 10

[0075] The embodiment of the present invention provides a titanium-aluminum alloy target material. The only difference between the preparation method of the titanium-aluminum alloy target material and that of embodiment 1 is that in step (2), the median particle size of the titanium powder is 10 μm.

[0076] Embodiment 11

[0077] The embodiment of the present invention provides a titanium-aluminum alloy target material. The only difference between the preparation method of the titanium-aluminum alloy target material and that of embodiment 1 is that in step (2), the median particle size of the titanium powder is 70 μm.

[0078] Example 12

[0079] The embodiment of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of embodiment 1 is that in step (2), mixing is performed at a rotation speed of 20 r / min for 5 hours.

[0080] Comparative Example 1

[0081] The comparative example of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of Example 1 is that in step (4), the temperature of hot isostatic pressing is 350°C.

[0082] Comparative Example 2

[0083] The comparative example of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of Example 1 is that in step (4), the temperature of hot isostatic pressing is 650°C.

[0084] Comparative Example 3

[0085] The comparative example of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of Example 1 is that in step (4), the hot isostatic pressing pressure is 60 MPa.

[0086] Comparative Example 4

[0087] The comparative example of the present invention provides a titanium aluminum alloy target material. The only difference between the preparation method of the titanium aluminum alloy target material and that of Example 1 is that in step (4), the hot isostatic pressing pressure is 160 MPa.

[0088] Effect example

[0089] The effect examples of the present invention verify the performance of the titanium aluminum alloy targets prepared by Examples 1-12 and Comparative Examples 1-4, including the following aspects:

[0090] 1. Density: tested by Archimedes drainage method;

[0091] 2. Surface flatness: tested with a three-coordinate measuring instrument;

[0092] 3. Fine and uniform grain structure: Use metallographic microscope and SEM to test and record the average grain size;

[0093] The obtained results are shown in Table 1;

[0094] Table 1

[0095]

[0096]

[0097] It can be seen from Table 1 that the titanium aluminum alloy target prepared by the technical solution provided by the present invention has excellent comprehensive properties. Specifically, the density of the prepared titanium aluminum alloy target is above 99.90%, the surface flatness is below 4.2 mm, the grain structure is fine and uniform, and the average grain size is below 88 μm. The titanium aluminum alloy target prepared in Example 1 was observed by microscopic morphology, and the obtained figure is as follows: Figure 2 As shown, from Figure 2 It can be seen that the particle size and structure of the prepared titanium aluminum alloy target are fine and uniform.

[0098] It can be seen from Example 1 and Comparative Examples 1-4 that when the temperature and pressure of the hot isostatic pressing treatment are not within the range given in the present invention, the obtained product cannot simultaneously achieve the goals of high density, fine grains and smooth surface.

[0099] Finally, it should be noted that the above embodiments are intended to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A method for preparing a titanium aluminum alloy target, characterized in that: The preparation method comprises the following steps: (1) placing graphite paper and a separator in the bottom of the bag in sequence, then spreading the premixed titanium powder and aluminum powder on the separator to obtain a mixed powder layer, then placing the pretreated titanium-aluminum alloy residual target on the mixed powder layer, then spreading the premixed titanium powder and aluminum powder in the bag containing the titanium-aluminum alloy residual target, and finally placing the graphite paper and the separator in sequence and welding; (2) Degassing the welded sheath, and after degassing, hot isostatic pressing at 400-600° C. and 80-140 MPa, and then removing the sheath to obtain a titanium aluminum alloy target.

2. The preparation method according to claim 1, characterized in that: The hot isostatic pressing has a temperature of 450-550° C., a pressure of 100-120 MPa, and a time of 3-8 hours.

3. The preparation method according to claim 1, characterized in that: Calculated on the mass of the titanium-aluminum alloy residual target, the mass percentage of the premixed titanium powder and aluminum powder is 40-60%.

4. The preparation method according to claim 1, characterized in that: The mass ratio of the titanium powder to the aluminum powder is (3-6):(4-7).

5. The preparation method according to claim 1, characterized in that: The purity of the titanium powder is greater than 99.9%, and the median particle size of the titanium powder is 30-50 μm; And / or, the purity of the aluminum powder is greater than 99.9%, and the median particle size of the aluminum powder is 30-50 μm.

6. The preparation method according to claim 1, characterized in that: The premixing method of titanium powder and aluminum powder is as follows: adding titanium powder and aluminum powder into a mixer, and mixing the powders at a speed of 6-12 r / min for 5-10 hours.

7. The preparation method according to claim 1, characterized in that: The pressure in the package after degassing is ≤5×10 - 4 Pa.

8. The preparation method according to claim 1, characterized in that: The pretreatment method of the titanium-aluminum alloy residual target is: machining the titanium-aluminum alloy residual target, then sequentially alkali washing, water washing, organic solvent washing, and drying to obtain the pretreated titanium-aluminum alloy residual target.

9. A titanium aluminum alloy target, characterized in that: The titanium aluminum alloy target is prepared by the preparation method according to any one of claims 1 to 8.

10. Use of the titanium aluminum alloy target material as claimed in claim 9 in vacuum coating.

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