Niobium oxide rotating target material and preparation method thereof

Abstract

The invention provides a niobium oxide rotating target material and a preparation method thereof, and belongs to the technical field of preparation of target materials. In the preparation process of the niobium oxide rotating target material, the base coat with the specific thickness and the niobium oxide spraying powder with the specific average particle size are selected, the stress concentration problem caused by the small outer diameter of the base body pipe is effectively relieved, and the niobium oxide rotating target material with the outer diameter smaller than or equal to 90 mm, the thickness larger than or equal to 8 mm, the density larger than 4.7 g / cm < 3 >, compact tissue, uniform components, no cracks, the resistivity smaller than or equal to 0.09 omega.cm and the thickness larger than or equal to 8 mm is obtained. The deposition rate of the niobium oxide rotating target material is 45% or above. In the sputtering process of the niobium oxide rotating target material, the air pressure required by arcing can be reduced, the sputtering efficiency and the quality of a sputtered film are improved, and the service life of the target material is prolonged.

Description

Technical Field

[0001] The present invention relates to the technical field of target preparation, and particularly relates to a niobium oxide rotary target and a preparation method thereof. Background Art

[0002] Niobium oxide materials have excellent ultraviolet absorption ability, can be used to make heat-sensitive films, have a high refractive index, and are widely used in the fields of touch screens and optical glass. At present, plasma-sprayed niobium oxide targets have a huge market in their coating fields. Currently, the main size of the back tube of the niobium oxide target for spraying is 133 mm. However, due to the excessive thickness, the utilization rate of the target after spraying is low. When the outer diameter of the spraying back tube is small, the magnetic field intensity per unit area on the surface of the sprayed target will be higher, which helps to confine electrons, thereby reducing the air pressure required for arc ignition and improving the sputtering efficiency. In addition, the target sprayed by the small outer diameter back tube can be consumed more evenly during the sputtering process, thereby prolonging the service life of the target.

[0003] Since the smaller the outer diameter of the back tube, the larger the radian of the powder deposition surface, the more likely it is to cause stress concentration. Coupled with the high thermal expansion coefficient of niobium oxide materials, the thermal stress generated during the spraying process is not easily released, resulting in the target being more prone to cracking and affecting the spraying thickness of the target. Currently, Patent 103045995B describes that the outer diameter of the back tube is 66 mm, the bottom layer is 0.05 - 0.3 mm, the powder particle size is 48 - 106 μm, and the spraying thickness is only 5 mm thick; Patent 104831243B describes that the outer diameter of the back tube is 133 mm, the bottom layer is 0.5 mm, the powder particle size ≤ 150 μm, and the spraying thickness is unknown.

[0004] Therefore, how to obtain a small-size niobium oxide rotary target with a high thickness is an urgent problem to be solved at present. Summary of the Invention

[0005] The purpose of the present disclosure is to overcome the deficiencies of the prior art and provide a niobium oxide rotary target and a preparation method thereof.

[0006] To achieve the above purpose, the technical solutions adopted by the present disclosure are as follows:

[0007] In the first aspect, a niobium oxide rotary target is provided, wherein the outer diameter of the matrix tube of the niobium oxide rotary target is ≤ 90 mm, the thickness is ≥ 8 mm, and the density is 4.7 g / cm 3 or more.

[0008] In the second aspect, a preparation method of the niobium oxide rotary target is provided, including the following steps: treatment of the matrix tube for spraying, spraying the bottom layer, and spraying niobium oxide spraying powder on the matrix tube by a plasma spraying process; wherein the thickness of the bottom layer is 0.6 - 0.9 mm, and the average particle size of the niobium oxide spraying powder is 50 - 120 μm.

[0009] In some embodiments, the purity of the niobium oxide spraying powder is 99.95 - 99.99%, and the loose bulk density is 1.5 - 2 g / cm 3 .

[0010] In some embodiments, the treatment of the spraying substrate tube includes cleaning, grinding to remove the dirt and oxide layer on the surface of the substrate tube, and then sandblasting to roughen the surface of the substrate tube.

[0011] In some embodiments, the primer layer refers to spraying an alloy coating with a thickness of 0.6 - 0.9 mm on the surface of the substrate tube.

[0012] In some embodiments, the alloy coating is sprayed with nickel - coated aluminum, nickel - chromium, nickel - chromium - aluminum, nickel - cobalt - chromium - aluminum - yttrium powder by plasma spraying method, or aluminum bronze or nickel - aluminum alloy wire is sprayed by arc spraying method;

[0013] In some embodiments, during the process of spraying niobium oxide spraying powder on the substrate tube by plasma spraying process, the substrate tube is controlled to rotate around the central axis at a speed of 250 - 300 r / min, the distance between the spray gun and the substrate tube is maintained at 180 - 220 mm, and the spray gun reciprocates back and forth uniformly along the direction of the substrate tube at a speed of 30 - 90 mm / min;

[0014] In some embodiments, the substrate tube is cooled with water during the plasma spraying process;

[0015] In some embodiments, during the plasma spraying process, the surface of the target is cooled with compressed gas or cryogenic cooling fluid, and the surface temperature of the target is controlled at 100 - 130 °C.

[0016] In some embodiments, the compressed gas is compressed air or inert gas;

[0017] In some embodiments, the cryogenic cooling fluid is carbon dioxide or liquid nitrogen.

[0018] In some embodiments, the cooling of the surface of the target with compressed gas or cryogenic cooling fluid is achieved by a cooling temperature control device. The cooling control device includes a trachea support parallel to the spraying substrate. Two parallel blowing pipes are installed on the trachea support. The blowing pipes are perpendicular to the spraying substrate, and a gas flowmeter is installed at the air inlet of the blowing pipes.

[0019] In some embodiments, the inner diameter of the blowing pipe is 8 - 10 mm, the outer diameter is 6 - 8 mm, and the length is 150 - 200 mm;

[0020] In some embodiments, the distance between the pipe end of the blowing pipe and the coating during spraying is 20 - 30 mm;

[0021] In some embodiments, the distance between the two parallel blow pipes is 100-200 mm.

[0022] Compared with the prior art, the beneficial effects of the present disclosure are as follows: In the preparation process of the niobium oxide rotary target, a specific thickness of the underlayer and niobium oxide spraying powder with a specific average particle size are selected, effectively alleviating the stress concentration problem caused by the small outer diameter of the substrate tube, and obtaining a substrate tube with an outer diameter ≤ 90 mm, a thickness ≥ 8 mm, and a density of 4.7 g / cm 3 As described above, a niobium oxide rotary target with a dense structure, uniform composition, no cracks, a resistivity ≤ 0.09 Ω·cm, and a deposition rate of more than 45%. During the sputtering process of the niobium oxide rotary target of the present invention, the air pressure required for arc ignition can be reduced, the sputtering efficiency and the quality of the sputtered thin film can be improved, and the service life of the target can be extended. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic structural diagram of the dust removal and cooling device on the surface of the plasma spraying rotary target in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0024] To facilitate the understanding of the present disclosure, the present disclosure will be described more comprehensively below. However, the present disclosure can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure content of the present disclosure more thorough and comprehensive.

[0025] As used herein, the terms:

[0026] "Prepared from" is synonymous with "comprising". As used herein, the terms "comprising", "including", "having", "containing" or any other variation thereof are intended to cover non-exclusive inclusion. For example, a composition, step, method, article or device containing the listed elements is not necessarily limited to those elements, but may include other elements not explicitly listed or elements inherent to such composition, step, method, article or device.

[0027] The connecting word "consisting of" excludes any unstated element, step or component. If used in a claim, this phrase will make the claim closed, excluding materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of" appears in a clause of the claim body rather than immediately following the subject, it only limits the elements described in that clause; other elements are not excluded from the claim as a whole.

[0028] When an equivalent, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper preferred values and lower preferred values, this should be understood to specifically disclose all ranges formed by any pairing of any range upper limit or preferred value with any range lower limit or preferred value, regardless of whether the range is disclosed individually. For example, when the range "1 - 5" is disclosed, the described range should be interpreted to include ranges such as "1 - 4", "1 - 3", "1 - 2", "1 - 2 and 4 - 5", "1 - 3 and 5", etc. When a numerical range is described herein, unless otherwise specified, the range is intended to include its endpoint values and all integers and fractions within the range.

[0029] In these embodiments, unless otherwise specified, the parts and percentages are by mass.

[0030] "Parts by mass" refers to the basic measurement unit representing the mass ratio relationship of multiple components. 1 part can represent any unit mass, such as 1 g or 2.689 g, etc. If we say that the mass of component A is a parts by mass and the mass of component B is b parts by mass, it means the mass ratio of component A to component B is a:b. Or, it means the mass of component A is aK and the mass of component B is bK (K is any number representing a multiple factor). It should not be misunderstood that, different from the number of parts by mass, the sum of the parts by mass of all components is not limited to 100 parts.

[0031] "And / or" is used to indicate that either or both of the described situations may occur. For example, A and / or B includes (A and B) and (A or B).

[0032] The smaller the outer diameter of the substrate tube of the niobium oxide rotating target, the larger the radian of the deposition surface of the niobium oxide spraying powder, the easier it is to cause stress concentration, and the niobium oxide has a high coefficient of thermal expansion, and the thermal stress generated during the plasma spraying process is not easily released, resulting in the niobium oxide rotating target being prone to cracking, and the thickness of the niobium oxide rotating target is low. To solve the above problems, in the first aspect of the present invention, a niobium oxide rotating target is provided, and the outer diameter of the substrate tube of the niobium oxide rotating target is ≤90 mm, the thickness is ≥8 mm, and the density is 4.7 g / cm 3 or more.

[0033] The niobium oxide rotating target prepared by the present invention has a dense structure, uniform composition, no cracks, a resistivity of ≤0.09 Ω·cm, and a deposition rate of more than 45%; during the sputtering process, it can reduce the gas pressure required for arc ignition, improve the sputtering efficiency and the quality of the sputtered thin film, and extend the service life of the target.

[0034] Specifically, the outer diameter of the substrate tube of the niobium oxide rotating target is 60 - 90 mm.

[0035] Specifically, the thickness of the niobium oxide rotating target is 8-12 mm.

[0036] Specifically, the density of the niobium oxide rotating target is 4.7-4.95 g / cm 3 .

[0037] Specifically, the resistance of the niobium oxide rotating target is 0.04-0.09 Ω·cm.

[0038] Specifically, the deposition rate of the niobium oxide rotating target is 45-70%.

[0039] In a second aspect, a method for preparing the niobium oxide rotating target is provided, including the following steps: treatment of the substrate tube, spraying a primer layer, and spraying niobium oxide spraying powder on the substrate tube by a plasma spraying process; wherein the thickness of the primer layer is 0.6-0.9 mm, and the average particle size of the niobium oxide spraying powder is 50-120 μm.

[0040] In the preparation process of the niobium oxide rotating target of the present invention, a primer layer with a specific thickness and niobium oxide spraying powder with a specific average particle size are selected, effectively alleviating the stress concentration problem caused by the small outer diameter of the substrate tube, and obtaining a niobium oxide rotating target with an outer diameter of the substrate tube ≤90 mm, a thickness ≥8 mm, a density of 4.7 g / cm 3 as above, with a dense structure, uniform composition, no cracks, a resistivity ≤0.09 Ω·cm, and a deposition rate of more than 45%.

[0041] Specifically, the thickness of the primer layer can be, but is not limited to, 0.6 mm, 0.65 mm, 0.7 mm, 0.75 mm, 0.8 mm, 0.85 mm, 0.9 mm.

[0042] If the thickness of the primer layer is too small or too large, it will cause cracking of the niobium oxide target, and a niobium oxide rotating target with a thickness ≥8 mm cannot be obtained.

[0043] Specifically, the average particle size of the niobium oxide spraying powder is 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, 120 μm; the test method is GB / T 19077-2016.

[0044] If the average particle size of the niobium oxide spraying powder is too small or too large, it will cause cracking of the niobium oxide target, and a niobium oxide rotating target with a thickness ≥8 mm cannot be obtained.

[0045] Specifically, the niobium oxide spraying powder of the present invention can be obtained by purchasing commercially available products or prepared by methods well-known in the art.

[0046] In some embodiments, the purity of the niobium oxide spraying powder is 99.95-99.99%; the loose bulk density is 1.5-2 g / cm3 , for example, it can be but not limited to 1.5 g / cm 3 , 1.6 g / cm 3 , 1.7 g / cm 3 , 1.8 g / cm 3 , 1.9 g / cm 3 , 2 g / cm 3 .

[0047] In some embodiments, the treatment of the sprayed substrate tube includes cleaning, grinding to remove dirt and oxide layers on the surface of the substrate tube, and then sandblasting to roughen the surface of the substrate tube.

[0048] By performing the above treatment on the sprayed substrate tube, the substrate tube has a certain roughness, which is beneficial to the spraying of the bottom layer and improves the bonding force between the bottom layer and the substrate tube.

[0049] In some embodiments, the bottom layer refers to an alloy coating with a thickness of 0.6 - 0.9 mm sprayed on the surface of the substrate tube.

[0050] In some embodiments, the alloy coating is sprayed with nickel - aluminide, nickel - chromium, nickel - chromium - aluminum, nickel - cobalt - chromium - aluminum - yttrium powder by plasma spraying method, or aluminum bronze or nickel - aluminum alloy wire is sprayed by arc spraying method;

[0051] In some embodiments, during the process of spraying niobium oxide spraying powder on the substrate tube by plasma spraying process, the substrate tube is controlled to rotate around the central axis at a speed of 250 - 300 r / min, and the spray gun is kept at a distance of 180 - 220 mm from the substrate tube and reciprocates uniformly along the direction of the substrate tube at a speed of 30 - 90 mm / min.

[0052] Specifically, the plasma spraying process parameters for spraying niobium oxide spraying powder on the substrate tube are shown in Table 1 below.

[0053] Table 1

[0054]

[0055]

[0056] In some embodiments, during the plasma spraying process, the substrate tube is cooled with water so that the water temperature inside the substrate tube is 70 - 80 °C. Within this water temperature range, it can not only promote the bonding between the target blank and the substrate tube, but also timely take away the heat generated during spraying, avoiding cracking caused by thermal stress concentration.

[0057] In some embodiments, during the plasma spraying process, it further includes a dust removal step, and the dust removal frequency is 30 - 50 Hz. Within this frequency range, it can timely take away the molten powder that has not been deposited on the target material, avoiding the increase in the temperature of the target material.

[0058] In some embodiments, during the plasma spraying process, the surface of the target is cooled with compressed gas or cryogenic cooling fluid to control the surface temperature of the target at 100 - 130 °C;

[0059] Cooling the surface of the target with compressed gas or cryogenic cooling fluid can timely reduce the surface temperature of the target and avoid cracking caused by the accumulation of thermal stress.

[0060] After the niobium oxide spraying powder is sprayed, it is cooled to room temperature within 100 - 120 min. At the same time, the water temperature inside the matrix tube is reduced from 70 - 80 °C to room temperature, avoiding excessive temperature difference inside and outside the niobium oxide rotating target and generating stress difference leading to cracking. At the same time, the step of cooling can further improve the spraying quality.

[0061] In some embodiments, the compressed gas is compressed air or compressed inert gas;

[0062] In some embodiments, the cryogenic cooling fluid is carbon dioxide or liquid nitrogen.

[0063] As Figure 1 shown, in some embodiments, cooling the surface of the target with the compressed gas or cryogenic cooling fluid is achieved by a cooling device. The cooling device includes an inlet pipe parallel to the spraying matrix. Two parallel blowing pipes are installed on the inlet pipe. The blowing pipes are perpendicular to the spraying matrix. A gas flow meter is installed at the inlet of the inlet pipe.

[0064] Specifically, the inlet pipe is arranged on the surface of the target far from the gun outlet.

[0065] In some embodiments, the inner diameter of the blowing pipe is 8 - 10 mm, the outer diameter is 6 - 8 mm, and the length is 150 - 200 mm;

[0066] In some embodiments, the distance between the end of the blowing pipe and the coating during spraying is 20 - 30 mm;

[0067] In some embodiments, the distance between the two parallel blowing pipes is 100 - 200 mm.

[0068] The matrix tubes used in the following examples and comparative examples are stainless steel back tubes with an outer diameter of 88 mm and a length of 850 mm.

[0069] In the following examples and comparative examples, during the spraying of niobium oxide spraying powder, as Figure 1The shown cooling device blows and cools the surface of the target. The cooling device includes an air inlet pipe parallel to the spraying substrate. Two parallel blowing pipes are installed on the air inlet pipe. The blowing pipes are perpendicular to the spraying substrate. A gas flow meter is installed at the air inlet of the air inlet pipe;

[0070] The inner diameter of the blowing pipe is 10 mm, the outer diameter is 8 mm, and the length is 200 mm; the distance between the pipe end and the coating during spraying is 25 mm.

[0071] Example 1

[0072] This example provides a method for preparing a niobium oxide rotary target, including the following steps:

[0073] Treatment of the spraying substrate pipe: Remove surface dirt and oxide layer by cleaning and mechanical grinding methods, and perform sandblasting to make the substrate surface reach a certain roughness.

[0074] Spray the bottom layer: Spray a NiAl alloy layer with a thickness of 0.7 mm by arc spraying. The process parameters of arc spraying are a current of 230 A and a voltage of 30 V.

[0075] Spray niobium oxide spraying powder: Spray niobium oxide spraying powder on the bottom layer by plasma spraying process. During plasma spraying, the inside of the substrate pipe is cooled with water, and the water temperature inside the substrate pipe is controlled at 70 °C. Use the Figure 1 shown cooling device to blow and cool the surface of the target with compressed air. The blowing pressure is 3 kg, and the surface temperature of the target is controlled at 110 °C; among them, the parameters of the niobium oxide spraying powder are: purity of 99.9%, loose bulk density of 1.5 g / cm 3 , average particle size of 90 μm; the process parameters of plasma spraying are shown in Table 2;

[0076] After the spraying of niobium oxide spraying powder is completed, continue to use the cooling air pipe to blow and cool the surface of the target with compressed air, so that the surface of the target is cooled to room temperature within 110 min, and at the same time, the water temperature inside the substrate pipe is reduced from 70 °C to 30 °C to obtain a niobium oxide target; during the cooling of the target, the rotation speed of the target is 50 rpm.

[0077] Table 2

[0078]

[0079]

[0080] The thickness of the niobium oxide rotary target prepared in this example is 10 mm. The target structure is dense, the composition is uniform, there are no cracks, and the density of the target measured by the Archimedes method is 4.84 g / cm 3, the average resistivity is 0.06 Ω·cm and the deposition rate is 56%.

[0081] Example 2

[0082] This example provides a method for preparing a niobium oxide rotating target, including the following steps:

[0083] Treatment of the sprayed substrate tube: Remove surface dirt and oxide layer by cleaning and mechanical grinding, and perform sandblasting to make the substrate surface reach a certain roughness.

[0084] Spray the bottom layer: Spray a NiAl alloy layer with a thickness of 0.6 mm by arc spraying. The process parameters of arc spraying are a current of 230 A and a voltage of 30 V.

[0085] Spray niobium oxide spraying powder: Spray niobium oxide spraying powder on the bottom layer by plasma spraying. During the plasma spraying process, the inside of the substrate tube is cooled with water, and the water temperature inside the substrate tube is controlled at 80°C. Use a cooling gas pipe to blow and cool the surface of the target with compressed air, and the blowing pressure is 4 kg. Control the surface temperature of the target at 130°C; among them, the parameters of the niobium oxide spraying powder are: purity of 99.9%, loose bulk density of 1.5 g / cm 3 , average particle size of 90 μm; the process parameters of plasma spraying are shown in Table 3;

[0086] After the spraying of the niobium oxide spraying powder is completed, continue to use the cooling gas pipe to blow and cool the surface of the target with compressed air, so that the surface of the target is cooled to room temperature within 120 minutes. At the same time, reduce the water temperature inside the substrate tube from 80°C to 20°C to obtain a niobium oxide target; during the cooling of the target, the rotation speed of the target is 80 rpm.

[0087] Table 3

[0088] Process parameters Parameter value Current / A 500 Current / V 60 Gun distance / mm 200 <![CDATA[Spray gun moving speed / mm·min -1 > 60 Target rotation speed / rpm 260 <![CDATA[Argon flow rate / nL·h -1 > 2300 <![CDATA[Hydrogen flow rate / nL·h -1 > 250 <![CDATA[Powder feeding rate / g·min -1 > 120 <![CDATA[Carrier gas flow rate / nL·min -1 > 2

[0089] The thickness of the niobium oxide rotating target prepared in this example is 10.4 mm. The target structure is dense, the composition is uniform, and there are no cracks. The density of the target measured by the Archimedes method is 4.83 g / cm 3 , average resistivity of 0.056 Ω·cm, and deposition rate of 55%.

[0090] Example 3

[0091] This example provides a method for preparing a niobium oxide rotating target, which is only different from Example 1 in that: the thickness of the bottom layer in this example is 0.9 mm; the remaining steps and parameters are the same as those in Example 1.

[0092] The thickness of the niobium oxide rotating target prepared in this example is 10.5 mm. The target structure is dense, the composition is uniform, and there are no cracks. The density of the target measured by the Archimedes method is 4.82 g / cm 3 , the average resistivity is 0.054 Ω·cm, and the deposition rate is 58%.

[0093] Example 4

[0094] This example provides a method for preparing a niobium oxide rotating target, which is only different from Example 1 in that: the average particle size of the niobium oxide spraying powder in this example is 50 μm; the remaining steps and parameters are the same as those in Example 1.

[0095] The thickness of the niobium oxide rotating target prepared in this example is 10.3 mm. The target structure is dense, the composition is uniform, and there are no cracks. The density of the target measured by the Archimedes method is 4.91 g / cm 3 , the average resistivity is 0.043 Ω·cm, and the deposition rate is 65%.

[0096] Example 5

[0097] This example provides a method for preparing a niobium oxide rotating target, which is only different from Example 1 in that: the average particle size of the niobium oxide spraying powder in this example is 70 μm; the remaining steps and parameters are the same as those in Example 1.

[0098] The thickness of the niobium oxide rotating target prepared in this example is 10.6 mm. The target structure is dense, the composition is uniform, and there are no cracks. The density of the target measured by the Archimedes method is 4.89 g / cm 3 , the average resistivity is 0.052 Ω·cm, and the deposition rate is 60%.

[0099] Example 6

[0100] This example provides a method for preparing a niobium oxide rotating target, which is only different from Example 1 in that: the average particle size of the niobium oxide spraying powder in this example is 110 μm; the remaining steps and parameters are the same as those in Example 1.

[0101] The thickness of the niobium oxide rotating target prepared in this example is 10.3 mm. The target structure is dense, the composition is uniform, and there are no cracks. The density of the target measured by the Archimedes method is 4.79 g / cm 3 , the average resistivity is 0.074 Ω·cm, and the deposition rate is 52%.

[0102] Example 7

[0103] This example provides a method for preparing a niobium oxide rotating target, which is only different from Example 1 in that: the average particle size of the niobium oxide spraying powder in this example is 120 μm; the remaining steps and parameters are the same as those in Example 1.

[0104] The thickness of the niobium oxide rotating target prepared in this example is 10.5 mm. The target structure is dense, the composition is uniform, and there are no cracks. The density of the target measured by the Archimedes method is 4.70 g / cm 3 , the average resistivity is 0.089 Ω·cm, and the deposition rate is 46%.

[0105] Comparative Example 1

[0106] This comparative example provides a preparation method of a niobium oxide rotating target, and the difference from Example 1 is only that: the thickness of the underlayer in this comparative example is 0.5 mm; the remaining steps and parameters are the same as those in Example 1.

[0107] The thickness of the niobium oxide rotating target prepared in this example is 9.7 mm. There are reticular cracks in the target. The density of the target measured by the Archimedes method is 4.82 g / cm 3 , the average resistivity is 0.05 Ω·cm, and the deposition rate is 54%.

[0108] Comparative Example 2

[0109] This comparative example provides a preparation method of a niobium oxide rotating target, and the difference from Example 1 is only that: the thickness of the underlayer in this comparative example is 1.1 mm; the remaining steps and parameters are the same as those in Example 1.

[0110] The thickness of the niobium oxide rotating target prepared in this example is 10.1 mm. There are through cracks in the target. The density of the target measured by the Archimedes method is 4.84 g / cm 3 , the average resistivity is 0.056 Ω·cm, and the deposition rate is 58%.

[0111] Comparative Example 3

[0112] This comparative example provides a preparation method of a niobium oxide rotating target, and the difference from Example 1 is only that: the average particle size of the niobium oxide spraying powder in this comparative example is 40 μm; the remaining steps and parameters are the same as those in Example 1.

[0113] The thickness of the niobium oxide rotating target prepared in this comparative example is 9.5 mm. There are reticular cracks in the target. The density of the target measured by the Archimedes method is 4.79 g / cm 3 , the average resistivity is 0.05 Ω·cm, and the deposition rate is 52%.

[0114] Comparative Example 4

[0115] This comparative example provides a preparation method of a niobium oxide rotating target, and the difference from Example 1 is only that: the average particle size of the niobium oxide spraying powder in this comparative example is 150 μm; the remaining steps and parameters are the same as those in Example 1.

[0116] The thickness of the niobium oxide rotating target prepared in this comparative example is 10.4 mm, and there are microcracks in the target. The density of the target measured by the Archimedes method is 4.68 g / cm 3 , the average resistivity is 0.1 Ω·cm, and the deposition rate is 42%.

[0117] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present disclosure rather than to limit the protection scope of the present disclosure. Although the present disclosure has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present disclosure can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present disclosure.

Claims

1. A niobium oxide rotary target, characterized in that, The outer diameter of the substrate tube of the niobium oxide rotating target is ≤90 mm, the thickness is ≥8 mm, and the density is 4.7 g / cm 3 or more.

2. A method for preparing a niobium oxide rotary target as described in claim 1, characterized in that, It includes the following steps: Treatment of the sprayed substrate tube, spraying the primer layer, and spraying niobium oxide spraying powder on the substrate tube by plasma spraying process; wherein the thickness of the primer layer is 0.6 - 0.9 mm, and the average particle size of the niobium oxide spraying powder is 50 - 120 μm.

3. The method for preparing a niobium oxide rotating target according to claim 2, wherein The purity of the niobium oxide spraying powder is 99.95 - 99.99%, and the loose bulk density is 1.5 - 2 g / cm 3 .

4. The method for preparing a niobium oxide rotary target according to claim 2, characterized in that The treatment of the sprayed substrate tube includes cleaning, grinding to remove dirt and oxide layer on the surface of the substrate tube, and then roughening the surface of the substrate tube by sandblasting; And / or, the primer layer refers to spraying an alloy coating with a thickness of 0.6 - 0.9 mm on the surface of the substrate tube.

5. The method for preparing a niobium oxide rotary target according to claim 4, wherein The alloy coating is sprayed with nickel - coated aluminum, nickel - chromium, nickel - chromium - aluminum, nickel - cobalt - chromium - aluminum - yttrium powder by plasma spraying method, or spraying aluminum bronze or nickel - aluminum alloy wire by arc spraying method.

6. The method for preparing a niobium oxide rotary target according to claim 2, characterized in that, During the process of spraying niobium oxide spraying powder on the substrate tube by plasma spraying process, control the substrate tube to rotate around the central axis at a speed of 250 - 300 r / min, keep the distance between the spray gun and the substrate tube at 180 - 220 mm, and reciprocate and move uniformly along the direction of the substrate tube at a speed of 30 - 90 mm / min.

7. The method for preparing a niobium oxide rotary target according to claim 2, characterized in that, During the plasma spraying process, the substrate tube is cooled by water; And / or, during the plasma spraying process, the surface of the target is cooled by compressed gas or low - temperature cooling fluid, and the surface temperature of the target is controlled at 100 - 130 °C.

8. The method for preparing a niobium oxide rotating target according to claim 7, wherein The compressed gas is compressed air or inert gas; And / or, the low - temperature cooling fluid is carbon dioxide or liquid nitrogen.

9. The method for preparing a niobium oxide rotary target according to claim 7, characterized in that, The cooling of the surface of the target by the compressed gas or low - temperature cooling fluid is realized by a cooling and temperature - control device. The cooling control device includes a trachea bracket parallel to the sprayed substrate. Two parallel air - blowing pipes are installed on the trachea bracket. The air - blowing pipes are perpendicular to the sprayed substrate, and a gas flowmeter is installed at the air inlet of the air - blowing pipes.

10. The method for preparing a niobium oxide rotating target according to claim 7, wherein The inner diameter of the air - blowing pipe is 8 - 10 mm, the outer diameter is 6 - 8 mm, and the length is 150 - 200 mm; And / or, the distance between the tube end of the air - blowing pipe and the coating during spraying is 20 - 30 mm; And / or, the distance between the two parallel air - blowing pipes is 100 - 200 mm.

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