CrTiCuAl alloy tube target material and preparation method thereof

CrTiCuAl alloy powder was prepared by vacuum induction smelting and mechanical ball milling treatment, and combined with thermal isostatic pressing technology, the problem of brittle cracking of CrTiCuAl alloy target was solved, and the preparation of CrTiCuAl alloy tube target with high purity and high relative density was achieved, improving the uniformity and stability of the coating.

CN119800191APending Publication Date: 2025-04-11AEROSPACE LONG MARCH ARIMT TECH CO LTD

Patent Information

Application Number
CN202411934971.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-26
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

The prior art is difficult to effectively prepare CrTiCuAl alloy targets, resulting in brittle cracking of the target material and unstable coating quality.

Method used

Vacuum induction melting was carried out using high-purity chromium and aluminum to obtain pre-alloyed CrAl alloy ingots, and were processed by mechanical ball milling and screening. Then, mechanical ball milling was mixed with Cr, Ti, and Cu powders under a protective atmosphere to form CrTiCuAl alloy powder. Then the packing was filled and argon arc welding was performed, followed by vacuum heat degassing and thermal isostatic sintering and binding were carried out simultaneously to prepare the CrTiCuAl alloy tube target.

Benefits of technology

The high purity and high relative density of the CrTiCuAl alloy tube target material are achieved, the brittle cracking problem of target material is avoided, the uniformity and stability of the coating are improved, the process flow is simplified and the production efficiency is improved.

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Abstract

The invention provides a CrTi CuAl alloy tube target material and a preparation method thereof, and the CrTi CuAl alloy tube target material takes CrAl pre-alloyed powder, Cr powder, Ti powder and Cu powder as raw material powder; the preparation method comprises the following steps: controlling an alloying reaction through CrAl pre-alloying, matching the particle sizes of pre-alloyed powder and metal elementary substance powder, mechanically ball-milling and mixing, filling powder, carrying out vacuum hot degassing on a sheath, synchronously carrying out hot isostatic pressing sintering and binding, machining and the like, and carrying out pre-alloying treatment on Cr powder and A powder to control the alloying reaction. The CrTi-CuAl alloy tube target material prepared by the preparation method disclosed by the invention has the characteristics of high purity, nearly full compactness, uniform and fine structure, small circle jump degree, large length-diameter ratio and the like, and the CrTi-CuAl alloy tube target material is prepared by synchronously sintering and binding by utilizing a hot isostatic pressing technology, and the preparation method has the advantages of short preparation process flow and high production efficiency.
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Description

Technical Field

[0001] The invention relates to the technical field of preparation of tubular target materials for magnetron sputtering, in particular to a CrTiCuAl alloy tubular target material and a preparation method thereof. Background Art

[0002] Magnetron sputtering technology refers to the process of using energetic particles to bombard the target material under the action of an electric field, causing the target material to sputter, and the sputtered particles are deposited on the plated workpiece to form a thin film. In the field of glass coating, the target material is mainly used to prepare low-radiation glass and smart glass. By coating a film system composed of multiple layers of metals or their compounds on the glass surface, energy saving, light control, and decoration are achieved. It is mainly used in the fields of construction, room decoration, automobiles, mirror making, etc., among which the largest application is in the construction field. The targets widely used in the field of glass coating include metal targets such as Cr, Ti, Cu, and Ag. With the continuous development of magnetron sputtering technology and target material preparation technology, it is possible to achieve high-quality films with strong bonding, good uniformity, and stable and reliable quality on large areas of glass.

[0003] The coating method using a single-element target and multiple targets will lead to problems such as uneven distribution of film composition and unstable quality. The alloy target composed of Cr, Ti, Cu and Al elements can improve the adhesion of the sputtered film on the glass substrate and improve the uniformity of the film composition. Since the melting point of Al element is very different from that of Cr, Ti, Cu and other elements, and Al element undergoes a complex alloying reaction with Cr, Ti and Cu at about 500°C to generate a variety of brittle intermetallic compounds, resulting in brittle cracking of the target material, it is difficult to prepare CrTiCuAl alloy targets by conventional vacuum melting and powder metallurgy methods.

[0004] Patent CN 116804265A discloses a CrAlCuFe alloy target material and a preparation method thereof, the preparation method comprising: separating the CrAlCuFe cold pressed billets and the CrAlCuFe cold pressed billets from the sheath with a TiAl bottom layer, and performing a pre-alloying heat treatment, so that the Al and Cu / Fe in the sheath are pre-alloyed to a certain extent, thereby reducing the heat release of the intense alloying reaction during the HIP process. The target material prepared by this method is a planar target, and the mixed powder is pre-molded by molding, and the pre-alloying is performed after vacuum degassing. The process is cumbersome, the production cycle is long, and the batch production efficiency is low.

[0005] Target material is the main consumable in the magnetron sputtering coating process. Improving the utilization rate of target material can extend the cycle of target material replacement, maintain the stability of coating process, and improve production efficiency, thereby achieving the purpose of reducing production costs and improving product stability. Compared with flat target materials, tube target materials can not only expand the coating area, but also significantly improve the utilization rate of target materials, greatly extend the cycle of target material replacement, and improve the continuity and stability of coating. Therefore, in the field of magnetron sputtering coating, with the market competition becoming increasingly fierce, tube target materials have been widely favored by the coating industry. However, at present, there is no report on the preparation process of CrTiCuAl alloy large aspect ratio tube target materials. Summary of the invention

[0006] The technical problem to be solved by the present invention is to provide a CrTiCuAl alloy tube target material.

[0007] Another technical problem to be solved by the present invention is to provide a method for preparing the CrTiCuAl alloy tube target material.

[0008] In order to solve the above technical problems, the technical solution of the present invention is:

[0009] A CrTiCuAl alloy tube target material comprises the following components by mass percentage: 60-70wt% of Cr, 15-25wt% of Ti, 5-15wt% of Al and 5-10wt% of Cu.

[0010] Preferably, the above-mentioned CrTiCuAl alloy tube target material has the following components in percentage by mass: Cr 65wt%, Ti 20wt%, Al 10wt%, Cu 5wt%.

[0011] The preparation method of the CrTiCuAl alloy tube target material comprises the following specific steps:

[0012] (1) High-purity chromium (purity ≥ 99.95%) and high-purity aluminum (purity ≥ 99.99%) are used for vacuum induction melting to obtain a pre-alloyed CrAl alloy ingot, and the CrAl alloy ingot is mechanically ball-milled into a CrAl alloy powder and sieved. The chemical composition of the alloy powder is 40-60wt% Cr and 60-40wt% Al. The Cr powder and Al powder are pre-alloyed to control the alloying reaction process and avoid the problem of brittle cracking of the target material;

[0013] (2) The pre-alloyed CrAl alloy powder of step (1) is mixed uniformly with Cr powder, Ti powder and Cu powder by mechanical ball milling under a protective atmosphere, wherein Cr is 60-70wt%, Ti is 15-25wt%, Al is 5-15wt%, Cu is 5-10wt%, the ball-to-material ratio is 3-1:1, and the powder mixing time is 12-24h;

[0014] (3) The mixed powder uniformly mixed in step (2) is filled into the annular space formed by the outer surface of the inner tube of the sheath and the inner surface of the outer tube of the sheath, and the relative density of the mixed powder filling is ≥64% (the ratio of the volume density of the mixed powder filling to the theoretical density of the corresponding material, and the theoretical density is calculated based on the density of each component of the CrTiCuAl alloy target and their proportion in the alloy), and the maximum deviation of the gap in the annular space is ≤0.15mm, and the maximum deviation of the gap is the difference between the maximum gap and the minimum gap, so as to ensure the uniformity of the powder filling in the annular space, so as to ensure the uniformity of the wall thickness of the target layer after hot isostatic pressing and the roundness of the target layer is ≤1.5mm;

[0015] (4) Argon arc welding is performed on the package filled with powder in step (3), and a degassing port is reserved on the outer package. The vacuum heat degassing temperature is 500-700°C and the vacuum degree is ≤1×10 -3 Pa, insulation time is 3 to 10 hours;

[0016] (5) The sheath obtained by vacuum heat degassing in step (4) is subjected to hot isostatic pressing sintering and bonding simultaneously by hot isostatic pressing technology to prepare a CrTiCuAl alloy tube target with a large aspect ratio, wherein the hot isostatic pressing temperature is 700 to 950° C., the pressure is 100 to 150 MPa, and the holding time is 2 to 5 h;

[0017] (6) The outer sheath of the tube target blank which is simultaneously hot isostatically pressed and bound in step (5) is removed by mechanical processing to obtain a CrTiCuAl alloy tube target material for sputtering.

[0018] The CrTiCuAl alloy tube target material obtained by the preparation method has a purity of ≥99.9%, a relative density of ≥99%, an average grain size of ≤100 μm, a roundness of ≤1.5 mm, and an aspect ratio of greater than 18:1.

[0019] Preferably, in the method for preparing the above-mentioned CrTiCuAl alloy tube target material, the protective atmosphere is nitrogen.

[0020] Preferably, in the method for preparing the above-mentioned CrTiCuAl alloy tube target material, the particle size of the CrAl alloy powder is -250 mesh.

[0021] Preferably, in the preparation method of the CrTiCuAl alloy tube target material, the purity of the Cr powder is ≥99.9%, and the particle size is -250 mesh; the purity of the Ti powder is ≥99.9%, and the particle size is -250 mesh; the purity of the Cu powder is ≥99.9%, and the particle size is -250 mesh. The particle size ratio of the pre-alloyed powder and the metal element powder has a higher powder packing density.

[0022] Beneficial effects:

[0023] The above-mentioned CrTiCuAl alloy tube target material adopts Cr powder and Al powder pre-alloying treatment to control the alloying reaction and avoid the problem of brittle cracking of the target material. It has the characteristics of high purity, nearly full density, uniform and fine structure, small roundness jump, large aspect ratio, etc. The purity of the target material is ≥99.9%, the relative density is ≥99%, the average grain size is ≤100μm, the roundness jump is ≤1.5mm, and the aspect ratio is greater than 18:1; the CrTiCuAl alloy tube target material is prepared by hot isostatic pressing technology to realize simultaneous sintering and binding, and the preparation method has the advantages of short preparation process and high production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a metallographic photograph of the CrTiCuAl alloy target layer in the CrTiCuAl alloy tube target in the embodiment.

[0025] Figure 2 This is a photo of the finished appearance of the CrTiCuAl alloy tube target material in the embodiment. DETAILED DESCRIPTION

[0026] In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0027] Example 1

[0028] A method for preparing a CrTiCuAl alloy tube target material, the specific steps are as follows:

[0029] (1) A Cr block with a purity of 99.95% and an Al block with a purity of 99.99% were prepared with a mass percentage of 1:1, and vacuum induction melting was performed to obtain a pre-alloyed CrAl alloy ingot with a mass ratio of 1:1, the CrAl alloy ingot was mechanically ball-milled into a CrAl alloy powder, and the CrAl alloy powder was sieved to obtain a pre-alloyed CrAl alloy powder with a particle size of -250 mesh. The pre-alloying treatment of Cr powder and Al powder was used to control the alloying reaction process and avoid the problem of brittle cracking of the target material.

[0030] (2) Pre-alloyed CrAl alloy powder, Cr powder, Ti powder and Cu powder were weighed in a mass ratio of Cr:Ti:Cu:Al=65:20:5:10 and then mechanically ball-milled and mixed in a V-type mixer under nitrogen protection. The ball-to-material ratio was 2:1 and the mixing time was 12 hours to obtain CrTiCuAl alloy tube target layer powder, wherein the specification parameters of each raw material powder were: Cr powder purity ≥99.9%, particle size -250 mesh, Ti powder purity ≥99.9%, particle size -250 mesh, Cu powder purity ≥99.9%, particle size -250 mesh. The purpose of selecting a specific powder particle size ratio for mixing in this embodiment is to make the mixed powder have a higher packing density. The higher powder packing density avoids the difficulty in controlling the size caused by excessive shrinkage during the hot isostatic pressing sintering process.

[0031] (3) The uniformly mixed CrTiCuAl mixed powder is filled into the annular space formed by the outer surface of the inner tube of the sheath and the inner surface of the outer tube of the sheath. The filling density of the mixed powder is 65%, and the maximum deviation of the annular space gap is 0.10 mm. The maximum deviation of the gap is the difference between the maximum gap and the minimum gap. The uniformity of the powder filling in the annular space is ensured to ensure the uniformity of the wall thickness of the target material layer after hot isostatic pressing and a smaller roundness.

[0032] (4) Argon arc welding is performed on the package after powder filling. A degassing port is reserved on the outer package. The vacuum heat degassing temperature is 600°C and the vacuum degree is ≤1×10 -3 Pa, the holding time is 8h.

[0033] (5) The package that has been vacuum degassed is subjected to hot isostatic pressing sintering and binding simultaneously, with the hot isostatic pressing temperature being 900°C, the pressure being 120 MPa, and the holding time being 3 h.

[0034] (6) The outer sheath of the tube target blank that has been simultaneously hot isostatically pressed and bound is removed by mechanical processing, and then the tube target blank is machined according to the drawing to obtain a CrTiCuAl alloy tube target for sputtering.

[0035] In this example, the finished CrTiCuAl alloy tube target material has a relative density of 100.8%, a uniform microstructure, an average grain size of less than 100 μm, a roundness of 1.0 mm, and an aspect ratio of 18.8.

[0036] Figure 1 This is a metallographic photograph of the CrTiCuAl alloy target layer in the CrTiCuAl alloy tube target in this embodiment; Figure 2 This is a photo of the finished appearance of the CrTiCuAl alloy tube target material in this embodiment.

[0037] Example 2

[0038] A method for preparing a CrTiCuAl alloy tube target material, the specific steps are as follows:

[0039] (1) A Cr block with a purity of 99.95% and an Al block with a purity of 99.99% were prepared with a mass percentage of 3:2, and vacuum induction melting was performed to obtain a pre-alloyed CrAl alloy ingot with a mass ratio of 3:2, the CrAl alloy ingot was mechanically ball-milled into a CrAl alloy powder, and the CrAl alloy powder was sieved to obtain a pre-alloyed CrAl alloy powder with a particle size of -250 mesh. The pre-alloying treatment of Cr powder and Al powder was used to control the alloying reaction process and avoid the problem of brittle cracking of the target material.

[0040] (2) Pre-alloyed CrAl alloy powder, Cr powder, Ti powder and Cu powder were weighed in a mass ratio of Cr:Ti:Cu:Al=70:15:5:10 and then mechanically ball-milled and mixed in a V-type mixer under nitrogen protection. The ball-to-material ratio was 2:1 and the mixing time was 12 hours to obtain CrTiCuAl alloy tube target layer powder, wherein the specification parameters of each raw material powder were: Cr powder purity ≥99.9%, particle size -250 mesh, Ti powder purity ≥99.9%, particle size -250 mesh, Cu powder purity ≥99.9%, particle size -250 mesh. The purpose of selecting a specific powder particle size ratio for mixing in this embodiment is to make the mixed powder have a higher packing density. The higher powder packing density avoids the difficulty in controlling the size caused by excessive shrinkage during the hot isostatic pressing sintering process.

[0041] (3) The uniformly mixed CrTiCuAl mixed powder is filled into the annular space formed by the outer surface of the inner tube of the sheath and the inner surface of the outer tube of the sheath. The filling density of the mixed powder is 64%, and the maximum deviation of the annular space gap is 0.08 mm. The maximum deviation of the gap is the difference between the maximum gap and the minimum gap. The uniformity of the powder filling in the annular space is ensured to ensure the uniformity of the wall thickness of the target material layer after hot isostatic pressing and a smaller roundness.

[0042] (4) Argon arc welding is performed on the package after powder filling. A degassing port is reserved on the outer package. The vacuum heat degassing temperature is 500°C and the vacuum degree is ≤1×10 -3 Pa, the holding time is 10h.

[0043] (5) The package that has been vacuum degassed is subjected to hot isostatic pressing sintering and binding simultaneously, with the hot isostatic pressing temperature being 750°C, the pressure being 150 MPa, and the holding time being 4 h.

[0044] (6) The outer sheath of the tube target blank that has been simultaneously hot isostatically pressed and bound is removed by mechanical processing, and then the tube target blank is machined according to the drawing to obtain a CrTiCuAl alloy tube target for sputtering.

[0045] The finished CrTiCuAl alloy tube target material in this example has a relative density of 99.8%, a uniform microstructure, an average grain size of less than 100 μm, a roundness of 1.0 mm, and an aspect ratio of 18.8.

[0046] Example 3

[0047] A method for preparing a CrTiCuAl alloy tube target material, the specific steps are as follows:

[0048] (1) A Cr block with a purity of 99.95% and an Al block with a purity of 99.99% were prepared with a mass percentage of 1:1, and vacuum induction melting was performed to obtain a pre-alloyed CrAl alloy ingot with a mass ratio of 1:1, the CrAl alloy ingot was mechanically ball-milled into a CrAl alloy powder, and the CrAl alloy powder was sieved to obtain a pre-alloyed CrAl alloy powder with a particle size of -250 mesh. The pre-alloying treatment of Cr powder and Al powder was used to control the alloying reaction process and avoid the problem of brittle cracking of the target material.

[0049] (2) Pre-alloyed CrAl alloy powder, Cr powder, Ti powder and Cu powder were weighed in a mass ratio of Cr:Ti:Cu:Al=65:20:5:10 and then mechanically ball-milled and mixed in a V-type mixer under nitrogen protection. The ball-to-material ratio was 2:1 and the mixing time was 12 hours to obtain CrTiCuAl alloy tube target layer powder, wherein the specification parameters of each raw material powder were: Cr powder purity ≥99.9%, particle size -250 mesh, Ti powder purity ≥99.9%, particle size -250 mesh, Cu powder purity ≥99.9%, particle size -250 mesh. The purpose of selecting a specific powder particle size ratio for mixing in this embodiment is to make the mixed powder have a higher packing density. The higher powder packing density avoids the difficulty in controlling the size caused by excessive shrinkage during the hot isostatic pressing sintering process.

[0050] (3) The uniformly mixed CrTiCuAl mixed powder is filled into the annular space formed by the outer surface of the inner tube of the sheath and the inner surface of the outer tube of the sheath. The filling density of the mixed powder is 65%, and the maximum deviation of the annular space gap is 0.10 mm. The maximum deviation of the gap is the difference between the maximum gap and the minimum gap. The uniformity of the powder filling in the annular space is ensured to ensure the uniformity of the wall thickness of the target material layer after hot isostatic pressing and a smaller roundness.

[0051] (4) Argon arc welding is performed on the package after powder filling. A degassing port is reserved on the outer package. The vacuum heat degassing temperature is 600°C and the vacuum degree is ≤1×10 -3 Pa, the holding time is 4h.

[0052] (5) The package that has been vacuum degassed is subjected to hot isostatic pressing sintering and binding simultaneously, with the hot isostatic pressing temperature being 850° C., the pressure being 140 MPa, and the holding time being 3 h.

[0053] (6) The outer sheath of the tube target blank that has been simultaneously hot isostatically pressed and bound is removed by mechanical processing, and then the tube target blank is machined according to the drawing to obtain a CrTiCuAl alloy tube target for sputtering.

[0054] The relative density of the finished CrTiCuAl alloy tube target material in this example is 100.4%, the microstructure is uniform, the average grain size is less than 100 μm, the roundness is 1.2 mm, and the aspect ratio is 20.

[0055] Example 4

[0056] A method for preparing a CrTiCuAl alloy tube target material, the specific steps are as follows:

[0057] (1) A Cr block with a purity of 99.95% and an Al block with a purity of 99.99% were prepared with a mass percentage of 1:1, and vacuum induction melting was performed to obtain a pre-alloyed CrAl alloy ingot with a mass ratio of 1:1, the CrAl alloy ingot was mechanically ball-milled into a CrAl alloy powder, and the CrAl alloy powder was sieved to obtain a pre-alloyed CrAl alloy powder with a particle size of -250 mesh. The pre-alloying treatment of Cr powder and Al powder was used to control the alloying reaction process and avoid the problem of brittle cracking of the target material.

[0058] (2) Pre-alloyed CrAl alloy powder, Cr powder, Ti powder and Cu powder were weighed in a mass ratio of Cr:Ti:Cu:Al=60:25:10:5 and then mechanically ball-milled and mixed evenly in a V-type mixer under nitrogen protection, with a ball-to-material ratio of 2:1 and a mixing time of 12 hours to obtain a CrTiCuAl alloy tube target layer powder, wherein the specification parameters of each raw material powder are: Cr powder purity ≥99.9%, particle size of -250 mesh, Ti powder purity ≥99.9%, particle size of -250 mesh, Cu powder purity ≥99.9%, particle size of -250 mesh. The purpose of selecting a specific powder particle size ratio for mixing in this embodiment is to make the mixed powder have a higher packing density, and a higher powder packing density avoids the difficulty in controlling the size caused by excessive shrinkage during the hot isostatic pressing sintering process.

[0059] (3) The uniformly mixed CrTiCuAl mixed powder is filled into the annular space formed by the outer surface of the inner tube of the sheath and the inner surface of the outer tube of the sheath. The filling density of the mixed powder is 65%, and the maximum deviation of the annular space gap is 0.10 mm. The maximum deviation of the gap is the difference between the maximum gap and the minimum gap. The uniformity of the powder filling in the annular space is ensured to ensure the uniformity of the wall thickness of the target material layer after hot isostatic pressing and a smaller roundness.

[0060] (4) Argon arc welding is performed on the package after powder filling. A degassing port is reserved on the outer package. The vacuum heat degassing temperature is 600°C and the vacuum degree is ≤1×10 -3 Pa, the holding time is 8h.

[0061] (5) The package that has been vacuum degassed is subjected to hot isostatic pressing sintering and binding simultaneously, with the hot isostatic pressing temperature being 900°C, the pressure being 120 MPa, and the holding time being 3 h.

[0062] (6) The outer sheath of the tube target blank that has been simultaneously hot isostatically pressed and bound is removed by mechanical processing, and then the tube target blank is machined according to the drawing to obtain a CrTiCuAl alloy tube target for sputtering.

[0063] The relative density of the finished CrTiCuAl alloy tube target material in this example is 101.4%, the microstructure is uniform, the average grain size is less than 100 μm, the roundness is 1.0 mm, and the aspect ratio is 18.8.

[0064] In summary, the CrTiCuAl alloy tube target material of the present invention adopts Cr powder and Al powder pre-alloying treatment to achieve control of the alloying reaction process and avoid the problem of brittle cracking of the target material. The particle size ratio of the pre-alloyed powder and the metal element powder makes the mixed powder have a higher powder filling density, and the control of the gap deviation of the annular powder filling space ensures the uniformity of the powder filling to ensure the uniformity of the target layer wall thickness after hot isostatic pressing. The hot isostatic pressing technology is used to realize simultaneous sintering and binding. The prepared target material has high purity, purity ≥99.9%, close to full density, relative density ≥99%, uniform and fine structure, average grain size ≤100μm, small roundness, roundness ≤1.5mm, aspect ratio greater than 18:1, etc. The preparation method has the advantages of short preparation process and high production efficiency.

[0065] Example 5

[0066] The CrTiCuAl alloy tube target material described in Example 1 is used as a consumable in magnetron sputtering, and the specific steps are as follows:

[0067] (1) Using alloy tube targets with a mass ratio of Cr:Ti:Cu:Al = 65:20:5:10, magnetron sputtering coating equipment was used to perform glass color coating;

[0068] (2) Cleaning the substrate and target before coating, and installing the cleaned substrate and target in the vacuum chamber of the coating equipment;

[0069] (3) Close the coating equipment door and start the vacuum pump to evacuate the vacuum chamber of the coating machine until the vacuum state in the vacuum chamber reaches 10 -6 Torr;

[0070] (4) Turn on the coating machine substrate heating device to heat the substrate to be coated, heating it to 300° C. to meet the coating requirements;

[0071] (5) Since the color of the film generated by sputtering is obtained by the reaction between the target material and the gas, the gas flow rate and partial pressure will have a significant impact on the color of the film. The gas introduced contains argon and oxygen, and the gas flow rate and partial pressure can be adjusted;

[0072] (6) The substrate rotates to achieve uniform coating on the substrate, with a rotation speed of 2 r / min;

[0073] (7) The coating was performed for 20 min, the film thickness was 300 nm, and the prepared film exhibited color characteristics.

[0074] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A CrTiCuAl alloy tube target, characterized in that: The composition is calculated by mass percentage: Cr 60-70wt%, Ti 15-25wt%, Al 5-15wt%, Cu 5-10wt%.

2. The CrTiCuAl alloy tube target according to claim 1, characterized in that: The composition is calculated by mass percentage: Cr 65wt%, Ti 20wt%, Al 10wt%, Cu 5wt%.

3. The method for preparing the CrTiCuAl alloy tube target material according to claim 1, characterized in that: The specific steps are as follows: (1) high purity chromium and high purity aluminum are subjected to vacuum induction melting to obtain a pre-alloyed CrAl alloy ingot, the CrAl alloy ingot is mechanically ball-milled into a CrAl alloy powder and the alloy powder is sieved, wherein the chemical composition of the alloy powder is 40-60 wt % of Cr and 60-40 wt % of Al; (2) The pre-alloyed CrAl alloy powder of step (1) is mixed uniformly with Cr powder, Ti powder and Cu powder by mechanical ball milling under a protective atmosphere, wherein Cr is 60-70wt%, Ti is 15-25wt%, Al is 5-15wt%, Cu is 5-10wt%, the ball-to-material ratio is 3-1:1, and the powder mixing time is 12-24h; (3) filling the mixed powder uniformly mixed in step (2) into the annular space formed by the outer surface of the inner tube of the sheath and the inner surface of the outer tube of the sheath, wherein the relative density of the mixed powder filling is ≥ 64%, and the maximum deviation of the gap in the annular space is ensured to be ≤ 0.15 mm; (4) Argon arc welding is performed on the package filled with powder in step (3), and a degassing port is reserved on the outer package. The vacuum heat degassing temperature is 500-700°C and the vacuum degree is ≤1×10 -3 Pa, insulation time is 3 to 10 hours; (5) The package that has been vacuum degassed in step (4) is subjected to hot isostatic pressing sintering and binding simultaneously by hot isostatic pressing technology, wherein the hot isostatic pressing temperature is 700-950° C., the pressure is 100-150 MPa, and the holding time is 2-5 h; (6) The outer sheath of the tube target blank which is simultaneously hot isostatically pressed and bound in step (5) is removed by mechanical processing to obtain a CrTiCuAl alloy tube target material for sputtering.

4. The method for preparing the CrTiCuAl alloy tube target according to claim 3, characterized in that: The protective atmosphere is nitrogen.

5. The method for preparing the CrTiCuAl alloy tube target according to claim 3, characterized in that: The particle size of the CrAl alloy powder is -250 mesh.

6. The method for preparing the CrTiCuAl alloy tube target according to claim 3, characterized in that: The purity of the Cr powder is ≥99.9% and the particle size is -250 mesh; 7. The method for preparing the CrTiCuAl alloy tube target according to claim 3, characterized in that: The purity of the Ti powder is ≥99.9% and the particle size is -250 mesh.

8. The method for preparing the CrTiCuAl alloy tube target according to claim 3, characterized in that: The Cu powder has a purity of ≥99.9% and a particle size of -250 mesh.

Citation Information

Patent Citations

  • CrAlCuFe alloy target material and preparation method thereof

    CN116804265A

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