CN111575659A - Preparation method of titanium-aluminum alloy target material - Google Patents
Preparation method of titanium-aluminum alloy target material Download PDFInfo
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- CN111575659A CN111575659A CN202010425088.7A CN202010425088A CN111575659A CN 111575659 A CN111575659 A CN 111575659A CN 202010425088 A CN202010425088 A CN 202010425088A CN 111575659 A CN111575659 A CN 111575659A
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- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000013077 target material Substances 0.000 title claims abstract description 66
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 92
- 238000007731 hot pressing Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001238 wet grinding Methods 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical group 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000001513 hot isostatic pressing Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
Abstract
The application relates to a preparation method of a titanium-aluminum alloy target, which comprises the following steps: providing titanium-aluminum alloy target material powder; uniformly mixing raw material powder of a titanium-aluminum alloy target material according to a proportion to obtain blank powder; crushing the blank powder in a protective gas atmosphere to obtain powder; mixing the powder and the bonding coating agent, granulating, and performing compression molding to obtain a parison; and degumming the parison in a reducing atmosphere, and carrying out hot-pressing sintering to obtain the titanium-aluminum alloy target material. The method does not need expensive equipment such as a hot isostatic pressing sintering furnace, can also effectively improve the density and purity of the titanium-aluminum alloy target material, has simple preparation method and low production cost, and is beneficial to industrial popularization.
Description
Technical Field
The invention relates to the technical field of alloy targets, in particular to a preparation method of a titanium-aluminum alloy target.
Background
The target material is a sputtering source for magnetron sputtering coating, and the quality of the target material plays a crucial role in the performance of the film, so that the high-quality target material is the premise and the basis for ensuring the quality of the film, and a large number of researches show that the factors influencing the quality of the target material mainly comprise: purity, compactness, structural orientation, grain size and distribution, size, shape and the like, wherein the most important indexes for measuring the quality of the target material are the relative density, purity, crystalline orientation and uniformity of microstructure of the target material.
The sputtering process has high requirements on the compactness of the target material, and if the compactness of the target material structure is poor, when Ar & lt + & gt with high energy density bombards the target material, large substances on the surface of the target material are peeled off, so that the surface of the thin film has more large particles. This will seriously affect the flatness of the film surface, eventually leading to deterioration of the film properties. In addition, the high energy density of Ar + bombardment during magnetron sputtering also leads to a heating of the target material, and in order to better withstand the thermal stress inside the target material, it is necessary to obtain a high density and high strength target material.
The titanium-aluminum alloy is an alloy sputtering target material for vacuum coating, and titanium-aluminum alloy target materials with different characteristics can be obtained by regulating the contents of titanium and aluminum in the alloy. The titanium-aluminum intermetallic compound belongs to a hard and brittle material, has good wear resistance, and can effectively prolong the service time of the cutter by coating a layer of titanium-aluminum intermetallic compound on the surface of a common cutter. If the sputtering is carried out by matching with the nitrogen discharge arc striking, the surface film with high hardness and low friction coefficient can be obtained, and the method is particularly suitable for surface coatings of various cutters, grinding tools and other wearing parts, thereby having better application prospect in the machining industry.
The preparation of the titanium-aluminum alloy target is difficult. According to the phase diagram of the titanium-aluminum alloy, various intermetallic compounds can be formed between titanium and aluminum, so that the titanium-aluminum alloy has the processing brittleness, and particularly when the aluminum content in the alloy exceeds 50% (atomic ratio), the oxidation resistance of the alloy is suddenly reduced, and the oxidation is serious. Meanwhile, due to heat release and expansion in the alloying process, bubbles, shrinkage cavities and shrinkage porosity are easy to generate, so that the porosity of the alloy is high, and the requirement on the density of the target material cannot be met.
According to the research report of the production process of the titanium-aluminum alloy target at home and abroad, the main preparation technology of the titanium-aluminum alloy target at present comprises the following steps: hot isostatic pressing sintering. Although the titanium-aluminum alloy target material prepared by the hot isostatic pressing sintering method has high density and wide size specification range, the method needs a hot isostatic pressing sintering furnace with high price, so that the production cost is high, and the industrialized popularization is difficult.
Disclosure of Invention
Based on the above, a preparation method of the titanium-aluminum alloy target material with simple preparation method and low production cost is needed, and the titanium-aluminum alloy target material prepared by the method meets the requirements of density, purity and the like, and the specific scheme is as follows:
a preparation method of a titanium-aluminum alloy target comprises the following steps:
providing titanium-aluminum alloy target material powder;
uniformly mixing the titanium-aluminum alloy target material raw material powder in proportion to obtain blank powder;
in a protective gas atmosphere, crushing the blank powder to obtain powder;
mixing the powder and the bonding coating agent, granulating, and performing compression molding to obtain a parison;
and degumming the parison in a reducing atmosphere, and carrying out hot-pressing sintering to obtain the titanium-aluminum alloy target material.
In one embodiment, the method for pulverizing the blank powder comprises the following steps: and (3) putting the blank powder into a jet mill for crushing treatment.
In one embodiment, the powder has a particle size of 180-300 mesh.
In one embodiment, the bonding coating agent is paraffin or polyethylene glycol with the average molecular weight of 200-2000.
In one embodiment, the powder and the binding coating agent are mixed and then granulated to obtain particles with the particle size of 1-50 μm.
In one embodiment, the reducing atmosphere is hydrogen, and the flow rate of the hydrogen is 10ml/min to 100 ml/min; the degumming time is 0.5-4 hours, and the degumming temperature is 200-800 ℃.
In one embodiment, the hot-pressing sintering method is segmented hot pressing or plasma rapid sintering assisted segmented hot pressing.
In one embodiment, the segmented hot pressing method comprises the following steps: hot pressing for 0.5-2 hours at 300-800 MPa and 0-400 ℃; hot pressing for 0.5-2 hours at 400-800 MPa and 50-400 ℃; hot pressing for 1-4 hours at 400-800 MPa and 100-400 ℃; hot pressing for 0.5-2 hours at the temperature of 100-400 ℃ and the pressure of 800-1200 MPa.
In one embodiment, the hot pressing sintering method is microwave vibration assisted plasma rapid sintering.
In one embodiment, the method for uniformly mixing the titanium-aluminum alloy target material powder in proportion comprises the following steps: and mixing the titanium-aluminum alloy target material powder and a wet grinding medium in proportion, and stirring at a rotating speed of 50-150 rpm for 1-4 hours.
According to the preparation method of the titanium-aluminum alloy target, the blank powder is crushed in a protective atmosphere, an oxide film on the surface of the blank powder is damaged, a subsequent target interface is purified, the interface bonding force is activated, the porosity is reduced, and the density is improved; and then the powder and the bonding coating agent are mixed and granulated, so that the surface of the powder is coated by the bonding coating agent, the surface of the powder is prevented from being oxidized, and then the powder is degummed in a reducing atmosphere, so that the surface of the parison has excellent activation energy, activation pressing in a hot pressing process is formed, and the density and the purity of the titanium-aluminum alloy target are effectively improved.
The method has the advantages that expensive equipment such as a hot isostatic pressing sintering furnace is not needed in the preparation process, the preparation method is simple, the production cost can be effectively reduced, and the industrial popularization is facilitated.
Drawings
FIG. 1 is a scanning electron microscope image of a titanium-aluminum alloy target material prepared in example 2, magnified 300 times;
FIG. 2 is a scanning electron microscope image of the titanium-aluminum alloy target material prepared in comparative example 1, magnified 300 times.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The method for preparing the titanium-aluminum alloy target material of the embodiment comprises the following steps of S110 to S150:
s110, providing titanium-aluminum alloy target material powder.
In the present embodiment, the titanium-aluminum alloy target material powder is: pure titanium powder and pure aluminum powder.
S120, uniformly mixing the titanium-aluminum alloy target material powder in proportion to obtain blank powder.
In the present embodiment, the method for uniformly mixing the raw material powders of the titanium-aluminum alloy target material in proportion is as follows: and mixing the titanium-aluminum alloy target material powder and a wet grinding medium in proportion, and stirring at a rotating speed of 50-150 rpm for 1-4 hours. Wherein, the wet grinding medium can be ethanol or other common wet grinding media, so long as the subsequent discharge is easy and impurities are not introduced.
Furthermore, the volume ratio of the titanium-aluminum alloy target material powder to the wet grinding medium is (2-1): 1.
It is understood that, in other embodiments, the titanium-aluminum alloy target material powder may be mixed by other methods as long as it is homogenized to form a green powder.
And S130, crushing the blank powder in a protective gas atmosphere to obtain powder.
Wherein the protective gas atmosphere is nitrogen or argon.
In the present embodiment, the method of pulverizing the green powder includes: and (3) putting the blank powder into an airflow mill for crushing treatment. Compressed nitrogen or compressed argon is sprayed out at high speed through a nozzle, and the high-speed jet flow drives the blank powder to move at high speed, so that the blank powder is collided, rubbed and crushed.
Furthermore, the particle size of the powder is 180-300 meshes.
The blank powder is placed in an air flow mill for crushing treatment, and the obtained powder has the characteristics of narrow particle size distribution, smooth particle surface, regular particle shape, high purity, high activity, good dispersibility and the like, and is beneficial to reducing powder agglomeration, reducing porosity and improving density.
It should be noted that, in order to prevent impurities from being introduced during the pulverization process, the inner surfaces of the jet mills contacting the raw powder are coated with polymer materials, and even if the polymer materials are mixed into the raw powder during the pulverization process, the polymer materials can be removed by degumming or hot-pressing sintering, so that the purity of the target material can be effectively improved, and the performance of the target material can be improved.
In the protective gas atmosphere, the blank powder is crushed, so that an oxide film on the surface of the blank powder can be damaged, a subsequent target material interface is purified, the interface binding force is activated, the porosity is reduced, and the density is improved.
And S140, mixing the powder and the bonding coating agent, granulating, and performing compression molding to obtain a parison.
In the present embodiment, the binder coating agent is paraffin or polyethylene glycol having an average molecular weight of 200 to 2000.
It should be noted that the bonding coating agent is not limited to the paraffin or polyethylene glycol described above, and other high molecular polymers may be used as long as the bonding coating agent can coat the surface of the powder to prevent the powder from being oxidized, and can be removed by degumming or hot-pressing sintering at a later stage.
The powder and the bonding coating agent are mixed and then granulated, so that the surface of the powder is coated by the bonding coating agent, and the surface of the powder is prevented from being oxidized.
The granularity of particles obtained by mixing and granulating the powder and the bonding coating agent is controlled to be 1-50 mu m, and meanwhile, the granulated powder with different particle sizes is controlled to be distributed according to a certain proportion, so that the filling density among the powder in the pressing process can be effectively improved, and the density of the titanium-aluminum alloy target material is improved.
And S150, degumming the parison in a reducing atmosphere, and carrying out hot-pressing sintering to obtain the titanium-aluminum alloy target material.
Wherein the reducing atmosphere is hydrogen. The degumming time is 0.5-4 hours, and the degumming temperature is 200-800 ℃. The flow rate of the hydrogen is 10 ml/min-100 ml/min.
In the present embodiment, the hot pressing sintering method is segmented hot pressing or plasma rapid sintering assisted segmented hot pressing.
Further, the segmented hot pressing method comprises the following steps: hot pressing for 0.5-2 hours at 300-800 MPa and 0-400 ℃; hot pressing for 0.5-2 hours at 400-800 MPa and 50-400 ℃; hot pressing for 1-4 hours at 400-800 MPa and 100-400 ℃; hot pressing for 0.5-2 hours at the temperature of 100-400 ℃ and the pressure of 800-1200 MPa.
In other embodiments, the hot pressing sintering method can also be microwave vibration assisted plasma rapid sintering.
According to the preparation method of the titanium-aluminum alloy target, the blank powder is crushed in the protective gas atmosphere, an oxide film on the surface of the blank powder is damaged, a subsequent target interface is purified, the interface bonding force is activated, and the porosity is reduced and the density is improved; and finally, the parison is degummed in a reducing atmosphere, so that the surface of the parison has excellent activation energy, the subsequent hot pressing process forms activation pressing, expensive equipment such as a hot isostatic pressing sintering furnace is not needed, the density and the purity of the titanium-aluminum alloy target material can be effectively improved, the preparation method is simple, the production cost is low, and the industrial popularization is facilitated.
The following are specific examples.
Example 1
Taking pure titanium powder and pure aluminum powder in a mass ratio of 33:67 as raw material powder, adding ethanol in a volume ratio of 1:1 with the raw material powder, placing the mixture in a ball milling barrel of a polypropylene inner container, stirring the mixture for 2 hours at a rotating speed of 60rpm, and drying the mixture in vacuum to obtain blank powder. And under the protection of nitrogen, the blank powder is crushed in a jet mill to obtain powder with the particle size of 180-300 meshes.
The powder is mixed with paraffin wax and then granulated, and the obtained granules have the grain diameter of 1-20 mu m accounting for about 10 wt%, the grain diameter of 20-35 mu m accounting for about 30 wt% and the grain diameter of 35-50 mu m accounting for about 60 wt%. And (4) pressing and forming to obtain a parison. Degumming the parison in a hydrogen atmosphere at 430 ℃ for 2 hours, and then carrying out hot pressing at 300MPa and 200 ℃ for 0.5 hour; hot pressing at 400MPa and 300 deg.c for 1 hr; hot pressing for 1 hour at 600MPa and 400 ℃; hot pressing for 1 hour at 900MPa and 400 ℃ to obtain the titanium-aluminum alloy target.
Example 2
Taking pure titanium powder and pure aluminum powder in a mass ratio of 33:67 as raw material powder, adding ethanol in a volume ratio of 1:1 with the raw material powder, placing the mixture in a ball milling barrel of a polypropylene inner container, stirring the mixture for 2 hours at a rotating speed of 50rpm, and drying the mixture in vacuum to obtain blank powder. And under the protection of nitrogen, the blank powder is crushed in a jet mill to obtain powder with the particle size of 180-300 meshes.
Mixing the powder with polyethylene glycol with the average molecular weight of 200, and granulating to obtain granules with the particle size of 1-20 μm accounting for about 5 wt%, the particle size of 20-35 μm accounting for about 30 wt%, and the particle size of 35-50 μm accounting for about 65 wt%. And (4) pressing and forming to obtain a parison. Degumming the parison in a hydrogen atmosphere at 430 ℃ for 2 hours, and then carrying out hot pressing at 400MPa and 200 ℃ for 0.6 hour; hot pressing at 400MPa and 300 deg.c for 1 hr; hot pressing at 800MPa and 300 deg.c for 1 hr; hot pressing for 1 hour at 900MPa and 400 ℃ to obtain the titanium-aluminum alloy target.
Comparative example 1
Comparative example 1 is substantially the same as example 2 except that comparative example 1 does not perform a pulverization treatment after obtaining a green powder, but directly mixes the green powder with polyethylene glycol having an average molecular weight of 200 and then pelletizes.
FIG. 1 is a scanning electron microscope image of a titanium-aluminum alloy target material prepared in example 2, magnified 300 times; FIG. 2 is a scanning electron microscope image of the titanium-aluminum alloy target material prepared in comparative example 1, magnified 300 times. As can be seen from comparison between fig. 1 and fig. 2, the titanium-aluminum alloy target material prepared in example 2 has higher uniformity, smaller particle size distribution area, higher overall density, and no obvious pores caused by accumulation of particles, compared with the titanium-aluminum alloy target material prepared in comparative example 1.
Comparative example 2
Comparative example 2 is substantially the same as example 2 except that comparative example 2 does not perform pulverization treatment after obtaining the green powder, but directly mixes the green powder with polyethylene glycol having an average molecular weight of 200 and then pelletizes, and in addition, comparative example 2 does not perform segmented hot pressing after degumming but performs hot pressing sintering by using a conventional hot isostatic pressing method.
Example 3
Taking pure titanium powder and pure aluminum powder in a mass ratio of 33:67 as raw material powder, adding ethanol in a volume ratio of 1:1 with the raw material powder, placing the mixture in a ball milling barrel of a polypropylene inner container, stirring the mixture for 2 hours at a rotating speed of 70rpm, and drying the mixture in vacuum to obtain blank powder. And under the protection of nitrogen, the blank powder is crushed in a jet mill to obtain powder with the particle size of 180-300 meshes.
Mixing the above powder and polyethylene glycol with average molecular weight of 2000, and granulating to obtain granule with particle size of 1-20 μm accounting for about 5 wt%, particle size of 20-35 μm accounting for about 30 wt%, and particle size of 35-50 μm accounting for about 65 wt%. And (4) pressing and forming to obtain a parison. Degumming the parison in a hydrogen atmosphere at 450 ℃ for 2 hours, and hot-pressing at 300MPa and 200 ℃ for 0.5 hour; hot pressing at 400MPa and 300 deg.c for 1 hr; hot pressing for 1 hour at 600MPa and 400 ℃; hot pressing at 900MPa and 400 deg.c for 1 hr. And obtaining the titanium-aluminum alloy target.
The titanium-aluminum alloy targets prepared in examples 1 to 3 and comparative examples 1 and 2 were subjected to performance tests, and the results are shown in table 1.
TABLE 1
As can be seen from table 1, the titanium-aluminum alloy target material prepared by the method of the present application has lower oxygen content and iron content, and shows excellent purity; and the density is higher, which shows that the titanium-aluminum alloy target material prepared by the method has an advantage in densification effect compared with the traditional isostatic pressing mode.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the titanium-aluminum alloy target is characterized by comprising the following steps:
providing titanium-aluminum alloy target material powder;
uniformly mixing the titanium-aluminum alloy target material raw material powder in proportion to obtain blank powder;
in a protective gas atmosphere, crushing the blank powder to obtain powder;
mixing the powder and the bonding coating agent, granulating, and performing compression molding to obtain a parison;
and degumming the parison in a reducing atmosphere, and carrying out hot-pressing sintering to obtain the titanium-aluminum alloy target material.
2. The method for preparing the titanium-aluminum alloy target material according to claim 1, wherein the method for pulverizing the raw powder comprises the following steps: and (3) putting the blank powder into a jet mill for crushing treatment.
3. The method for preparing the titanium-aluminum alloy target material according to claim 1 or 2, wherein the powder has a particle size of 180-300 meshes.
4. The method for preparing the titanium-aluminum alloy target material according to claim 1, wherein the bonding coating agent is paraffin or polyethylene glycol with an average molecular weight of 200-2000.
5. The method for preparing the titanium-aluminum alloy target material according to claim 1 or 4, wherein the grain size of the grains obtained by mixing and granulating the powder material and the bonding coating agent is 1 μm to 50 μm.
6. The method for preparing the titanium-aluminum alloy target material according to claim 1, wherein the reducing atmosphere is hydrogen, and the flow rate of the hydrogen is 10ml/min to 100 ml/min; the degumming time is 0.5-4 hours, and the degumming temperature is 200-800 ℃.
7. The method for preparing the titanium-aluminum alloy target material according to claim 1, wherein the hot pressing sintering method is segmented hot pressing or plasma rapid sintering assisted segmented hot pressing.
8. The method for preparing the titanium-aluminum alloy target material according to claim 7, wherein the step of hot pressing comprises the following steps: hot pressing for 0.5-2 hours at 300-800 MPa and 0-400 ℃; hot pressing for 0.5-2 hours at 400-800 MPa and 50-400 ℃; hot pressing for 1-4 hours at 400-800 MPa and 100-400 ℃; hot pressing for 0.5-2 hours at the temperature of 100-400 ℃ and the pressure of 800-1200 MPa.
9. The method for preparing the titanium-aluminum alloy target material according to claim 1, wherein the hot-pressing sintering method is microwave vibration assisted plasma rapid sintering.
10. The method for preparing the titanium-aluminum alloy target material according to claim 1, wherein the method for uniformly mixing the raw material powder of the titanium-aluminum alloy target material in proportion comprises the following steps: and mixing the titanium-aluminum alloy target material powder and a wet grinding medium in proportion, and stirring at a rotating speed of 50-150 rpm for 1-4 hours.
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