CN117364035A - Titanium-aluminum target and preparation method thereof - Google Patents
Titanium-aluminum target and preparation method thereof Download PDFInfo
- Publication number
- CN117364035A CN117364035A CN202311331843.5A CN202311331843A CN117364035A CN 117364035 A CN117364035 A CN 117364035A CN 202311331843 A CN202311331843 A CN 202311331843A CN 117364035 A CN117364035 A CN 117364035A
- Authority
- CN
- China
- Prior art keywords
- powder
- titanium
- aluminum
- aluminum target
- sheath
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001301 oxygen Substances 0.000 claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 21
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 21
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 18
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 18
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008117 stearic acid Substances 0.000 claims abstract description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 241001122767 Theaceae Species 0.000 claims abstract description 9
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 9
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 8
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 claims abstract description 7
- 229940083982 sodium phytate Drugs 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000007872 degassing Methods 0.000 claims description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 29
- 229910002804 graphite Inorganic materials 0.000 claims description 29
- 239000010439 graphite Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000013077 target material Substances 0.000 abstract description 10
- 239000010936 titanium Substances 0.000 description 17
- 235000006708 antioxidants Nutrition 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 13
- 238000000576 coating method Methods 0.000 description 13
- 238000005192 partition Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 239000011265 semifinished product Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000003801 milling Methods 0.000 description 5
- 238000003466 welding Methods 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910001060 Gray iron Inorganic materials 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910004349 Ti-Al Inorganic materials 0.000 description 1
- 229910010037 TiAlN Inorganic materials 0.000 description 1
- 229910004692 Ti—Al Inorganic materials 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- QRRWWGNBSQSBAM-UHFFFAOYSA-N alumane;chromium Chemical compound [AlH3].[Cr] QRRWWGNBSQSBAM-UHFFFAOYSA-N 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- 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
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
Abstract
The application belongs to the technical field of target production, and discloses a preparation method of a titanium-aluminum target, which comprises the following steps of: 5-6, then putting titanium powder, aluminum powder and an antioxidant into a mixer for mixing to obtain powder I, wherein the antioxidant is at least one of stearic acid, sodium phytate and tea polyphenol, and the adding amount of the antioxidant is 0.1-0.5% of the total mass of the titanium powder and the aluminum powder; then ball milling is carried out on the first powder under the atmosphere of nitrogen or argon to obtain second powder, and the ball milling time is 6-12 hours; finally, carrying out hot isostatic pressing sintering on the powder II, then cooling and discharging to obtain the titanium-aluminum target material, and preparing the titanium-aluminum target material with low oxygen content, high density and excellent mechanical property by the preparation method.
Description
Technical Field
The invention relates to the technical field of target preparation, in particular to a titanium-aluminum target and a preparation method thereof.
Background
The hard alloy coating material is widely applied to the machining fields of cutting tools, wear-resistant parts and the like due to the good wear resistance, corrosion resistance, high-temperature oxidation resistance and other characteristics. Materials currently available for coating fabrication include titanium aluminum (TiAl), chromium aluminum (CrAl), titanium silicon (TiSi), tungsten carbide (WC), and nitride materials, wherein the titanium aluminum target produced from titanium aluminum alloy is nitrogen (N) 2 ) The coating is prepared in a magnetron sputtering mode in atmosphere, and can provide an antioxidant nitride coating (TiAlN) for cutters such as drills, milling cutters, numerical control blades, gear hobbing cutters and the like in machining, so that the service life of the cutters is prolonged, meanwhile, the binding force of the cutter coating is influenced by the oxygen content in a coating material, when the oxygen content is high, the binding force of the coating and the cutters is not strong, the coating is very easy to fall off from the cutters during turning, and therefore the cutters are broken, blunt cutters and the like.
Because the melting points of titanium (Ti) and aluminum (Al) are 1668 ℃ and 660 ℃ respectively, the difference between the melting points is larger, and the TiAl alloy with relatively uniform tissue distribution is difficult to prepare by adopting a vacuum smelting mode, the TiAl alloy is prepared by adopting a mode of mixing Ti powder and Al powder and further pressurizing and densifying at present, the oxygen content of the TiAl alloy is greatly dependent on the oxygen content in raw materials and the oxygen introducing amount in the process, and for oxygen in the raw materials, dense alumina (Al) is formed on the surface of aluminum powder 2 O 3 ) The film suppresses further oxidation of the Al powder as a whole, and since Al is an active metal, even if the surface alumina film is removed by some means, it is rapidly oxidized in actual operation. In addition, when Ti powder and Al powder are mixed, in order to mix uniformly, a ball milling powder mixing mode is generally adopted, and although inert gas (such as argon and nitrogen) is used for protection, the ball milling powder mixing can cause particle breakage, and oxygen is inevitably introduced in the transportation after powder mixing, so that the oxygen content is improved.
The Chinese patent application 200910043144.4 discloses a rapid hot-pressing sintering molding process of a titanium-aluminum alloy target, which adopts a hot-pressing powder rapid molding process to sinter and mold materials under the combined action of heat and force, and utilizes the low melting point of aluminum in a Ti-Al mixture to bond titanium powder together so as to obtain titanium-aluminum targets with various components required, so that titanium-aluminum targets with different components and various dimensions can be prepared.
Chinese patent application 201911425902.9 discloses a titanium-aluminum alloy target and a preparation method, wherein yttrium with the mass percentage of 0.3-2wt% is doped into the titanium-aluminum alloy target, and the slippage of a grain boundary is prevented and the diffusion of oxygen at the grain boundary is organized through the strengthening effect of yttrium on the grain boundary.
Chinese patent application 201410842607.4 discloses a titanium-aluminum alloy target and a method for preparing the same by doping Co, cr, ta, W, nb, mo, zr, V, B, si, Y, la, ce or Se in the titanium-aluminum target. According to the invention, through the addition of various elements, various forms of nitriding, carbonizing and nitrogen carbonizing composite film materials can be formed; further densification of the product is facilitated by improved heat treatment processes; the oxygen content is effectively controlled through the improved powder mixing and degassing process, and the powder mixing and degassing process in the scheme is as follows:
(1) Selecting raw materials, and mixing according to a proportion;
(2) Putting the mixed materials into a steel ladle sleeve, and performing argon arc welding without air leakage;
(3) Placing the steel ladle in a well type heat treatment furnace for degassing treatment;
(4) Welding the steel ladle after the degassing treatment;
(5) Placing the steel ladle after the degassing treatment in hot isostatic pressing equipment for hot isostatic pressing treatment;
(6) Cooling to 100-200deg.C, taking out, cooling to room temperature with cooling rate of 10-50deg.C/hr;
(7) Removing the sheath, and cutting the target material into a specified shape;
(8) And detecting the purity, oxygen content, density, grain size and metallographic parameters of the target material.
The problem that this scheme needs to solve: how to provide a titanium-aluminum target material with low oxygen content, high density and good mechanical properties of a coating prepared later and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a preparation method of a titanium-aluminum target, which can prepare the titanium-aluminum target with low oxygen content and good mechanical property of a coating prepared later under the condition of low requirement on the oxygen content of raw materials.
In order to achieve the above purpose, the present application discloses a preparation method of a titanium aluminum target, comprising the following steps:
step 1: the titanium powder and the aluminum powder are 4 to 5: 5-6, then putting titanium powder, aluminum powder and an antioxidant into a mixer for mixing to obtain powder I, wherein the antioxidant is at least one of stearic acid, sodium phytate and tea polyphenol, and the adding amount of the antioxidant is 0.1-0.5% of the total mass of the titanium powder and the aluminum powder;
step 2: ball milling is carried out on the first powder prepared in the step 1 in the atmosphere of nitrogen or argon to prepare second powder, and the ball milling time is 6-12 h;
step 3: and (3) carrying out hot isostatic pressing sintering on the powder II obtained in the step (2), and then cooling and discharging to obtain the titanium-aluminum target.
Preferably, in the step 1, the titanium powder is acid-washed titanium powder, and the acid-washed titanium powder is prepared by washing the titanium powder for 2-10 min through weak acid with the concentration of 0.5-3 mol/L and drying, wherein the weak acid is at least one selected from glacial acetic acid, dilute hydrochloric acid and silicic acid.
Preferably, the step 3 specifically comprises: placing the powder II prepared in the step 2 into a sheath with the inner surface covered with graphite paper, and sealing the sheath by using a cover plate to finish die filling;
degassing the die-filled sheath, placing the degassed sheath into a hot isostatic pressing sintering furnace for hot isostatic pressing sintering, wherein the heating rate in the hot isostatic pressing sintering process is 2-10 ℃/min, the temperature is kept for 3-8 h after the temperature is increased to 400-550 ℃, and the pressure in the hot isostatic pressing sintering process is 80-140 MPa;
and after the hot isostatic pressing sintering is finished, cooling to 100 ℃ or below along with the furnace, reducing the pressure to the standard atmospheric pressure, and discharging to obtain the titanium-aluminum target.
Preferably, step 1 is accomplished in an inert gas glove box.
Preferably, the degassing temperature of the degassing process of step 3 is 400-550 ℃.
In addition, the application also discloses a titanium-aluminum target material, which is prepared by the preparation method of the titanium-aluminum target material.
Preferably, the oxygen content of the titanium aluminum target is less than 1700ppm.
Preferably, the density of the titanium aluminum target is greater than 99.5%.
The beneficial effects of this application are: according to the method, the antioxidant is added into the titanium powder and the aluminum powder while the titanium powder and the aluminum powder are mixed, wherein the stearic acid can be used for blocking contact between metal ions and substances such as oxygen and water due to the fact that phytic acid molecules in the sodium phytate have a plurality of carboxyl groups and phosphoric acid groups, so that oxidation reaction of metals is reduced;
simultaneously, the hydroxyl and the phenolic groups in the tea polyphenol can coordinate with metal ions to form a stable complex. The complexing effect can block metal ions from participating in oxidation reaction, so that oxidation damage of metal is reduced;
and, stearic acid may form a protective oxide film with the metal surface. The oxide film can prevent the metal from contacting with substances such as external oxygen, water and the like, thereby reducing the oxidation reaction of the metal. The carboxyl group in the stearic acid molecule can form a complex with the metal surface to further stabilize the formation of the oxide film.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which specific conditions, either conventional or manufacturer-suggested, are not explicitly stated. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Step 1: washing Ti powder for 3 minutes by 2mol/L glacial acetic acid, fully removing surface oxide, drying the Ti powder in a vacuum oven at 110 ℃ for 1 hour, and rapidly transferring the dried Ti powder into an inert gas glove box, wherein the mass ratio of Ti to Al in the inert gas glove box is 46.64:53.36 and adding stearic acid accounting for 0.15% of the total mass of titanium powder and aluminum powder, and then carrying out preliminary powder mixing in an inert gas glove box through a three-dimensional mixer for 20 minutes to obtain powder I.
Step 2: and (3) ball milling and mixing the powder I prepared in the step (1) under argon atmosphere to further mix titanium powder and aluminum powder in the powder I, wherein the mixing time is 8 hours, and thus powder II is obtained.
Step 3: preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a partition plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, a through hole is formed in the cover plate, the degassing pipe is arranged at the through hole, and the partition plate and the graphite paper pad are arranged in a cylindrical accommodating space formed by the bottom plate, the outer side plate and the cover plate. Wherein, the thickness of the baffle is 3mm; the thickness of the graphite paper is 0.38mm; the outer diameter of the degassing pipe is 10mm, and the wall thickness of the degassing pipe is 3mm; the bottom plate, the outer side plate, the baffle plate, the cover plate and the deaeration pipe are made of low carbon steel. The installation modes of the bottom plate and the outer side plate, the cover plate and the outer side plate and the cover plate and the air removing pipe are all argon arc welding and fixing;
assembling a bottom plate and an outer side plate to form a semi-finished product of a sheath with an opening at one end, padding graphite paper at the inner wall of the outer side plate, sequentially padding graphite paper, a partition plate and graphite paper at the bottom of the semi-finished product of the sheath, pouring mixed powder II onto the graphite paper, tamping, sequentially padding the graphite paper, the partition plate and the graphite paper on the powder II, finally sealing and fixing the opening of the semi-finished product of the sheath by using a cover plate, and installing a degassing pipe at a through hole of the cover plate to finish die filling;
putting the die-filled sheath into a furnace, heating while vacuumizing and degassing the sheath through a degassing pipe, and when the vacuum degree in the sheath is less than 5 multiplied by 10 -4 After Pa, stopping heating and degassing, and sealing a degassing pipe, wherein the degassing temperature is 460 ℃;
and (3) placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and carrying out vacuumizing, pressurizing, heating and sintering, cooling and pressure recovery. In the heating sintering process, the heating rate is 5 ℃/min, the sintering temperature is 500 ℃, the pressure is 120MPa, and the heat preservation time is 4h; and after the heating and sintering are finished, cooling and pressure recovery are carried out, when the temperature is less than 100 ℃, and the pressure of the hot isostatic pressing sintering furnace is standard atmospheric pressure, discharging, and removing the sheath to obtain the titanium aluminum target.
Example 2
Step 1: washing Ti powder for 3 minutes by 0.5mol/L dilute hydrochloric acid, fully removing surface oxide, drying the Ti powder in a vacuum oven at 110 ℃ for 1 hour, and rapidly transferring the dried Ti powder into an inert gas glove box, wherein the mass ratio of Ti to Al in the inert gas glove box is 40:60, namely weighing materials, adding stearic acid accounting for 0.1% of the total mass of titanium powder and aluminum powder, and then carrying out preliminary powder mixing in an inert gas glove box through a three-dimensional mixer for 20 minutes to obtain powder I.
Step 2: and (3) ball milling and mixing the powder I prepared in the step (1) in an argon atmosphere to further mix titanium powder and aluminum powder in the powder I, wherein the mixing time is 6 hours, and thus powder II is obtained.
Step 3: preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a partition plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, a through hole is formed in the cover plate, the degassing pipe is arranged at the through hole, and the partition plate and the graphite paper pad are arranged in a cylindrical accommodating space formed by the bottom plate, the outer side plate and the cover plate; wherein, the thickness of the baffle is 3mm; the thickness of the graphite paper is 0.38mm; the outer diameter of the degassing pipe is 10mm, and the wall thickness of the degassing pipe is 3mm; the bottom plate, the outer side plate, the baffle plate, the cover plate and the deaeration pipe are made of low carbon steel. The connection mode of the bottom plate and the outer side plate, the cover plate and the outer side plate and the cover plate and the gas removal pipe is argon arc welding and fixing;
assembling a bottom plate and an outer side plate to form a semi-finished product of a sheath with an opening at one end, padding graphite paper at the inner wall of the outer side plate, sequentially padding graphite paper, a partition plate and graphite paper at the bottom of the semi-finished product of the sheath, pouring mixed powder II onto the graphite paper, tamping, sequentially padding the graphite paper, the partition plate and the graphite paper on the powder II, finally sealing and fixing the opening of the semi-finished product of the sheath by using a cover plate, and installing a degassing pipe at a through hole of the cover plate to finish die filling;
putting the die-filled sheath into a furnace, heating while vacuumizing and degassing the sheath through a degassing pipe, and when the vacuum degree in the sheath is less than 5 multiplied by 10 -4 After Pa, stopping heating and degassing, and sealing a degassing pipe, wherein the degassing temperature is 400 ℃;
and (3) placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and carrying out vacuumizing, pressurizing, heating and sintering, cooling and pressure recovery. In the heating sintering process, the heating rate is 2 ℃/min, the sintering temperature is 400 ℃, the pressure is 140MPa, and the heat preservation time is 8 hours; and after the heating and sintering are finished, cooling and pressure recovery are carried out, when the temperature is less than 100 ℃, and the pressure of the hot isostatic pressing sintering furnace is standard atmospheric pressure, discharging, and removing the sheath to obtain the titanium aluminum target.
Example 3
Step 1: washing Ti powder for 3 minutes through 3mol/L silicic acid, fully removing surface oxide, drying the Ti powder in a vacuum oven at 110 ℃ for 1 hour, and rapidly transferring the dried Ti powder into an inert gas glove box, wherein the mass ratio of Ti to Al in the inert gas glove box is 50:50, weighing materials, adding stearic acid accounting for 0.5% of the total mass of titanium powder and aluminum powder, and then carrying out preliminary powder mixing in an inert gas glove box through a three-dimensional mixer for 20 minutes to obtain powder I.
Step 2: and (3) ball milling and mixing the powder I prepared in the step (1) in an argon atmosphere to further mix titanium powder and aluminum powder in the powder I, wherein the mixing time is 12 hours, and thus powder II is obtained.
Step 3: preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a partition plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, a through hole is formed in the cover plate, the degassing pipe is arranged at the through hole, and the partition plate and the graphite paper pad are arranged in a cylindrical accommodating space formed by the bottom plate, the outer side plate and the cover plate; wherein, the thickness of the baffle is 3mm; the thickness of the graphite paper is 0.38mm; the outer diameter of the degassing pipe is 10mm, and the wall thickness of the degassing pipe is 3mm; the bottom plate, the outer side plate, the baffle plate, the cover plate and the deaeration pipe are made of low carbon steel. The connection mode of the bottom plate and the outer side plate, the cover plate and the outer side plate and the cover plate and the gas removal pipe is argon arc welding and fixing;
assembling a bottom plate and an outer side plate to form a semi-finished product of a sheath with an opening at one end, padding graphite paper at the inner wall of the outer side plate, sequentially padding graphite paper, a partition plate and graphite paper at the bottom of the semi-finished product of the sheath, pouring mixed powder II onto the graphite paper, tamping, sequentially padding the graphite paper, the partition plate and the graphite paper on the powder II, finally sealing and fixing the opening of the semi-finished product of the sheath by using a cover plate, and installing a degassing pipe at a through hole of the cover plate to finish die filling;
putting the die-filled sheath into a furnace, heating while vacuumizing and degassing the sheath through a degassing pipe, and when the vacuum degree in the sheath is less than 5 multiplied by 10 -4 After Pa, stopping heating and degassing, and sealing a degassing pipe, wherein the degassing temperature is 550 ℃;
and (3) placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and carrying out vacuumizing, pressurizing, heating and sintering, cooling and pressure recovery. In the heating sintering process, the heating rate is 10 ℃/min, the sintering temperature is 550 ℃, the pressure is 80MPa, and the heat preservation time is 3h; and after the heating and sintering are finished, cooling and pressure recovery are carried out, when the temperature is less than 100 ℃, and the pressure of the hot isostatic pressing sintering furnace is standard atmospheric pressure, discharging, and removing the sheath to obtain the titanium aluminum target.
Example 4
Substantially the same as in example 1, except that the titanium powder was washed with 5mol/L glacial acetic acid for 3 minutes in this example.
Example 5
Substantially the same as in example 1, except that the antioxidant is a mixture of stearic acid and tea polyphenol, and the mass ratio of stearic acid to tea polyphenol is 1:1.
example 6
Substantially the same as in example 1, except that the antioxidant is a mixture of stearic acid and sodium phytate, and the mass ratio of stearic acid to tea polyphenol is 1:1.
example 7
Substantially the same as in example 1, except that the antioxidant is a mixture of stearic acid, sodium phytate, tea polyphenols, and the mass ratio of stearic acid, sodium phytate, and tea polyphenols is 2:1:1.
comparative example 1
Substantially the same as in example 1, except that in step 1, no antioxidant was added during the mixing of the titanium powder and the aluminum powder.
Comparative example 2
Substantially the same as in example 1, except that in step 1, ascorbic acid was used instead of stearic acid.
Comparative example 3
Substantially the same as in example 1, except that sodium sulfite was used instead of stearic acid in step 1.
Comparative example 4
Substantially the same as in example 1, except that in step 1, the antioxidant was added in an amount of 2.0% by mass of the total mass of the titanium powder and the aluminum powder.
Performance test:
1. testing the oxygen content in the target material by an oxygen-nitrogen analyzer;
2. the prepared target is manufactured into a coating on the surface of a milling cutter in a magnetron sputtering mode, and the service life standard is tested in a milling and turning mode, wherein the milling cutter adopts WNGU080608-GM, the workpiece material adopts TH250 gray cast iron, the machining mode is square shoulder milling, the service life standard takes a collapse value of more than or equal to 0.3mm as a standard, and the comparison is 100% in the embodiment 1; wherein the turning tool specification adopts CNMG120408-LM, the workpiece material is 304 stainless steel, and the processing mode is continuous;
3. testing the compactness of the target material by using an Archimedes drainage method;
the test results are shown in table 1:
TABLE 1
Analysis of results:
1. it is seen from examples 1 to 3 that, after adjusting the mass ratio of titanium to aluminum and the addition amount of stearic acid, the target material does not have a certain performance difference in oxygen content, density and mechanical properties of the coating prepared by subsequent processing, but the difference is not obvious;
2. as can be seen from examples 1 and examples 5 to 7, after the antioxidant is compounded, the oxygen content in the target is obviously reduced, the compactness is improved to a certain extent, more importantly, the mechanical properties of the coating subsequently prepared by the target obtained in examples 5 to 7 are obviously improved, and the unexpected improvement effect is obtained in example 7;
3. it can be seen from example 1 and comparative examples 1 to 3 that the oxygen content of the target, the density and the mechanical properties of the coating layer produced by the subsequent processing are reduced to different extents, whether the addition of the antioxidant is omitted or other substances having antioxidant ability are used instead of the antioxidant in the present application, and that the antioxidant in the present application is indispensable and irreplaceable.
The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the titanium aluminum target is characterized by comprising the following steps of:
step 1: the titanium powder and the aluminum powder are 4 to 5: 5-6, then putting titanium powder, aluminum powder and an antioxidant into a mixer for mixing to obtain powder I, wherein the antioxidant is at least one of stearic acid, sodium phytate and tea polyphenol, and the adding amount of the antioxidant is 0.1-0.5% of the total mass of the titanium powder and the aluminum powder;
step 2: ball milling is carried out on the first powder prepared in the step 1 in the atmosphere of nitrogen or argon to prepare second powder, and the ball milling time is 6-12 h;
step 3: and (3) carrying out hot isostatic pressing sintering on the powder II obtained in the step (2), and then cooling and discharging to obtain the titanium-aluminum target.
2. The method for preparing a titanium-aluminum target according to claim 1, wherein in the step 1, the titanium powder is acid-washed titanium powder, the acid-washed titanium powder is prepared by washing titanium powder for 2-10 min through weak acid with the concentration of 0.5-3 mol/L, and drying the titanium powder, and the weak acid is at least one selected from glacial acetic acid, diluted hydrochloric acid and silicic acid.
3. The method for preparing a titanium aluminum target according to claim 1, wherein the step 3 specifically comprises: placing the powder II prepared in the step 2 into a sheath with the inner surface covered with graphite paper, and sealing the sheath by using a cover plate to finish die filling;
degassing the die-filled sheath, placing the degassed sheath into a hot isostatic pressing sintering furnace for hot isostatic pressing sintering, wherein the heating rate in the hot isostatic pressing sintering process is 2-10 ℃/min, the temperature is kept for 3-8 h after the temperature is increased to 400-550 ℃, and the pressure in the hot isostatic pressing sintering process is 80-140 MPa;
and after the hot isostatic pressing sintering is finished, cooling to 100 ℃ or below along with the furnace, reducing the pressure to the standard atmospheric pressure, and discharging to obtain the titanium-aluminum target.
4. The method for preparing a titanium aluminum target according to claim 1, wherein the step 1 is completed in an inert gas glove box.
5. The method for producing a titanium-aluminum target according to claim 3, wherein the degassing temperature in the degassing process of step 3 is 400 to 550 ℃.
6. A titanium-aluminum target, characterized by being produced by the method for producing a titanium-aluminum target according to any one of claims 1 to 5.
7. The titanium aluminum target of claim 6, wherein the oxygen content of the titanium aluminum target is less than 1700ppm.
8. The titanium aluminum target of claim 6, wherein the density of the titanium aluminum target is greater than 99.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311331843.5A CN117364035A (en) | 2023-10-13 | 2023-10-13 | Titanium-aluminum target and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311331843.5A CN117364035A (en) | 2023-10-13 | 2023-10-13 | Titanium-aluminum target and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117364035A true CN117364035A (en) | 2024-01-09 |
Family
ID=89392271
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311331843.5A Pending CN117364035A (en) | 2023-10-13 | 2023-10-13 | Titanium-aluminum target and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117364035A (en) |
-
2023
- 2023-10-13 CN CN202311331843.5A patent/CN117364035A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108060322B (en) | Preparation method of hard high-entropy alloy composite material | |
| CN109972015B (en) | Ti (C, N) -based metal ceramic cutter material and preparation method thereof | |
| EP2462083B1 (en) | Tough coated hard particles consolidated in a tough matrix material | |
| CN104451277B (en) | Chromium-aluminum alloy target and manufacturing method thereof | |
| CN110273092B (en) | CoCrNi particle reinforced magnesium-based composite material and preparation method thereof | |
| CN112647009A (en) | High-strength high-wear-resistance medium-entropy alloy and preparation method thereof | |
| CN112743080B (en) | Method for preparing Ti (C, N) -based metal ceramic cutter material with high heat resistance through in-situ integration | |
| CN110358960B (en) | Preparation method of high-strength and high-toughness Ti (C, N) -based metal ceramic | |
| CN111349839B (en) | Whisker toughened FCC (fluid catalytic cracking) high-entropy alloy composite material and preparation method thereof | |
| CN113234950B (en) | Preparation method of Ti (C, N) -based metal ceramic | |
| EP0646186B1 (en) | Sintered extremely fine-grained titanium based carbonitride alloy with improved toughness and/or wear resistance | |
| CN114635069A (en) | High-strength-toughness medium-entropy alloy binding phase Ti (C, N) -based metal ceramic and preparation method thereof | |
| CN115725944A (en) | Preparation method of tungsten-titanium sputtering target material | |
| CN112725676B (en) | Preparation method of high-strength hard alloy with good red hardness | |
| CN112981265A (en) | Carbon-free high-speed steel and preparation method thereof | |
| CN113151724A (en) | Method for preparing dual-performance DP-Ti (C, N) cermet by adopting oxidation material | |
| CN117364035A (en) | Titanium-aluminum target and preparation method thereof | |
| CN112024891A (en) | Hard alloy composite material and manufacturing method thereof | |
| CN111763843A (en) | Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy | |
| CN115679282A (en) | Preparation method of titanium-silicon target material | |
| CN116079055A (en) | CrAlFe-based alloy target and preparation method thereof | |
| CN112877578A (en) | Ultra-fine grain hard alloy and preparation method thereof | |
| JP5063129B2 (en) | cermet | |
| CN113088909A (en) | Nickel-chromium alloy sputtering target material and hot-pressing preparation method thereof | |
| CN108220735B (en) | Reinforced phase system for preparing metal ceramic and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |