CN111375758A - Sintering method of titanium or titanium alloy powder - Google Patents
Sintering method of titanium or titanium alloy powder Download PDFInfo
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- CN111375758A CN111375758A CN202010325032.4A CN202010325032A CN111375758A CN 111375758 A CN111375758 A CN 111375758A CN 202010325032 A CN202010325032 A CN 202010325032A CN 111375758 A CN111375758 A CN 111375758A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000010936 titanium Substances 0.000 title claims abstract description 104
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 103
- 239000000843 powder Substances 0.000 title claims abstract description 100
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000005245 sintering Methods 0.000 title claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 89
- 230000005672 electromagnetic field Effects 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 238000005238 degreasing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000009694 cold isostatic pressing Methods 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000001746 injection moulding Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000010146 3D printing Methods 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 238000005097 cold rolling Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 239000000375 suspending agent Substances 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 11
- 239000006260 foam Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 239000007943 implant Substances 0.000 description 4
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000000399 orthopedic effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
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- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
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- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
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- 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
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- B22F3/1134—Inorganic fillers
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
- C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
- C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F2003/1053—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by induction
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
Abstract
The invention belongs to the field of materials, and particularly relates to a sintering method of titanium or titanium alloy powder. The technical scheme of the invention is as follows: a sintering method of titanium or titanium alloy powder comprises the following steps: 1) preparing powder; 2) the heating body heats the powder; 3) the electromagnetic field heats the powder. According to the sintering method of the titanium or titanium alloy powder, heat is transmitted to the titanium or titanium alloy powder in contact with the heating body through the heating body, the non-conductive titanium dioxide oxide layer on the surface of the titanium or titanium alloy powder in the contact layer is damaged and dissolved, the titanium or titanium alloy powder is mutually connected and conducts electricity, the powder is rapidly heated layer by layer under the action of an alternating electromagnetic field, and finally a complete sintered body is obtained. The method has the advantages of high heating speed, short sintering time, small size shrinkage of the sintered body and simple process, and can be used for preparing porous titanium or titanium alloy and fully-compact titanium or titanium alloy sintered bodies with different pore gas rates.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a sintering method of titanium or titanium alloy powder.
Background
The porous material is a structural function integrated material, and due to the existence of pores, the specific surface of the material is increased, the density of the material is reduced, and the porous material has the functional properties of adsorption, filtration, noise reduction, heat insulation and the like. The product is widely applied to the fields of aerospace, medicine, environmental protection, metallurgy, electrochemistry and the like. The existing technology for preparing the porous material has the disadvantages of complex process, long production period, high technical requirement, high production equipment cost and difficult realization.
Titanium and titanium alloys have been widely used as structural materials in aerospace, automotive, diving, medical implants due to their high specific strength, low modulus, excellent biocompatibility, corrosion resistance. The porous titanium and the titanium alloy have the functional properties of high surface area and low modulus by introducing the holes, and the application of the titanium and the titanium alloy in orthopedic implant materials, battery electrode materials, sound absorption materials and filter materials is extended. The pore structure of porous titanium can be divided into two types: closed cell structures and open cell structures. The closed pore structure porous titanium has the functions of high damping, sound absorption and heat insulation due to the closed pores, and is mainly applied to sound absorption materials and thermal protection materials. The open-pore structure porous titanium has the functional attribute of closed-pore structure porous titanium due to the mutual penetration of the pores, has filtering property, and is mainly applied to orthopedic implant materials, battery electrode materials and filtering materials.
At present, the preparation method of porous titanium and titanium alloy is mainly the traditional powder metallurgy technology, and comprises powder loose sintering, pore-forming agent adding method, organic foam immersion method, freezing casting, fiber sintering and the like. In which I.H.Oh et al (scriptaMaterialia,2003,49,1197) prepared porous titanium with a through-hole structure having a porosity of 37% by vacuum sintering of spherical titanium powder, and its Young's modulus and flexural strength were close to those of human bones. Manonukul et al (Powder Technology,2014,266,129) prepared porous titanium with a porosity of 84% by dipping polyurethane foam in titanium Powder slurry by an organic foam dipping method, degreasing and vacuum sintering, and the Young's modulus of the porous titanium could reach 0.58 GPa. In the preparation technology of the porous titanium, because a compact titanium dioxide oxide film exists on the surface of titanium powder, electron migration between the titanium powder which is in contact with each other is hindered, the titanium powder can not be sintered in a mode of rapid heating through an electromagnetic field, heat can only be conducted to powder through the heating elements to be sintered under a vacuum condition, the heating rate is slow, the temperature rise time is long, the size shrinkage of a sintered body is large, the size of a product is difficult to control, and the preparation technology is not suitable for preparing the porous titanium and the titanium alloy with high porosity.
Disclosure of Invention
The invention provides a sintering method of titanium or titanium alloy powder, which transmits heat to titanium or titanium alloy powder contacted with a heating body through the heating body, destroys and dissolves a non-conductive titanium dioxide oxide layer on the surface of the titanium or titanium alloy powder in a contact layer, so that the titanium or titanium alloy powder is mutually connected and conductive, and the powder is rapidly heated layer by layer under the action of an alternating electromagnetic field, and finally a complete sintered body is obtained. The method has the advantages of high heating speed, short sintering time, small size shrinkage of the sintered body and simple process, and can be used for preparing porous titanium or titanium alloy and fully-compact titanium or titanium alloy sintered bodies with different pore gas rates.
The technical scheme of the invention is as follows:
a sintering method of titanium or titanium alloy powder comprises the following steps:
1) preparing powder; preparing titanium or titanium alloy powder into powder;
2) the heating body heats the powder; under the protective atmosphere of vacuum or inert gas, the powder is contacted with a heating body to be rapidly heated;
3) heating the powder by an electromagnetic field; the heating body heats the powder through heat conduction, and simultaneously, the powder is quickly heated through an electromagnetic field to prepare a sintered body.
Further, in the sintering method of the titanium or titanium alloy powder, the powder preparation mode in the step 1) is as follows: mixing titanium or titanium alloy powder with the granularity of less than 1000 mu m with a pore-forming agent and an organic adhesive, preparing a green body by cold pressing, warm pressing, 3D printing, cold isostatic pressing, cold rolling or injection molding, and degreasing the green body to obtain the titanium or titanium alloy powder.
Further, in the sintering method of the titanium or titanium alloy powder, the powder preparation mode in the step 1) is as follows: adding titanium or titanium alloy powder with the granularity of less than 1000 mu m, a binder, a dispersant, a suspending agent, a defoaming agent, a titrant, water or an organic solvent into a container in proportion, preparing powder slurry by stirring, dipping an organic template into the powder slurry, and carrying out curing and degreasing treatment to obtain the titanium or titanium alloy powder.
Further, in the sintering method of the titanium or titanium alloy powder, the powder preparation mode in the step 1) is as follows: the titanium or titanium alloy powder is directly spread on the heating body.
Further, the sintering method of the titanium or titanium alloy powder comprises the step of sintering the titanium or titanium alloy powder, wherein the pore-forming agent is NaCl, sucrose, magnesium, urea or starch.
Further, the sintering method of the titanium or titanium alloy powder is characterized in that the pressure for preparing the green body by the cold pressing or cold isostatic pressing process is 0.1-1500 MPa; the pressure of the green blank prepared by the warm pressing process is 0.1-1500MPa, and the temperature is 50-500 ℃.
Further, in the sintering method of the titanium or titanium alloy powder, the heating body is made of silicon carbide, silicon nitride, aluminum oxide, graphite, tungsten, molybdenum, steel, copper, titanium or titanium alloy.
Further, in the sintering method of titanium or titanium alloy powder, in the step 2), the vacuum condition is as follows: degree of vacuum 10-2~10-5Pa, inert gas is: argon or helium.
Further, in the sintering method of the titanium or titanium alloy powder, the heating temperature of the heating body is 200-1500 ℃.
Further, the sintering method of the titanium or titanium alloy powder comprises the following electromagnetic field heating modes: microwave heating, induction heating, plasma heating or pulse heating; the heating temperature of the electromagnetic field is 600-1500 ℃, and the heat preservation time is 0.01-2400 minutes.
Further, according to the sintering method of the titanium or titanium alloy powder, the green body is prepared on a pure titanium or titanium alloy heating body, the titanium or titanium alloy powder, a pore-forming agent and an organic adhesive are mixed to obtain a mixture, the pure titanium or titanium alloy heating body is placed at the bottom of a mold, the mixture is placed into the mold, cold press molding is carried out, and a molded body comprises the green body and the pure titanium or titanium alloy heating body.
The invention has the beneficial effects that: the invention transmits heat to the titanium or titanium alloy powder contacted with the heating body, can effectively destroy and dissolve the titanium dioxide oxide layer on the surface of the titanium or titanium alloy powder, and realizes the rapid heating of the powder under the action of the alternating electromagnetic field. The obtained sintered body has a porosity of 0.01-99%, and is suitable for preparing fully compact or porous titanium or titanium alloy products, and a porous titanium or titanium alloy coating can be prepared on a titanium or titanium alloy heating body. The method has the advantages that the heating speed can reach 1000 degrees per minute, the shrinkage rate of the sintered product is 0.1-90 percent, and the pore structure, the pore size, the pore rate and the size deviation of the sintered body of the porous titanium and the titanium alloy can be accurately controlled. The invention has simple production equipment, low raw material cost and controllable process, can realize large-scale industrial production, and can be widely applied to the fields of biomedical implants, photocatalysis, filtration, adsorption, noise reduction, heat insulation and the like.
Drawings
FIG. 1 is a cross-sectional gold phase diagram of porous titanium in example 1;
FIG. 2 is a cross-sectional gold phase diagram of porous titanium in example 2;
FIG. 3 is a metallographic structure chart of a fully dense titanium sintered body in example 2.
Detailed Description
Example 1
A method of sintering titanium powder comprising the steps of:
step 1: uniformly mixing pure titanium powder with the particle size of less than 45 mu m and urea particles with the particle size of less than 70 mu m according to the volume ratio of 3:7, putting 100 g of the mixture into a mold, cold-pressing the mixture into a green body with the diameter of 30 mm under the pressure of 100MPa, and putting the green body under the vacuum condition and the vacuum degree of less than 10-2Pa, degreasing to remove urea to obtain powder, wherein the degreasing temperature is 350 ℃, the heating rate is 10 ℃/min, and the degreasing time is 2 h.
Step 2: and placing the powder on a silicon carbide heating body, and heating the silicon carbide heating body under a vacuum condition, wherein the surface temperature of the silicon carbide heating body reaches 1000 ℃, and the heating rate is 500 ℃/min.
And step 3: the powder is heated to 1000 ℃ by pulse current, and the temperature is kept for 5 minutes to prepare porous titanium, wherein the cross section metallographic structure of the porous titanium is shown in figure 1; the porosity of the porous titanium is 68 percent, and the through porosity is 100 percent.
Example 2
A sintering method of titanium alloy powder comprises the following steps:
step 1: spreading spherical Ti-6Al-4V titanium alloy powder with the particle size of less than 149 microns on a silicon nitride heating body, placing the silicon nitride heating body in an induction heating coil, heating the silicon nitride heating body under the protection of argon gas, wherein the oxygen content is less than 100ppm, and the surface temperature of the silicon nitride heating body reaches 900 ℃, and the heating rate is 450 ℃/min.
And step 3: introducing induction current, heating the powder to 900 ℃ through an alternating electromagnetic field in the induction coil, and preserving heat for 10 minutes to prepare porous titanium, wherein the cross section metallographic structure of the porous titanium is shown in figure 2; the porosity of the porous titanium is 32%, and the through porosity is 100%.
Example 3
A sintering method of titanium alloy powder comprises the following steps:
step 1: heating polypropylene, polyethylene glycol and carnauba wax to 150 ℃ according to the mass ratio of 25:70:5, uniformly mixing to prepare a binder, mixing the binder and spherical Ti-6Al-4V titanium alloy powder with the same volume and the particle size of less than 44 mu m, heating to 150 ℃, uniformly mixing, heating the mixture to 150 ℃ through an injection molding machine, performing injection molding to obtain a green body with the diameter of 20 mm, and performing vacuum injection on the green body under the vacuum condition with the vacuum degree of less than 10-2Pa, heating to 900 ℃, preserving heat for 1 hour, degreasing and removing the binder to obtain powder, wherein the heating rate is 10 ℃/min.
Step 2: and placing the powder on a graphite heating body with the diameter of 40 mm, heating the graphite heating body under the argon protective atmosphere, wherein the oxygen content is lower than 100ppm, and the surface temperature of the graphite heating body reaches 1000 ℃, and the heating rate is 500 ℃/min.
And step 3: heating the powder to 1100 ℃ by using plasma, and preserving the heat for 2 hours to prepare a fully-compact titanium sintered body, wherein the cross section metallographic structure of the fully-compact titanium sintered body is shown in a figure 3; the relative density was 99%.
Example 4
A sintering method of titanium alloy powder comprises the following steps:
step 1: uniformly mixing Ti-6Al-4V titanium alloy powder with the particle size of less than 45 mu m, PVA, a dispersing agent and water in a mass ratio of 75:1:1:23 by a magnetic stirrer to prepare titanium powder slurry, soaking organic foam with the thickness of 20 mm in the slurry, repeating the soaking step for multiple times until the organic foam is completely coated by the slurry, taking out the organic foam, placing the organic foam in air, standing at room temperature for 24 hours until the organic foam is solidified, and placing the organic foam under a vacuum condition with the vacuum degree of less than 10-2Pa, heating to 600 ℃, preserving heat for 2 hours, degreasing and removing organic foam to obtain powder, wherein the heating rate is 10 ℃/min.
Step 2: placing the powder on a tungsten heating body with the area of 400 square centimeters, wherein the vacuum degree is lower than 10 under the vacuum condition-2Pa, heating the tungsten heating body, wherein the surface temperature of the tungsten heating body reaches 1100 ℃, and the heating rate is 500 ℃/min.
And step 3: heating the powder to 1100 ℃ by microwave, and keeping the temperature for 5 minutes to prepare porous titanium; the porosity of the porous titanium is 90%, and the through porosity is 100%.
Example 5
A method of sintering titanium powder comprising the steps of:
step 1: uniformly mixing pure titanium powder with the particle size of less than 45 mu m and NaCl particles with the particle size of less than 2mm according to the volume ratio of 3:7, placing a pure titanium heating body with the diameter of 30 mm at the center position at the bottom of a mould with the diameter of 30 mm, wherein the thickness of the pure titanium heating body is 20 mm, pouring 10 g of the mixture of the pure titanium powder and the NaCl particles into the mould, carrying out cold press molding on the mould under the pressure of 800MPa, coating the surface of the pure titanium heating body with the mixture of the pure titanium powder and the NaCl particles, removing NaCl from the molded body including a coating layer and the titanium heating body in deionized water, and placing the molded body at room temperature for 48 hours, and replacing the deionized.
Step 2: and (2) introducing pulse current to heat the coating layer and the titanium heating body, keeping the temperature of the titanium heating body to 1000 ℃, heating at the rate of 100 ℃/min, keeping the temperature until the temperature of the coating layer reaches 1000 ℃, and stopping heating to prepare the porous titanium coating on the pure titanium heating body, wherein the porosity of the porous titanium is 69% and the porosity of the through hole is 100%.
The above description describes only a few embodiments of the invention, and does not limit the scope of the invention. All changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (10)
1. A method for sintering titanium or titanium alloy powder, characterized by comprising the steps of:
1) preparing powder; preparing titanium or titanium alloy powder into powder;
2) the heating body heats the powder; under the protective atmosphere of vacuum or inert gas, the powder is contacted with a heating body to be rapidly heated;
3) heating the powder by an electromagnetic field; the heating body heats the powder through heat conduction, and simultaneously, the powder is quickly heated through an electromagnetic field to prepare a sintered body.
2. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the powder is prepared in the following manner in the step 1): mixing titanium or titanium alloy powder with the granularity of less than 1000 mu m with a pore-forming agent and an organic adhesive, preparing a green body by cold pressing, warm pressing, 3D printing, cold isostatic pressing, cold rolling or injection molding, and degreasing the green body to obtain the titanium or titanium alloy powder.
3. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the powder is prepared in the following manner in the step 1): adding titanium or titanium alloy powder with the granularity of less than 1000 mu m, a binder, a dispersant, a suspending agent, a defoaming agent, a titrant, water or an organic solvent into a container in proportion, preparing powder slurry by stirring, dipping an organic template into the powder slurry, and carrying out curing and degreasing treatment to obtain the titanium or titanium alloy powder.
4. The sintering method for preparing porous titanium by sintering titanium or titanium alloy powder according to claim 1, wherein the powder preparation mode in the step 1) is as follows: the titanium or titanium alloy powder is directly spread on the heating body.
5. The method for sintering titanium or titanium alloy powder according to claim 2, wherein the pore-forming agent is NaCl, sucrose, magnesium, urea, or starch.
6. The method for sintering titanium or titanium alloy powder according to claim 2, wherein the pressure at which the green body is prepared by the cold pressing or cold isostatic pressing process is between 0.1 and 1500 MPa; the pressure of the green blank prepared by the warm pressing process is 0.1-1500MPa, and the temperature is 50-500 ℃.
7. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the heater is made of silicon carbide, silicon nitride, alumina, graphite, tungsten, molybdenum, steel, copper, titanium or titanium alloy.
8. The method for preparing porous titanium by sintering titanium or titanium alloy powder according to claim 1, wherein in the step 2), the vacuum condition is as follows: degree of vacuum 10-2~10-5Pa, inert gas is: argon or helium, wherein the heating temperature of the heating body is 200-1500 ℃.
9. The method for sintering titanium or titanium alloy powder according to claim 1, wherein the electromagnetic field heating means is: microwave heating, induction heating, plasma heating or pulse heating; the heating temperature of the electromagnetic field is 600-1500 ℃, and the heat preservation time is 0.01-2400 minutes.
10. The method for sintering titanium or titanium alloy powder according to claim 2, wherein the green body is prepared on a pure titanium or titanium alloy heating body, the titanium or titanium alloy powder is mixed with a pore-forming agent and an organic binder to obtain a mixture, the pure titanium or titanium alloy heating body is placed at the bottom of the mold, the mixture is placed into the mold, and cold press molding is performed, wherein a molded body comprises the green body and the pure titanium or titanium alloy heating body.
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