CN116079051A - Preparation method of high-density titanium alloy fitting - Google Patents
Preparation method of high-density titanium alloy fitting Download PDFInfo
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- CN116079051A CN116079051A CN202211712084.2A CN202211712084A CN116079051A CN 116079051 A CN116079051 A CN 116079051A CN 202211712084 A CN202211712084 A CN 202211712084A CN 116079051 A CN116079051 A CN 116079051A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005238 degreasing Methods 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 150000003608 titanium Chemical class 0.000 claims abstract description 17
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 230000003197 catalytic effect Effects 0.000 claims abstract description 12
- 238000005498 polishing Methods 0.000 claims abstract description 12
- 238000000280 densification Methods 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 4
- 229920006324 polyoxymethylene Polymers 0.000 claims description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 9
- -1 Polyoxymethylene Polymers 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 7
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000001746 injection moulding Methods 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 2
- 239000000806 elastomer Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims 1
- 102220043159 rs587780996 Human genes 0.000 claims 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 210000001161 mammalian embryo Anatomy 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 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
- 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
- B22F3/005—Loading or unloading powder metal objects
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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
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
-
- 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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
-
- 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
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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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
- B22F3/24—After-treatment of workpieces or articles
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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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
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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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
- B22F3/1025—Removal of binder or filler not by heating only
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses a preparation method of a high-density titanium alloy fitting, which comprises the following steps: s1: selecting hydrogenated dehydrogenated titanium alloy powder with oxygen content of 0.1-0.15% and granularity of 10-50 μm for ball milling crushing and sphericizing; s2: feeding the hydrogenated and dehydrogenated titanium alloy particles obtained in the step S1; s3: injecting the feed obtained in the step S2 into a mould to obtain a green body; s4: carrying out catalytic degreasing on the green body obtained in the step S3 to obtain a degreased blank; s5: densification sintering is carried out on the degreasing blank obtained in the step S4, the sintering temperature is 1050-1150 ℃, the heat preservation is carried out for 3 hours, argon protection is adopted in the thermal degreasing stage, the air flow is 20-50 mL/min, and high vacuum sintering is adopted in the stage, so that a sintered part is obtained; s6: and carrying out mirror polishing treatment on the sintered part to obtain a final product.
Description
Technical Field
The invention relates to the technical field of metal fitting production, in particular to a preparation method of a high-density titanium alloy fitting.
Background
Titanium and titanium alloys are widely used in the fields of aviation, military industry, medical treatment, etc. because of their high strength, low density, excellent corrosion resistance and biocompatibility. With the rapid development of intelligent wearing equipment, the intelligent watch shell, the intelligent glasses frame and the like provide higher requirements on the appearance mirror polishing performance of the material and the light weight of the material. The titanium alloy is a better choice, and the titanium alloy is difficult to sinter to be fully compact, so that the mirror polishing of the titanium alloy can only achieve the matte effect, sand holes, fine scratches and the like on the surface of the titanium metal can not be completely eliminated, meanwhile, the processing cost is higher due to the poor processing performance of the titanium alloy, the powder price is high, and the application and popularization of the titanium alloy are further limited.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the preparation method of the high-density titanium alloy accessory is capable of reducing production cost and enabling the accessory to obtain a good polished mirror surface.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the high-density titanium alloy fitting comprises the following steps:
s1: selecting hydrogenated dehydrogenated titanium alloy powder with oxygen content of 0.1-0.15% and granularity of 10-50 μm for ball milling crushing and sphericizing;
s2: feeding the titanium alloy powder obtained in the step S1;
s3: injecting the feed obtained in the step S2 into a mould to obtain a green body;
s4: carrying out catalytic degreasing on the green body obtained in the step S3 to obtain a degreased blank;
s5: densification sintering is carried out on the degreasing blank obtained in the step S4, the sintering temperature is 1050-1150 ℃, the heat preservation is carried out for 3 hours, argon protection is adopted in the thermal degreasing stage, the air flow is 20-50 mL/min, and high vacuum sintering is adopted in the stage, so that a sintered part is obtained;
s6: and carrying out mirror polishing treatment on the sintered part to obtain a final product.
The invention has the beneficial effects that: the hydrogenation dehydrogenation titanium alloy powder is selected as the raw material, so that the development and production cost of the titanium alloy is obviously reduced by 30 percent; the hydrogenation dehydrogenation titanium alloy powder has higher activity, higher sintering densification degree and higher relative density of more than 99 percent, and the surface polishing degree of the polished titanium alloy fitting is good by improving the density of a sintered part.
Drawings
FIG. 1 is a diagram of a product produced by a method of producing a high density titanium alloy fitting of the present invention;
FIG. 2 is a microscopic view of the polished surface of a product produced by the method for producing a high density titanium alloy fitting of the present invention;
FIG. 3 is a microscopic view of the polished surface of the product prepared by the preparation method in the comparative example of the present invention.
Detailed Description
In order to describe the technical content, the achieved objects and effects of the present invention in detail, the following description is made with reference to the embodiments and the drawings.
The preparation method of the high-density titanium alloy fitting comprises the following steps:
s1: selecting hydrogenated dehydrogenated titanium alloy powder with oxygen content of 0.1-0.15% and granularity of 10-50 μm for ball milling crushing and sphericizing;
s2: feeding the titanium alloy powder obtained in the step S1;
s3: injecting the feed obtained in the step S2 into a mould to obtain a green body;
s4: carrying out catalytic degreasing on the green body obtained in the step S3 to obtain a degreased blank;
s5: densification sintering is carried out on the degreasing blank obtained in the step S4, the sintering temperature is 1050-1150 ℃, the heat preservation is carried out for 3 hours, argon protection is adopted in the thermal degreasing stage, the air flow is 20-50 mL/min, and high vacuum sintering is adopted in the stage, so that a sintered part is obtained;
s6: and carrying out mirror polishing treatment on the sintered part to obtain a final product. The working principle of the invention is as follows: the invention selects the hydrogenation dehydrogenation titanium alloy powder as the raw material to reduce the production cost, and processes such as powder injection molding, surface pretreatment, sintering and the like are carried out to break the oxide layer on the surface of the powder, so that the oxidation dehydrogenation titanium alloy is prepared
From the above description, the beneficial effects of the invention are as follows: the hydrogenation dehydrogenation titanium alloy powder is selected as the raw material, so that the development and production cost of the titanium alloy is obviously reduced by 30 percent; the hydrogenation dehydrogenation titanium alloy powder has higher activity, higher sintering densification degree and higher relative density of more than 99 percent, and the surface polishing degree of the polished titanium alloy fitting is good by improving the density of a sintered part.
Further, the specific operation of S1 is as follows: adding hydrogenated and dehydrogenated titanium alloy powder into a container, crushing and spheroidizing at 200-500 rpm for 8-15 hr, and introducing argon as protecting gas at 0.01-0.05MPa.
Preferably, crushing and sphericizing are carried out at a rotation speed of 400 rpm for 13 hours, argon is introduced as shielding gas, and the argon pressure is 0.03MPa.
Further, the feeding binder in the step S2 is at least one of Polyoxymethylene (POM), polyvinyl butyral (PVB), paraffin (PW), glycerol, polyethylene octene co-elastomer (POE) and dioctyl phthalate (DOP).
Preferably, the feed binder is polyoxymethylene.
Further, the feeding conditions of the S2 are as follows: the banburying temperature is 160-170 ℃ and the banburying time is 1h, the vacuum protection is carried out, and the feeding is taken out and crushed after the banburying is finished.
Preferably, the banburying temperature is 165 ℃, the banburying time is 1h, the vacuum protection is carried out, and the feed is taken out and crushed after the banburying is finished.
From the above description, the vacuum protection mode can prevent the titanium alloy from being oxidized in the honey refining process, and ensure the surface brightness of the titanium alloy product.
Further, the specific operation of S2 is as follows: preheating the powder to 175 ℃ and preserving heat for 30min, then adding polyformaldehyde, heating to 175 ℃, adding the rest feeding binder when the polyformaldehyde is completely melted, cooling to 170 ℃, and carrying out banburying for 30min.
From the above description, the polymerization degree of each component can be improved by the sectional banburying method, and the thermal stability is good, so that the sintered titanium alloy product has high density and high surface smoothness.
Further, the specific operation of S3 is as follows: the feed is injected into a mould, and the injection temperature is 170-185 ℃ and the injection pressure is 90-120 MPa during injection molding.
Further, the specific operation of S4 is as follows: degreasing temperature is 110-150 ℃, degreasing time is 8-12 h, and acid flux is 4.5-6.0 g/min.
Preferably, the specific operation of S4 is as follows: the degreasing temperature is 130 ℃, the degreasing time is 10 hours, and the acid flux is 6.0g/min.
Further, the green embryo in the step S4 is placed in an oxalic acid degreasing furnace for catalytic degreasing.
As is apparent from the above description, the conventional titanium alloy is generally degreased by a nitric acid degreasing method, and the oxalic acid degreasing method in the present invention can prevent the titanium alloy from reacting with nitric acid to affect the appearance and performance of the sintered part.
Example 1
The preparation method of the high-density titanium alloy fitting comprises the following steps:
s1: the hydrogenated and dehydrogenated titanium alloy powder with the oxygen content of 0.1-0.15% and the powder D50 particle diameter of 20 mu m is selected for ball milling and crushing and spheroidizing, specifically, the titanium alloy powder is added into a container for crushing and spheroidizing, the rotating speed is 500 r/min, the time is 8h, argon is introduced as protective gas, and the argon pressure is 0.04MPa.
S2: feeding the hydrogenated-dehydrogenated titanium alloy powder obtained in the step S1, wherein the feeding conditions are as follows: the banburying temperature is 160-170 ℃ and the banburying time is 1h, the vacuum protection is carried out, and the feeding is taken out and crushed after the banburying is finished; preferably, the feed binders are Polyoxymethylene (POM) and. Further, the hydrogenated and dehydrogenated titanium alloy powder was heated to 175℃and kept at that temperature for 30 minutes for preheating, followed by addition of a polymerFormaldehyde is heated to 175 ℃, polyvinyl butyral is added when the polyformaldehyde is completely melted, and the temperature is reduced to 170 ℃ for continuous banburying for 30min. Wherein the vacuum degree of the vacuumized air is 10 -(2～3) Pa。
S3: injecting the feed obtained in the step S2 into a die of a molding machine, wherein the injection temperature is 185 ℃ and the injection pressure is 110MPa during injection molding, so as to obtain a green body; in this step, the mold temperature at the time of injection should be 90℃to 120℃and the holding pressure 80MPa to 110MPa. Preferably, the mold temperature at the time of injection in this example is 110℃and the holding pressure is 100MPa.
S4: carrying out catalytic degreasing on the green body obtained in the step S3 to obtain a degreased blank; specifically, the green embryo is placed into an oxalic acid degreasing furnace for catalytic degreasing, argon protection is selected in a thermal degreasing stage, the degreasing temperature is 140 ℃, the total degreasing time is 10 hours, the catalytic degreasing is carried out in a sectional acid-introducing mode, and the acid-introducing amount of each stage is 4.5g/min, 5g/min and 5.5g/min respectively. The temperature of the thermal stripping stage is raised at a rate of 2-2.5 ℃/min.
S5: densification sintering is carried out on the degreasing blank obtained in the step S4, the sintering temperature is 1130 ℃, the heat preservation is carried out for 3 hours, the air flow is 40mL/min, and high vacuum sintering is adopted at the stage to obtain a sintered piece; wherein, the high vacuum refers to the vacuum degree of 10 -(2～3) Vacuum environment of Pa. The high temperature sintering stage is heated at a rate of 3-3.5 ℃/min.
S6: and carrying out mirror polishing treatment on the sintered part to obtain a final product.
Example two
The preparation method of the high-density titanium alloy fitting comprises the following steps:
s1: the hydrogenated and dehydrogenated titanium alloy powder with the oxygen content of 0.1-0.15% and the powder D50 particle diameter of 20 mu m is selected for ball milling and crushing and spheroidizing, specifically, the titanium alloy powder is added into a container for crushing and spheroidizing, the rotating speed is 500 r/min, the time is 8h, argon is introduced as protective gas, and the argon pressure is 0.04MPa.
S2: feeding the hydrogenated-dehydrogenated titanium alloy powder obtained in the step S1, wherein the feeding conditions are as follows: banburying at 160-170 deg.cThe time is 1h, vacuum protection is carried out, and the feed is taken out and crushed after banburying is finished; preferably, the feed binder is Polyoxymethylene (POM). Further, heating hydrogenated and dehydrogenated titanium alloy powder to 175 ℃ and preserving heat for 30min to preheat, then adding polyformaldehyde, heating to 175 ℃ at a speed of 3-3.5 ℃/min, adding polyvinyl butyral when the polyformaldehyde is completely melted, cooling to 170 ℃, and banburying for 30min. Wherein the vacuum degree of the vacuumized air is 10 -(2～3) Pa。
S3: injecting the feed obtained in the step S2 into a die of a molding machine, wherein the injection temperature is 170 ℃ and the injection pressure is 110MPa during injection molding, so as to obtain a green body; in this step, the mold temperature at the time of injection should be 90℃to 120℃and the holding pressure 80MPa to 110MPa.
S4: carrying out catalytic degreasing on the green body obtained in the step S3 to obtain a degreased blank; specifically, the green embryo is placed into an oxalic acid degreasing furnace for catalytic degreasing, argon protection is selected in a thermal degreasing stage, the degreasing temperature is 140 ℃, the degreasing time is 10 hours, the catalytic degreasing is carried out in a sectional acid-introducing mode, and the acid-introducing amount in each stage is 4g/min, 5g/min and 6g/min respectively. The temperature of the thermal stripping stage is raised at a rate of 2-2.5 ℃/min.
S5: densification sintering is carried out on the degreasing blank obtained in the step S4, the sintering temperature is 1150 ℃, the heat preservation is carried out for 3 hours, the air flow is 50mL/min, and high vacuum sintering is adopted at the stage to obtain a sintered piece; wherein, the high vacuum refers to the vacuum degree of 10 -(2～3) Vacuum environment of Pa. The high temperature sintering stage is heated at a rate of 3-3.5 ℃/min.
S6: and carrying out mirror polishing treatment on the sintered part to obtain a final product.
Comparative example: in contrast to the first and second embodiments, the aerosolized spherical powder was selected and no surface treatment was performed.
The performance test was performed on the first, second and comparative examples, and the results were as follows:
| powder cost (RMB/Kg) | Relative sintered density (%) | Sintered state | Polishing state | |
| Example 1 | 307 | 99.4 | Good quality | Good quality |
| Example two | 307 | 99.1 | Good quality | Good quality |
| Comparative example | 588 | 95.5 | Deformation of | Multiple holes |
In summary, the invention provides a method for preparing a high-density titanium alloy accessory, which comprises the steps of carrying out surface treatment on hydrogenated and dehydrogenated titanium alloy powder, reducing powder gaps, improving powder sintering activity, enabling a sintered piece to obtain high density, obtaining a surface compact layer, enabling the sintering density to be more than 99%, further enabling the sintered piece to obtain a mirror effect after polishing, and achieving high brightness.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent changes made in the specification and drawings of the present invention, or direct or indirect application in the relevant art, are included in the scope of the present invention.
Claims (8)
1. The preparation method of the high-density titanium alloy fitting is characterized by comprising the following steps of:
s1: selecting hydrogenated dehydrogenated titanium alloy powder with oxygen content of 0.1-0.15% and granularity of 10-50 μm for ball milling crushing and sphericizing;
s2: feeding the hydrogenated and dehydrogenated titanium alloy particles obtained in the step S1;
s3: injecting the feed obtained in the step S2 into a mould to obtain a green body;
s4: carrying out catalytic degreasing on the green body obtained in the step S3 to obtain a degreased blank;
s5: densification sintering is carried out on the degreasing blank obtained in the step S4, the sintering temperature is 1050-1150 ℃, the heat preservation is carried out for 3 hours, argon protection is adopted in the thermal degreasing stage, the air flow is 20-50 mL/min, and high vacuum sintering is adopted in the stage, so that a sintered part is obtained;
s6: and carrying out mirror polishing treatment on the sintered part to obtain a final product.
2. The method for manufacturing a high-density titanium alloy fitting according to claim 1, wherein the specific operation of S1 is: adding the hydrogenated and dehydrogenated titanium alloy powder into a container, crushing and spheroidizing, wherein the rotating speed is 200-500 rpm, the time is 8-15h, and argon is introduced as a protective gas, the argon pressure is 0.01-0.05MPa, and the hydrogenated and dehydrogenated titanium alloy powder D50=20-50 μm.
3. The method for manufacturing a high-density titanium alloy fitting according to claim 1, wherein the feeding binder in S2 is at least one of Polyoxymethylene (POM), polyvinyl butyral (PVB), paraffin Wax (PW), glycerin, polyethylene octene co-elastomer (POE) and dioctyl phthalate (DOP).
4. The method for manufacturing a high density titanium alloy fitting according to claim 1, wherein the feeding conditions of S2 are: the banburying temperature is 160-170 ℃ and the banburying time is 1h, the vacuum protection is carried out, and the feeding is taken out and crushed after the banburying is finished.
5. A method for producing a high-density titanium alloy fitting according to claim 3, wherein the specific operation of S2 is: preheating hydrogenated and dehydrogenated titanium alloy powder to 175 ℃ and preserving heat for 30min, then adding polyformaldehyde, heating to 175 ℃, adding the rest feeding binder when the polyformaldehyde is completely melted, cooling to 170 ℃, and continuing banburying for 30min.
6. The method for manufacturing a high-density titanium alloy fitting according to claim 1, wherein the specific operation of S3 is: the feed is injected into a mould, and the injection temperature is 170-185 ℃ and the injection pressure is 90-120 MPa during injection molding.
7. The method for manufacturing a high-density titanium alloy fitting according to claim 1, wherein the specific operation of S4 is: degreasing temperature is 110-150 ℃, degreasing time is 8-12 h, and acid flux is 4.5-6.0 g/min.
8. The method for manufacturing a high-density titanium alloy fitting according to claim 1, wherein the green body in S4 is placed in an oxalic acid degreasing furnace for catalytic degreasing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211712084.2A CN116079051A (en) | 2022-12-29 | 2022-12-29 | Preparation method of high-density titanium alloy fitting |
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| CN106475914A (en) * | 2016-10-31 | 2017-03-08 | 南京航空航天大学 | A kind of titanium alloy surface amino film plastics abrasive air Jet Polishing method |
| CN106566472A (en) * | 2016-10-31 | 2017-04-19 | 常州乔尔塑料有限公司 | Preparation method and purpose of amino molding compound abrasive for abrasive air jet finishing |
| CN113319280A (en) * | 2021-04-14 | 2021-08-31 | 济南大学 | Metal powder injection molding MIM production process of novel titanium and titanium alloy material |
| CN114769591A (en) * | 2022-04-15 | 2022-07-22 | 北京科技大学 | Sintering method of high-strength high-plasticity powder titanium alloy |
| CN114985743A (en) * | 2022-04-26 | 2022-09-02 | 北京科技大学 | Titanium powder for powder injection molding and preparation method and product thereof |
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| CN106475914A (en) * | 2016-10-31 | 2017-03-08 | 南京航空航天大学 | A kind of titanium alloy surface amino film plastics abrasive air Jet Polishing method |
| CN106566472A (en) * | 2016-10-31 | 2017-04-19 | 常州乔尔塑料有限公司 | Preparation method and purpose of amino molding compound abrasive for abrasive air jet finishing |
| CN113319280A (en) * | 2021-04-14 | 2021-08-31 | 济南大学 | Metal powder injection molding MIM production process of novel titanium and titanium alloy material |
| CN114769591A (en) * | 2022-04-15 | 2022-07-22 | 北京科技大学 | Sintering method of high-strength high-plasticity powder titanium alloy |
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