CN107513642B - Co-based alloy powder and its preparation method and application - Google Patents
Co-based alloy powder and its preparation method and application Download PDFInfo
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- CN107513642B CN107513642B CN201710967273.7A CN201710967273A CN107513642B CN 107513642 B CN107513642 B CN 107513642B CN 201710967273 A CN201710967273 A CN 201710967273A CN 107513642 B CN107513642 B CN 107513642B
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- 239000000956 alloy Substances 0.000 title claims abstract description 129
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 96
- 239000000843 powder Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 53
- 239000010941 cobalt Substances 0.000 claims abstract description 53
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 43
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 40
- 239000011733 molybdenum Substances 0.000 claims abstract description 40
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 39
- 239000010937 tungsten Substances 0.000 claims abstract description 39
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 37
- 239000011651 chromium Substances 0.000 claims abstract description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 57
- 150000004706 metal oxides Chemical class 0.000 claims description 57
- 238000000889 atomisation Methods 0.000 claims description 49
- 238000010438 heat treatment Methods 0.000 claims description 38
- 238000010146 3D printing Methods 0.000 claims description 29
- 238000002844 melting Methods 0.000 claims description 24
- 230000008018 melting Effects 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 17
- 239000011159 matrix material Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 7
- 229910000531 Co alloy Inorganic materials 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 20
- 239000002245 particle Substances 0.000 abstract description 5
- 125000004122 cyclic group Chemical group 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 25
- 239000000155 melt Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 229910052573 porcelain Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- QBACCBHDCANWCQ-UHFFFAOYSA-N chromium cobalt molybdenum tungsten Chemical compound [Co][Cr][Mo][W] QBACCBHDCANWCQ-UHFFFAOYSA-N 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 125000003636 chemical group Chemical group 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910002064 alloy oxide Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003564 dental alloy Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000002320 enamel (paints) Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 208000037805 labour Diseases 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- B22F1/0003—
-
- 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
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
- B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- 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
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Abstract
The present invention relates to a kind of Co-based alloy powders and its preparation method and application, by weight percentage, the Co-based alloy powder is made of following chemical component: 22-32% chromium, 4-10% molybdenum, 4-10% tungsten, 0-1% silicon, 0-0.75% iron, 0-0.35% carbon, 0.05-0.2% nitrogen, surplus are cobalt.Good fluidity, the partial size of Co-based alloy powder of the present invention be small and centralized particle diameter, Co-base alloy material mechanical performance made from the Co-based alloy powder can reach 5 types/type5 of the requirement of GB17168/ISO 22674, and tensile strength reaches 1326MPa, nonproportional cyclic straining reaches 948MPa；Elasticity modulus reaches 206GPa, fracture elongation up to 13.8%.
Description
Technical field
The present invention relates to medical material tech field, more particularly to a kind of Co-based alloy powder and its preparation and method and
Using.
Background technique
With the extensive use of ceramometal restoration, the problem of more and more repairing failures, is displayed.A large amount of research knot
Fruit shows that ceramometal restoration collapses incidence highest of the porcelain in golden porcelain repairing failure, is primarily due in complicated oral environment
In, ceramometal restoration will receive the masticatory force of all directions, and good Metal-ceramic combining strength, alloy high strength are to prevent from repairing
Body collapses the basis of porcelain and the deformation of thin-walled tooth.Currently, the dental alloy such as preparation material ASTM F75 of dental prosthesis, stainless steel
Intensity is only capable of reaching 4 types/type4 of the requirement of GB17168/ISO 22674, when causing to be embedded in tooth body dental prosthesis deformation or
Dental prosthesis crackled glaze in person's use process.
In addition, using precinct laser fusion technology, i.e. metal three-dimensional printing technology, in aerospace, mold, personalized justice
Tooth and medical domain etc. have huge applications space.Especially in terms of manufacturing personalized dental prosthesis, precinct laser melting
Technology can satisfy the manufacture characteristics such as personalization, high-precision, the labyrinth of dental prosthesis；However, precinct laser melts skill
The research of art raw material is always the bottleneck promoted of the technology, precinct laser melting original material mainly based on dusty material,
It is required that dusty material has good mobility, chemical purity height etc..
Medical Cobalt-Based Alloys are to mainly contain the alloying elements such as cobalt, chromium, molybdenum using cobalt and chromium as the solid solution of basis；
The tissue of cobalt-base alloys is mainly made of austenitic matrix and carbide reinforced matrix.Medical Cobalt-Based Alloys are due to good
Corrosion resistance and golden porcelain associativity are widely used in artificial tooth in gear division reparation, bracket, various casting crowns, inlay and solid
Determine the manufacture of bridge.But that there are still alloy strengths is not high enough so as to cause repairing failure for Co-base alloy material in the prior art
The problem of.
Summary of the invention
Based on this, it is necessary to which for cobalt-base alloys in the prior art, that there are still alloy strengths is not high enough so as to cause reparation
The problem of failure, provide a kind of Co-based alloy powder.The Co-based alloy powder alloy strength is high.
To achieve the above object, specific technical solution is as follows:
A kind of Co-based alloy powder, by weight percentage, the Co-based alloy powder are made of following chemical component:
22-32% chromium, 4-10% molybdenum, 4-10% tungsten, 0-1% silicon, 0-0.75% iron, 0-0.35% carbon, 0.05-0.2%
Nitrogen, surplus are cobalt, wherein molybdenum is identical with the weight percent of tungsten in the Co-based alloy powder.
In wherein some embodiments, by weight percentage, the Co-based alloy powder is made of following chemical component:
22-28% chromium, 4.8-7.5% molybdenum, 4.8-7.5% tungsten, 0-1% silicon, 0-0.75% iron, 0-0.35% carbon, 0.05-
0.1% nitrogen, surplus are cobalt, wherein molybdenum is identical with the weight percent of tungsten in the Co-based alloy powder.
In wherein some embodiments, the partial size of the Co-based alloy powder is 10-63 μm.Co-based alloy powder partial size is
At 10-63 microns, which can be suitable for SLM (selective laser melting) technology 3D printing.
It is a further object of the present invention to provide the preparation methods of above-mentioned Co-based alloy powder.
A kind of preparation method of above-mentioned Co-based alloy powder, includes the following steps:
(1) raw metal of the Co-based alloy powder is taken, the raw metal is chromium, molybdenum, tungsten and cobalt, described in removal
The metal oxide layer on raw metal surface, the chromium that metal oxide layer must be removed, the molybdenum for removing metal oxide layer, removal metal oxidation
The tungsten of layer and the cobalt for removing metal oxide layer；
(2) smelting furnace is added as matrix in the 30-70wt% of the cobalt of the removal metal oxide layer, adds described go
Except the chromium of metal oxide layer, after heating melting, the molybdenum and tungsten for adding the removal metal oxide layer add after melting completely
Enter the cobalt of remaining removal metal oxide layer, completely after melting, heating obtains melt；
(3) using high pressure nitrogen as atomization gas, step (2) melt is sprayed into atomisation tower and is atomized, mist is obtained
Droplet after change；It keeps being full of nitrogen in atomisation tower in atomization process and keeps less than 1 atmosphere of pressure in atomisation tower
Pressure；
(4) droplet after atomization is cooling, it collects powder after cooling and carries out the pre-heat treatment to get the cobalt-base alloys
Powder.
In wherein some embodiments, the step (4) the pre-heat treatment includes: that the powder after cooling exists
1-12h is kept the temperature under conditions of 300-500 DEG C.When being atomized due to melt by high pressure nitrogen, the droplet after atomization can absorb nitrogen,
The part nitrogen and the droplet after atomization of absorption chemically react, and unreacted nitrogen still wraps up after atomization small
In drop, after cooling, still there is unreacted nitrogen in Co-based alloy powder, by the pre-heat treatment, makes unreacted nitrogen
Gas is further chemically reacted with chromium, so the method for warming up is most important for Co-based alloy powder fixed nitrogen,
Ductility and hardness after directly affecting Co-based alloy powder machine-shaping (such as: 3D printing technique).
It is 0.1- that the pressure in atomisation tower is kept in wherein some embodiments, in step (3) described atomization process
0.9MPa。
In wherein some embodiments, the penetrating pressure of high pressure nitrogen described in step (3) is 1-5MPa, in step (2)
The temperature of the melt is 1650-1700 DEG C.
It is yet another object of the invention to provide above-mentioned Co-based alloy powders to prepare the application in dental prosthesis.
It is yet another object of the invention to provide a kind of dental prosthesis.
A kind of dental prosthesis, preparing raw material includes above-mentioned Co-based alloy powder.
It is yet another object of the invention to provide the preparation methods of above-mentioned dental prosthesis.
A kind of preparation method of above-mentioned dental prosthesis, includes the following steps:
(1) 3D printing: 3D printing is carried out by raw material of above-mentioned cobalt billon powder, the condition of the 3D printing includes: sharp
Optical power is 50-180W, and scanning speed 80-400mm/s, sweep span 0.06-0.12mm obtain 3D printing dummy；
(2) it is heat-treated: step (1) the 3D printing dummy being placed in nitrogen atmosphere, in 800-1150 DEG C of condition
Lower heat preservation 1-2h, then it is air-cooled to room temperature, obtain the dental prosthesis.
In wherein some embodiments, the heat treatment are as follows: step (1) the 3D printing dummy is placed in nitrogen atmosphere
In, 1.5h is kept the temperature under the conditions of 1100 DEG C, then be air-cooled to room temperature, obtains dental prosthesis.
In the preparation process of above-mentioned dental prosthesis, 3D printing dummy is placed in nitrogen atmosphere, in 800-1150
1-2h is kept the temperature under the conditions of DEG C, then is air-cooled to room temperature, is heat-treated to dental prosthesis, for the mechanics of dental prosthesis
Performance is particularly significant, and aging temp is too low or excessively high, and all causing different phases, (there are two types of allotrope, Fcc and hcp's) for cobalt
Transformation causes dental prosthesis to occur splitting porcelain during subsequent upper porcelain, collapse phenomena such as porcelain, excessive high hardness, ductility are deteriorated, from
And the function of causing the alloy formula of this dental prosthesis to design cannot be effectively played；Secondly, the heat treatment method is into one
It can guarantee to step that nitrogen is sufficiently acted on chromium in dental prosthesis, prevents crisp phase constitution (the hcp phase or intermetallic of matrix cobalt
The σ brittlement phase of object) it generates, and stablize dental prosthesis ductility；In addition, the heat treatment method can make equivalent molybdenum and tungsten with
Cobalt is dissolved to form hardening constituent, to play the role of the thermal expansion coefficient of stable dental prosthesis；In addition, the heat treatment method can
Further be precipitated the molybdenum tungsten hardening constituent to be formed a small amount of, make the enhanced strength of dental prosthesis again will not hardness it is too high.
In the present invention, the effect for the chemical constituent that the Co-based alloy powder contains is as follows:
The chemical component cobalt contained in Co-based alloy powder of the present invention is basic metallic element, plays other conjunctions of solid solution
The effect of gold.
The chemical component chromium contained in Co-based alloy powder of the present invention, effect mainly enhance the corrosion resistance of alloy
And intensity, but excessive chromium can make alloy become fragile, ductility reduction.
The chemical component molybdenum contained in Co-based alloy powder of the present invention enhances the strong of alloy by acting synergistically with tungsten
Degree, hardness.
When the chemical component W content contained in Co-based alloy powder of the present invention is 4-10wt%, alloy oxidation is hindered
Film generates, and keeps alloy oxide film thinning, fine and close, enhancing cobalt-base alloys matrix and enamel coating gold porcelain binding force；Secondly, the weight hundred of tungsten
When content being divided to be greater than 4wt%, facilitate the linear expansion coefficient of stable alloy with the molybdenum synergistic effect of equal weight percent；By
After heat treatment, the tungsten of weight percent is waited to form second-phase strength phase with molybdenum, enhances the intensity of cobalt-base alloys matrix.
The chemical component nitrogen contained in Co-based alloy powder of the present invention, which can consume, easily makes matrix cobalt from the (modeling of Fcc phase
Property phase) the excessive chemical component chromium that changes to σ phase (brittlement phase), closed after processing Co-based alloy powder of the present invention
Golden material plasticity enhancing, hardness are unlikely to increase.
Compared with prior art, the invention has the following advantages:
Good fluidity, the partial size of Co-based alloy powder of the present invention be small and centralized particle diameter.Cobalt-based of the present invention
Co-base alloy material mechanical performance made from alloy powder can reach 5 types/type5 of the requirement of GB17168/ISO 22674, stretch
Intensity can reach 1326MPa, nonproportional cyclic straining can reach 948MPa；Elasticity modulus reaches 206GPa, fracture elongation can
Reach 13.8%.Inventor further improves the preparation method of Co-based alloy powder, by a large amount of creative labors
It was found that being added in two portions cobalt as matrix, the preparation method relative to conventional method during raw metal melting
(cobalt is once added), cobalt, which is added in two portions, can reduce cobalt loss as caused by gasification during melt-processed, further
Improve the mechanical performance of the Co-base alloy material of Co-based alloy powder preparation of the present invention in ground.
Specific embodiment
Of the invention is described in further detail below in conjunction with specific embodiment, but protection scope of the present invention is unlimited
In specific embodiment.
Embodiment 1
The dosage of the raw metal of 1 embodiment 1 of table
| Raw material | Cobalt | Chromium | Molybdenum | Tungsten |
| Dosage (wt%) | 62 | 28 | 5 | 5 |
The preparation method of the present embodiment Co-based alloy powder, includes the following steps:
(1) according to the dosage of table 1, chromium, molybdenum, tungsten and cobalt are taken, removes chromium, molybdenum, tungsten and the metal oxide layer on cobalt surface,
The chromium that metal oxide layer must be removed, the molybdenum for removing metal oxide layer, the tungsten for removing metal oxide layer and removal metal oxide layer
Cobalt；
(2) smelting furnace is added as matrix in the 35wt% of the cobalt of the removal metal oxide layer, adds the removal
The chromium of metal oxide layer, after heating melting, the molybdenum and tungsten for adding the removal metal oxide layer are added after melting completely
The cobalt of remaining removal metal oxide layer, completely after melting, heating obtains the melt that temperature is 1695 DEG C；
(3) using high pressure nitrogen as atomization gas, step (2) melt and high pressure nitrogen are sprayed into atomisation tower, high pressure
The penetrating pressure of nitrogen is 3.4MPa, and the melt is atomized under the action of high pressure nitrogen, it is atomized after droplet；
Keeping being full of nitrogen in atomisation tower and keeping the pressure in atomisation tower in atomization process is 0.85MPa；
(4) droplet after atomization is cooling, the powder that partial size is 10-63 μm after collection is cooling carries out the pre-heat treatment, i.e.,
Obtain Co-based alloy powder.Wherein, the pre-heat treatment condition are as follows: through 320 DEG C of heat preservation 8h.
Co-based alloy powder described in the present embodiment is processed using 3D printing technique, is included the following steps:
(1) 3D printing: Co-based alloy powder described in embodiment 1 is put into selective laser printer, and laser function is arranged
Rate 120W, 30 μm of powdering thickness, scanning speed 250mm/s, sweep span 0.06mm obtain 3D printing sample；
(2) it is heat-treated: step (1) the 3D printing sample being heat-treated together with substrate, the heat treatment includes
1.5h is kept the temperature under the conditions of 1100 DEG C in nitrogen atmosphere, then is air-cooled to room temperature, obtains the Co-base alloy material of the present embodiment, gained cobalt
The chemical composition of base alloy material is as shown in table 2.
The chemical composition of 2 embodiment of table, 1 Co-base alloy material
Embodiment 2
The dosage of the raw metal of 3 embodiment 2 of table
| Raw material | Cobalt | Chromium | Molybdenum | Tungsten |
| Dosage (wt%) | 57 | 27 | 8 | 8 |
Co-based alloy powder described in the present embodiment is processed using 3D printing technique, is included the following steps:
(1) according to the dosage of table 3, chromium, molybdenum, tungsten and cobalt are taken, removes chromium, molybdenum, tungsten and the metal oxide layer on cobalt surface,
The chromium that metal oxide layer must be removed, the molybdenum for removing metal oxide layer, the tungsten for removing metal oxide layer and removal metal oxide layer
Cobalt；
(2) smelting furnace is added as matrix in the 68wt% of the cobalt of the removal metal oxide layer, adds the removal
The chromium of metal oxide layer, after heating melting, the molybdenum and tungsten for adding the removal metal oxide layer are added after melting completely
The cobalt of remaining removal metal oxide layer, completely after melting, heating obtains the melt that temperature is 1660 DEG C；
(3) using high pressure nitrogen as atomization gas, step (2) melt and high pressure nitrogen are sprayed into atomisation tower, high pressure
The penetrating pressure of nitrogen is 4.5MPa, and the melt is atomized under the action of high pressure nitrogen, it is atomized after droplet；
Keeping being full of nitrogen in atomisation tower and keeping the pressure in atomisation tower in atomization process is 0.55MPa；
(4) droplet after atomization is cooling, the powder that partial size is 10-63 μm after collection is cooling carries out the pre-heat treatment, i.e.,
Obtain Co-based alloy powder.Wherein, the pre-heat treatment is through 480 DEG C of heat preservation 1.5h.
Co-based alloy powder described in the present embodiment is processed using 3D printing technique, is included the following steps:
(1) 3D printing: Co-based alloy powder described in the present embodiment is put into selective laser printer, and laser function is arranged
Rate 120W, 30 μm of powdering thickness, scanning speed 250mm/s, sweep span 0.06mm obtain 3D printing sample；
(2) it is heat-treated: step (1) the 3D printing sample being heat-treated with substrate, the heat treatment is included in nitrogen
Atmosphere keeps the temperature 2h under the conditions of 850 DEG C in enclosing, then is air-cooled to room temperature, obtains the Co-base alloy material of the present embodiment, gained cobalt-base alloys
The chemical composition of material is as shown in table 4.
The chemical composition of 4 embodiment of table, 2 Co-base alloy material
Embodiment 3
The dosage of the raw metal of 5 embodiment 3 of table
| Raw material | Cobalt | Chromium | Molybdenum | Tungsten |
| Dosage (wt%) | 58.2 | 23 | 9.4 | 9.4 |
Co-based alloy powder described in the present embodiment is processed using 3D printing technique, is included the following steps:
(1) according to the dosage of table 5, chromium, molybdenum, tungsten and cobalt are taken, removes chromium, molybdenum, tungsten and the metal oxide layer on cobalt surface,
The chromium that metal oxide layer must be removed, the molybdenum for removing metal oxide layer, the tungsten for removing metal oxide layer and removal metal oxide layer
Cobalt；
(2) smelting furnace is added as matrix in the 55wt% of the cobalt of the removal metal oxide layer, adds the removal
The chromium of metal oxide layer, after heating melting, the molybdenum and tungsten for adding the removal metal oxide layer are added after melting completely
The cobalt of remaining removal metal oxide layer, completely after melting, heating obtains the melt that temperature is 1680 DEG C；
(3) using high pressure nitrogen as atomization gas, step (2) melt and high pressure nitrogen are sprayed into atomisation tower, high pressure
The penetrating pressure of nitrogen is 1.5MPa, and the melt is atomized under the action of high pressure nitrogen, it is atomized after droplet；
Keeping being full of nitrogen in atomisation tower and keeping the pressure in atomisation tower in atomization process is 0.3MPa；
(4) droplet after atomization is cooling, the powder that partial size is 10-63 μm after collection is cooling carries out the pre-heat treatment, i.e.,
Obtain Co-based alloy powder.Wherein, the pre-heat treatment is through 450 DEG C of heat preservation 1.5h.
Co-based alloy powder described in the present embodiment is processed using 3D printing technique, is included the following steps:
(1) 3D printing: Co-based alloy powder described in the present embodiment is put into selective laser printer, and laser function is arranged
Rate 120W, 30 μm of powdering thickness, scanning speed 250mm/s, sweep span 0.06mm obtain 3D printing sample；
(2) it is heat-treated: step (1) the 3D printing sample being heat-treated with substrate, the heat treatment is included in nitrogen
Atmosphere keeps the temperature 1h under the conditions of 850 DEG C in enclosing, then is air-cooled to room temperature, obtains the Co-base alloy material of the present embodiment, gained cobalt-base alloys
The chemical composition of material is as shown in table 6.
The chemical composition of 6 embodiment of table, 3 Co-base alloy material
Embodiment 4
The dosage of the raw metal of 7 embodiment 4 of table
| Raw material | Cobalt | Chromium | Molybdenum | Tungsten |
| Dosage (wt%) | 61 | 31.0 | 4.0 | 4.0 |
The preparation method of the present embodiment Co-based alloy powder, includes the following steps:
(1) according to the dosage of table 7, chromium, molybdenum, tungsten and cobalt are taken, removes chromium, molybdenum, tungsten and the metal oxide layer on cobalt surface,
The chromium that metal oxide layer must be removed, the molybdenum for removing metal oxide layer, the tungsten for removing metal oxide layer and removal metal oxide layer
Cobalt；
(2) smelting furnace is added as matrix in the 35wt% of the cobalt of the removal metal oxide layer, adds the removal
The chromium of metal oxide layer, after heating melting, the molybdenum and tungsten for adding the removal metal oxide layer are added after melting completely
The cobalt of remaining removal metal oxide layer, completely after melting, heating obtains the melt that temperature is 1695 DEG C；
(3) using high pressure nitrogen as atomization gas, step (2) melt and high pressure nitrogen are sprayed into atomisation tower, high pressure
The penetrating pressure of nitrogen is 3.4MPa, and the melt is atomized under the action of high pressure nitrogen, it is atomized after droplet；
Keeping being full of nitrogen in atomisation tower and keeping the pressure in atomisation tower in atomization process is 0.85MPa；
(4) droplet after atomization is cooling, the powder that partial size is 10-63 μm after collection is cooling carries out the pre-heat treatment, i.e.,
Obtain Co-based alloy powder.Wherein, the pre-heat treatment is through 250 DEG C of heat preservation 8h.
The preparation method is the same as that of Example 1 for the Co-base alloy material of the present embodiment, the chemical group of Co-base alloy material obtained
Cheng Rubiao 8.
The chemical composition of 8 embodiment of table, 4 Co-base alloy material
Comparative example 1
The dosage of the raw metal of 9 comparative example 1 of table
| Raw material | Cobalt | Chromium | Molybdenum | Tungsten |
| Dosage (wt%) | 62 | 28 | 4 | 6 |
The preparation method is the same as that of Example 1 for the Co-based alloy powder of this comparative example.
The preparation method is the same as that of Example 1 for the Co-base alloy material of this comparative example, the chemical group of Co-base alloy material obtained
Cheng Rubiao 10.
The chemical composition of 10 comparative example of table, 1 Co-base alloy material
Comparative example 2
The dosage of the raw metal of 11 comparative example 2 of table
| Raw material | Cobalt | Chromium | Molybdenum | Tungsten |
| Dosage (wt%) | 62 | 28 | 5 | 5 |
The preparation method of this comparative example Co-based alloy powder, includes the following steps:
(1) according to the dosage of table 11, chromium, molybdenum, tungsten and cobalt, removal chromium, molybdenum, tungsten and the oxidation of the metal on cobalt surface are taken
Layer, the chromium that metal oxide layer must be removed, the molybdenum for removing metal oxide layer, the tungsten for removing metal oxide layer and removal metal oxidation
The cobalt of layer；
(2) smelting furnace is added as matrix in the cobalt of the removal metal oxide layer, adds the removal metal oxidation
The chromium of layer after heating melting, adds the molybdenum and tungsten of the removal metal oxide layer, after melting completely, heating, obtaining temperature is
1695 DEG C of melt；
(3) using high pressure nitrogen as atomization gas, step (2) melt and high pressure nitrogen are sprayed into atomisation tower, high pressure
The penetrating pressure of nitrogen is 3.4MPa, and the melt is atomized under the action of high pressure nitrogen, it is atomized after droplet；
Keeping being full of nitrogen in atomisation tower and keeping the pressure in atomisation tower in atomization process is 0.85MPa；
(4) droplet after atomization is cooling, the powder that partial size is 10-63 μm after collection is cooling carries out the pre-heat treatment, i.e.,
Obtain Co-based alloy powder.Wherein, the pre-heat treatment is through 320 DEG C of heat preservation 8h.
The preparation method is the same as that of Example 1 for the Co-base alloy material of this comparative example, the chemical group of Co-base alloy material obtained
Cheng Rubiao 12.
The chemical composition of 12 comparative example of table, 2 Co-base alloy material
5 Co-based alloy powder performance test of embodiment
Test purpose:
The performance of the Co-based alloy powder of embodiment 1-4 and comparative example 1 is tested.
Test result:
Co-based alloy powder performance test is as shown in table 13.
The performance test results of 13 Co-based alloy powder of table
Interpretation of result: as shown in Table 1, the Co-based alloy powder Hall flow velocity of embodiment 1-4 is in 17.5s/50g-28.6s/
In the range of 50g, therefore the Co-based alloy powder good fluidity of embodiment 1-4, in the Co-based alloy powder of comparative example 1 due to molybdenum and
The content of tungsten is not identical and difference is larger, and Hall flow velocity is 31.3s/50g, and the Co-based alloy powder mobility of comparative example 1 is opposite
It is poor in the cobalt-base alloys of embodiment 1-4；By the D50 numerical value of powder size distribution it is found that embodiment 1-4 Co-based alloy powder
D50 of the D50 slightly than 1 Co-based alloy powder of comparative example is small, therefore the Co-based alloy powder integral particle partial size of embodiment 1-4 is opposite
It is smaller in the partial size of comparative example 1 Co-based alloy powder entirety；In addition, by the result of (D90-D10)/D50 it is found that embodiment 1-4
Co-based alloy powder partial size it is more narrower than the particle diameter distribution of the Co-based alloy powder of comparative example 1.It follows that of the present invention
The good fluidity of cobalt-base alloys, partial size is small and centralized particle diameter.
6 Co-base alloy material performance test of embodiment
Test purpose:
The performance of the Co-base alloy material of embodiment 1-4 and comparative example 1-2 is tested.
Test result:
Co-base alloy material performance test is as shown in table 14.
14 Co-base alloy material the performance test results of table
Interpretation of result: as seen from the above table, the tensile strength of the Co-base alloy material of embodiment 1-4, nonproportional cyclic straining
Can respectively be up to 1173MPa, 506MPa or more, the especially tensile strength of the Co-base alloy material of embodiment 1 be 1326MPa,
206MPa；And the tensile strength and nonproportional cyclic straining of the Co-base alloy material of comparative example 1 respectively be only 887MPa,
468MPa, main cause are that the molybdenum that the Co-base alloy material of comparative example 1 contains and tungsten difference are larger, lead to the cobalt-based of comparative example 1
The more difficult formation hardening constituent of alloy material；The fracture elongation 9.5-13.8% of the Co-base alloy material of embodiment 1-4, hence it is evident that be greater than
The fracture elongation of comparative example 1 and comparative example 2 shows that the Co-base alloy material of embodiment 1-4 has good ductility；Implement
The elasticity modulus of example 1-4 is up to 190Gpa or more, bigger than the elasticity modulus of comparative example 1-2；The Co-base alloy material of comparative example 2 by
It is disposable addition cobalt in preparation process, causes the loss of cobalt in process to increase, to cause in comparative example 2
The overall mechanical properties of Co-base alloy material are deteriorated.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (9)
1. a kind of Co-based alloy powder, which is characterized in that by weight percentage, the Co-based alloy powder by following chemistry at
It is grouped as:
22.29-27.26% chromium, 5.02-9.82% molybdenum, 5.04-9.75% tungsten, 0.46-0.81% silicon, 0.23-0.32% iron,
0.0089-0.0096% carbon, 0.0784-0.1734% nitrogen, surplus are cobalt, wherein prepare the metal of the Co-based alloy powder
Molybdenum is identical with the weight percent of tungsten in raw material.
2. Co-based alloy powder according to claim 1, which is characterized in that the partial size of the Co-based alloy powder is 10-63 μ
m。
3. a kind of preparation method of the Co-based alloy powder as described in claim any one of 1-2, which is characterized in that including walking as follows
It is rapid:
(1) raw metal of the Co-based alloy powder is taken, the raw metal is chromium, molybdenum, tungsten and cobalt, removes the metal
The metal oxide layer on raw material surface, the chromium that must remove metal oxide layer, remove metal oxide layer at the molybdenum for removing metal oxide layer
Tungsten and the cobalt for removing metal oxide layer；
(2) smelting furnace is added as matrix in the 30-70wt% of the cobalt of the removal metal oxide layer, adds the removal gold
The chromium for belonging to oxide layer after heating melting, adds the molybdenum and tungsten of the removal metal oxide layer, after melting completely, is added surplus
The cobalt of remaining removal metal oxide layer, completely after melting, heating obtains melt；
(3) using high pressure nitrogen as atomization gas, step (2) melt is sprayed into atomisation tower and is atomized, after atomized
Droplet；It keeps being full of nitrogen in atomisation tower in atomization process and keeps less than 1 atmospheric pressure of pressure in atomisation tower；
(4) droplet after atomization is cooling, it collects powder after cooling and carries out the pre-heat treatment to get the cobalt-based alloy powder
End.
4. the preparation method of Co-based alloy powder according to claim 3, which is characterized in that step (4) described the pre-heat treatment
It include: that the powder after cooling is kept the temperature into 1-12h under conditions of 300-500 DEG C.
5. according to the preparation method of any one of the claim 3-4 Co-based alloy powder, which is characterized in that step (3) is described
It is 0.1-0.9MPa that the pressure in atomisation tower is kept in atomization process.
6. according to the preparation method of any one of the claim 3-4 Co-based alloy powder, which is characterized in that institute in step (3)
The penetrating pressure for stating high pressure nitrogen is 1-5MPa, and the temperature of melt described in step (2) is 1650-1700 DEG C.
7. a kind of dental prosthesis, which is characterized in that it includes any one of claim 1-2 cobalt-based alloy powder that it, which prepares raw material,
End.
8. a kind of preparation method of dental prosthesis as claimed in claim 7, which comprises the steps of:
(1) 3D printing: 3D printing is carried out by raw material of the described in any item Co-based alloy powders of claim 1-2, the 3D is beaten
The condition of print includes: that laser power is 50-180W, and scanning speed 80-400mm/s, sweep span 0.06-0.12mm are obtained
3D printing dummy；
(2) it is heat-treated: step (1) the 3D printing dummy being placed in nitrogen atmosphere, is protected under conditions of 800-1150 DEG C
Warm 1-2h, then it is air-cooled to room temperature, obtain the dental prosthesis.
9. the preparation method of dental prosthesis according to claim 8, which is characterized in that the heat treatment are as follows: by step (1)
The 3D printing dummy is placed in nitrogen atmosphere, is kept the temperature 1.5h under the conditions of 1100 DEG C, then be air-cooled to room temperature, is obtained dental prosthetic
Body.
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| EP3872202A4 (en) * | 2019-12-26 | 2022-04-06 | Mitsubishi Power, Ltd. | Cobalt-based alloy product |
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