CN110331394A - A kind of method of cold spraying increasing material manufacturing bio-medical Ti-Ta composite material - Google Patents
A kind of method of cold spraying increasing material manufacturing bio-medical Ti-Ta composite material Download PDFInfo
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- CN110331394A CN110331394A CN201910673087.1A CN201910673087A CN110331394A CN 110331394 A CN110331394 A CN 110331394A CN 201910673087 A CN201910673087 A CN 201910673087A CN 110331394 A CN110331394 A CN 110331394A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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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
- C23C24/087—Coating with metal alloys or metal elements only
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- Materials For Medical Uses (AREA)
Abstract
The invention belongs to cold spraying material increasing fields, and in particular to a kind of method of cold spraying increasing material manufacturing bio-medical Ti-Ta composite material.First micron order Ta powder is made into mixed-powder with Ti powder according to a certain percentage and is uniformly mixed with mixed powder equipment；Cold air power spraying and coating equipment is used again, it is using metal material De Laval spray gun, the mixed-powder of preparation is spray deposited on Ti substrate under certain condition, Ti-Ta composite deposition object is formed, and it is removed from Ti substrate, obtains Ti-Ta composite material.The method of the present invention can prepare the high-strength low mould body implanting material of bio-medical, the Viability of prosthetic replacement operation will be improved, biocompatibility after improving Using prosthesis human body (there is no the releases of harmful element), and (elasticity modulus is low for mechanical compatibility, reduce stress shielding effect), be able to solve prepare high temperature required for tantalum at present and the problems such as bring harsh conditions.
Description
Technical field
The invention belongs to cold spraying material increasing fields, and in particular to a kind of cold spraying increasing material manufacturing bio-medical Ti-Ta
The method of composite material.
Background technique
Currently, titanium and its alloy have many advantages, such as that density is low, specific strength is high, good corrosion resistance, good biocompatibility, recognized
To be important biomaterial.But titanium (110GPa), compared with body bone tissue (4~30GPa), elasticity modulus is high, it may
It will lead to planting material and surrounding natural bone mismatch, i.e., so-called stress shielding effect, to hinder answering extensively for titanium alloy
With.In addition, human body fluid environment complicated under blood, protein and action of mechanical pressure can promote releasing for alloying elements
It puts, such as: V, Ni, Al may cause allergic reaction and serious chronic health problems.Therefore, do not have cytotoxic alloy
Element is developed, to overcome above-mentioned restricted problem.Tantalum (Ta), niobium (Nb), zirconium (Zr) and its alloy are quickly becoming mostly
The tempting selection of number biomedical applications.
Wherein, tantalum is one of most promising metallic biomaterial, and inside and outside biocompatibility is even better than titanium, and has
There is good corrosion resistance.Therefore, tantalum has been applied to bone graft substitute, operation suture thread, hip joint, knee joint et al.
The fields such as work joint replacement.About the preparation of tantalum and tantalum-base alloy, there are many reports, have good biomedical applications
Prospect.But the shortcomings that tantalum is also apparent from: (1) fusing point is high (3000 DEG C)；(2) very dense (16.65g/cm3)；(3) raw material
It is at high cost；(4) there is very strong affinity to oxygen.Due to disadvantages mentioned above, tantalum is not considered for block planting material.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, should
Method can prepare the high-strength low mould body implanting material of bio-medical, will improve the Viability of prosthetic replacement operation, improve prosthese
(elasticity modulus is low, and reduction is answered for biocompatibility (there is no the releases of harmful element) and mechanical compatibility after being implanted into human body
Power screen effect), be able to solve prepare high temperature required for tantalum at present and the problems such as bring harsh conditions.
Technical scheme is as follows:
A kind of method of cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, comprising the following steps:
(1) by micron order Ta powder and Ti powder according to atomic ratio 1:(1~20) it is made into mixed-powder, and mixed with mixed powder equipment
Uniformly；
(2) cold air power spraying and coating equipment is used, the mixed-powder of preparation is spray deposited on Ti substrate, form Ti-Ta
Composite sedimentary layer, and it is removed from Ti substrate, obtain Ti-Ta composite material.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, in step (1), the pattern of Ta powder
For spherical or irregular pattern, particle size range is 10~60 μm.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, in step (1), the pattern of Ti powder
For spherical or irregular pattern, particle size range is 10~60 μm.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, in step (2), cold air powered spray
Painting uses compressed air as working gas, and 200~600 DEG C of temperature, 1.5~2.5MPa of pressure, 10~40mm of spray distance,
Ti-Ta composite sedimentary layer with a thickness of 5mm or more.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material is right before spraying in step (2)
Ti substrate carries out coarse sand blasting treatment.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, in step (2) deposition process, spray
Powder is smooth out for a long time for rifle, unplugged.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material in step (2), deposits
Ti-Ta composite material, Ta are evenly distributed with Ti two-phase.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, as needed to Ti-Ta composite wood
Material is post-processed.
The method of the cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, in step (3), post-processing is true
Sky heat treatment, vacuum heat treatment temperature are 750~1500 DEG C, and soaking time is 1~10 hour.
Design philosophy of the invention is:
Studies have shown that tantalum can show bioactivity more superior than titanium and bio-compatible in people's bone prosthesis
Property, it is medically highly desirable biocompatible material.But tantalum is but because of the expensive and high fusing point of itself
(nearly 3000 DEG C), and oxygen affinity is stronger, so that it is become difficult by conventional machining.In order to solve this problem, cold spraying
Undoubtedly become the optimal selection for preparing tantalum and its composite material far below the technical characteristic of material melting point with its operating temperature.Cold spray
Being coated with high pressure gas is power, and the material solid state deposition under low-temperature condition may be implemented, small on the influence of materials microstructure structure, is sunk
Product is high-efficient, and there are compression in lithosomic body, can be used for increasing material manufacturing block materials.
The invention has the advantages and beneficial effects that:
1. being the β phase stable element of Ti using Ta of the present invention, the elasticity modulus of β-Ti is lower, and springform can be effectively reduced in this
Amount is allowed to be adapted with body bone tissue.
2. being infinitely dissolved therebetween using Ta of the present invention and Ti, intermetallic compound is not present therebetween.
3. use Ta of the present invention can significantly improve Ti alloy strength, to bear external force, to extend the use longevity of material
Life.
4. there is good inside and outside biocompatibility using Ta of the present invention.
5. can have certain porosity in the Ti-Ta composite material of cold spraying increasing material manufacturing of the present invention, this can equally be dropped
The elasticity modulus of low planting body reduces stress shielding effect, and the presence of hole has the biological fixation conducive to osteocyte.
The advantages of 6. the method for the present invention combination biocompatibility is high, good mechanical performance, it is intended to explore a kind of new clinic
Application material.
Detailed description of the invention
Fig. 1 be spray state Ti-50Ta (atomic ratio) composite material (a) cross-sectional scans electromicroscopic photograph and enlarged drawing, (b) three
Stress-displacement curve of point bend test.
Fig. 2 is (a) cross-sectional scans Electronic Speculum of Ti-50Ta (atomic ratio) composite material after 1000 DEG C of+2h vacuum heat treatments
Photo and enlarged drawing, (b) stress-displacement curve of three point bending test.
Fig. 3 be spray state Ti-25Ta (atomic ratio) composite material (a) cross-sectional scans electromicroscopic photograph and enlarged drawing, (b) three
Stress-displacement curve of point bend test.
Fig. 4 is that (a) cross-sectional scans Electronic Speculum of Ti-25Ta (atomic ratio) composite material after 900 DEG C of+5h vacuum heat treatments is shone
Piece and enlarged drawing, (b) stress-displacement curve of three point bending test.
Specific embodiment
In the specific implementation process, the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material of the present invention, first
Micron order Ta powder is made into mixed-powder with Ti powder according to a certain percentage and is uniformly mixed with mixed powder equipment；Again using cold air powered
Spraying equipment, it is using metal material De Laval spray gun, the mixed-powder of preparation is spray deposited to Ti base under certain condition
On plate, Ti-Ta composite deposition object is formed, and it is removed from Ti substrate, obtain Ti-Ta composite material.It finally can also be right
This Ti-Ta composite material carries out a degree of post-processing, such as heat treatment.Specific step is as follows for this method:
Step 1 mixes powder: micron order Ta powder being made into mixed-powder with Ti powder according to a certain percentage and is mixed with mixed powder equipment
Uniformly.
Wherein, 10~60 μm of the particle size range of Ta powder, the particle size range of Ti powder are 10~60 μm, two kinds of powder morphologies
Think spherical or irregular pattern.
Step 2 spraying: using cold air power spraying and coating equipment, arrives the mixed-powder of preparation is spray deposited under certain condition
On Ti substrate, Ti-Ta composite deposition object is formed, and it is removed from Ti substrate, obtain Ti-Ta composite material.Cold spraying is set
Standby operating condition is 200~600 DEG C of temperature, 1.5~2.5MPa of pressure, 10~40mm of spray distance, and compressed air is selected to make
For blasting medium.Ti substrate needs to carry out coarse sand blasting treatment before spraying.
Wherein, cold spray apparatus refer to Chinese invention patent (patent No.: 01128130.8, Authorization Notice No.:
CN1161188C a kind of cold air driven spray painter) mentioned or other commercial cold spraying, dynamic spraying or low pressure cold sprayings are set
It is standby.Spray gun uses metal material De Laval spray gun, and powder is smooth out for a long time for spray gun in deposition process, unplugged.Deposition obtains
Ti-Ta composite material, Ta is evenly distributed with Ti two-phase.
Step 3 post-processing: a degree of post-processing can also be finally carried out to this Ti-Ta composite material, is such as heat-treated
Etc..Wherein, post-processing can be vacuum heat treatment, and temperature is 750~1500 DEG C (preferably 800~1000 DEG C), heat preservation
Time is 1~10 hour (preferably 3~6 hours).
The present invention is described in detail with reference to the accompanying drawings and embodiments, is implemented under premised on inventive technique scheme, is provided
Detailed embodiment and specific operation process, but protection scope of the present invention is not limited to the following examples.
Embodiment 1
In the present embodiment, by 10~60 μm of granularity of spherical Ta powder and 10~60 μm of granularity of irregular Ti powder in mixed powder
It is mixed 8 hours in equipment.Wherein, the atomic ratio of Ta powder is 50%, and reduced mass score is about 79%.Cold spraying operation temperature
Being 450 DEG C, operating pressure 2.0MPa, spray distance 20mm selects compressed air as blasting medium.Substrate selects technical pure Ti
Plate, the Ti-Ta thickness of composite material about 5mm deposited on it are thick.
As shown in Figure 1a, from prepared Ti-Ta composite material cross-sectional scans electromicroscopic photograph, it can be seen that Ti, Ta
Two-phase is uniformly distributed, and is consistent substantially with the ratio in raw material powder, and there are a small amount of holes, about 0.35% for material internal.
As shown in Figure 1 b, three point bending test can be calculated spraying state Ti-Ta composite material bending elastic modulus be about
20.9GPa, bending strength reach 144.3MPa, extremely similar to people's bone.
Embodiment 2
In the present embodiment, by the Ti-Ta composite material in embodiment 1 through vacuum heat treatment, heat treatment temperature is 1000 DEG C,
Soaking time is 2 hours, then furnace cooling.As shown in Figure 2 a, it is shone from prepared Ti-Ta composite material cross-sectional scans Electronic Speculum
Piece observation, it can be seen that Ti, Ta two-phase are thermally treated, occur obvious diffusion region therebetween, and are endless perfect diffusion, in material
Also there is the kirkendall hole generated due to counterdiffusion in portion, and about 2.11%.As shown in Figure 2 b, three point bending test can be with
The bending elastic modulus that Ti-Ta composite material after being heat-treated is calculated is about 53.6GPa, and bending strength reaches 610.5MPa,
Although elasticity modulus is risen after heat treatment, but it is maintained at a lower level, and the strength of materials improves 4 times.
Embodiment 3
In the present embodiment, by 30~40 μm of granularity of spherical Ta powder and 30~40 μm of granularity of irregular Ti powder in mixed powder
It is mixed 8 hours in equipment.Wherein, the atomic ratio of Ta powder is 25%, and reduced mass score is about 55.7%.Cold spraying operation temperature
Degree selects compressed air as blasting medium for 450 DEG C, operating pressure 2.5MPa, spray distance 20mm.Substrate selects technical pure
Ti plate, the Ti-Ta thickness of composite material about 7mm deposited on it are thick.
As shown in Figure 3a, from prepared Ti-Ta composite material cross-sectional scans electromicroscopic photograph, it can be seen that Ti, Ta
Two-phase is uniformly distributed, and is consistent substantially with the ratio in raw material powder, and there are a small amount of holes, about 0.48% for material internal.
As shown in Figure 3b, three point bending test can be calculated spraying state Ti-Ta composite material bending elastic modulus be about
33.4GPa, bending strength reach 186.9MPa, extremely similar to people's bone.
Embodiment 4
In the present embodiment, by the Ti-Ta composite material in embodiment 3 through vacuum heat treatment, heat treatment temperature is 900 DEG C,
Soaking time is 5 hours, then furnace cooling.As shown in fig. 4 a, it is shone from prepared Ti-Ta composite material cross-sectional scans Electronic Speculum
Piece observation, it can be seen that Ti, Ta two-phase are thermally treated, occur obvious diffusion region therebetween, and are endless perfect diffusion, in material
Also there are a large amount of kirkendall holes generated due to counterdiffusion in portion, and about 3.94%.As shown in Figure 4 b, three point bending test
The bending elastic modulus that Ti-Ta composite material after being heat-treated can be calculated is about 35.9GPa, and bending strength reaches
508.5MPa, elasticity modulus is held essentially constant after heat treatment, and the strength of materials improves nearly 3 times.
Embodiment the result shows that, the method for the present invention is easy to operate, save the cost, without the harsh conditions such as high temperature, high pressure, also
Without using He or N2The expensive gases such as gas only can be achieved with cold spraying using compressed air under intermediate-temperaande ande medium-pressure condition and increase material system
Ti-Ta composite material is made, the Ti-Ta composite material prepared, two-phase is evenly distributed, and functional.
Claims (9)
1. a kind of method of cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, which comprises the following steps:
(1) by micron order Ta powder and Ti powder according to atomic ratio 1:(1~20) it is made into mixed-powder, and mixed with mixed powder equipment
It is even；
(2) cold air power spraying and coating equipment is used, the mixed-powder of preparation is spray deposited on Ti substrate, it is compound to form Ti-Ta
Sedimentary, and it is removed from Ti substrate, obtain Ti-Ta composite material.
2. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In in step (1), the pattern of Ta powder is spherical or irregular pattern, and particle size range is 10~60 μm.
3. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In in step (1), the pattern of Ti powder is spherical or irregular pattern, and particle size range is 10~60 μm.
4. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In, in step (2), cold air power spraying and coating uses compressed air as working gas, and 200~600 DEG C of temperature, pressure 1.5~
2.5MPa, spray distance 10~40mm, Ti-Ta composite sedimentary layer with a thickness of 5mm or more.
5. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In in step (2), to the progress coarse sand blasting treatment of Ti substrate before spraying.
6. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In in step (2) deposition process, powder is smooth out for a long time for spray gun, unplugged.
7. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In in step (2), the Ti-Ta composite material deposited, Ta is evenly distributed with Ti two-phase.
8. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material described in accordance with the claim 1, feature exist
In being post-processed as needed to Ti-Ta composite material.
9. the method for cold spraying increasing material manufacturing bio-medical Ti-Ta composite material, feature exist according to claim 8
In in step (3), post-processing as vacuum heat treatment, vacuum heat treatment temperature is 750~1500 DEG C, and soaking time is 1~10 small
When.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112809007A (en) * | 2019-11-15 | 2021-05-18 | 沈阳工业大学 | Method for preparing titanium alloy and nickel-based superalloy functionally gradient material |
| CN114871445A (en) * | 2022-05-12 | 2022-08-09 | 西安交通大学 | Method for manufacturing nano-structure copper-based bimetal composite material through cold spraying solid additive |
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| CN106735280A (en) * | 2016-11-23 | 2017-05-31 | 西北有色金属研究院 | A kind of preparation method of spherical TiTa alloy powders |
| CN108728844A (en) * | 2018-07-25 | 2018-11-02 | 中国兵器科学研究院宁波分院 | A kind of cold spraying preparation method of medical bio coating |
| US20190084048A1 (en) * | 2017-09-18 | 2019-03-21 | Tosoh Smd, Inc. | Titanium-tantalum powders for additive manufacturing |
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2019
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| CN104342583A (en) * | 2014-09-25 | 2015-02-11 | 中南大学 | Ti-Ta alloy as well as preparation method and application thereof |
| CN106735280A (en) * | 2016-11-23 | 2017-05-31 | 西北有色金属研究院 | A kind of preparation method of spherical TiTa alloy powders |
| US20190084048A1 (en) * | 2017-09-18 | 2019-03-21 | Tosoh Smd, Inc. | Titanium-tantalum powders for additive manufacturing |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112809007A (en) * | 2019-11-15 | 2021-05-18 | 沈阳工业大学 | Method for preparing titanium alloy and nickel-based superalloy functionally gradient material |
| CN114871445A (en) * | 2022-05-12 | 2022-08-09 | 西安交通大学 | Method for manufacturing nano-structure copper-based bimetal composite material through cold spraying solid additive |
| CN114871445B (en) * | 2022-05-12 | 2023-08-18 | 西安交通大学 | Method for manufacturing nano-structure copper-based bimetal composite material by cold spraying solid-state additive |
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Application publication date: 20191015 |