CN101285136A - Preparation method for porous titanium and porous titanium alloy - Google Patents
Preparation method for porous titanium and porous titanium alloy Download PDFInfo
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- CN101285136A CN101285136A CNA2008100181995A CN200810018199A CN101285136A CN 101285136 A CN101285136 A CN 101285136A CN A2008100181995 A CNA2008100181995 A CN A2008100181995A CN 200810018199 A CN200810018199 A CN 200810018199A CN 101285136 A CN101285136 A CN 101285136A
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Abstract
The invention relates to a method for preparing porous titanium and tporous titanium alloy, which is characterized in that the preparing steps are as follows: Ti powder or Ti alloy powder is baked in an oven; grit-blasting coursing pretreatment is performed on the surface of a flat shape matrix or the surface of a club-shaped matrix; the cold spraying method is used to spray the prepared Ti powder or the Ti alloy powder on the matrix; and then a coating layer gained in step three is put in a vacuum heat treatment furnace for heat treatment. The invention has the characteristics of simple technology, short production cycle and low cost. The porosity of the porous titanium and the porous titanium alloy prepared by the method is distributed evenly with good controllability. The porosity of the porous titanium and the porous titanium alloy prepared by the method can be changed in the range of between 5 and 50 percent, and the intensity can be changed in the range between 30 and 75 MPa according to the porosity. The controllability of the method is good and the production efficiency is high, which is favorable for industrialization.
Description
Technical field
The present invention relates to the preparation method of a kind of POROUS TITANIUM and porous titanium alloy, adopt the cold spraying forming technique, cooperate vacuum heat treatment to obtain required porous material.Mainly be applicable to biomaterial, also can be used for structured material in particular cases.
Background technology
Metal foam or metal polyporous material are a kind of physical function that develops rapidly in the world in the later stage eighties and structure-integrated new engineering material.It is a kind ofly to have good penetrability, hole and controllable aperture, dimensionally stable, high temperature resistant, anti-thermal shock, the functional materials of property such as can regenerate, can process.Metal polyporous material is widely used in the technologies such as the filtration, separation, noise reduction, gas distribution, catalysis, heat exchange of industries such as Aeronautics and Astronautics, nuclear power, petrochemical industry, metallurgy, machinery, medicine, environmental protection.In recent years, each field has promoted its development greatly to the demand of metal polyporous material.On the other hand, titanium and titanium alloy are used widely in fields such as aerospace, biologies because of characteristics such as its excellent corrosion resisting performance, high specific tenacity, excellent biocompatibility.In its biologic applications, the preparation of POROUS TITANIUM and titanium alloy is the key issue that needs solve, and wherein also relates to the important indicator of porous material quality good or not: the homogeneity of bore hole size and shape.Present existing POROUS TITANIUM preparation method mainly contains: sintering process and hot spray process.Sintering process mainly is to pile up titanium ball, short titanium fiber, titanium net or TiH on titanium or titanium alloy substrate
2Carry out sintering (U.S. Pat 4206516, Chinese patent 03810032.0), but the POROUS TITANIUM and the matrix bond of this method preparation are relatively poor, the titanium fiber easily comes off.Hot spray process is mainly used in the preparation porous titanium coating.U.S. Pat 3605123 had been reported plasma spraying TiH in 1971
2The preparation porous titanium coating, but the porous nickel of gained coating is relatively poor.U.S. Pat 4542539 usefulness flame platings in 1985 have prepared gradient porous titanium coating, but anchoring strength of coating is low, only 7MPa.Japan Kobe Steel company adopts vacuum plasma spray coating to prepare the porous titanium coating of porosity 40～60%, Young's modulus 4.7GPa, compressive strength 85MPa.Sulzer Calcitek company successfully is applied to tooth implant with the porous titanium coating of vacuum plasma spray coating preparation, and obtains the FDA authentication in 1997, comes into the market.But the vacuum plasma spray coating apparatus expensive, and still there are porous nickel and the connective relatively poor problem of perforate.Nearest [the W.-Y.Li that studies show that, et al., Ti and Ti-6Al-4V coatings by cold spraying and microstructure modification by heattreatment, Advanced Engineering Materials, 2007,9 (5), 418-423], cold spraying can be used for preparing Ti and Ti alloy coat, and coatings prepared shows higher void content; After the prepared coating thermal treatment, coating and high base strength are improved.But these preliminary researchs only relate to than shallow layer preparation, and the performance of prepared coating own is not characterized, and spraying coating process and thermal treatment process are single, lack systemic.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes the preparation method of a kind of POROUS TITANIUM and porous titanium alloy, and the POROUS TITANIUM of this method preparation is even with the titanium alloy distribution of porosity, controllability is better, and equipment, technology are simple, with short production cycle, low production cost.
Technical scheme
Basic thought of the present invention is: at first the cold spraying shaping prepares titanium or titanium alloy coat on matrix, carries out vacuum heat treatment then, and the one, increase the bonding strength between deposited particles, the 2nd, improve hole and distribution thereof.
The preparation method of a kind of POROUS TITANIUM and porous titanium alloy is characterized in that preparation process is as follows:
Step 1:, in 80～100 ℃ baking oven, toasted 1～4 hour with the Ti powder or the Ti powdered alloy of size range at 5～200 μ m;
Step 2: tabular matrix surface or bar-shaped matrix surface are carried out sandblast alligatoring pre-treatment;
Step 3: adopt cold spray-coating method to spray Ti powder or the Ti powdered alloy of preparing in the step 1 on above-mentioned matrix, powder sending quantity is during spraying: 10～100g/min; Coat thickness is: 100 μ m～50mm;
Step 4: the coat that step 3 is obtained places in the vacuum heat treatment furnace heat-treats, and vacuum degree in vacuum chamber requires less than 10
-3Pa; Holding temperature is at 600～900 ℃; Soaking time was at 1～8 hour.
When matrix need be peeled off, matrix should be peeled off before the thermal treatment of step 4.
The selection principle of the powder size of described Ti powder or Ti powdered alloy is: select the powder of granularity 5～100 μ m less than 20%～40% the time when requiring to spray porosity after finishing; When requiring to spray hole after finishing greater than 40% the time, select the powder of 100～200 μ m.
Described sandblast pretreatment is adopted-24 purpose sand grains for titanium or titanium alloy substrate; Matrix adopting-100 purpose the sand grains of peeling off for need.
Beneficial effect
The POROUS TITANIUM of proposition of the present invention and the preparation method of porous titanium alloy, it is simple to have technology, with short production cycle, the characteristics of low production cost.POROUS TITANIUM that the method for utilizing the present invention to propose prepares and porous titanium alloy distribution of porosity are even, controllability is better.The POROUS TITANIUM of the inventive method preparation can be in 5%～50% range with the porosity of porous titanium alloy, and intensity is according to porosity 30～75MPa variation that do not coexist.This method controllability is good, production efficiency is high, helps industrial applications.
Description of drawings
Fig. 1: for implementing starting powder pattern photo involved in the present invention, wherein (a) is the Ti powder, and granularity 11-45 μ m (b) is the Ti powder, and granularity 45-160 μ m (c) is the Ti-6Al-4V powder, granularity 11-63 μ m;
Fig. 2: for adopting the prepared porous material section of Fig. 1 (a) Ti powder light microscopic photo, wherein (a) (b) is heat treatment state for the spraying attitude;
Fig. 3: for adopting the prepared porous material section of Fig. 1 (b) Ti powder light microscopic photo, wherein (a) (b) is heat treatment state for the spraying attitude;
Fig. 4: for adopting the prepared porous material section of Fig. 1 (c) Ti-6Al-4V powder light microscopic photo, wherein (a) (b) is heat treatment state for the spraying attitude;
Fig. 5: for adopting Fig. 1 (a) Ti powder prepared porous Ti coating section light microscopic photo on the Ti-6Al-4V matrix, wherein (a) (b) is heat treatment state for the spraying attitude.
Embodiment
Now in conjunction with the embodiments the present invention is further described:
Embodiment 1:
Select 11-45 μ m titanium valve for use.Matrix is 45mm * 30mm * 4mm mild steel plate, adopts-100 order aluminum oxide fine sands to carry out surface coarsening before the spraying and handles.The cold spraying working gas is a pressurized air, spray gun ingress gaseous tension 2.7MPa, 500～520 ℃ of gas temperatures; Powder feeding gas is argon gas, pressure 3.0MPa; The about 30g/min of powder feeding rate; Spray distance 30mm, spray gun translational speed 150mm/s.The about 5mm of coat thickness.Peel off matrix after the spraying, carry out vacuum heat treatment then, 850 ℃ of thermal treatment temps, soaking time 4 hours, furnace cooling is to room temperature then.Observe the coating fractography, as shown in Figure 2, gas cell distribution is more even in the coating.Spraying attitude mean porosities is about 11%, heat treatment state mean porosities about 15%.After the thermal treatment, in the coating between particle the contact interface reach metallurgical binding, bonding strength obviously improves, from the spraying attitude 25MPa about to more than the 75MPa of heat treatment state.
Embodiment 2:
Select 45-160 μ m titanium valve for use.Matrix is 45mm * 30mm * 4mm mild steel plate, adopts-100 order aluminum oxide fine sands to carry out surface coarsening before the spraying and handles.The cold spraying working gas is a pressurized air, spray gun ingress gaseous tension 2.8MPa, about 550 ℃ of gas temperature; Powder feeding gas is argon gas, pressure 3.1Mpa; The about 30g/min of powder feeding rate; Spray distance 30mm, spray gun translational speed 150mm/s.The about 5mm of coat thickness.Peel off matrix after the spraying, carry out vacuum heat treatment then, 850 ℃ of thermal treatment temps, soaking time 4 hours, furnace cooling is to room temperature then.Observe the coating fractography, as shown in Figure 3, gas cell distribution is more even in the coating.Spraying attitude mean porosities is about 15%, heat treatment state mean porosities about 18%.After the thermal treatment, in the coating between particle the contact interface reach metallurgical binding, bonding strength obviously improves, from the spraying attitude 18MPa about to more than the 70MPa of heat treatment state.
Embodiment 3:
Select the Ti-6Al-4V powder of 11-63 μ m for use.Matrix is 45mm * 30mm * 4mm mild steel plate, adopts-100 order aluminum oxide fine sands to carry out surface coarsening before the spraying and handles.The cold spraying working gas is a pressurized air, spray gun ingress gaseous tension 2.8MPa, about 550 ℃ of gas temperature; Powder feeding gas is argon gas, pressure 3.1MPa; The about 30g/min of powder feeding rate; Spray distance 30mm, spray gun translational speed 150mm/s.The about 5mm of coat thickness.Peel off matrix after the spraying, carry out vacuum heat treatment then, 850 ℃ of thermal treatment temps, soaking time 4 hours, furnace cooling is to room temperature then.Observe the coating fractography, as shown in Figure 4, gas cell distribution is more even in the coating.Because of titanium alloy intensity height, deformability is poor, and prepared coating porosity is higher, and spraying attitude mean porosities is about 28%, heat treatment state mean porosities about 38%.After the thermal treatment, in the coating between particle the contact interface reach metallurgical binding, bonding strength obviously improves, from about the 10MPa of spraying attitude to about the 55MPa of heat treatment state.
Embodiment 4:
Select 11-45 μ m titanium valve for use.Matrix is the Ti-6Al-4V disc shaped test piece of diameter 25.4mm, length 10mm, adopts-24 order aluminum oxide fine sands to carry out surface coarsening before the spraying and handles.The cold spraying working gas is a pressurized air, spray gun ingress gaseous tension 3.0MPa, 500～520 ℃ of gas temperatures; Powder feeding gas is argon gas, pressure 3.3MPa; The about 30g/min of powder feeding rate; Spray distance 30mm, spray gun translational speed 150mm/s.The about 0.7mm of coat thickness.Directly carry out vacuum heat treatment after the spraying, 800 ℃ of thermal treatment temps, soaking time 4 hours, furnace cooling is to room temperature then.Observe the coating fractography, as shown in Figure 5, coating top layer 300 μ m inner air vent distribution uniform, and void content is higher.Coating and matrix bond are good.Spraying attitude mean porosities is about 7%, heat treatment state mean porosities about 13%.After the thermal treatment, in the coating between particle the contact interface reach metallurgical binding, bonding strength obviously improves, from the spraying attitude 25MPa about to more than the 70MPa of heat treatment state.
When implementing the inventive method, powder size and scope wait according to requirement porosity and pore dimension and select, and when requiring porosity less than 20%～40%, select granularity 5～100 μ m; When requiring hole greater than 40% the time, select the powder of 100～200 μ m to spray.
The body material kind is selected, and decides according to required matrix biomaterial kind, so that form POROUS TITANIUM or porous titanium alloy.When requiring independent POROUS TITANIUM or porous titanium alloy material, need to consider peeling off of preparation coat, select the general industry metallic substance get final product as matrix, as carbon steel etc., employing mechanical impact or machining process are peeled off matrix after spraying.
Sandblast pretreatment also is to decide according to application need, for titanium or titanium alloy substrate, requires the sandblast alligatoring effective, and surfaceness is big, adopts-24 order sand grains; For the matrix surface that need are peeled off, simply sandblasting, surfaceness is little, adopts-100 order sand grains.
The preparation of coat, powder sending quantity is at 10～100g/min when requiring spraying.
Claims (4)
1. the preparation method of POROUS TITANIUM and porous titanium alloy is characterized in that preparation process is as follows:
Step 1:, in 80～100 ℃ baking oven, toasted 1～4 hour with the Ti powder or the Ti powdered alloy of size range at 5～200 μ m;
Step 2: tabular matrix surface or bar-shaped matrix surface are carried out sandblast alligatoring pre-treatment;
Step 3: adopt cold spray-coating method to spray Ti powder or the Ti powdered alloy of preparing in the step 1 on above-mentioned matrix, powder sending quantity is during spraying: 10～100g/min; Coat thickness is: 100 μ m～50mm;
Step 4: the coat that step 3 is obtained places in the vacuum heat treatment furnace heat-treats, and vacuum degree in vacuum chamber requires less than 10
-3Pa; Holding temperature is at 600～900 ℃; Soaking time was at 1～8 hour.
2. the preparation method of POROUS TITANIUM according to claim 1 and porous titanium alloy is characterized in that: when matrix need be peeled off, matrix should be peeled off before the thermal treatment of step 4.
3. the preparation method of POROUS TITANIUM according to claim 1 and porous titanium alloy is characterized in that: the selection principle of the powder size of described Ti powder or Ti powdered alloy is: select the powder of granularity 5～100 μ m less than 20%～40% the time when requiring to spray porosity after finishing; When requiring to spray hole after finishing greater than 40% the time, select the powder of 100～200 μ m.
4. the preparation method of POROUS TITANIUM according to claim 1 and 2 and porous titanium alloy is characterized in that: described sandblast pretreatment, adopt-24 purpose sand grains for titanium or titanium alloy substrate; Matrix adopting-100 purpose the sand grains of peeling off for need.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838785A (en) * | 2010-06-01 | 2010-09-22 | 中国航空工业集团公司北京航空材料研究院 | Post weld vacuum heat treatment process of TC18 titanium alloy welding component |
| CN102303117A (en) * | 2011-08-27 | 2012-01-04 | 北京科技大学 | Method for preparing porous heat exchange surface of TiAl-based intermetallic compound |
| CN102443796A (en) * | 2011-12-02 | 2012-05-09 | 九江学院 | Porous Fe-Al intermetallic compound coating and preparation method thereof |
| CN107523717A (en) * | 2016-06-21 | 2017-12-29 | 张家港市思杰五金工具有限公司 | A kind of preparation method of POROUS TITANIUM |
| CN108309063A (en) * | 2017-01-17 | 2018-07-24 | 佛山市顺德区美的电热电器制造有限公司 | The preparation method of cookware, cooking apparatus and cookware |
| CN109207988A (en) * | 2017-07-25 | 2019-01-15 | 中国航空制造技术研究院 | A kind of reparation of thin-wall workpiece surface damage cold spraying powder and restorative procedure |
| CN114411140A (en) * | 2022-01-19 | 2022-04-29 | 西部宝德科技股份有限公司 | Preparation method of porous titanium coating |
-
2008
- 2008-05-15 CN CNA2008100181995A patent/CN101285136A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838785A (en) * | 2010-06-01 | 2010-09-22 | 中国航空工业集团公司北京航空材料研究院 | Post weld vacuum heat treatment process of TC18 titanium alloy welding component |
| CN101838785B (en) * | 2010-06-01 | 2011-12-21 | 中国航空工业集团公司北京航空材料研究院 | Post weld vacuum heat treatment process of TC18 titanium alloy welding component |
| CN102303117A (en) * | 2011-08-27 | 2012-01-04 | 北京科技大学 | Method for preparing porous heat exchange surface of TiAl-based intermetallic compound |
| CN102443796A (en) * | 2011-12-02 | 2012-05-09 | 九江学院 | Porous Fe-Al intermetallic compound coating and preparation method thereof |
| CN102443796B (en) * | 2011-12-02 | 2014-01-22 | 九江学院 | Porous Fe-Al intermetallic compound coating and its preparation method |
| CN107523717A (en) * | 2016-06-21 | 2017-12-29 | 张家港市思杰五金工具有限公司 | A kind of preparation method of POROUS TITANIUM |
| CN108309063A (en) * | 2017-01-17 | 2018-07-24 | 佛山市顺德区美的电热电器制造有限公司 | The preparation method of cookware, cooking apparatus and cookware |
| CN109207988A (en) * | 2017-07-25 | 2019-01-15 | 中国航空制造技术研究院 | A kind of reparation of thin-wall workpiece surface damage cold spraying powder and restorative procedure |
| CN114411140A (en) * | 2022-01-19 | 2022-04-29 | 西部宝德科技股份有限公司 | Preparation method of porous titanium coating |
| CN114411140B (en) * | 2022-01-19 | 2024-01-30 | 西部宝德科技股份有限公司 | Preparation method of porous titanium coating |
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