CN102912263B - A kind of fibre reinforced titanium alloy composite material and preparation method thereof - Google Patents
A kind of fibre reinforced titanium alloy composite material and preparation method thereof Download PDFInfo
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- CN102912263B CN102912263B CN201210382504.5A CN201210382504A CN102912263B CN 102912263 B CN102912263 B CN 102912263B CN 201210382504 A CN201210382504 A CN 201210382504A CN 102912263 B CN102912263 B CN 102912263B
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Abstract
The invention discloses a kind of fibre reinforced titanium alloy composite material and preparation method thereof.The concrete steps of the method are: step 1, pre-treatment of carbon fiber; Step 2, carbon fiber surface electroless copper: utilize chemical plating method that copper-clad is overlying on carbon fiber surface; Step 3, chemical vapour deposition pure tungsten: obtain tungsten settled layer by chemical Vapor deposition process at the carbon fiber surface of coated copper; Step 4, obtained the carbon fiber of appropriate length by the method for cutting by design requirements; Step 5, to mix by titanium alloy component requirements of design and together load hot-forming in pressing mold with carbon fiber after powder and sinter the fibre reinforced titanium alloy composite material finally obtaining needing shape.Fibre reinforced titanium alloy material compound prepared by the present invention is good, and titanium alloy component is adjustable, and the distribution of carbon fiber is controlled, and carbon fiber decarburization can not occur.This matrix material has high specific modulus, and have low density, high specific tenacity, impelling strength and good anti-Adiabatic Shear destructiveness, be a kind of high performance structural material simultaneously.
Description
Technical field
The present invention relates to the preparation technology of Copper Plating of Carbon Fiber, copper coating surface vapor deposition pure tungsten and metal composite, belong to metallurgical technology field, particularly relate to a kind of preparation method of fibre reinforced titanium alloy composite material.
Background technology
Fibre reinforced titanium alloy composite material by there is the titanium alloy of high specific strength and there is high ratio modulus, the carbon fiber of stretch-proof is composited, and has that density is low, specific tenacity is high, stretch-proof and a specific modulus advantages of higher.Its mechanical property carries out the adjustment in certain limit by the control of the distribution of adjustment carbon fiber in titanium alloy and titanium alloy component, be a kind of high performance lightweight structural material.
Carbon fiber and metallic substance compound tense is used to take simple mechanical complex method more or directly the metallurgical mode of carbon fiber are compound in metal blocks in the material of construction of present stage.Its shortcoming is that the matrix material bonding force obtained like this is very low, in use de-taking out easily occurs, is difficult to give play to carbon fiber stretch-proof and shear-stable advantage.
The specific tenacity of titanium alloy Yin Qigao is usually used in shock resistance field.Present stage can prepare short carbon fiber reinforced titanium alloy composite material, but staple fibre to its anti-shear ability effect of raising significantly and the arrangement of carbon fiber be difficult to control.
Can there is weightlessness being heated to more than 450 DEG C in carbon fiber, and this temperature cannot reach the powder metallurgy temperature of titanium alloy, and have hydrophobicity and surface inertness because of it, cannot directly by powder metallurgic method and titanium alloy compound; Because pure tungsten to react generation wolfram varbide with carbon fiber, directly utilize vapour deposition carbon fiber can be caused at high temperature weightless in the method for carbon fiber surface deposition pure tungsten.
After the present invention utilizes pre-treatment of carbon fiber, electroless copper plating method is first by its surface metalation; the method of vapour deposition is utilized to deposit one deck pure tungsten on its surface again; and then in the powder metallurgy process of titanium alloy compound with it; solve the problem that carbon fiber cannot bear high temperature when powder metallurgy prepares titanium alloy, also solve directly utilize tungsten as during protective layer and carbon fiber react when high temperature and form the problem of wolfram varbide.The material made has high specific tenacity and specific modulus, and the composition of the shape of finished product and the distribution of internal carbon fibers thereof, titanium alloy is all controlled.
Summary of the invention
The object of the invention is to overcome carbon fiber be difficult to compound and enter in titanium alloy and to combine difference and surface deposition tungsten in case can the shortcomings such as wolfram varbide be formed when blocking fiber high temperature is weightless, provide a kind of and there is high specific tenacity, specific modulus and fibre reinforced titanium alloy composite material that carbon fiber distribution is controlled, titanium alloy component is controlled and preparation method thereof.
The present invention solves the problems of the technologies described above taked technical scheme: make it metallize to prevent it from reacting with tungsten under the high temperature conditions at carbon fiber surface by copper facing and generate wolfram varbide; The resistant to elevated temperatures characteristic of recycling tungsten adopts powder metallurgic method and titanium alloy compound, improves the bonding strength with titanium alloy; For the Spreading requirements of carbon fiber in titanium alloy, adopt mechanical bonding it to be arranged in advance in pressing mold, then carry out warm-pressing formation and make it to form precast billet by Spreading requirements and Titanium Powder and finally carry out sintering and obtain finished product.
The above-mentioned preparation method with the fibre reinforced titanium alloy of high specific strength and specific modulus is as follows:
Step 1, pre-treatment of carbon fiber;
Step 2, carbon fiber surface electroless copper: utilize chemical plating method that copper-clad is overlying on carbon fiber surface;
Step 3, chemical vapour deposition pure tungsten: obtain tungsten settled layer by chemical Vapor deposition process at the carbon fiber surface of coated copper;
Step 4, obtained the carbon fiber of appropriate length by the method for cutting by design requirements;
Step 5, to mix by titanium alloy component requirements of design and together load hot-forming in pressing mold with carbon fiber after powder and sinter the fibre reinforced titanium alloy composite material finally obtaining needing shape.
The present invention, relative to the existing fibre reinforced titanium alloy composite material obtained by simple and mechanical complex method, be it is advantageous that:
(1) make it metallize at carbon fiber surface by copper facing, prevent from again while improve itself and pure tungsten bonding force reacting with tungsten under the high temperature conditions generating wolfram varbide; The resistant to elevated temperatures characteristic of recycling tungsten adopts powder metallurgic method and titanium alloy compound, improves the bonding strength with titanium alloy; For the Spreading requirements of carbon fiber in titanium alloy, mechanical means is adopted it to be arranged in advance in pressing mold, carry out warm-pressing formation again to make it to form precast billet by Spreading requirements and Titanium Powder and finally carry out sintering and obtain finished product, finally make to obtain fibre reinforced titanium alloy composite material by powder metallurgic method and become possibility.
(2) the fibre reinforced titanium alloy composite material interface cohesion obtained by powder metallurgic method is good, de-taking out not easily occurs, ensure that the high ratio modulus of material.
(3) long carbon fiber titanium alloy composite material can be obtained, and the distribution of carbon fiber in titanium alloy and titanium alloy component all can control.
Embodiment
Below in conjunction with four specific embodiments, exemplary illustration and help understand the present invention further.But embodiment detail is only in order to the present invention is described, do not represent the present invention conceive under whole technical schemes, therefore can not be interpreted as the restriction to technical solution of the present invention.Some unsubstantialities not departing from the present invention's design are changed, such as, simply change with the technical characteristic with same or similar technique effect or replace, all belonging to rights protection scope of the present invention.
Embodiment 1
1, first adopt the air calcination method of 300 DEG C except glue to carbon fiber, use thereafter that composition is nitric acid, the coarsening solution alligatoring of potassium bichromate, hydrogen peroxide and ammonium persulphate, then apply 10%NaOH solution and it is neutralized and uses SnCl
2carry out sensitization as sensitizing solution, adopt composition to be PdCl afterwards
2activate with the activation solution of AgCl, the inferior sodium phosphate solution soaking carbon fiber 1 ~ 3min of final utilization 20g/L is to complete reduction process;
2, the method for electroless copper is adopted to process carbon fiber.Solution composition comprises CuSO
4, HCHO, NaKC
4h
4o
6.Plating solution pH value is 12.7, plating temperature 60 DEG C, plating time 20min.For keeping the independent and uniform distribution state in carbon fiber plating process, ultra-sonic oscillation method is adopted to carry out dispersed to chemical bronze plating liquid.Wash 15min with deionized water after taking-up, then in the hot blast of 70 ~ 80 DEG C dry 20min;
3, chemical vapor depsotition equipment is utilized to carry out the vapour deposition of pure tungsten to copper-plated carbon fiber.The raw material adopted during deposition pure tungsten is WF
6and H
2, be warming up to 450 DEG C after emptying air, continue in temperature-rise period to pass into hydrogen, the time is about 1h, regulates hydrogen flowing quantity to 2L/min, and pass into WF after temperature-stable
6gas, flow is 0.8L/min; Stop after 1h passing into WF
6, stopped reaction during slow cooling to 100 DEG C;
4, carbon fiber is cut into the length of 5mm;
5, powdered alloy is prepared according to TC10 titanium alloy component (aluminium: 6%, vanadium: 6%, tin: 2%, titanium residue); Thereon with the spacing of the 1cm carbon fiber cut arranged in parallel after the powdered alloy that even laid 2cm is thick in mould, repave the powdered alloy putting 2cm, after repetition said process to mould fills up, mould and powder are heated, temperature is 120 ~ 180 DEG C simultaneously, pressing pressure is 500MPa, pressurize 30s, then sinter in vacuum oven, sintering temperature is 1250 DEG C, insulation 3h, air cooling obtains finished product.
Embodiment 2
1, first adopt the air calcination method of 300 DEG C except glue to carbon fiber, use thereafter that composition is nitric acid, the coarsening solution alligatoring of potassium bichromate, hydrogen peroxide and ammonium persulphate, then apply 10%NaOH solution and it is neutralized and uses SnCl
2carry out sensitization as sensitizing solution, adopt composition to be PdCl afterwards
2activate with the activation solution of AgCl, the inferior sodium phosphate solution soaking carbon fiber 1 ~ 3min of final utilization 20g/L is to complete reduction process;
2, the method for electroless copper is adopted to process carbon fiber.Solution composition comprises CuSO
4, HCHO, NaKC
4h
4o
6.Plating solution pH value is 12.7, plating temperature 60 DEG C, plating time 20min.For keeping the independent and uniform distribution state in carbon fiber plating process, ultra-sonic oscillation method is adopted to carry out dispersed to chemical bronze plating liquid.Wash 15min with deionized water after taking-up, then in the hot blast of 70 ~ 80 DEG C dry 20min; 3, chemical vapor depsotition equipment is utilized to carry out the vapour deposition of pure tungsten to copper-plated carbon fiber.The raw material adopted during deposition pure tungsten is WF
6and H
2, be warming up to 550 DEG C after emptying air, continue in temperature-rise period to pass into hydrogen, the time is about 1h, regulates hydrogen flowing quantity to 2L/min, and pass into WF after temperature-stable
6gas, flow is 1.2L/min; Stop after 1.5h passing into WF
6, stopped reaction during slow cooling to 100 DEG C;
4, carbon fiber is cut into the length of 10mm;
5, powdered alloy is prepared according to TC10 titanium alloy component (aluminium: 6%, vanadium: 6%, tin: 2%, titanium residue); Put in the mode of meshy arrangement the carbon fiber cut thereon after the powdered alloy that even laid 1cm is thick in mould, between the parallel carbon fiber of two nearest neighbour, spacing is 1cm, then the powdered alloy of laid 1cm thereon, repeats after said process to mould fills up, mould and powder are heated simultaneously, temperature is 120 ~ 180 DEG C, and pressing pressure is 500MPa, pressurize 30s, sinter in vacuum oven again, sintering temperature is 1250 DEG C, and insulation 3h, air cooling obtains finished product.
Embodiment 3
1, first adopt the air calcination method of 300 DEG C except glue to carbon fiber, use thereafter that composition is nitric acid, the coarsening solution alligatoring of potassium bichromate, hydrogen peroxide and ammonium persulphate, then apply 10%NaOH solution and it is neutralized and uses SnCl
2carry out sensitization as sensitizing solution, adopt composition to be PdCl afterwards
2activate with the activation solution of AgCl, the inferior sodium phosphate solution soaking carbon fiber 1 ~ 3min of final utilization 20g/L is to complete reduction process;
2, the method for electroless copper is adopted to process carbon fiber.Solution composition comprises CuSO
4, HCHO, NaKC
4h
4o
6.Plating solution pH value is 12.7, plating temperature 60 DEG C, plating time 20min.For keeping the independent and uniform distribution state in carbon fiber plating process, ultra-sonic oscillation method is adopted to carry out dispersed to chemical bronze plating liquid.Wash 15min with deionized water after taking-up, then in the hot blast of 70 ~ 80 DEG C dry 20min;
3, chemical vapor depsotition equipment is utilized to carry out the vapour deposition of pure tungsten to copper-plated carbon fiber.The raw material adopted during deposition pure tungsten is WF
6and H
2, be warming up to 450 DEG C after emptying air, continue in temperature-rise period to pass into hydrogen, the time is about 1h, regulates hydrogen flowing quantity to 2L/min, and pass into WF after temperature-stable
6gas, flow is 0.8L/min; Stop after 1h passing into WF
6, stopped reaction during slow cooling to 100 DEG C;
4, carbon fiber is cut into the length of 5mm;
5, powdered alloy is prepared according to Ti153 titanium alloy component (vanadium: 15%, aluminium: 3%, chromium: 3%, tin: 3%, titanium residue); Put in the mode of meshy arrangement the carbon fiber cut thereon after the powdered alloy that even laid 1cm is thick in mould, between the parallel carbon fiber of two nearest neighbour, spacing is 1cm, then the powdered alloy of laid 1cm thereon, repeats after said process to mould fills up, mould and powder are heated simultaneously, temperature is 120 ~ 180 DEG C, and pressing pressure is 500MPa, pressurize 30s, sinter in vacuum oven again, sintering temperature is 1250 DEG C, and insulation 3h, air cooling obtains finished product.
Embodiment 4
1, first adopt the air calcination method of 300 DEG C except glue to carbon fiber, use thereafter that composition is nitric acid, the coarsening solution alligatoring of potassium bichromate, hydrogen peroxide and ammonium persulphate, then apply 10%NaOH solution and it is neutralized and uses SnCl
2carry out sensitization as sensitizing solution, adopt composition to be PdCl afterwards
2activate with the activation solution of AgCl, the inferior sodium phosphate solution soaking carbon fiber 1 ~ 3min of final utilization 20g/L is to complete reduction process;
2, the method for electroless copper is adopted to process carbon fiber.Solution composition comprises CuSO
4, HCHO, NaKC
4h
4o
6.Plating solution pH value is 12.7, plating temperature 60 DEG C, plating time 20min.For keeping the independent and uniform distribution state in carbon fiber plating process, ultra-sonic oscillation method is adopted to carry out dispersed to chemical bronze plating liquid.Wash 15min with deionized water after taking-up, then in the hot blast of 70 ~ 80 DEG C dry 20min;
3, chemical vapor depsotition equipment is utilized to carry out the vapour deposition of pure tungsten to copper-plated carbon fiber.The raw material adopted during deposition pure tungsten is WF
6and H
2, be warming up to 550 DEG C after emptying air, continue in temperature-rise period to pass into hydrogen, the time is about 1h, regulates hydrogen flowing quantity to 2L/min, and pass into WF after temperature-stable
6gas, flow is 1.2L/min; Stop after 1.5h passing into WF
6, stopped reaction during slow cooling to 100 DEG C;
4, carbon fiber is cut into the length of 10mm;
5, powdered alloy is prepared according to Ti153 titanium alloy component (vanadium: 15%, aluminium: 3%, chromium: 3%, tin: 3%, titanium residue); Thereon with the spacing of the 1cm carbon fiber cut arranged in parallel after the powdered alloy that even laid 2cm is thick in mould, repave the powdered alloy putting 2cm, after repetition said process to mould fills up, mould and powder are heated, temperature is 120 ~ 180 DEG C simultaneously, pressing pressure is 500MPa, pressurize 30s, then sinter in vacuum oven, sintering temperature is 1250 DEG C, insulation 3h, air cooling obtains finished product.
Claims (6)
1. a fibre reinforced titanium alloy composite material, it is characterized in that: carbon fiber is parallel or meshy arrangement is distributed in titanium alloy block, titanium alloy component is adjustable, carbon fiber distribution is controlled, and this matrix material is by adopting chemical Vapor deposition process to utilize WF on its surface again after carbon fiber surface electroless plating a layer thickness is the copper of 2 ~ 5 μm
6and H
2reactive deposition a layer thickness is the pure tungsten of 2 ~ 5 μm, finally utilizes powder metallurgic method the carbon fiber after process and the method for titanium alloy compound to be obtained.
2. material as claimed in claim 1, is characterized in that: the composition of titanium alloy allows to adjust as required.
3. material as claimed in claim 1, is characterized in that: distributing position, angle and the quantity of carbon fiber in the titanium alloy block that powder metallurgy is formed allows to adjust in the pressing mold used by powder metallurgy.
4. material as claimed in claim 1, is characterized in that: carbon fiber surface has thickness to be the copper plate of 2 ~ 5 μm, and layers of copper surface deposition has one deck to have thickness to be the pure tungsten of 2 ~ 5 μm;
Described material is prepared by following process: (1) carbon fiber will carry out 300 DEG C of air calcinations before use and remove photoresist, nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulfate solution alligatoring, and 10%NaOH solution neutralizes, SnCl
2solution sensitization, PdCl
2with inferior sodium phosphate solution soaking 1 ~ 3min reduction pretreatment of the activation of AgCl solution, 20g/L;
(2) adopt pH value be the method for chemical plating fluid copper facing 20min at 60 DEG C of 12.7 in carbon fiber surface plating, after taking-up with deionized water washing and in the hot blast of 70 ~ 80 DEG C dry 20min;
(3) chemical Vapor deposition process is adopted, the pure tungsten that carbon fibres deposit one deck after copper facing 2 ~ 5 μm is thick;
(4) by the dimensional requirement of design, cutting is carried out to carbon fiber;
(5) carry out mixed powder by the requirement of titanium alloy component of design, powder and carbon fiber are placed in pressing mold by design requirements and carry out warm-pressing formation, finally sinter.
5. the preparation method of a kind of fibre reinforced titanium alloy composite material as claimed in claim 1, is characterized in that:
(1) carbon fiber will carry out 300 DEG C of air calcinations before use and removes photoresist, nitric acid, potassium bichromate, hydrogen peroxide and ammonium persulfate solution alligatoring, and 10%NaOH solution neutralizes, SnCl
2solution sensitization, PdCl
2with inferior sodium phosphate solution soaking 1 ~ 3min reduction pretreatment of the activation of AgCl solution, 20g/L;
(2) adopt pH value be the method for chemical plating fluid copper facing 20min at 60 DEG C of 12.7 in carbon fiber surface plating, after taking-up with deionized water washing and in the hot blast of 70 ~ 80 DEG C dry 20min;
(3) chemical Vapor deposition process is adopted, the pure tungsten that carbon fibres deposit one deck after copper facing 2 ~ 5 μm is thick;
(4) by the dimensional requirement of design, cutting is carried out to carbon fiber;
(5) carry out mixed powder by the requirement of titanium alloy component of design, powder and carbon fiber are placed in pressing mold by design requirements and carry out warm-pressing formation, finally sinter.
6. preparation method as claimed in claim 5, is characterized in that:
(1), when carrying out electroless copper to carbon fiber, employing solution composition is CuSO
4, HCHO, NaKC
4h
4o
6; Or use composition to be CuSO
45H
2o, EDTA, KNaC
4h
4o
64H
2o, NaOH, HCHO, 2,2 ' 2 dipyridyls, K
4fe (CN)
63H
2the pH value that O is made into is the plating solution plating of 12.7;
(2), when the copper-plated carbon fiber of effects on surface carries out vapour deposition pure tungsten, the raw material of employing is WF
6and H
2, react front-seat net air; Continue in temperature-rise period to pass into hydrogen, the time is 1h, after substrate temperature reaches 450 DEG C and maintenance is stable, regulates hydrogen flowing quantity, passes into WF
6gas; Stop after 1h passing into WF
6, stop during slow cooling to 100 DEG C passing into H
2, pass into N
2until cooling terminates;
(3) what the copper carbon fiber of effects on surface deposition pure tungsten carried out adopting with the compound tense of titanium alloy is powder metallurgic method, the last interpolation internal lubricant of Titanium Powder that powder obtains predetermined component is mixed by the component requirements of titanium alloy, powder and carbon fiber are placed in pressing mold by the Spreading requirements designed, mould and powder are heated simultaneously and pressurize and carries out warm compaction molding, then sinter in vacuum oven.
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CN114438425B (en) * | 2022-02-09 | 2022-07-19 | 重庆金开泰达新材料科技有限公司 | Long carbon fiber reinforced titanium alloy composite material |
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