CN103435373B - Carbon/carbon composite material connection layer and preparation method - Google Patents
Carbon/carbon composite material connection layer and preparation method Download PDFInfo
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Abstract
The invention discloses a preparation method for a carbon/carbon composite material connection layer, which is used for preparing a metal connection layer on the surface of a carbon/carbon composite material by means of liquid-phase impregnation. The preparation method is characterized by comprising the steps of carbon/carbon composite material base layer blank preparation, liquid-phase impregnation, and calcining reduction, wherein the prepared carbon/carbon composite material connection layer comprises a carbon/carbon composite material base layer blank, and a metal particle layer on the surface of the carbon/carbon composite material base layer blank. The preparation method disclosed by the invention is simple in process; the metal connection layer is prepared on the surface of the carbon/carbon composite material by virtue of liquid-phase impregnation and calcining reduction, so that the chemical constitution and micro-geometrical structure of the surface of the carbon/carbon composite are changed; the attached metal connection layer is good in compatibility with a metal material, so that the connection strength between the carbon/carbon composite material and the metal material can be increased.
Description
Technical field
The present invention relates to a kind of carbon/carbon compound material, specifically a kind of Carbon/carbon composite material connection layer and preparation method.
Background technology
Carbon/carbon compound material has low density, high strength, high ratio modulus, high thermal conductivity, low-expansion coefficient, and thermal shock resistance is good, dimensional stability advantages of higher, is one of the most rising high-temperature material.Carbon/carbon compound material, due to the performance of its uniqueness, has been widely used in the fields such as aerospace, automotive industry, medical science aspect.
But, in some Application Areass and occasion, need carbon/carbon compound material to be connected with metal.But carbon/carbon compound material and metal have larger difference in crystalline structure, physics-chem characteristic etc., the wetting angle of carbon/carbon compound material and most metals is greater than 90 °, cannot directly connect.This just needs to add the third material at carbon/carbon compound material and metal two storeroom, prepares articulamentum, thus realizes the connection of carbon/carbon compound material and metal.
Document 1: " Cu-Cr alloy cladding surface modification carbon/carbon compound material; mining metallurgical engineering; 2007 (06): P58 ~ P60 ", Cu-Cr binary alloy is adopted to be raw material, in vacuum heater, temperature is 1200 ~ 1600 DEG C, under vacuum tightness is less than 10 Pa conditions, implements surface cladding process to carbon/carbon compound material.Result shows, cladding impels Cr enrichment of element in alloy in surface of carbon/carbon composite, and generates Cr with C element reaction in－situ
3c
2; This reactant be stratiform continuous distribution in surface of carbon/carbon composite, between carbon/carbon compound material and metal, play interfaces transition effect, contribute to the connectivity improved between the two.
Document 2: mention by surface of carbon/carbon composite brushing one deck Mo-Cr powdered alloy slip in " Direct joining of CFC to copper. Journal of Nuclear Materials; 2004. 329-333; Part B (0): P1563 ~ P1566 ", obtain the alloy coat that thickness is 5 ~ 10 μm in vacuum oven more than 1000 DEG C, and then carbon/carbon compound material directly can be connected with Cu.
The disclosed two kinds of methods of document 1, document 2 are by the metal connecting layer of high temperature, depression formation, all there is metal layer thickness to be difficult to control and uneven problem, metal skewness in process of setting simultaneously, much dendrite, twin and other lattice defect can be generated, cause the mechanical property of web member not high.
Summary of the invention
The object of this invention is to provide a kind of Carbon/carbon composite material connection layer and the preparation method that are prepared metal connecting layer by liquid impregnation at surface of carbon/carbon composite.
The present invention adopts following technical scheme to realize its goal of the invention, a kind of Carbon/carbon composite material connection layer, it is provided with metal particle layer in carbon/carbon composite material base layer billet surface, and described metal particle layer is that carbon/carbon composite material base layer base substrate is through liquid impregnation, the preparation of calcining reduction step.
The thickness of metal particle layer of the present invention is 0.01 μm ~ 100 μm.
A kind of Carbon/carbon composite material connection layer preparation method, it comprises the following steps:
(1) carbon/carbon composite material base layer body preparation: carbon/carbon composite material base layer base substrate carbon/carbon compound material base substrate being machined to desired shape, for subsequent use after washing, oven dry;
(2) flood: the container that carbon/carbon composite material base layer base substrate step (1) obtained puts into the alcohol solution be equipped with containing at least one metal ion floods 1h ~ 50h, then by solution warms to 80 DEG C ~ 150 DEG C, insulation 1h ~ 10h, after being cooled to room temperature, dry in the shade under carbon/carbon composite material base layer base substrate is taken out normal temperature from container, namely prepare metal-salt coating in carbon/carbon composite material base layer billet surface;
(3) articulamentum preparation: carbon/carbon composite material base layer base substrate step (2) obtained puts into reduction furnace, at 300 DEG C ~ 1200 DEG C, pass into hydrogen and carry out calcining reduction, the recovery time is 1h ~ 50h, be cooled to normal temperature afterwards, there is the carbon/carbon composite material base layer base substrate of metal particle layer on obtained surface.
For removing impurity in carbon/carbon composite material base layer base substrate, the present invention step (1) in, washing, dry before, obtained carbon/carbon composite material base layer base substrate is put into High Temperature Furnaces Heating Apparatus and carries out purification process, under vacuum or protective atmosphere condition, add heat abstraction wherein impurity.Cleansing temp is 1800 DEG C ~ 2500 DEG C, and soaking time is 2h ~ 6h.
The present invention step (2) in, the compound method of the described alcohol solution containing at least one metal ion is by soluble in water at least one metal-salt, the volume of dehydrated alcohol accounts for 5 ﹪ ~ 30 ﹪ of overall solution volume, aqueous solution of urea accounts for 5 ﹪ ~ 20 ﹪ of overall solution volume, the volume percent sum of water, dehydrated alcohol and aqueous solution of urea is 100 ﹪, add aqueous solution of urea and the dehydrated alcohol of 0.5mol/L ~ 3mol/L in the solution, be mixed with the aqueous solution that metal ion total concn is 0.05mol/L ~ 5mol/L.
Metal-salt of the present invention is one in nitrate soluble in water or vitriol or chlorate or combination.
The present invention step (2) in, described metal ion is one in cupric ion or aluminum ion or iron ion or nickel ion or lanthanum ion or chromium ion or combination.
The present invention step (3) in, the thickness of metal particle layer is 0.01 μm ~ 100 μm.
Owing to adopting technique scheme, the present invention achieves goal of the invention preferably, technique is simple, metal connecting layer is prepared at surface of carbon/carbon composite by liquid impregnation, calcining reduction, change chemical constitution and the micro-geometry of surface of carbon/carbon composite, and the metal connecting layer of attachment and metallic substance have good consistency, can improve the intensity that carbon/carbon compound material is connected with metallic substance.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
A kind of Carbon/carbon composite material connection layer preparation method, it comprises the following steps:
(1) carbon/carbon composite material base layer body preparation: the carbon/carbon composite material base layer base substrate 2 carbon/carbon compound material base substrate being machined to desired shape, for subsequent use after washing, oven dry;
Carbon/carbon compound material base substrate of the present invention is by the one in mold pressing or chemical vapour deposition or liquid impregnation method or combination preparation.Carbon fiber is first made carbon fiber basic unit precast body by desired structure and shape by the present embodiment, more obtained after chemical gas phase sinks density.
For removing impurity in carbon/carbon composite material base layer base substrate 2; the present invention step (1) in; before washing, oven dry; obtained carbon/carbon composite material base layer base substrate 2 is put into High Temperature Furnaces Heating Apparatus and carries out purification process; heat abstraction wherein impurity is added under vacuum or protective atmosphere condition; cleansing temp is 1800 DEG C ~ 2500 DEG C, and soaking time is 2h ~ 6h.The present embodiment cleansing temp is 2200 DEG C, and soaking time is 2h.
(2) flood: the container that the carbon/carbon composite material base layer base substrate 2 step (1) obtained puts into the alcohol solution be equipped with containing at least one metal ion floods 1h ~ 50h, then by solution warms to 80 DEG C ~ 150 DEG C, insulation 1h ~ 10h, after being cooled to room temperature, dry in the shade under carbon/carbon composite material base layer base substrate 2 being taken out from container normal temperature, namely prepare metal-salt coating on carbon/carbon composite material base layer base substrate 2 surface;
The present invention step (2) in, the compound method of the described alcohol solution containing at least one metal ion is by soluble in water at least one metal-salt, the volume of dehydrated alcohol accounts for 5 ﹪ ~ 30 ﹪ of overall solution volume, aqueous solution of urea accounts for 5 ﹪ ~ 20 ﹪ of overall solution volume, the volume percent sum of water, dehydrated alcohol and aqueous solution of urea is 100 ﹪, add aqueous solution of urea and the dehydrated alcohol of 0.5mol/L ~ 3mol/L in solution, be mixed with the aqueous solution that metal ion total concn is 0.05mol/L ~ 5mol/L.
Metal-salt of the present invention is one in nitrate soluble in water or vitriol or chlorate or combination.
The present invention step (2) in, described metal ion is one in cupric ion or aluminum ion or iron ion or nickel ion or lanthanum ion or chromium ion or combination.
Metal-salt described in the present embodiment is copper sulfate and chromium nitrate, when preparing alcohol solution, the volume of dehydrated alcohol accounts for 20 ﹪ of overall solution volume, aqueous solution of urea accounts for 10 ﹪ of overall solution volume, the volume percent sum of water, dehydrated alcohol and aqueous solution of urea is 100 ﹪, add aqueous solution of urea and the dehydrated alcohol of 2mol/L in solution, be mixed with the aqueous solution that metal ion total concn is 2mol/L.Wherein, in solution, cupric ion and chromium ion atom number ratio are 15:3.
During dipping, carbon/carbon composite material base layer base substrate 2 is put into the container that prepared alcohol solution is housed and floods 24h, then by solution warms to 125 DEG C, insulation 3h, after being cooled to room temperature, dry in the shade under carbon/carbon composite material base layer base substrate 2 being taken out from container normal temperature, namely have in the preparation of carbon/carbon composite material base layer base substrate 2 surface the coating comprising copper sulfate and chromium nitrate.
The present invention also can adopt spraying method to prepare metal-salt coating on carbon/carbon composite material base layer base substrate 2 surface.
(3) articulamentum preparation: the carbon/carbon composite material base layer base substrate 2 step (2) obtained puts into reduction furnace, at 300 DEG C ~ 1200 DEG C, pass into hydrogen and carry out calcining reduction, recovery time is 1h ~ 50h, be cooled to normal temperature afterwards, there is the carbon/carbon composite material base layer base substrate 2 of metal particle layer 1 on obtained surface.
The present invention step (3) in, the thickness of metal particle layer 1 is 0.01 μm ~ 100 μm.
The carbon/carbon composite material base layer base substrate 2 that (2) step obtains by the present embodiment puts into reduction furnace, at 900 DEG C, pass into hydrogen and carry out calcining reduction, recovery time is 3h, be cooled to normal temperature afterwards, obtained surface includes the carbon/carbon composite material base layer base substrate 2 of metal particle layer 1 of copper particle, chromium particle; The thickness of described metal particle layer 1 is 30 μm.
As shown in Figure 1, a kind of Carbon/carbon composite material connection layer, it is provided with metal particle layer 1 on carbon/carbon composite material base layer base substrate 2 surface, and described metal particle layer 1 is that carbon/carbon composite material base layer base substrate 2 is through liquid impregnation, the preparation of calcining reduction step.
The thickness of metal particle layer 1 of the present invention is 0.01 μm ~ 100 μm.
The goods prepared by aforesaid method comprise carbon/carbon composite material base layer base substrate 2, an articulamentum, and described articulamentum is the metal particle layer 1 being prepared in carbon/carbon composite material base layer base substrate 2 surface, and described in the present embodiment, the thickness of metal particle layer 1 is 30 μm.
The carbon/carbon composite material base layer base substrate 2 step (3) obtained and metal material base base substrate clamp, and metal particle layer on carbon/carbon composite material base layer base substrate 21 is adjacent with the joint face of metal material base base substrate, and (the present embodiment is prepared by metallic copper material, joint face carries out frosted process), then put it in vacuum oven, be heated to 500 DEG C ~ 2200 DEG C (the present embodiment is 1300 DEG C), be 0.05MPa at 0.01MPa ~ 10MPa(the present embodiment) under pressure, 10min ~ 500min(the present embodiment is kept to be 30min), the metal particle layer 1 on carbon/carbon composite material base layer base substrate 2 is made to form metallurgical binding with the joint face of metal material base base substrate, the i.e. web member of obtained carbon/carbon compound material and metallic copper material.
Through test, the shearing resistance at the present embodiment carbon/carbon composite material base layer base substrate 2, metallic copper material basic unit base substrate interface is 30MPa.
Embodiment 2:
The present invention step (2) in, metal-salt is chromium nitrate, and in alcohol solution, metal ion total concn is 2mol/L, and the preparation of carbon/carbon composite material base layer base substrate 2 surface has the coating of chromium nitrate.Step (3) in, there is the carbon/carbon composite material base layer base substrate 2 of the metal particle layer 1 of chromium particle on obtained surface, and the thickness of metal particle layer 1 is 20 μm.
After the carbon/carbon composite material base layer base substrate 2 that (3) step is obtained and metallic copper material basic unit base substrate compound, i.e. the web member of obtained carbon/carbon compound material and metallic copper material.
Through test, the shearing resistance at the present embodiment carbon/carbon composite material base layer base substrate 2, metallic copper material basic unit base substrate interface is 25MPa.
Remaining with embodiment 1.
Embodiment 3:
The present invention step (2) in, metal-salt is aluminum nitrate and chromium nitrate, and in alcohol solution, aluminum ion and chromium ion atom number are than being 15:4, and the preparation of carbon/carbon composite material base layer base substrate 2 surface has the coating of aluminum nitrate and chromium nitrate.Step (3) in, there is the carbon/carbon composite material base layer base substrate 2 of the metal particle layer 1 of aluminum particulate, chromium particle on obtained surface, and the thickness of described metal particle layer 1 is 28 μm.
After the carbon/carbon composite material base layer base substrate 2 that (3) step is obtained and metallic aluminum material basic unit base substrate compound, i.e. the web member of obtained carbon/carbon compound material and metallic aluminum material.Through test, the shearing resistance at the present embodiment carbon/carbon composite material base layer base substrate 2, metallic aluminum material basic unit base substrate interface is 30MPa.
Remaining with embodiment 1.
Embodiment 4:
The present invention step (2) in, metal-salt is nickelous nitrate and copper sulfate, and in alcohol solution, nickel ion and cupric ion atom number are than being 15:2, and the preparation of carbon/carbon composite material base layer base substrate 2 surface has the coating of nickelous nitrate and copper sulfate.Step (3) in, the carbon/carbon composite material base layer base substrate 2 step (2) obtained puts into reduction furnace, at 1100 DEG C, pass into hydrogen and carry out calcining reduction, recovery time is 3h, be cooled to normal temperature afterwards, obtained surface includes the carbon/carbon composite material base layer base substrate 2 of metal particle layer 1 of nickel particles, copper particle; The thickness of described metal particle layer 1 is 50 μm.
The carbon/carbon composite material base layer base substrate 2 step (3) obtained and obtained metallic iron material base layer base substrate clamp, then put it in vacuum oven, be heated to 1400 DEG C, under 0.05MPa pressure, keep 30min, the metal particle layer 1 carbon/carbon composite material base layer base substrate 2 including nickel particles and copper particle is made to form metallurgical binding with the joint face of metallic iron material base layer base substrate, i.e. the web member of obtained carbon/carbon compound material and metallic iron material.Remaining with embodiment 1.
Through test, the shearing resistance at the present embodiment carbon/carbon composite material base layer base substrate 2, metallic iron material base layer base substrate interface is 25MPa.
Remaining with embodiment 1.
Embodiment 5:
The present invention step (2) in, metal-salt is nickelous nitrate, lanthanum nitrate and aluminum nitrate, and nickel ion, lanthanum ion and aluminum ion atom number are than for 15:3:2, and the preparation of carbon/carbon composite material base layer base substrate 2 surface has the coating of nickelous nitrate, lanthanum nitrate and aluminum nitrate.Step (3) in, obtained surface includes the carbon/carbon composite material base layer base substrate 2 of the metal particle layer 1 of nickel particles, lanthanum particle and aluminum particulate, and the thickness of metal particle layer 1 is 35 μm.
The carbon/carbon composite material base layer base substrate 2 step (3) obtained and obtained metal stainless material basic unit base substrate clamp, then put it in vacuum oven, be heated to 1400 DEG C, under 0.05MPa pressure, keep 30min, the metal particle layer 1 carbon/carbon composite material base layer base substrate 2 including nickel particles and copper particle is made to form metallurgical binding with the joint face of metal stainless material basic unit base substrate, i.e. the web member of obtained carbon/carbon compound material and metal stainless material.
Through test, the shearing resistance at the present embodiment carbon/carbon composite material base layer base substrate 2, metal stainless material basic unit's base substrate interface is 20MPa.
Remaining with embodiment 1.
Claims (5)
1. a Carbon/carbon composite material connection layer preparation method, is characterized in that it comprises the following steps:
(1) carbon/carbon composite material base layer body preparation: carbon/carbon composite material base layer base substrate carbon/carbon compound material base substrate being machined to desired shape, for subsequent use after washing, oven dry;
(2) flood: the container that carbon/carbon composite material base layer base substrate step (1) obtained puts into the alcohol solution be equipped with containing at least one metal ion floods 1h ~ 50h, then by solution warms to 80 DEG C ~ 150 DEG C, insulation 1h ~ 10h, after being cooled to room temperature, dry in the shade under carbon/carbon composite material base layer base substrate is taken out normal temperature from container, namely prepare metal-salt coating in carbon/carbon composite material base layer billet surface; Step (2) in, the compound method of the described alcohol solution containing at least one metal ion is by soluble in water at least one metal-salt, the volume of dehydrated alcohol accounts for 5 ﹪ ~ 30 ﹪ of overall solution volume, aqueous solution of urea accounts for 5 ﹪ ~ 20 ﹪ of overall solution volume, the volume percent sum of water, dehydrated alcohol and aqueous solution of urea is 100 ﹪, add aqueous solution of urea and the dehydrated alcohol of 0.5mol/L ~ 3mol/L in the solution, be mixed with the aqueous solution that metal ion total concn is 0.05mol/L ~ 5mol/L;
(3) articulamentum preparation: carbon/carbon composite material base layer base substrate step (2) obtained puts into reduction furnace, at 300 DEG C ~ 1200 DEG C, pass into hydrogen and carry out calcining reduction, the recovery time is 1h ~ 50h, be cooled to normal temperature afterwards, there is the carbon/carbon composite material base layer base substrate of metal particle layer on obtained surface; The thickness of metal particle layer is 0.01 μm ~ 100 μm.
2. Carbon/carbon composite material connection layer preparation method according to claim 1; it is characterized in that step (1) in; before washing, oven dry, obtained carbon/carbon composite material base layer base substrate is put into High Temperature Furnaces Heating Apparatus and carries out purification process, under vacuum or protective atmosphere condition, add heat abstraction wherein impurity.
3. Carbon/carbon composite material connection layer preparation method according to claim 2, it is characterized in that cleansing temp is 1800 DEG C ~ 2500 DEG C, soaking time is 2h ~ 6h.
4. Carbon/carbon composite material connection layer preparation method according to claim 1, is characterized in that described metal-salt is one in nitrate soluble in water or vitriol or chlorate or combination.
5. Carbon/carbon composite material connection layer preparation method according to claim 1, it is characterized in that step (2) in, described metal ion is one in cupric ion or aluminum ion or iron ion or nickel ion or lanthanum ion or chromium ion or combination.
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| CN105887059B (en) * | 2016-06-14 | 2018-08-10 | 西北工业大学 | A kind of preparation method of highly-conductive hot carbon/carbon-carbon/carbon-copper composite material |
| CN106966753B (en) * | 2017-04-06 | 2021-04-02 | 哈尔滨工业大学 | Preparation method of C/Al-Si-X ablation-resistant composite material |
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| CN101279366A (en) * | 2008-05-28 | 2008-10-08 | 天津大学 | Method for producing diamond reinforced Cu-matrix compound material by surface metallization and chemical deposition |
| CN102586704A (en) * | 2012-03-23 | 2012-07-18 | 北京科技大学 | High thermal conductivity graphite whisker/copper composite and preparation method thereof |
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| CN101279366A (en) * | 2008-05-28 | 2008-10-08 | 天津大学 | Method for producing diamond reinforced Cu-matrix compound material by surface metallization and chemical deposition |
| CN102586704A (en) * | 2012-03-23 | 2012-07-18 | 北京科技大学 | High thermal conductivity graphite whisker/copper composite and preparation method thereof |
Non-Patent Citations (3)
| Title |
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| Cu-Cr合金熔覆表面改性炭/炭复合材料;张福勤等;《矿冶工程》;20071231;第27卷(第6期);第58-60页 * |
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Address after: 413000 Hunan province Yiyang Yingbin Road No. 2 Patentee after: Hunan gold carbon Limited by Share Ltd Address before: 413000 Hunan province Yiyang Yingbin Road No. 2 Patentee before: Hunan KBCarbon Composite Science and Technology Co., Ltd. |