CN106478125B - A kind of preparation method of the modified C/C-SiC brake material of B4C - Google Patents
A kind of preparation method of the modified C/C-SiC brake material of B4C Download PDFInfo
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- CN106478125B CN106478125B CN201610858805.9A CN201610858805A CN106478125B CN 106478125 B CN106478125 B CN 106478125B CN 201610858805 A CN201610858805 A CN 201610858805A CN 106478125 B CN106478125 B CN 106478125B
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- 239000000463 material Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 25
- 239000004917 carbon fiber Substances 0.000 claims abstract description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 23
- 230000003068 static effect Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 238000001764 infiltration Methods 0.000 claims abstract description 7
- 230000008595 infiltration Effects 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 10
- 239000000835 fiber Substances 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 239000002296 pyrolytic carbon Substances 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- 229910017082 Fe-Si Inorganic materials 0.000 claims description 2
- 229910017133 Fe—Si Inorganic materials 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 229910008341 Si-Zr Inorganic materials 0.000 claims 1
- 229910002796 Si–Al Inorganic materials 0.000 claims 1
- 229910006682 Si—Zr Inorganic materials 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 abstract description 15
- 238000000626 liquid-phase infiltration Methods 0.000 abstract description 6
- 239000000470 constituent Substances 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000002289 liquid silicon infiltration Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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Abstract
The present invention relates to a kind of B4The preparation method of the modified C/C-SiC brake material of C in initial density is about 0.4~0.6g/cm using vacuum pressure impregnating method3B is introduced in D refraction statics carbon felt4C powder, and the method for combining chemical vapor infiltration (CVI) and reactive melt infiltration (RMI) to prepare C/C-SiC brake material.Using B4C is modified C/C-SiC brake material, one side B4C has protective effect to carbon fiber and carbon base body as self-healing constituent element, can significantly improve the inoxidizability of material；On the other hand, B4C has higher specific heat capacity, can improve the whole specific heat of material, and brake temperature is effectively reduced, and improves material friction stability.
Description
Technical field
The invention belongs to the preparation methods of C/C-SiC composite material, are related to a kind of B4The modified C/C-SiC brake material of C
Preparation method, be it is a kind of using vacuum pressure impregnation by B4C powder introduces D refraction statics carbon fiber precast body, and passes through chemical gas
Mutually deposition association reaction melt Infiltration Technics prepare B4The method of the modified C/C-SiC brake material of C.
Background technique
Brake gear is aircraft, high-speed rail, automobile realization braking, ensures the core component of operational safety, mainly passes through friction
The relative motion on surface converts kinetic energy into thermal energy to realize the purpose of braking.In braking process, brake gear is when extremely short
It is interior to convert thermal energy for huge kinetic energy and diffuse out.
Document Krenkel W.Cost Effective Processing of Cmc Composites by Melt
Infiltration (Lsi‐Process)[M]//25th Annual Conference on Composites,Advanced
Ceramics, Materials,and Structures:A:Ceramic Engineering and Science
Proceedings, Volume 22, Issue 3.John Wiley&Sons, Inc., 2008:443-454. disclose a kind of logical
Cross controlled in porous carbon fiber precast body with liquid silicon infiltration process cost and obtain C/SiC brake material, at
Function is for the high-grade cars such as Porsche (Porsche9llTurbo), Bentley, Bugatti, Lamborghini sport car and Audi.Text
Offer Fan S, Zhang L, Cheng L, et al.Effect of braking pressure and braking speed on
the tribological properties of C/SiC aircraft brake materials[J].Composites
Science&Technology, 2010,70 (6): 959-965. discloses a kind of D refraction statics C/SiC brake material of preparing
Method, it is this using chemical vapor infiltration (CVI technique) combine liquid silicon infiltration (LSI technique) preparation brake material, at present this
Kind aircraft brake system realizes batch application at home.
Carbon is made pottery, and brake material is high and stable with coefficient of friction, and coefficient of friction decaying is small under hygrometric state condition, wear-resistant, by force
Degree is high, and the excellent properties such as long service life are the brake materials of new generation of great competitiveness.Since brake material is repeatedly hot
Work under conditions of impact, frictional interface temperature is high, brake interface will form heat spot cause in frictional interface pyrolytic carbon and
Carbon fiber oxidation, leads to material serious wear；More seriously, since brake temperature is excessively high, it is tight to will lead to brake disc junction
Re-oxidation deformation, causes Joint failure, and catastrophic failure occurs.Therefore, introducing can be anti-oxidation and be had in carbon pottery brake material
There are self-healing crackle ability, and the filler that specific heat capacity is high, the anti-of carbon pottery brake material carbon fiber and carbon base body can be effectively improved
Oxidability reduces brake temperature and is of great significance.
High Speed Train in China covering Speed 200 km/h is tight at 380 kilometers of speed per hour to 380 kilometers of each speed class at present
When bringing to a halt, brake temperature has been up to 900-1000 DEG C, reaches the operating limit of powder metallurgy or steel brake material.And high-speed rail is thought
To raise speed again, at present used in the brake demand of powder metallurgy or steel brake material when cannot bear emergency.Carbon
Brake material of making pottery will become ideal brake material of the speed per hour higher than 380 kilometers when, B4C modified carbon pottery brake material will be more applicable
It brakes in high-speed rail of the speed per hour higher than 380 kilometers.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of B4The preparation of the modified C/C-SiC brake material of C
Method can carry high aircraft disk type brake material for brake, in order to overcome brake temperature is excessively high to lead to friction and wear behavior
It is unstable, high specific heat ingredient is introduced in brake material, improves the specific heat capacity of brake material, reduces brake temperature；For disk/piece
Clamp-type brake system introduces the anti-oxidation constituent element of self-healing in brake material, to improve the ability of the anti-oxidant abrasion of brake material,
Improve the service life of brake material.
Technical solution
A kind of B4The preparation method of the modified C/C-SiC brake material of C, it is characterised in that steps are as follows:
Step 1: by B4C powder is added in the carboxymethyl fiber bundle sodium CMC aqueous solution that mass fraction is 0.5%~1.5%,
Spheroidal graphite 24~48 hours made above to obtain B4C slurry；
Step 2: being 0.4~0.6g/cm by density under vacuum conditions3D refraction statics carbon fiber felt immerses B4In C slurry,
It then passes to inert gas and is pressurized to 0.5~3MPa, 30~60min of pressure maintaining then takes out drying, obtains containing B4C powder
D refraction statics carbon fiber precast body；
Step 3: by D refraction statics carbon fiber precast body by chemical vapor infiltration CVI deposition pyrolytic carbon or by containing carbon poly
It closes object infiltration pyrolysis method PIP and obtains C/C composite material；Vacuum high-temperature heat treatment is carried out again；
Step 4: C/C composite material being subjected to siliconising processing in vacuum high temperature furnace, reaction melt is alloy containing Si, in furnace
Air pressure is lower than 50Pa, and reaction temperature is 1300~1900 DEG C, and soaking time is 0.5~4h, and subsequent cooled to room temperature obtains
B4C is modified C/C-SiC brake material.
It is 5: 1~2 (H that mass ratio is added in the step 12O:B4C B)4C powder.
Prepared by the step 3 contains B4The density of the C/C composite material of C powder is 1.3~1.7g/cm3, technological parameter
Are as follows: propylene is as precursor, and in the prefabricated internal deposition PyC of D refraction statics fiber C, depositing temperature is 930 DEG C, and sedimentation time is
300h。
The treatment temperature of the vacuum high-temperature heat treatment of the step 3 is 2500 DEG C, soaking time lh.
The B4The partial size of C powder is less than 5um.
Beneficial effect
A kind of B proposed by the present invention4The preparation method of the modified C/C-SiC brake material of C, B4C is hard with SiC as ceramic phase
Degree quite, is all high temperature resistant, wear-resistant ceramic, can improve the friction and wear behavior of material.The B of frictional interface4C is oxidized to B2O3
Can heal the defect of frictional interface, prevent the oxidative wear of pyrolytic carbon and carbon fiber, protect the toughening effect of carbon fiber, drop
The low brittle flaking off of frictional interface.B4C has higher specific heat, and a certain amount of B is added4C can effectively improve the ratio of material
Thermal capacitance reduces brake temperature, improves friction and wear behavior.
So introducing high specific heat modified filler B in carbon pottery brake material4C can effectively increase the specific heat of brake material, from
And brake temperature is reduced, and B4C can play a protective role to carbon fiber and carbon base body in oxidation process, reduce material oxidation
Abrasion, improves the stability of brake material friction and wear behavior, while improving the reliability that carbon pottery brake material is on active service.Therefore,
B4The modified C/C-SiC brake material of C will become carbon pottery brake material of new generation.
The present invention is about 0.4~0.6g/cm in initial density using vacuum pressure impregnating method3It is introduced in D refraction statics carbon felt
B4C powder, and the method for combining chemical vapor infiltration (CVI) and reactive melt infiltration (RMI) to prepare C/C-SiC brake material.
Using B4C is modified C/C-SiC brake material, one side B4C there is protection to make carbon fiber and carbon base body as self-healing constituent element
With the inoxidizability of material can be significantly improved；On the other hand, B4C has higher specific heat capacity, can improve the whole ratio of material
Brake temperature is effectively reduced in heat, improves material friction stability.
Detailed description of the invention
Fig. 1 is B4The preparation technology flow chart of the modified C/C-SiC brake material of C
Fig. 2 is C/C-B in the embodiment of the present invention 14C-SiC brake material XRD spectrum
Fig. 3 is C/C-B in the embodiment of the present invention 14C-SiC brake material surface SEM photograph
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Embodiment 1:
Step 1, the preparation of fiber C precast body:
Staple fiber tire net and laminated cloth is made in PAN base T-300 (6~50K) carbon fiber first, then by 0 ° of single layer without latitude
Cloth, tire net, 90 ° of laminated cloths, tire net circuit sequentially superposition laying, and needling technique is recycled to be integrally formed laminated cloth and tire net.
Thickness as needed obtains D refraction statics carbon fiber precast body by lamination repeatedly, needle thorn, lamination, needle thorn ....Precast body
Density is about 0.55g/cm3, tire stratum reticulare density is about 0.2g/cm3, laminated cloth layer density is about 0.6g/cm3, the body of carbon fiber
Product content is about 40%, and layer density is about 14 layers/10mm.
Step 2, B4The preparation of C slurry:
The CMC (sodium carboxymethylcellulose) of 0.5wt% is added in distilled water, be uniformly mixed and is adjusted with ammonium hydroxide and hydrochloric acid
For pH value to 11~12, it is 5:1 (H that mass ratio, which is then added,2O:B4C B)4C powder obtains uniformly mixed B through ball milling for 24 hours4C
Slurry.
Step 3, vacuum pressure impregnating slurry:
The obtained D refraction statics carbon fiber precast body of step 1 is put into impregnating autoclave, after vacuumizing 30min, injection
B4C slurry is forced into 0.9MPa by inert gas, takes out after impregnating about 30min, and dry 4h is contained under the conditions of 150 DEG C
There is B4The D refraction statics carbon fiber precast body of C powder.
Step 4, containing B4The preparation of the C/C composite material of C:
Using propylene as precursor, in the prefabricated internal deposition PyC of D refraction statics fiber C, depositing temperature is 930 DEG C, deposition
Time is 300h, and preparing density is 1.5g/cm3Contain B4The C/C composite material of C powder.Deposition is obtained containing B4The C/C of C
Composite material carries out vacuum high-temperature heat treatment, and treatment temperature is 2500 DEG C, soaking time lh.
Step 5, reaction melt infiltrates:
Step 4 is resulting containing B4The C/C composite material of C powder under vacuum conditions, passes through reaction melt Infiltration Technics
Prepare B4C is modified C/C-SiC brake material.Reaction melt is Si, and air pressure is lower than 50Pa in furnace, and reaction temperature is 1580 DEG C, is protected
The warm time is 1h.
B4The modified C/C-SiC brake material XRD result of C is as shown in Fig. 2, show material by C, SiC, B4Tetra- kinds of objects of C and Si
Phase composition.Material SEM photograph is as shown in figure 3, show B4C is primarily present in the macrovoid inside tire stratum reticulare.Modified C/C-
SiC material and the 700 DEG C of oxidation 10h mass loss comparisons of unmodified material are as shown in table 1:
Table 1
Mass loss rate after 1 material of table, 700 DEG C of oxidation 10h
As seen from table, B4C powder, which is introduced, has significant increase to itself inoxidizability of C/C-SiC material, plays to material
Effect is effectively protected.
Modified C/C-SiC material and the variation of unmodified quality of materials thermal capacitance J/ (gK) are as shown in table 2:
Table 2
The mass specific heat of 2 material of table
As seen from table, B4The introducing of C powder can effectively improve material specific heat, advantageously reduce brake temperature.
Embodiment 2:
Step 1, the preparation of fiber C precast body:
Staple fiber tire net and laminated cloth is made in PAN base T-300 (6~50K) carbon fiber first, then by 0 ° of single layer without latitude
Cloth, tire net, 90 ° of laminated cloths, tire net circuit sequentially superposition laying, and needling technique is recycled to be integrally formed laminated cloth and tire net.
Thickness as needed obtains D refraction statics carbon fiber precast body by lamination repeatedly, needle thorn, lamination, needle thorn ....Precast body
Density is about 0.55g/cm3, tire stratum reticulare density is about 0.2g/cm3, laminated cloth layer density is about 0.6g/cm3, the body of carbon fiber
Product content is about 40%, and layer density is about 14 layers/10mm.
Step 2, B4The preparation of C slurry:
The CMC (sodium carboxymethylcellulose) of 1.0wt% is added in distilled water, be uniformly mixed and is adjusted with ammonium hydroxide and hydrochloric acid
For pH value to 11~12, it is 5: 2 (H that mass ratio, which is then added,2O:B4C B)4C powder obtains uniformly mixed B through ball milling 48h4C
Slurry.
Step 3, vacuum pressure impregnating slurry:
The obtained D refraction statics carbon fiber precast body of step 1 is put into impregnating autoclave, after vacuumizing 30min, injection
B4C slurry is forced into 1.5MPa by inert gas, takes out after impregnating about 60min, and dry 4h is contained under the conditions of 150 DEG C
There is B4The D refraction statics carbon fiber precast body of C powder.
Step 4, containing B4The preparation of the C/C composite material of C:
Using propylene as precursor, in the prefabricated internal deposition PyC of D refraction statics fiber C, depositing temperature is 930 DEG C,
Sedimentation time is 300h, and preparing density is 1.6g/cm3Contain B4The C/C composite material of C powder.Deposition is obtained
Contain B4The C/C composite material of C carries out vacuum high-temperature heat treatment, and treatment temperature is 2500 DEG C, soaking time lh.
Step 5, reaction melt infiltrates:
Step 4 is resulting containing B4The C/C composite material of C powder under vacuum conditions, passes through reaction melt Infiltration Technics
Prepare B4C is modified C/C-SiC brake material.Reaction melt is Fe-Si alloy, and air pressure is lower than 50Pa in furnace, and reaction temperature is
1500 DEG C, soaking time 2h.
Claims (1)
1. a kind of B4The preparation method of the modified C/C-SiC brake material of C, it is characterised in that steps are as follows:
Step 1: by B4C powder is added in the sodium carboxymethylcellulose CMC aqueous solution that mass fraction is 0.5%~1.5%, spheroidal graphite
24~48 hours made above to obtain B4C slurry；
Step 2: being 0.4~0.6g/cm by density under vacuum conditions3D refraction statics carbon fiber felt immerses B4In C slurry, then
It is passed through inert gas and is pressurized to 0.5~3MPa, 30~60min of pressure maintaining then takes out drying, obtains containing B4The three-dimensional of C powder
Needled carbon fiber preform；
Step 3: by D refraction statics carbon fiber precast body by chemical vapor infiltration CVI deposition pyrolytic carbon or by containing carbon polymer
Infiltration pyrolysis method PIP obtains C/C composite material；Vacuum high-temperature heat treatment is carried out again；
Step 4: C/C composite material being subjected to siliconising processing in vacuum high temperature furnace, reaction melt is alloy containing Si, air pressure in furnace
Lower than 50Pa, reaction temperature is 1300~1900 DEG C, and soaking time is 0.5~4h, and subsequent cooled to room temperature obtains B4C
Modified C/C-SiC brake material；
It is 5: 1~2 (H that mass ratio is added in the step 12O:B4C B)4C powder；
The alloy containing Si is Si or Si-Zr alloy, Fe-Si alloy, Si-Al alloy；
Prepared by the step 3 contains B4The density of the C/C composite material of C powder is 1.3~1.7g/cm3, technological parameter are as follows: third
Alkene is as precursor, and in the prefabricated internal deposition PyC of D refraction statics fiber C, depositing temperature is 930 DEG C, sedimentation time 300h；
The treatment temperature of the vacuum high-temperature heat treatment of the step 3 is 2500 DEG C, soaking time lh；
The B4The partial size of C powder is less than 5 μm.
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| CN109306440B (en) * | 2018-12-08 | 2021-11-05 | 马鞍山市雷狮轨道交通装备有限公司 | C-C-B4C-combined tread sweeper grinder and preparation method thereof |
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| US20210387441A1 (en) * | 2020-06-15 | 2021-12-16 | Goodrich Corporation | Composites and methods of forming composites having an increased volume of ceramic particles |
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| CN114656275B (en) * | 2022-03-11 | 2023-08-04 | 西北工业大学 | SiC preparation by vacuum impregnation combined with reaction melt infiltration f Method for preparing/Si-Y-B-C composite material |
| CN115784759B (en) * | 2022-12-07 | 2023-09-26 | 湖南金博碳素股份有限公司 | Carbon/boron carbide composite material and preparation method and application thereof |
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