CN106478125A - A kind of B4The preparation method of C modification C/C SiC brake material - Google Patents
A kind of B4The preparation method of C modification C/C SiC brake material Download PDFInfo
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- CN106478125A CN106478125A CN201610858805.9A CN201610858805A CN106478125A CN 106478125 A CN106478125 A CN 106478125A CN 201610858805 A CN201610858805 A CN 201610858805A CN 106478125 A CN106478125 A CN 106478125A
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- 239000000463 material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 230000004048 modification Effects 0.000 title claims abstract description 21
- 238000012986 modification Methods 0.000 title claims abstract description 21
- 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
- 238000000034 method Methods 0.000 claims abstract description 19
- 230000003068 static effect Effects 0.000 claims abstract description 19
- 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
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000000151 deposition Methods 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 239000000835 fiber Substances 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 230000014759 maintenance of location Effects 0.000 claims description 7
- 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 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001467 acupuncture Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 150000002835 noble gases Chemical class 0.000 claims description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 4
- 239000002296 pyrolytic carbon Substances 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 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
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 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
- 239000002245 particle 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
- 229920000642 polymer Polymers 0.000 claims 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 abstract description 18
- 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 10
- 239000010410 layer Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000002289 liquid silicon infiltration Methods 0.000 description 2
- 230000001590 oxidative effect Effects 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
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005470 impregnation Methods 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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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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
- 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
- C04B35/573—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 obtained by reaction sintering or recrystallisation
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
The present invention relates to a kind of B4The preparation method of C modification C/C SiC brake material, is about 0.4～0.6g/cm using vacuum pressure impregnating method in initial density3B is introduced in D refraction statics carbon felt4C powder, and combine the method that chemical vapor infiltration (CVI) and reactive melt infiltration (RMI) prepare C/C SiC brake material.Using B4C modification C/C SiC brake material, one side B4C has protective effect as self-healing constituent element to carbon fiber and carbon base body, can significantly improve the non-oxidizability of material；On the other hand, B4C has higher specific heat capacity, can improve the overall specific heat of material, effectively reduces brake temperature, improves material friction stability.
Description
Technical field
The invention belongs to the preparation method of C/C-SiC composite, it is related to a kind of B4C modification C/C-SiC brake material
Preparation method, be a kind of using vacuum pressure impregnation by B4C powder introduces D refraction statics carbon fiber precast body, and by chemical gas
Mutually deposition association reaction melt Infiltration Technics preparation B4The method of C modification C/C-SiC brake material.
Background technology
Brake gear is aircraft, high ferro, automobile realization braking, ensures the core component running safety, mainly passes through friction
The relative motion on surface converts kinetic energy into heat energy to realize the purpose braked.In braking procedure, brake gear is when extremely short
Interior huge kinetic energy be converted into heat 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. disclosing a kind of logical
Cross to control cost the C/SiC brake material obtaining with liquid silicon infiltration process in porous carbon fiber precast body, become
Work(is used for the high-grade cars such as Porsche (Porsche9llTurbo), Bentley, Bugatti, Lamborghini sport car and Audi.Document
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 side preparing D refraction statics C/SiC brake material
Method, this employing chemical vapor infiltration (CVI technique) combines brake material prepared by liquid silicon infiltration (LSI technique), this at present
Aircraft brake system has realized batch application at home.
Carbon pottery brake material has coefficient of friction height and stable, and under hygrometric state condition, coefficient of friction decay is little, 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.Because brake material is in heat repeatedly
Work under conditions of impact, frictional interface temperature is high, brake interface can be formed heat spot cause in frictional interface pyrolytic carbon and
Carbon fiber aoxidizes, and leads to material serious wear；More seriously, because brake temperature is too high, brake disc junction can be led to tight
Re-oxidation deforms, and causes Joint failure, and catastrophic failure occurs.Therefore, in carbon pottery brake material, introducing energy is anti-oxidation and has
There is self-healing crackle ability, and a high filler of specific heat capacity, carbon can be effectively improved and make pottery the anti-of brake material carbon fiber and carbon base body
Oxidability, reduces brake temperature significant.
High Speed Train in China covers Speed 200 km/h to 380 kilometers of each speed class at present, tight in 380 kilometers of speed per hour
When bringing to a halt, up to 900-1000 DEG C of brake temperature, reach powder metallurgy or the operating limit of steel brake material.And high ferro is thought
To raise speed again, the powder metallurgy being used at present or steel brake material can not bear brake demand during emergency.Carbon
Pottery brake material will become the preferable brake material that speed per hour is higher than when 380 kilometers, B4The modified carbon pottery brake material of C will be more applicable
It is higher than 380 kilometers of high ferro brake in speed per hour.
Content of the invention
Technical problem to be solved
In place of the deficiencies in the prior art, the present invention proposes a kind of B4The preparation of C modification C/C-SiC brake material
Method, carries high aircraft disk type brake material for Brake Energy, brake temperature is too high to lead to friction and wear behavior in order to overcome
Unstable, brake material introduces high specific heat composition, improves the specific heat capacity of brake material, reduce 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 brake material antioxidation abrasion,
Improve the service life of brake material.
Technical scheme
A kind of B4The preparation method of C modification C/C-SiC brake material is it is characterised in that step is 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 is made above to obtain B4C slurry；
Step 2：Under vacuum, by density be 0.4～0.6g/cm3D refraction statics carbon fiber felt immerses B4In C slurry,
Then pass to noble gases and be pressurized to 0.5～3MPa, pressurize 30～60min, then take out drying, obtain containing B4C powder
D refraction statics carbon fiber precast body；
Step 3：D refraction statics carbon fiber precast body is deposited pyrolytic carbon or by containing carbon poly by chemical vapor infiltration CVI
Compound infiltration pyrolysis method PIP obtains C/C composite；Carry out vacuum high-temperature heat treatment again；
Step 4：C/C composite is carried out siliconising process in vacuum high temperature furnace, reaction melt is alloy containing Si, in stove
Air pressure is less than 50Pa, and reaction temperature is 1300～1900 DEG C, and temperature retention time is 0.5～4h, subsequently naturally cools to room temperature, obtains
B4C modification C/C-SiC brake material.
Mass ratio is added to be 5: 1～2 (H in described step 12O:B4C B)4C powder.
Prepared by described step 3 contains B4The density of the C/C composite of C powder is 1.3～1.7g/cm3, technological parameter
For：As precursor, in D refraction statics fiber C prefabricated internal deposition PyC, depositing temperature is 930 DEG C to propylene, and sedimentation time is
300h.
The treatment temperature of the vacuum high-temperature heat treatment of described step 3 is 2500 DEG C, and temperature retention time is lh.
Described B4The particle diameter of C powder is less than 5um.
Beneficial effect
A kind of B proposed by the present invention4The preparation method of C modification C/C-SiC brake material, 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 be healed the defect of frictional interface, stop the oxidative wear of pyrolytic carbon and carbon fiber, protect the toughening effect of carbon fiber, fall
The low brittle flaking off of frictional interface.B4C has higher specific heat, adds a certain amount of B4C, 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 be effectively increased the specific heat of brake material, from
And reduce brake temperature, and B4C can play a protective role to carbon fiber and carbon base body in oxidizing process, reduces material oxidation
Abrasion, improves the stability of brake material friction and wear behavior, improves the reliability that carbon pottery brake material is on active service simultaneously.Therefore,
B4C modification C/C-SiC brake material will become carbon pottery brake material of new generation.
The present invention adopts vacuum pressure impregnating method to be about 0.4～0.6g/cm in initial density3Introduce in D refraction statics carbon felt
B4C powder, and combine the method that chemical vapor infiltration (CVI) and reactive melt infiltration (RMI) prepare C/C-SiC brake material.
Using B4C modification C/C-SiC brake material, one side B4C has protection as self-healing constituent element and makees to carbon fiber and carbon base body
With the non-oxidizability of material can be significantly improved；On the other hand, B4C has higher specific heat capacity, can improve the entirety ratio of material
Heat, effectively reduces brake temperature, improves material friction stability.
Brief description
Fig. 1 is B4The preparation technology flow chart of C modification C/C-SiC brake material
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
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1：
Step 1, the preparation of fiber C precast body：
First PAN base T-300 (6～50K) carbon fiber is made chopped fiber tire net and laminated cloth, then by 0 ° of monolayer no latitude
Cloth, tire net, 90 ° of laminated cloth, tire nets circulate superposition laying successively, recycle needling technique so that laminated cloth and tire net is integrally formed.
Thickness as needed, through lamination repeatedly, acupuncture, lamination, acupuncture ..., obtains D refraction statics carbon fiber precast body.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 volume of carbon fiber
Content is about 40%, and layer density is about 14 layers/10mm.
Step 2, B4The preparation of C slurry：
Add the CMC (sodium carboxymethyl cellulose) of 0.5wt% in distilled water, mix homogeneously is simultaneously adjusted with ammonia and hydrochloric acid
PH value, to 11～12, is subsequently adding mass ratio for 5：1(H2O:B4C B)4C powder, the B being uniformly mixed through ball milling 24h4C
Slurry.
Step 3, vacuum pressure impregnating slurry：
D refraction statics carbon fiber precast body obtained by step 1 is put in impregnating autoclave, after evacuation 30min, injects B4C
Slurry, is forced into 0.9MPa by noble gases, takes out, 4h is dried and is contained under the conditions of 150 DEG C after dipping about 30min
B4The D refraction statics carbon fiber precast body of C powder.
Step 4, containing B4The preparation of the C/C composite of C：
Using propylene as precursor, in D refraction statics fiber C prefabricated internal deposition PyC, depositing temperature is 930 DEG C, deposition
Time is 300h, and preparing density is 1.5g/cm3Containing B4The C/C composite of C powder.Deposition is obtained containing B4The C/C of C
Composite carries out vacuum high-temperature heat treatment, and treatment temperature is 2500 DEG C, and temperature retention time is lh.
Step 5, reaction melt infiltrates：
By step 4 gained containing B4The C/C composite of C powder under vacuum, by reaction melt Infiltration Technics
Preparation B4C modification C/C-SiC brake material.Reaction melt is Si, and stove internal gas pressure is less than 50Pa, and reaction temperature is 1580 DEG C, protects
The warm time is 1h.
B4C modification C/C-SiC brake material XRD result is as shown in Fig. 2 show material by C, SiC, B4Tetra- kinds of thing phases of C and Si
Composition.Material SEM photograph is as shown in figure 3, show B4C is primarily present in the macrovoid within tire stratum reticulare.Modified C/C-SiC
Material is with unmodified 700 DEG C of oxidation 10h mass loss contrasts of material as shown in table 1：
Table 1
Mass loss rate after 700 DEG C of oxidation 10h of table 1 material
As seen from table, B4C powder introduces has significant increase to itself non-oxidizability of C/C-SiC material, and material is played
It is effectively protected effect.
Modified C/C-SiC material is with unmodified quality of materials thermal capacitance J/ (g K) change as shown in table 2：
Table 2
The mass specific heat of table 2 material
As seen from table, B4The introducing of C powder can effectively improve material specific heat, advantageously reduces brake temperature.
Embodiment 2：
Step 1, the preparation of fiber C precast body：
First PAN base T-300 (6～50K) carbon fiber is made chopped fiber tire net and laminated cloth, then by 0 ° of monolayer no latitude
Cloth, tire net, 90 ° of laminated cloth, tire nets circulate superposition laying successively, recycle needling technique so that laminated cloth and tire net is integrally formed.
Thickness as needed, through lamination repeatedly, acupuncture, lamination, acupuncture ..., obtains D refraction statics carbon fiber precast body.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 volume of carbon fiber
Content is about 40%, and layer density is about 14 layers/10mm.
Step 2, B4The preparation of C slurry：
Add the CMC (sodium carboxymethyl cellulose) of 1.0wt% in distilled water, mix homogeneously is simultaneously adjusted with ammonia and hydrochloric acid
PH value, to 11～12, is subsequently adding mass ratio for 5: 2 (H2O:B4C B)4C powder, the B being uniformly mixed through ball milling 48h4C
Slurry.
Step 3, vacuum pressure impregnating slurry：
D refraction statics carbon fiber precast body obtained by step 1 is put in impregnating autoclave, after evacuation 30min, injects B4C
Slurry, is forced into 1.5MPa by noble gases, takes out, 4h is dried and is contained under the conditions of 150 DEG C after dipping about 60min
B4The D refraction statics carbon fiber precast body of C powder.
Step 4, containing B4The preparation of the C/C composite of C：
Using propylene as precursor, in D refraction statics fiber C prefabricated internal deposition PyC, depositing temperature is 930 DEG C,
Sedimentation time is 300h, and preparing density is 1.6g/cm3Containing B4The C/C composite of C powder.Deposition is obtained
Containing B4The C/C composite of C carries out vacuum high-temperature heat treatment, and treatment temperature is 2500 DEG C, and temperature retention time is lh.
Step 5, reaction melt infiltrates：
By step 4 gained containing B4The C/C composite of C powder under vacuum, by reaction melt Infiltration Technics
Preparation B4C modification C/C-SiC brake material.Reaction melt is Fe-Si alloy, and stove internal gas pressure is less than 50Pa, and reaction temperature is
1500 DEG C, temperature retention time is 2h.
Claims (5)
1. a kind of B4The preparation method of C modification C/C-SiC brake material is it is characterised in that step is 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：Under vacuum, by density be 0.4～0.6g/cm3D refraction statics carbon fiber felt immerses B4In C slurry, then
It is passed through noble gases and is pressurized to 0.5～3MPa, pressurize 30～60min, then take out drying, obtain containing B4The three-dimensional of C powder
Acupuncture carbon fiber precast body；
Step 3：D refraction statics carbon fiber precast body is deposited pyrolytic carbon or by containing carbon polymer by chemical vapor infiltration CVI
Infiltration pyrolysis method PIP obtains C/C composite；Carry out vacuum high-temperature heat treatment again；
Step 4：C/C composite is carried out in vacuum high temperature furnace siliconising process, reaction melt is alloy containing Si, stove internal gas pressure
Less than 50Pa, reaction temperature is 1300～1900 DEG C, and temperature retention time is 0.5～4h, subsequently naturally cools to room temperature, obtains B4C
Modified C/C-SiC brake material.
2. B according to claim 14C modification C/C-SiC brake material preparation method it is characterised in that：In described step 1
Addition mass ratio is 5: 1～2 (H2O:B4C B)4C powder.
Described alloy containing Si is Si or Si-Zr alloy, Fe-Si alloy, Si-Al alloy.
3. B according to claim 1 or claim 24C modification C/C-SiC brake material preparation method it is characterised in that：Described step
3 preparation contain B4The density of the C/C composite of C powder is 1.3～1.7g/cm3, technological parameter is：Propylene is as pioneer
Body, in D refraction statics fiber C prefabricated internal deposition PyC, depositing temperature is 930 DEG C, and sedimentation time is 300h.
4. B according to claim 1 or claim 24C modification C/C-SiC brake material preparation method it is characterised in that：Described step
The treatment temperature of 3 vacuum high-temperature heat treatment is 2500 DEG C, and temperature retention time is lh.
5. B according to claim 1 or claim 24C modification C/C-SiC brake material preparation method it is characterised in that：Described B4C
The particle diameter of powder is less than 5um.
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