CN117466625A - 复合碳纤维的碳陶刹车盘的复合工艺 - Google Patents
复合碳纤维的碳陶刹车盘的复合工艺 Download PDFInfo
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- CN117466625A CN117466625A CN202311427909.0A CN202311427909A CN117466625A CN 117466625 A CN117466625 A CN 117466625A CN 202311427909 A CN202311427909 A CN 202311427909A CN 117466625 A CN117466625 A CN 117466625A
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- ceramic
- brake disc
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- 239000000919 ceramic Substances 0.000 title claims abstract description 93
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 44
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 40
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000008569 process Effects 0.000 title claims abstract description 21
- 238000013329 compounding Methods 0.000 title claims 7
- 239000002131 composite material Substances 0.000 claims abstract description 52
- 239000000835 fiber Substances 0.000 claims abstract description 50
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000010936 titanium Substances 0.000 claims abstract description 34
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 34
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 239000000853 adhesive Substances 0.000 claims description 18
- 230000001070 adhesive effect Effects 0.000 claims description 18
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 17
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 claims description 14
- 238000007731 hot pressing Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 claims description 9
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 9
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 9
- POJMWJLYXGXUNU-UHFFFAOYSA-N 6-(6-oxo-1h-pyridin-2-yl)-1h-pyridin-2-one Chemical compound N1C(=O)C=CC=C1C1=CC=CC(=O)N1 POJMWJLYXGXUNU-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- SKOWZLGOFVSKLB-UHFFFAOYSA-N hypodiboric acid Chemical compound OB(O)B(O)O SKOWZLGOFVSKLB-UHFFFAOYSA-N 0.000 claims description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 7
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 7
- 244000226021 Anacardium occidentale Species 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
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- 239000001038 titanium pigment Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 7
- 239000011347 resin Substances 0.000 abstract description 7
- ZOCHARZZJNPSEU-UHFFFAOYSA-N diboron Chemical group B#B ZOCHARZZJNPSEU-UHFFFAOYSA-N 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 2
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- 238000000465 moulding Methods 0.000 abstract description 2
- 239000011241 protective layer Substances 0.000 abstract description 2
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- 125000002524 organometallic group Chemical group 0.000 description 24
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920006282 Phenolic fiber Polymers 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002783 friction material Substances 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 238000005475 siliconizing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
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- -1 high strength Chemical compound 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D65/00—Parts or details
- F16D65/02—Braking members; Mounting thereof
- F16D65/12—Discs; Drums for disc brakes
- F16D65/125—Discs; Drums for disc brakes characterised by the material used for the disc body
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C04B33/36—Reinforced clay-wares
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Abstract
本发明涉及刹车盘技术领域，具体关于一种复合碳纤维的碳陶刹车盘的复合工艺；本发明的二硼基团的有机金属钛改性陶瓷纤维制备的复合碳纤维的碳陶刹车盘，有机金属钛促进了碳纤维与陶瓷基体的界面反应；此外，有机金属钛还可以通过化学气相沉积等方法在碳纤维表面形成一层致密的钛碳化物保护层，提高碳纤维的抗氧化性能；将制备好的复合碳纤维与陶瓷纤维进行混合，然后在一定温度和压力下进行热压成型，得到碳陶刹车盘；由于复合碳纤维的增强作用以及二硼基团和有机金属钛的改性效果，使得碳陶刹车盘的摩擦磨损性能得到显著提高；具有较好的摩擦磨损性能，线磨损率远远低于树脂基刹车片。
Description
技术领域
本发明属于刹车盘技术领域，具体涉及一种复合碳纤维的碳陶刹车盘的复合工艺。
背景技术
刹车片是动力机械和机动车辆必须装配的制动材料，其性能直接影响车辆、设备使用的稳定性和可靠性。碳纤维复合材料刹车片，是采用碳纤维为增强材料制成的一类摩擦材料，充分利用了碳纤维在物理性能上具有强度大、模量高、密度低、导热好、耐热、耐摩擦等特点。
中国专利CN116373074A：公开了复合碳纤维的碳陶刹车盘的复合工艺及其设备，具体包括以下步骤：S1、高温回收：在复合碳纤维的碳陶刹车盘生产过程中，在进行浸渗固化处理、热处理、碳化处理等高温处理(温度≥100℃)工序时，均在回收机构的高温烘室内部进行，且在高温烘室内部高温处理后，一侧水箱由保温室运动至高温烘室内部，通过内部液态水对热量进行吸收；S2、余热烘干：在低温烘室进行短切碳纤维预浸料烘干等低温处理(温度＜100℃)工序时，涉及碳纤维复合材料制造技术领域，解决了现有碳纤维碳陶刹车盘生产工艺，在生产过程中需要使用较多加热设备，以及加热后热量浪费，不仅增大了生产成本，且不符合节能环保的问题。
中国专利CN111892416A：提供了一种碳陶刹车材料的制备方法。该方法通过将低密度碳/碳坯体置于硅粉浸渍浆料中，浸渍完成后烘干，然后将硅粉浸渍后的碳/碳坯体装入硅化处理炉中，高温下碳坯体内的硅粉与坯体表面的沉积碳原位发生熔融化学反应，形成SiC陶瓷相。该方法无需在熔融渗硅过程中使用工装坩埚，节省了装炉空间和渗硅原材料。且工艺简单，实施方便，渗硅量易控易调，形成的陶瓷相弥散性、均匀性好，残留硅含量低，性能稳定。
以上专利及现有技术制备的刹车盘，主要使用半金属摩擦材料、无石棉有机摩擦材料及少量石棉刹车片；由于石棉是强致癌物质，不符合环保要求；无石棉有机制动材料存在耐热性能低；半金属摩擦材料又存在密度较大、产生噪音等不足；尽管C/C复合材料性能优异，但其成本较高，通常只能在飞机及高档赛车上使用。
发明内容
针对上述常规方法制备的刹车盘的缺陷，本发明的目的在于提供一种复合碳纤维的碳陶刹车盘的复合工艺。
本发明限定的一种复合碳纤维的碳陶刹车盘的复合工艺，制备得到的碳陶刹车盘的摩擦磨损性能得到显著提高，具有较好的摩擦磨损性能，线磨损率远远低于树脂基刹车片。具体操作步骤：
S1：按重量份，称取5-10份改性磷酸盐胶黏剂，20-30份有机金属钛改性陶瓷纤维，2-7份矿物纤维、1-3份芳纶纤维，10-20份石墨，5-10份腰果壳油摩擦粉，20-30份填料，3-5份环氧改性酚醛树脂，混合均匀后，热压；
S2：热压后的复合材料，在真空条件下，进行热处理；
S3：热处理后的复合材料，经加工成型，得复合碳纤维的碳陶刹车盘。
进一步地，其中所述的S1的热压温度为150-180℃。
进一步地，其中所述的S2的热处理温度为1500-1600℃。
进一步地，其中所述的填料为高岭土、滑石粉、硅灰石、钛白粉、重晶石粉中的一种或多种。
进一步地，其中所述的改性磷酸盐胶黏剂的制备方法为：
A1：按重量份，称取10-20份磷酸、3-7份氢氧化铝，于反应釜中，升温至80-100℃，反应50-90min；
A2：继续加入质量分数为2-10％的氧化铬粉末，继续在反应50-90min；
A3：反应结束后，冷却至室温，最后加入0.5-2份固化剂，升温至40-60℃，反应50-70min，得到改性磷酸盐胶黏剂。
进一步地，其中所述的有机金属钛改性陶瓷纤维的制备方法为：
B1：按照质量份数，取100-120份陶瓷纤维放于1500-1800份水中，加入3-6份3-异氰酸酯基丙基三甲氧基硅烷，于32-45℃下反应50-100分钟，过滤，烘干，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
B2：按照质量份数，取3-6份硝酸钛，0.06-0.3份硝酸镧，5-10份6,6'-二羟基-2,2'-联吡啶，500-750份N,N-二甲基甲酰胺中，通入氮气，于32-45℃下反应40-80分钟，得到钛/镧有机金属前驱体；
B3：在反应釜中再加入80-100份3-异氰酸酯基硅烷处理的陶瓷纤维，0.08-0.6份四羟基二硼，2-4份辛酸亚锡，60-85℃下反应40-80分钟，过滤，干燥，得到有机金属钛改性陶瓷纤维。
进一步地，其中所述的固化剂为氧化铬、氧化铝、氧化镁、二氧化硅。
上述有机金属钛改性陶瓷纤维的制备方法为：
S1：陶瓷纤维表面羟基与3-异氰酸酯基丙基三甲氧基硅烷，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
S2：硝酸钛，硝酸镧与6,6'-二羟基-2,2'-联吡啶生成金属配合物，得到钛/镧有机金属前驱体；
S3：3-异氰酸酯基硅烷处理的陶瓷纤维与四羟基二硼的羟基发生缩合反应，3-异氰酸酯基硅烷处理的陶瓷纤维与钛/镧有机金属前驱体的羟基的发生缩合反应，得到含二硼基团的有机金属钛改性陶瓷纤维。
通过采用上述技术，与现有技术相比，本发明的有益效果如下：
1、本发明制备的复合碳纤维的碳陶刹车盘，具有较高的抗弯强度、断裂韧性，可大幅提高刹车盘的力学性能；
2、含二硼基团的有机金属钛改性陶瓷纤维制备的复合碳纤维的碳陶刹车盘，有机金属钛促进了碳纤维与陶瓷基体的界面反应；此外，有机金属钛还可以通过化学气相沉积(CVD)等方法在碳纤维表面形成一层致密的钛碳化物(TiC)保护层，提高碳纤维的抗氧化性能。
3、碳陶刹车盘的制备及性能提升：将制备好的复合碳纤维与陶瓷纤维进行混合，然后在一定温度和压力下进行热压成型，得到碳陶刹车盘；由于复合碳纤维的增强作用以及二硼基团和有机金属钛的改性效果，使得碳陶刹车盘的摩擦磨损性能得到显著提高；具有较好的摩擦磨损性能，线磨损率远远低于树脂基刹车片；
4、含二硼基团的有机金属钛改性陶瓷纤维制备的复合碳纤维的碳陶刹车盘，具有密度适中、使用寿命长、制动舒适、环保、价格适宜等优点。
具体实施方式
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此。
本发明具体实施方式制备得到的刹车片性能评价方法参考如下：
1、抗弯强度：参照ASTMC1341-00标准，采用三点弯曲法测试材料的弯曲强度，加载速度为0.5mm/min；
2、断裂韧性：参照ASTME399-74标准，采用单边切口梁法测试材料的断裂韧性，加载速度为0.05mm/min；
3、线磨损率：采用MM-1000型摩擦磨损试验机测试。
实施例1
一种复合碳纤维的碳陶刹车盘的复合工艺，其操作步骤为：
S1：称取5g改性磷酸盐胶黏剂，20g有机金属钛改性陶瓷纤维，2g矿物纤维、1g芳纶纤维，10g石墨，5g腰果壳油摩擦粉，20g填料，3g环氧改性酚醛树脂，混合均匀后，热压；
S2：热压后的复合材料，在真空条件下，进行热处理；
S3：热处理后的复合材料，经加工成型，得复合碳纤维的碳陶刹车盘。
所述的S1的热压温度为150℃。
所述的S2的热处理温度为1500℃。
所述的填料为高岭土。
所述的改性磷酸盐胶黏剂的制备方法为：
A1：称取10g磷酸、3g氢氧化铝，于反应釜中，升温至80℃，反应50min；
A2：继续加入质量分数为2％的氧化铬粉末，继续在反应50min；
A3：反应结束后，冷却至室温，最后加入0.5g固化剂，升温至40℃，反应50min，得到改性磷酸盐胶黏剂。
所述的有机金属钛改性陶瓷纤维的制备方法为：
B1：取100g陶瓷纤维放于1500g水中，加入3g3-异氰酸酯基丙基三甲氧基硅烷，于32℃下反应50分钟，过滤，烘干，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
B2：取3g硝酸钛，0.06g硝酸镧，5g6,6'-二羟基-2,2'-联吡啶，500gN,N-二甲基甲酰胺中，通入氮气，于32℃下反应40分钟，得到钛/镧有机金属前驱体；
B3：在反应釜中再加入80g3-异氰酸酯基硅烷处理的陶瓷纤维，0.08g四羟基二硼，2g辛酸亚锡，60℃下反应40分钟，过滤，干燥，得到有机金属钛改性陶瓷纤维。
所述的固化剂为氧化铬。
实施例2
一种复合碳纤维的碳陶刹车盘的复合工艺，其操作步骤为：
S1：称取6g改性磷酸盐胶黏剂，24g有机金属钛改性陶瓷纤维，4g矿物纤维、2g芳纶纤维，14g石墨，6g腰果壳油摩擦粉，24g填料，4g环氧改性酚醛树脂，混合均匀后，热压；
S2：热压后的复合材料，在真空条件下，进行热处理；
S3：热处理后的复合材料，经加工成型，得复合碳纤维的碳陶刹车盘。
所述的S1的热压温度为160℃。
所述的S2的热处理温度为1540℃。
所述的填料为滑石粉。
所述的改性磷酸盐胶黏剂的制备方法为：
A1：称取14g磷酸、4g氢氧化铝，于反应釜中，升温至85℃，反应60min；
A2：继续加入质量分数为5％的氧化铬粉末，继续在反应60min；
A3：反应结束后，冷却至室温，最后加入1g固化剂，升温至45℃，反应55min，得到改性磷酸盐胶黏剂。
所述的有机金属钛改性陶瓷纤维的制备方法为：
B1：取105g陶瓷纤维放于1600g水中，加入4g3-异氰酸酯基丙基三甲氧基硅烷，于36℃下反应60分钟，过滤，烘干，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
B2：取4g硝酸钛，0.1g硝酸镧，6g6,6'-二羟基-2,2'-联吡啶，550gN,N-二甲基甲酰胺中，通入氮气，于36℃下反应50分钟，得到钛/镧有机金属前驱体；
B3：在反应釜中再加入85g3-异氰酸酯基硅烷处理的陶瓷纤维，0.2g四羟基二硼，3g辛酸亚锡，70℃下反应50分钟，过滤，干燥，得到有机金属钛改性陶瓷纤维。
所述的固化剂为氧化铝。
实施例3
一种复合碳纤维的碳陶刹车盘的复合工艺，其操作步骤为：
S1：称取8g改性磷酸盐胶黏剂，28g有机金属钛改性陶瓷纤维，6g矿物纤维、2g芳纶纤维，18g石墨，8g腰果壳油摩擦粉，28g填料，4g环氧改性酚醛树脂，混合均匀后，热压；
S2：热压后的复合材料，在真空条件下，进行热处理；
S3：热处理后的复合材料，经加工成型，得复合碳纤维的碳陶刹车盘。
所述的S1的热压温度为170℃。
所述的S2的热处理温度为1580℃。
所述的填料为硅灰石。
所述的改性磷酸盐胶黏剂的制备方法为：
A1：称取18g磷酸、6g氢氧化铝，于反应釜中，升温至95℃，反应80min；
A2：继续加入质量分数为8％的氧化铬粉末，继续在反应80min；
A3：反应结束后，冷却至室温，最后加入1.5g固化剂，升温至55℃，反应65min，得到改性磷酸盐胶黏剂。
所述的有机金属钛改性陶瓷纤维的制备方法为：
B1：取115g陶瓷纤维放于1700g水中，加入5g3-异氰酸酯基丙基三甲氧基硅烷，于40℃下反应90分钟，过滤，烘干，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
B2：取5g硝酸钛，0.2g硝酸镧，8g6,6'-二羟基-2,2'-联吡啶，700gN,N-二甲基甲酰胺中，通入氮气，于40℃下反应70分钟，得到钛/镧有机金属前驱体；
B3：在反应釜中再加入95g3-异氰酸酯基硅烷处理的陶瓷纤维，0.4g四羟基二硼，3g辛酸亚锡，80℃下反应70分钟，过滤，干燥，得到有机金属钛改性陶瓷纤维。
所述的固化剂为氧化镁。
实施例4
一种复合碳纤维的碳陶刹车盘的复合工艺，其操作步骤为：
S1：称取10g改性磷酸盐胶黏剂，30g有机金属钛改性陶瓷纤维，7g矿物纤维、3g芳纶纤维，20g石墨，10g腰果壳油摩擦粉，30g填料，5g环氧改性酚醛树脂，混合均匀后，热压；
S2：热压后的复合材料，在真空条件下，进行热处理；
S3：热处理后的复合材料，经加工成型，得复合碳纤维的碳陶刹车盘。
所述的S1的热压温度为180℃。
所述的S2的热处理温度为1600℃。
所述的填料为重晶石粉。
所述的改性磷酸盐胶黏剂的制备方法为：
A1：称取20g磷酸、7g氢氧化铝，于反应釜中，升温至100℃，反应90min；
A2：继续加入质量分数为10％的氧化铬粉末，继续在反应90min；
A3：反应结束后，冷却至室温，最后加入2g固化剂，升温至60℃，反应70min，得到改性磷酸盐胶黏剂。
所述的有机金属钛改性陶瓷纤维的制备方法为：
B1：取120g陶瓷纤维放于1800g水中，加入6g3-异氰酸酯基丙基三甲氧基硅烷，于45℃下反应100分钟，过滤，烘干，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
B2：取6g硝酸钛，0.3g硝酸镧，10g6,6'-二羟基-2,2'-联吡啶，750gN,N-二甲基甲酰胺中，通入氮气，于45℃下反应80分钟，得到钛/镧有机金属前驱体；
B3：在反应釜中再加入100g3-异氰酸酯基硅烷处理的陶瓷纤维，0.6g四羟基二硼，4g辛酸亚锡，85℃下反应80分钟，过滤，干燥，得到有机金属钛改性陶瓷纤维。
所述的固化剂为二氧化硅。
对比例1
与实施例1不同的是在有机金属钛改性陶瓷纤维的制备过程中不加入3-异氰酸酯基丙基三甲氧基硅烷，其余保持一致。
对比例2
与实施例1不同的是在有机金属钛改性陶瓷纤维的制备过程中不加入6,6'-二羟基-2,2'-联吡啶，其余保持一致。
对比例3
与实施例1不同的是在有机金属钛改性陶瓷纤维的制备过程中不加入四羟基二硼，其余保持一致。
表1实施例测试结果
通过以上实施例与对比例数据分析，本发明制备的复合碳纤维的碳陶刹车盘，具有较高的抗弯强度、断裂韧性，可大幅提高刹车盘的力学性能；本发明制备的复合碳纤维的碳陶刹车盘，耐氧化性提升率可达到155％，提高了碳纤维的抗氧化性能。
本说明书实施例所述的内容仅仅是对发明构思的实现形式的列举，本发明的保护范围的不应当被视为仅限于实施例所陈述的具体形式，本发明的保护范围也及于本领域技术人员根据本发明构思所能够想到的等同技术手段。
Claims (7)
1.一种复合碳纤维的碳陶刹车盘的复合工艺，其操作步骤为：
S1：按重量份，称取5-10份改性磷酸盐胶黏剂，20-30份有机金属钛改性陶瓷纤维，2-7份矿物纤维、1-3份芳纶纤维，10-20份石墨，5-10份腰果壳油摩擦粉，20-30份填料，3-5份环氧改性酚醛树脂，混合均匀后，热压；
S2：热压后的复合材料，在真空条件下，进行热处理；
S3：热处理后的复合材料，经加工成型，得复合碳纤维的碳陶刹车盘。
2.根据权利要求1所述的复合碳纤维的碳陶刹车盘的复合工艺，其特征在于：所述的S1的热压温度为150-180℃。
3.根据权利要求1所述的复合碳纤维的碳陶刹车盘的复合工艺，其特征在于：所述的S2的热处理温度为1500-1600℃。
4.根据权利要求1所述的复合碳纤维的碳陶刹车盘的复合工艺，其特征在于：所述的填料为高岭土、滑石粉、硅灰石、钛白粉、重晶石粉中的一种或多种。
5.根据权利要求1所述的复合碳纤维的碳陶刹车盘的复合工艺，其特征在于：所述的改性磷酸盐胶黏剂的制备方法为：
A1：按重量份，称取10-20份磷酸、3-7份氢氧化铝，于反应釜中，升温至80-100℃，反应50-90min；
A2：继续加入质量分数为2-10％的氧化铬粉末，继续在反应50-90min；
A3：反应结束后，冷却至室温，最后加入0.5-2份固化剂，升温至40-60℃，反应50-70min，得到改性磷酸盐胶黏剂。
6.根据权利要求5所述的复合碳纤维的碳陶刹车盘的复合工艺，其特征在于：所述的固化剂为氧化铬、氧化铝、氧化镁、二氧化硅。
7.根据权利要求1所述的复合碳纤维的碳陶刹车盘的复合工艺，其特征在于：所述的有机金属钛改性陶瓷纤维的制备方法为：
B1：按照质量份数，取100-120份陶瓷纤维放于1500-1800份水中，加入3-6份3-异氰酸酯基丙基三甲氧基硅烷，于32-45℃下反应50-100分钟，过滤，烘干，制得3-异氰酸酯基硅烷处理的陶瓷纤维；
B2：按照质量份数，取3-6份硝酸钛，0.06-0.3份硝酸镧，5-10份6,6'-二羟基-2,2'-联吡啶，500-750份N,N-二甲基甲酰胺中，通入氮气，于32-45℃下反应40-80分钟，得到钛/镧有机金属前驱体；
B3：在反应釜中再加入80-100份3-异氰酸酯基硅烷处理的陶瓷纤维，0.08-0.6份四羟基二硼，2-4份辛酸亚锡，60-85℃下反应40-80分钟，过滤，干燥，得到有机金属钛改性陶瓷纤维。
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