CN114478015A - 氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料的制备方法 - Google Patents
氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料的制备方法 Download PDFInfo
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- CN114478015A CN114478015A CN202210157304.3A CN202210157304A CN114478015A CN 114478015 A CN114478015 A CN 114478015A CN 202210157304 A CN202210157304 A CN 202210157304A CN 114478015 A CN114478015 A CN 114478015A
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- Prior art keywords
- silicon carbide
- alumina fiber
- carbide ceramic
- sintering
- drying
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 110
- 239000000835 fiber Substances 0.000 title claims abstract description 87
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000000919 ceramic Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 23
- 238000005245 sintering Methods 0.000 claims abstract description 77
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 61
- 239000004744 fabric Substances 0.000 claims abstract description 41
- -1 boric acid saturated alcohol Chemical class 0.000 claims abstract description 40
- 239000004327 boric acid Substances 0.000 claims abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000003825 pressing Methods 0.000 claims abstract description 33
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 32
- QOKYJGZIKILTCY-UHFFFAOYSA-J hydrogen phosphate;zirconium(4+) Chemical compound [Zr+4].OP([O-])([O-])=O.OP([O-])([O-])=O QOKYJGZIKILTCY-UHFFFAOYSA-J 0.000 claims abstract description 29
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims abstract description 29
- 239000000413 hydrolysate Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000007598 dipping method Methods 0.000 claims abstract description 16
- 238000011049 filling Methods 0.000 claims abstract description 9
- 239000005388 borosilicate glass Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 72
- 239000000203 mixture Substances 0.000 claims description 64
- 238000001035 drying Methods 0.000 claims description 63
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 39
- 229920003257 polycarbosilane Polymers 0.000 claims description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 34
- 229910011255 B2O3 Inorganic materials 0.000 claims description 33
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 claims description 33
- 229910052681 coesite Inorganic materials 0.000 claims description 33
- 229910052906 cristobalite Inorganic materials 0.000 claims description 33
- 239000000377 silicon dioxide Substances 0.000 claims description 33
- 229910052682 stishovite Inorganic materials 0.000 claims description 33
- 229910052905 tridymite Inorganic materials 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 28
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 28
- 239000011261 inert gas Substances 0.000 claims description 28
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 26
- 238000002791 soaking Methods 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 23
- 239000011268 mixed slurry Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 22
- 239000003960 organic solvent Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 17
- 238000005470 impregnation Methods 0.000 claims description 17
- 235000015895 biscuits Nutrition 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 14
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 14
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 12
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229910001593 boehmite Inorganic materials 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 7
- 230000002708 enhancing effect Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 7
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- 229960001484 edetic acid Drugs 0.000 claims description 5
- 238000005338 heat storage Methods 0.000 abstract description 2
- 239000012782 phase change material Substances 0.000 abstract description 2
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002679 ablation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 1
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Abstract
本发明提供氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,包括以下步骤:改性氧化铝纤维布的制备,浸渍、压制和烧结,空隙填充,增强。本发明还提供了上述方法制得的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料。本发明提供了碳化硅陶瓷材料内部设有改性氧化铝纤维布层,同时在纤维布层上沉积磷酸氢锆氧化铝纤维布层与碳化硅的接触面积大大提高,不仅提高了材料强度,而且提高了材料韧性,同时在碳化硅内掺杂石墨粉末等材料,形成硼硅酸盐玻璃,并利用硼酸饱和醇溶液、硅酸乙酯水解液填充于碳化硅陶瓷内部空隙中,硼硅酸盐玻璃不仅可起到填充作用,而且为相变材料,可起到储热作用,减缓陶瓷材料高温应用时急剧变化,提高其应用寿命。
Description
技术领域
本发明属于新材料领域,特别涉及一种氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料的制备方法及制得的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料。
背景技术
陶瓷材料所具有的诸多优点是其他材料所不能比拟的,但是它的脆性也是不可避免的致命缺点,陶瓷材料的脆性在很大程度上影响了材料性能的可靠性和一致性。陶瓷材料都是由离子键或共价键所组成的多晶结构,它缺乏能促使材料变形的滑移系统,材料一旦受到外加的负荷,再加上陶瓷工艺所很难避免的在材料表面所构成的微缺陷的存在,它们都有可能构成裂纹源,应力就会在这些裂纹的尖端集中,在陶瓷材料中又没有其他可以消耗外来能量的系统,只有以新的自由能予以交换,所谓新的自由能就是裂纹尖端的扩展所形成的新的表面所吸收的能量,这样的结果就造成裂纹的快速扩展而表现为所谓脆性断裂。由此可知,陶瓷材料的脆性是物质的化学键合性质和它的显微结构所决定的。因此要使碳化硅发挥其优异的耐磨性能,首先应该克服其脆性,即提高碳化硅陶瓷的韧性。
HfC陶瓷是目前熔点最高的超高温陶瓷之一,其熔点高达3930℃,热膨胀系数为6.7×10-6/K-1,对应其氧化物(HfO2)的熔点为2700℃,CTE为5.6×10-6/K-1。HfC晶体属于面心立方结构(FCC),空间群是Fm3m,碳原子占据密排Hf原子立方晶格的八面体间隙位置,所以其成键方式包含共价键、金属键以及离子键,导致其具有优异的力学性能。与其他碳化物相比,HfC具有较高的弹性模量,硬度以及强度。因此,HfC被广泛应用于工业切削刀具、航空航天器的热结构部件及高超声速飞行器及推进系统(例如导弹)、第四代核反应堆的包壳材料等。除此之外,由于HfC陶瓷中存在金属键,因此具有较高的电导率和热导率,在电催化产氢、高温电极材料、高温太阳能吸收剂及储能材料等领域也具有很好的应用前景。
然而,HfC陶瓷本身固有的极强的共价键和较低的自扩散系数,导致其存在难以烧结致密化和断裂韧性较低这两大缺点。再者,HfC在温度超过500℃的有氧环境中极易氧化生成HfO2,而且在超高温极端服役环境下抗烧蚀性能差,烧蚀后的氧化层结构疏松易被机械冲刷、剥离,导致该材料在氧化烧蚀后力学性能大幅度降低,限制了其作为高温结构材料在极端环境下应用因此,解决HfC陶瓷烧结问题、提高HfC陶瓷断裂韧性以及抗氧化、烧蚀性能成为其作为高温结构材料应用于极端环境下的关键。
发明内容
技术问题:为了解决现有技术的缺陷,本发明提供了一种氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料的制备方法及制得的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料。
技术方案:本发明提供氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,包括以下步骤:
(1)改性氧化铝纤维布的制备:室温下将磷酸氢锆分散于水中得磷酸氢锆分散体;在真空以及室温下,采用磷酸氢锆分散体对氧化铝纤维布进行真空浸渍;将经过真空浸渍后的氧化铝纤维布晾干,即得改性氧化铝纤维布;
(2)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将改性氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
(3)空隙填充:将步骤(2)的碳化硅陶瓷材料置于硼酸饱和醇溶液中浸渍,取出烘干,再置于硅酸乙酯水解液中浸渍,取出烘干,再置于真空炉中中烧结;
(4)增强:将步骤(3)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2-3MPa,以5-10℃/min的速度升温至1500-1600℃,保温2-4h,随炉冷却至600-850℃并保温1-2h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.05-0.5mol/L时,以5-10℃/min的速率加热至1200-1400℃并保温4-8h;随后停止通入聚碳硅烷,保持惰性气体流量100-200ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
步骤(1)中,磷酸氢锆分散体中还包括乙二胺四乙酸,调pH至3-4;磷酸氢锆、水的用量比为1g:(100-300)mL;晾干条件为:室温下放置10~15h或在50~70℃下保温1~2h。
步骤(2)中,碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:(100-200):(40~50):(10~15):(2~5):(1~5):(0.5~3):(0.5~2);烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2-4%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的1-3倍;氧化铝纤维布与混合浆料的重量比为10:(40-80)。
步骤(2)中,浸渍时间为1-2h;压制压力为150-250MPa/cm2,压制时间为1-10s;烧结温度为2100-2200℃,烧结时间为1-3h。
步骤(3)中,硼酸饱和醇溶液的制备方法为:将硼酸粉末和甲醇于温度为60-70℃的油浴下恒温搅拌1-2h,即得硼酸饱和醇溶液,所述硼酸粉末和甲醇的用量比为(10-20)g:100ml;所述硅酸乙酯水解液的制备方法为:将硅酸乙酯、蒸馏水和甲醇混匀,滴入浓盐酸调pH 3-4,室温搅拌1-2h,即得硅酸乙酯水解液。
步骤(3)中,硼酸饱和醇溶液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;硅酸乙酯水解液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;烧结条件为:5~10℃/min的升温速率,将真空炉升温至1000~1200℃,保温烧结1-2h。
步骤(4)中,所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡0.5-2小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为(5-15):100,记为溶液2;
(c)将混合物1倒入溶液2中,60-80℃水浴加热,搅拌2-6小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至5-10MPa;按照一定的升温程序升温至500-520℃,保温12-24小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
本发明还提供了上述方法制得的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料。
本发明还提供了氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,包括:分散有硼硅酸盐玻璃的碳化硅材料,碳化硅材料内设置的多层改性氧化铝纤维布层,所述改性氧化铝纤维布为表面分散磷酸氢锆的氧化铝纤维布。
有益效果:本发明提供了碳化硅陶瓷材料内部设有改性氧化铝纤维布层,同时在纤维布层上沉积磷酸氢锆氧化铝纤维布层与碳化硅的接触面积大大提高,不仅提高了材料强度,而且提高了材料韧性,同时在碳化硅内掺杂石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2等材料,形成硼硅酸盐玻璃,并利用硼酸饱和醇溶液、硅酸乙酯水解液填充于碳化硅陶瓷内部空隙中,硼硅酸盐玻璃不仅可起到填充作用,而且为相变材料,可起到储热作用,减缓陶瓷材料高温应用时急剧变化,提高其应用寿命。
具体实施方式
下面对本发明作出进一步说明。
本发明中,使用的烧结助剂为MgO。
实施例1
氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,包括以下步骤:
(1)改性氧化铝纤维布的制备:室温下将磷酸氢锆分散于水中得磷酸氢锆分散体;在真空以及室温下,采用磷酸氢锆分散体对氧化铝纤维布进行真空浸渍;将经过真空浸渍后的氧化铝纤维布晾干,即得改性氧化铝纤维布;
磷酸氢锆分散体中还包括乙二胺四乙酸,调pH至3-4;磷酸氢锆、水的用量比为1g:200mL;晾干条件为:室温下放置12h或在60℃下保温1.5h。
(2)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将改性氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:150:45:12:3:3:2:1;烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的3%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2倍;氧化铝纤维布与混合浆料的重量比为10:60。
浸渍时间为1.5h;压制压力为200MPa/cm2,压制时间为5s;烧结温度为2150℃,烧结时间为2h。
(3)空隙填充:将步骤(2)的碳化硅陶瓷材料置于硼酸饱和醇溶液中浸渍,取出烘干,再置于硅酸乙酯水解液中浸渍,取出烘干,再置于真空炉中中烧结;
硼酸饱和醇溶液的制备方法为:将硼酸粉末和甲醇于温度为65℃的油浴下恒温搅拌1.5h,即得硼酸饱和醇溶液,所述硼酸粉末和甲醇的用量比为15g:100ml;所述硅酸乙酯水解液的制备方法为:将硅酸乙酯、蒸馏水和甲醇混匀,滴入浓盐酸调pH 3-4,室温搅拌1.5h,即得硅酸乙酯水解液。
硼酸饱和醇溶液中浸渍时间为30h,烘干时间为0.5h,烘干温度为160℃;硅酸乙酯水解液中浸渍时间为30h,烘干时间为0.5h,烘干温度为160℃;烧结条件为:8℃/min的升温速率,将真空炉升温至1100℃,保温烧结1.5h。
(4)增强:将步骤(3)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2.5MPa,以8℃/min的速度升温至1550℃,保温3h,随炉冷却至750℃并保温1.5h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.3mol/L时,以8℃/min的速率加热至1300℃并保温6h;随后停止通入聚碳硅烷,保持惰性气体流量150ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡1小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为10:100,记为溶液2;
(c)将混合物1倒入溶液2中,70℃水浴加热,搅拌4小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至8MPa;按照一定的升温程序升温至510℃,保温18小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
实施例2
氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,包括以下步骤:
(1)改性氧化铝纤维布的制备:室温下将磷酸氢锆分散于水中得磷酸氢锆分散体;在真空以及室温下,采用磷酸氢锆分散体对氧化铝纤维布进行真空浸渍;将经过真空浸渍后的氧化铝纤维布晾干,即得改性氧化铝纤维布;
磷酸氢锆分散体中还包括乙二胺四乙酸,调pH至3-4;磷酸氢锆、水的用量比为1g:(100-300)mL;晾干条件为:室温下放置10~15h或在50~70℃下保温1~2h。
(2)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将改性氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:(100-200):(40~50):(10~15):(2~5):(1~5):(0.5~3):(0.5~2);烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2-4%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的1-3倍;氧化铝纤维布与混合浆料的重量比为10:(40-80)。
浸渍时间为1-2h;压制压力为150-250MPa/cm2,压制时间为1-10s;烧结温度为2100-2200℃,烧结时间为1-3h。
(3)空隙填充:将步骤(2)的碳化硅陶瓷材料置于硼酸饱和醇溶液中浸渍,取出烘干,再置于硅酸乙酯水解液中浸渍,取出烘干,再置于真空炉中中烧结;
硼酸饱和醇溶液的制备方法为:将硼酸粉末和甲醇于温度为60-70℃的油浴下恒温搅拌1-2h,即得硼酸饱和醇溶液,所述硼酸粉末和甲醇的用量比为(10-20)g:100ml;所述硅酸乙酯水解液的制备方法为:将硅酸乙酯、蒸馏水和甲醇混匀,滴入浓盐酸调pH3-4,室温搅拌1-2h,即得硅酸乙酯水解液。
硼酸饱和醇溶液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;硅酸乙酯水解液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;烧结条件为:5~10℃/min的升温速率,将真空炉升温至1000~1200℃,保温烧结1-2h。
(4)增强:将步骤(3)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2-3MPa,以5-10℃/min的速度升温至1500-1600℃,保温2-4h,随炉冷却至600-850℃并保温1-2h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.05-0.5mol/L时,以5-10℃/min的速率加热至1200-1400℃并保温4-8h;随后停止通入聚碳硅烷,保持惰性气体流量100-200ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡2小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为15:100,记为溶液2;
(c)将混合物1倒入溶液2中,60℃水浴加热,搅拌6小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至5MPa;按照一定的升温程序升温至520℃,保温24小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
实施例3
氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,包括以下步骤:
(1)改性氧化铝纤维布的制备:室温下将磷酸氢锆分散于水中得磷酸氢锆分散体;在真空以及室温下,采用磷酸氢锆分散体对氧化铝纤维布进行真空浸渍;将经过真空浸渍后的氧化铝纤维布晾干,即得改性氧化铝纤维布;
磷酸氢锆分散体中还包括乙二胺四乙酸,调pH至3-4;磷酸氢锆、水的用量比为1g:(100-300)mL;晾干条件为:室温下放置10~15h或在50~70℃下保温1~2h。
(2)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将改性氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:(100-200):(40~50):(10~15):(2~5):(1~5):(0.5~3):(0.5~2);烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2-4%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的1-3倍;氧化铝纤维布与混合浆料的重量比为10:(40-80)。
浸渍时间为1-2h;压制压力为150-250MPa/cm2,压制时间为1-10s;烧结温度为2100-2200℃,烧结时间为1-3h。
(3)空隙填充:将步骤(2)的碳化硅陶瓷材料置于硼酸饱和醇溶液中浸渍,取出烘干,再置于硅酸乙酯水解液中浸渍,取出烘干,再置于真空炉中中烧结;
硼酸饱和醇溶液的制备方法为:将硼酸粉末和甲醇于温度为60-70℃的油浴下恒温搅拌1-2h,即得硼酸饱和醇溶液,所述硼酸粉末和甲醇的用量比为(10-20)g:100ml;所述硅酸乙酯水解液的制备方法为:将硅酸乙酯、蒸馏水和甲醇混匀,滴入浓盐酸调pH3-4,室温搅拌1-2h,即得硅酸乙酯水解液。
硼酸饱和醇溶液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;硅酸乙酯水解液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;烧结条件为:5~10℃/min的升温速率,将真空炉升温至1000~1200℃,保温烧结1-2h。
(4)增强:将步骤(3)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2-3MPa,以5-10℃/min的速度升温至1500-1600℃,保温2-4h,随炉冷却至600-850℃并保温1-2h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.05-0.5mol/L时,以5-10℃/min的速率加热至1200-1400℃并保温4-8h;随后停止通入聚碳硅烷,保持惰性气体流量100-200ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡0.5小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为5:100,记为溶液2;
(c)将混合物1倒入溶液2中,80℃水浴加热,搅拌2小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至10MPa;按照一定的升温程序升温至500℃,保温12小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
对比例1
碳化硅陶瓷复合材料,包括以下步骤:
(1)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:150:45:12:3:3:2:1;烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的3%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2倍;氧化铝纤维布与混合浆料的重量比为10:60。
浸渍时间为1.5h;压制压力为200MPa/cm2,压制时间为5s;烧结温度为2150℃,烧结时间为2h。
(2)空隙填充:将步骤(1)的碳化硅陶瓷材料置于硼酸饱和醇溶液中浸渍,取出烘干,再置于硅酸乙酯水解液中浸渍,取出烘干,再置于真空炉中中烧结;
硼酸饱和醇溶液的制备方法为:将硼酸粉末和甲醇于温度为65℃的油浴下恒温搅拌1.5h,即得硼酸饱和醇溶液,所述硼酸粉末和甲醇的用量比为15g:100ml;所述硅酸乙酯水解液的制备方法为:将硅酸乙酯、蒸馏水和甲醇混匀,滴入浓盐酸调pH 3-4,室温搅拌1.5h,即得硅酸乙酯水解液。
硼酸饱和醇溶液中浸渍时间为30h,烘干时间为0.5h,烘干温度为160℃;硅酸乙酯水解液中浸渍时间为30h,烘干时间为0.5h,烘干温度为160℃;烧结条件为:8℃/min的升温速率,将真空炉升温至1100℃,保温烧结1.5h。
(3)增强:将步骤(2)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2.5MPa,以8℃/min的速度升温至1550℃,保温3h,随炉冷却至750℃并保温1.5h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.3mol/L时,以8℃/min的速率加热至1300℃并保温6h;随后停止通入聚碳硅烷,保持惰性气体流量150ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡1小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为10:100,记为溶液2;
(c)将混合物1倒入溶液2中,70℃水浴加热,搅拌4小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至8MPa;按照一定的升温程序升温至510℃,保温18小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
对比例2
碳化硅陶瓷复合材料,包括以下步骤:
(1)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:150:45:12:3:3:2:1;烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的3%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2倍;氧化铝纤维布与混合浆料的重量比为10:60。
浸渍时间为1.5h;压制压力为200MPa/cm2,压制时间为5s;烧结温度为2150℃,烧结时间为2h。
(2)增强:将步骤(2)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2.5MPa,以8℃/min的速度升温至1550℃,保温3h,随炉冷却至750℃并保温1.5h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.3mol/L时,以8℃/min的速率加热至1300℃并保温6h;随后停止通入聚碳硅烷,保持惰性气体流量150ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡1小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为10:100,记为溶液2;
(c)将混合物1倒入溶液2中,70℃水浴加热,搅拌4小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至8MPa;按照一定的升温程序升温至510℃,保温18小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
对比例3
碳化硅陶瓷复合材料,包括以下步骤:
浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:150:45:12:3:3:2:1;烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的3%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2倍;氧化铝纤维布与混合浆料的重量比为10:60。
浸渍时间为1.5h;压制压力为200MPa/cm2,压制时间为5s;烧结温度为2150℃,烧结时间为2h。
实验例
测试实施例1至3以及对比例1至3的产品性能。结果如下:
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (9)
1.氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:包括以下步骤:
(1)改性氧化铝纤维布的制备:室温下将磷酸氢锆分散于水中得磷酸氢锆分散体;在真空以及室温下,采用磷酸氢锆分散体对氧化铝纤维布进行真空浸渍;将经过真空浸渍后的氧化铝纤维布晾干,即得改性氧化铝纤维布;
(2)浸渍、压制和烧结:将碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂混合后球磨,再加入至乙醇中分散,得混合浆料;将改性氧化铝纤维布置于混合浆料中浸渍,用蒸汽干燥箱将其烘干;烘干后加入钢模中加压使压制成型,得碳化硅陶瓷素坯;将碳化硅陶瓷素坯置于真空炉中烧结,得碳化硅陶瓷材料;
(3)空隙填充:将步骤(2)的碳化硅陶瓷材料置于硼酸饱和醇溶液中浸渍,取出烘干,再置于硅酸乙酯水解液中浸渍,取出烘干,再置于真空炉中中烧结;
(4)增强:将步骤(3)的碳化硅陶瓷材料置于反应釜中,通入惰性气体,加压至2-3MPa,以5-10℃/min的速度升温至1500-1600℃,保温2-4h,随炉冷却至600-850℃并保温1-2h;以惰性气体为载气,向反应釜中通入聚碳硅烷;当反应釜内聚碳硅烷浓度达到0.05-0.5mol/L时,以5-10℃/min的速率加热至1200-1400℃并保温4-8h;随后停止通入聚碳硅烷,保持惰性气体流量100-200ml/min,随炉冷却至室温;即得氧化铝纤维增强碳化硅陶瓷材料。
2.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:步骤(1)中,磷酸氢锆分散体中还包括乙二胺四乙酸,调pH至3-4;磷酸氢锆、水的用量比为1g:(100-300)mL;晾干条件为:室温下放置10~15h或在50~70℃下保温1~2h。
3.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:步骤(2)中,碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2和烧结助剂的重量比为1000:(100-200):(40~50):(10~15):(2~5):(1~5):(0.5~3):(0.5~2);烧结助剂的重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的2-4%;乙醇重量为碳化硅粉末、石墨粉末、SiO2、B2O3、BaO、硼酸铝、K2O、TiO2的总重量的1-3倍;氧化铝纤维布与混合浆料的重量比为10:(40-80)。
4.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:步骤(2)中,浸渍时间为1-2h;压制压力为150-250MPa/cm2,压制时间为1-10s;烧结温度为2100-2200℃,烧结时间为1-3h。
5.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:步骤(3)中,硼酸饱和醇溶液的制备方法为:将硼酸粉末和甲醇于温度为60-70℃的油浴下恒温搅拌1-2h,即得硼酸饱和醇溶液,所述硼酸粉末和甲醇的用量比为(10-20)g:100ml;所述硅酸乙酯水解液的制备方法为:将硅酸乙酯、蒸馏水和甲醇混匀,滴入浓盐酸调pH 3-4,室温搅拌1-2h,即得硅酸乙酯水解液。
6.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:步骤(3)中,硼酸饱和醇溶液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;硅酸乙酯水解液中浸渍时间为20-40h,烘干时间为0.5-1h,烘干温度为150-180℃;烧结条件为:5~10℃/min的升温速率,将真空炉升温至1000~1200℃,保温烧结1-2h。
7.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:步骤(4)中,所述聚碳硅烷的制备方法为:
(a)将纳米勃姆石均匀分散在KH550的水溶液中,超声震荡0.5-2小时,得混合物1;
(b)聚二甲基硅烷PDMS蒸馏,收集103℃的馏分,干燥;随后向其中滴加有机溶剂并不断搅拌,直至有机溶剂与聚二甲基硅烷PDMS质量比为(5-15):100,记为溶液2;
(c)将混合物1倒入溶液2中,60-80℃水浴加热,搅拌2-6小时,得混合物3;
(d)将混合物3放入反应釜,通入CO2和惰性气体的混合气体,加压至5-10MPa;按照一定的升温程序升温至500-520℃,保温12-24小时;随炉冷却至室温,得粗产物4;
(e)将粗产物4溶解在有机溶剂中,过滤,抽真空减压蒸馏,得产物聚碳硅烷PCS。
8.根据权利要求1所述的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于:权利要求1至7任一项方法制得的氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料。
9.氧化铝纤维增强硼硅酸盐掺杂碳化硅陶瓷复合材料,其特征在于,包括:分散有硼硅酸盐玻璃的碳化硅材料,碳化硅材料内设置的多层改性氧化铝纤维布层,所述改性氧化铝纤维布为表面分散磷酸氢锆的氧化铝纤维布。
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