CN112062574B - 一种高性能纳米碳化硅陶瓷及其制备方法和应用 - Google Patents
一种高性能纳米碳化硅陶瓷及其制备方法和应用 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 47
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 12
- 238000005452 bending Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000005336 cracking Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 239000011812 mixed powder Substances 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 3
- 239000010439 graphite Substances 0.000 claims abstract description 3
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 230000005476 size effect Effects 0.000 abstract description 4
- 229910052575 non-oxide ceramic Inorganic materials 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract description 2
- 239000011225 non-oxide ceramic Substances 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明属于非氧化物陶瓷材料领域，公开一种高性能纳米的碳化硅陶瓷及其制备方法和应用。该碳化硅陶瓷是将聚碳硅烷作为前驱体和烧结助剂Al2O3‑CeO2球磨混合后，在保护气氛下，先升温至200～400℃保温，再升温至500～1200℃裂解，得到混合粉体；再将混合粉体进行球磨、造粒，装入石墨模具中，施加压力1～20MPa，在保护气氛下1200～1450℃进行烧结制得。本发明通过尺寸效应，控制样品厚度，使其致密度为97％以上，维氏硬度为25～35GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为800～1300MPa，可广泛应用于核能领域中。
Description
技术领域
本发明属于非氧化物陶瓷材料技术领域，更具体地，涉及一种高性能纳米碳化硅陶瓷及其制备方法和应用。
背景技术
科学技术的发展对材料提出了更高的要求，陶瓷基的复合材料表现出的高强度、高热导、耐腐蚀和抗高温等优点与合金材料相比优势较大，其中，碳化硅(SiC)材料正是一种典型的陶瓷材料，在高温环境下表现出的高硬度、热稳定性与抗化学腐蚀性使其在高温零部件、核能薄壁件等领域得到广泛的应用。
但由于碳化硅拥有结合力很强的共价键，导致其熔点很高，烧结工艺性差，致密度低。碳化硅的常规热压烧结温度超过2000℃，导致晶粒粗大；利用液相烧结促进致密化可降低烧结温度，但引入了较多的烧结助剂，严重影响了成品材料在高温应用时的性能，制约了碳化硅陶瓷的进一步应用。。
因此，需要发明一种碳化硅陶瓷的烧结工艺，能使碳化硅陶瓷在较低的温度下实现较高致密度的烧结，并且不引入过多的烧结助剂。
发明内容
为了解决上述现有技术存在的不足和缺点，提供一种高性能纳米碳化硅陶瓷的制备方法。该方法利用尺寸效应，通过加压裂解的高活性纳米级碳化硅坯料，降低了烧结的温度和烧结助剂的含量，选定了较优的工艺参数。
本发明的另一目的在于提供上述方法制得的高性能纳米碳化硅陶瓷。
本发明的再一目的在于提供上述高性能纳米碳化硅陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种高性能纳米碳化硅陶瓷的制备方法，包括如下步骤：
S1.将聚碳硅烷作为前驱体和烧结助剂Al2O3-CeO2球磨混合后，在保护气氛下，先升温至200～400℃保温，再升温至500～1200℃裂解，得到混合粉体；
S2.将混合粉体进行球磨、造粒，装入石墨模具中，施加压力为1～20MPa，在保护气氛下1200～1450℃进行烧结，制得高性能纳米的碳化硅陶瓷材料。
优选地，步骤S1中所述Al2O3与CeO2的纯度均为99～99.9wt.％，所述Al2O3与CeO2粉的粒径为10～100nm。
优选地，步骤S2中所述碳化硅陶瓷中碳化硅的粒径为30～100nm。
优选地，步骤S1中所述球磨为辊式球磨，是以无水乙醇为溶剂，以氮化硅球为球磨介质，球磨转速为150～500r/min，所述球磨的时间为8～24h。
优选地，步骤S1中所述的聚碳硅烷和烧结助剂的质量比为(95.5～98)：(2～4.5)，所述Al2O3和CeO2的质量比为(1～99)：(1～99)。
优选地，步骤S1中所述升温至200～400℃的速率为1～5℃/min，保温时间为0.5～2h；所述升温至500～1200℃的速率为5～15℃/min。
优选地，步骤S1和S2中所述保护气氛为氮气或氩气。
优选地，步骤S2中所述烧结的时间为10～60min；所述烧结的升温速率为5～200℃/min。
一种高性能纳米碳化硅陶瓷材料是由所述的方法制得。
优选地，所述纳米碳化硅陶瓷的致密度为97％以上，维氏硬度为25～35GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为800～1300MPa。
所述的高性能纳米碳化硅陶瓷材料在核能领域中的应用。
本发明通过以聚碳硅烷(PCS)作为前驱体，在不同的温度下加压进行加热裂解，得到高活性的纳米级碳化硅陶瓷材料；结合SPS烧结等烧结工艺并通过控制裂解产物的烧结厚度(10～1000μm)，借助尺寸效应，只需加入量的烧结助剂(2～4.5wt％)，即可在较低的烧结温度下得到尺寸各异、性能有所差别但致密度高的高性能纳米碳化硅陶瓷材料，从而降低了生产成本，提高了生产效率，应用前景广泛。
与现有技术相比，本发明具有以下有益效果：
1.本发明利用聚碳硅烷前驱体裂解得到的碳化硅陶瓷粉体，其具有较高的烧结活性，与传统常规的高温高压烧结条件相比，烧结温度较低，效率高，大幅降低了成本，实现环保节能。
2.本发明借助尺寸效应制备的高性能纳米级碳化硅陶瓷致密件，只需加入少量的烧结助剂即可实现高致密度的烧结，从而保证了成品在高温、高辐射应用环境下性能与强度的稳定性。
3.本发明的制造的高性能的纳米碳化硅陶瓷材料，可灵活改变烧结坯体的模具尺寸、施压的力度大小，从而实现对材料形状、尺寸、致密度以及结构特性的控制，在保障强度的同时满足各种生产需求。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.制备
(1)以产率为60wt％的聚碳硅烷作为前驱体，以Al2O3-CeO2为烧结助剂，聚碳硅烷、Al2O3与CeO2的质量百分比分别为96％、2％与2％。将聚碳硅烷和烧结助剂混合，用Si3N4球在辊式球磨下以150r/min的转数进行球磨混合8h，制得混合粉体；
(2)在氮气气氛下，加压10MPa，先以2℃/min升温至200℃保温1h，再以10℃/min升温至800℃保温1h，得到裂解产物；
(3)将裂解产物进行球磨造粒处理，以无水乙醇为溶剂，利用Si3N4球在辊式球磨，以400r/min的转数进行球磨混合24h，对混合完成后的浆料进行干燥。
(4)将干燥的粉体装入烧结模具，预压压力为10MPa，控制烧结厚度为500μm；将预压后的粉体放入SPS烧结设备中，在氮气气氛下，加压15MPa，以150℃/min升温至1600℃进行SPS烧结，保温20min，制得致密的纳米碳化硅陶瓷，其中，碳化硅的粒径为30～100nm。
2.性能测试：本实施例所得的纳米碳化硅陶瓷的致密度为98％，维氏硬度为25GPa，抗弯强度为1000MPa，断裂韧性为8MPa·m1/2，在1200℃下高温强度为800MPa。
实施例2
与实施例1不同的在于：步骤(2)中先升温至300℃，再升温至1000℃，得到裂解产物。
本实施例所得的纳米碳化硅陶瓷的致密度为97％，维氏硬度为24GPa，抗弯强度为900MPa，断裂韧性为7MPa·m1/2，在1200℃下高温强度为700MPa。
实施例3
与实施例1不同的在于：步骤(5)中所述轴向加压为50MPa，所述烧结温度为1500℃；保温时间为50min。
步骤(1)中所述聚碳硅烷前驱体、Al2O3与CeO2的质量百分比分别为98％、1％与1％。
本实施例所得的纳米碳化硅陶瓷的致密度为99％，维氏硬度为26GPa，抗弯强度为1000MPa，断裂韧性为9MPa·m1/2，在1200℃下高温强度为800MPa。
实施例4
与实施例1不同的在于：步骤(4)中所述控制烧结的厚度为100μm。
本实施例所得的纳米碳化硅陶瓷的致密度为99％，维氏硬度为28GPa，抗弯强度为800MPa，断裂韧性为7MPa·m1/2，在1200℃下高温强度为800MPa。
实施例5
与实施例1不同的在于：步骤(5)所述加压的压力为20MPa。
本实施例所得的纳米碳化硅陶瓷的致密度为98％，维氏硬度为24GPa，抗弯强度为1000MPa，断裂韧性为10MPa·m1/2，在1200℃下高温强度为700MPa。
本发明的纳米碳化硅陶瓷的致密度为97％以上，维氏硬度为25～35GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为800～1300MPa，该高性能纳米碳化硅陶瓷材料可应用在核能领域中。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (5)
1.一种高性能纳米碳化硅陶瓷的制备方法，其特征在于，包括如下步骤：
S1.将聚碳硅烷作为前驱体和烧结助剂Al2O3-CeO2球磨混合后，在保护气氛氮气或氩气下，先以1～5℃/min升温至200～400℃保温0.5～2h，再以5～15℃/min升温至500～1200℃裂解，得到混合粉体；所述Al2O3与CeO2的纯度均为99～99.9wt.％，所述Al2O3与CeO2粉的粒径为10～100nm；所述的聚碳硅烷和烧结助剂的质量比为(95.5～98)：(2～4.5)，所述Al2O3和CeO2的质量比为(1～99)：(1～99)；
S2.将混合粉体进行球磨、造粒，装入石墨模具中，施加压力为1～20MPa，控制烧结厚度为10～1000μm；在保护气氛氮气或氩气下以5～200℃/min升温至1200～1450℃烧结10～60min，制得高性能纳米的碳化硅陶瓷；所述碳化硅陶瓷中碳化硅的粒径为30～100nm，所述纳米碳化硅陶瓷的致密度为97％以上，维氏硬度为25～35GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为800～1300MPa。
2.根据权利要求1所述的高性能纳米的碳化硅陶瓷的制备方法，其特征在于，步骤S1中所述球磨为辊式球磨，是以无水乙醇为溶剂，以氮化硅球为球磨介质，球磨转速为150～500r/min，所述球磨的时间为8～24h。
3.一种高性能纳米碳化硅陶瓷，其特征在于，所述纳米碳化硅陶瓷是由权利要求1或2所述的方法制得。
4.根据权利要求3所述的高性能纳米碳化硅陶瓷，其特征在于，所述纳米碳化硅陶瓷的致密度为97％以上，维氏硬度为25～35GPa，抗弯强度为700～1200MPa，断裂韧性为6～12MPa·m1/2，在1200℃下高温强度为800～1300MPa。
5.权利要求3或4所述的高性能纳米碳化硅陶瓷在核能领域中的应用。
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