CN108191403A - 一种抗冲击散热纳米陶瓷材料的制备方法 - Google Patents
一种抗冲击散热纳米陶瓷材料的制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 19
- 230000035939 shock Effects 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000005855 radiation Effects 0.000 title claims description 10
- 239000000843 powder Substances 0.000 claims abstract description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 42
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 239000005350 fused silica glass Substances 0.000 claims abstract description 24
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 21
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000835 fiber Substances 0.000 claims abstract description 14
- 239000010445 mica Substances 0.000 claims abstract description 14
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 14
- 239000000440 bentonite Substances 0.000 claims abstract description 8
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 8
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 21
- 239000011268 mixed slurry Substances 0.000 claims description 15
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 239000002114 nanocomposite Substances 0.000 claims description 13
- 229930006000 Sucrose Natural products 0.000 claims description 12
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000005720 sucrose Substances 0.000 claims description 12
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- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
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- 235000019441 ethanol Nutrition 0.000 claims description 3
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- 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 4
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- 229910026161 MgAl2O4 Inorganic materials 0.000 abstract 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
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- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
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- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
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- 238000009938 salting Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
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Abstract
本发明公开了一种抗冲击纳米复合陶瓷材料的制备方法，纳米熔融石英粉、氧化镁、MgAl2O4、膨润土、氮化铝、氮化硅纤维、云母粉、氧化铝陶瓷粉和碳化钛微粉为主要原料，经过料浆制备、注凝脱模、烧结成型步骤所得的复合陶瓷致密度得到了显著提高,并且机械强度也得到了提升,所得陶瓷的致密度和抗冲击韧性得到了提高；本发明通过制备出陶瓷材料具有优异的抗冲击性及散热性能。
Description
技术领域
本发明本发明涉及一种抗冲击散热纳米陶瓷材料的制备方法，属于陶瓷制备领域。
背景技术
多孔陶瓷散热片具有尺寸小巧、绝缘性能好、不产生电磁波噪音、热膨胀系数小、耐腐蚀、抗氧化、散热表面积大等特点,越来越受到市场的青睐,主要材质为导热率一般的氧化铝和导热率较高的碳化硅,现有的陶瓷散热片采用多孔结构增大了散热面积,促进冷热空气对流,提高了散热能力。但是多孔结构同时严重降低了陶瓷材料的导热能力,在提高散热能力的同时牺牲了导热能力。现有的多孔碳化硅散热片大多都采用了低热导率的氧化硅、氧化铝等低温烧结助剂,进一步降低了热导率，本发明要解决的技术问题是,提供一种体积小、导热能力好以及散热性能好的抗冲击陶瓷散热片。
发明内容
本发明的目的在于提供一种抗冲击散热纳米复合陶瓷材料的制备方法,通过该方法制备的材料具有优异的耐磨效果。
一种抗冲击散热纳米复合陶瓷材料的制备方法，该方法包括以下步骤：
步骤1、称取10g3-氨丙基三乙氧基硅烷加入到烧瓶中,向烧瓶中再加入300份无水乙醇,搅拌,再加入20份氧化镁,搅拌,静置浸泡26h,得到预处理后的氧化镁混合液；
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
步骤3、最后将上述混合浆料加入到12000r/min的球磨机中,再依次加入无水乙醇、3份膨润土、0.5份十二烷基苯磺酸钠、3份甲基丙烯酸羟丙酯、12份氧化铝陶瓷粉、6份碳化钛微粉,混合研磨4h,将混合完全的物料放入模具中压制成型,将成型的材料在氮气保护、180℃烧结7h,再自然冷却至室温,即得一种抗冲击复合陶瓷散热材料。
所述的纳米熔融石英粉制备方法如下：
步骤1、用球磨机将熔融石英球磨成粉末,取能过200目筛的粉末备用；
步骤2、去34份蔗糖溶于去200份去离子水中,然后在搅拌的情况下向蔗糖溶液中缓慢加入18份上述熔融石英粉,混合均匀,置于干燥箱中,80℃下进行烘干,冷却,放入柑锅中
步骤3、将坩埚置于高温气氛炉中,在氮气的保护下,以10℃的升温速率加热至700℃保温1h,进行蔗糖热分解,将所得粉末冷却备用；
步骤4、将步骤3所得熔融石英粉末,置于微波反应炉中,先抽真空后,以5L/min的速度通氮气,
一段时间后,以10℃/min的升温速率加热至1050℃进行碳热还原反应,1.5h后冷却取出,然后放入马弗炉中进行加热处理,炉门不完全封闭,在600℃处理2h,去除反应剩余的碳,得到纳米熔融石英粉。
有益效果：本发明制备的抗冲击散热纳米复合陶瓷材料，经过料浆制备、注凝脱模、烧结成型步骤所得的复合陶瓷致密度得到了显著提高,并且机械强度也得到了提升,所得陶瓷的致密度和抗冲击韧性得到了提高；采用纳米石英粉与氮化铝、氮化硅构成骨架粒子,保证其在径向和轴向上都具有高的导热性和稳定性,氮化硅在烧结过程中,会被氧气氧化,生成液相的二氧化硅从而填充基体的孔隙,达到致密化,同时由于氮元素可以降低熔融石英粉末的氧含量,从而可以在一定程度下抑制熔融石英粉末析晶，使得陶瓷具有优异导热性的同时，也具备良好的抗冲击性。
具体实施方式
实施例1
一种高冲击耐磨型纳米复合陶瓷材料的制备方法，该方法包括以下步骤：
步骤1、称取10g3-氨丙基三乙氧基硅烷加入到烧瓶中,向烧瓶中再加入300份无水乙醇,搅拌,再加入20份氧化镁,搅拌,静置浸泡26h,得到预处理后的氧化镁混合液；
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
步骤3、最后将上述混合浆料加入到12000r/min的球磨机中,再依次加入无水乙醇、3份膨润土、0.5份十二烷基苯磺酸钠、3份甲基丙烯酸羟丙酯、12份氧化铝陶瓷粉、6份碳化钛微粉,混合研磨4h,将混合完全的物料放入模具中压制成型,将成型的材料在氮气保护、180℃烧结7h,再自然冷却至室温,即得一种抗冲击复合陶瓷散热材料。
所述的纳米熔融石英粉制备方法如下：
步骤1、用球磨机将熔融石英球磨成粉末,取能过200目筛的粉末备用；
步骤2、去34份蔗糖溶于去200份去离子水中,然后在搅拌的情况下向蔗糖溶液中缓慢加入18份上述熔融石英粉,混合均匀,置于干燥箱中,80℃下进行烘干,冷却,放入柑锅中
步骤3、将坩埚置于高温气氛炉中,在氮气的保护下,以10℃的升温速率加热至700℃保温1h,进行蔗糖热分解,将所得粉末冷却备用；
步骤4、将步骤3所得熔融石英粉末,置于微波反应炉中,先抽真空后,以5L/min的速度通氮气,
一段时间后,以10℃/min的升温速率加热至1050℃进行碳热还原反应,1.5h后冷却取出,然后放入马弗炉中进行加热处理,炉门不完全封闭,在600℃处理2h,去除反应剩余的碳,得到纳米熔融石英粉。
实施例2
步骤2、将7份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例3
步骤2、将3份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例4
步骤2、将1份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例5
步骤2、将11份纳米熔融石英粉加入到11份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例6
步骤2、将11份纳米熔融石英粉加入到5.5份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例7
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入4份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例8
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、3份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
实施例9
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
所述的NiAl—SBA-15纳米介孔材料制备方法如下：
步骤1、将500g份SBA-15原粉放入石英管中，在氮气流下以3℃/min的速度从25℃升到540℃焙烧，然后置于马弗炉540℃再焙烧3h以除去模板剂，将焙烧后的MCM-22用足量的2mol/L的硝酸铵溶液于80℃离子交换12h后，在马弗炉中于540℃焙烧3h；
步骤2、将上述焙烧后得到SBA-15加入含有氢氧化钠0.5mol和无水碳酸钠0.1mol的混合碱溶液里超声30min，上述混合溶液在室温剧烈搅拌下加入到含有硝酸镍0.75mol和硝酸铝0.25mol的盐溶液中得到悬浮液；
步骤3、将0.2mol的氢氧化钠溶液加入到上述悬浮液里调节溶液的PH=10.5，然后在60℃晶化6小时后溶液冷却至室温,用去离子水洗涤三次离心,60℃下干燥24h，得到NiAl—SBA-15纳米介孔材料。
其余制备和实施例1相同。
实施例10
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入16份纳米氮化铝、1份氮化硅纤维、1份云母粉,搅拌30min,得到混合浆料；
其余制备和实施例1相同。
对照例1
与实施例1不同点在于：纳米复合陶瓷材料制备的步骤2中，将11份二氧化硅粉加入到22份氧化镁混合液中，其余步骤与实施例1完全相同。
对照例2
与实施例1不同点在于：纳米复合陶瓷材料制备的步骤2中，不再加入石英粉，加入33份氧化镁混合液中，其余步骤与实施例1完全相同。
对照例3
与实施例1不同点在于：纳米复合陶瓷材料制备的步骤3中，再依次加入无水乙醇、1份膨润土、0.5份十二烷基苯磺酸钠、8份甲基丙烯酸羟丙酯、6份碳化钛微粉,混合研磨4h，其余步骤与实施例1完全相同。
对照例4
与实施例1不同点在于：纳米复合陶瓷材料制备的步骤3中，再依次加入无水乙醇、1份膨润土、2份十二烷基苯磺酸钠、16份甲基丙烯酸羟丙酯、12份氧化铝陶瓷粉,混合研磨4h，，其余步骤与实施例1完全相同。
对照例5
与实施例1不同点在于：纳米复合陶瓷材料制备的步骤3中，再依次加入无水乙醇、1份膨润土、0.5份十二烷基苯磺酸钠、8份甲基丙烯酸羟丙酯、6份氧化铝陶瓷粉、6份碳化钛微粉,混合研磨4h，，其余步骤与实施例1完全相同。
对照例6
与实施例1不同点在于：纳米复合陶瓷材料制备的步骤3中，再依次加入无水乙醇、1份膨润土、0.5份十二烷基苯磺酸钠、8份甲基丙烯酸羟丙酯、12份氧化铝陶瓷粉、1份碳化钛微粉,混合研磨4h，，其余步骤与实施例1完全相同。
对照例7
与实施例1不同点在于：纳米熔融石英粉制备的步骤3中，在CO2气体的保护下,以10℃的升温速率加热至700℃保温1h,进行蔗糖热分解，其余步骤与实施例1完全相同。
对照例8
与实施例1不同点在于：纳米熔融石英粉制备的步骤3中，在H2气体的保护下,以10℃的升温速率加热至700℃保温1h,进行蔗糖热分解，其余步骤与实施例1完全相同。
对照例9
与实施例1不同点在于：纳米熔融石英粉制备的步骤4中，以10℃/min的升温速率加热至750℃进行碳热还原反应，其余步骤与实施例1完全相同。
对照例10
与实施例1不同点在于：纳米熔融石英粉制备的步骤4中，以10℃/min的升温速率加热至1550℃进行碳热还原反应，其余步骤与实施例1完全相同。
选取制备得到的抗冲击散热纳米陶瓷材料分别进行性能检测，
冲击韧性采用GB/T14389-1993《工程陶瓷冲击韧性试验方法》；
GB/T5598-2015导热系数（热导率）测定方法；
测试结果
实验结果表明本发明提供的抗冲击散热纳米陶瓷纳米复合材料具有良好的散热效果，材料在标准测试条件下，抗冲击韧性一定，导热率越高，说明散热效果越好，反之，效果越差；实施例2到实施例10，分别改变散热陶瓷纳米复合材料中各个原料组成的配比，对材料的耐磨性能均有不同程度的影响，在纳米熔融石英粉、纳米氮化铝、氮化硅纤维、云母粉质量配比为11:8：7：:4，其他配料用量固定时，散热效果最好；值得注意的是实施例9加入NiAl—SBA-15纳米介孔材料，散热效果明显提高，说明纳米介孔材料对陶瓷填料结构的散热性能有更好的优化作用；对照例1至对照例2不再加入纳米石英粉并使用二氧化硅，导热率明显降低，说明纳米石英粉对材料的散热性产生重要影响；对照例3至对照例,6改变陶瓷浆料的辅助用料，说明在氧化铝陶瓷粉、碳化钛微粉质量比为2:1效果较好；对照例7至例8改变了蔗糖热分解的气体氛围，散热效果明显降低，说明氮气对纳米石英粉结构的复合改性影响很大；对照例9至对照例10，改变碳热还原反应的温度，使得材料的反应不完全，散热效果明显降低；因此使用本发明制备的抗冲击纳米陶瓷复合材料具有良好的散热效果。
Claims (2)
1.一种抗冲击散热纳米复合陶瓷材料的制备方法，其特征在于该方法包括以下步骤：
步骤1、称取10g3-氨丙基三乙氧基硅烷加入到烧瓶中,向烧瓶中再加入300份无水乙醇,搅拌,再加入20份氧化镁,搅拌,静置浸泡约26h,得到预处理后的氧化镁混合液；
步骤2、将11份纳米熔融石英粉加入到22份氧化镁混合液中,搅拌20min，再依次加入8份纳米氮化铝、7份氮化硅纤维、4份云母粉,搅拌30min,得到混合浆料；
步骤3、最后将上述混合浆料加入到12000r/min的球磨机中,再依次加入无水乙醇、3份膨润土、0.5份十二烷基苯磺酸钠、3份甲基丙烯酸羟丙酯、12份氧化铝陶瓷粉、6份碳化钛微粉,混合研磨4h,将混合完全的物料放入模具中压制成型,将成型的材料在氮气保护、180℃烧结7h,再自然冷却至室温,即得一种抗冲击复合陶瓷散热材料。
2.根据权利要求1所述一种抗冲击散热纳米陶瓷材料的制备方法，其特征在于所述，
所述的纳米熔融石英粉制备方法如下：
步骤1、用球磨机将熔融石英球磨成粉末,取能过200目筛的粉末备用；
步骤2、去34份蔗糖溶于去200份去离子水中,然后在搅拌的情况下向蔗糖溶液中缓慢加入18份上述熔融石英粉,混合均匀,置于干燥箱中,80℃下进行烘干,冷却,放入柑锅中
步骤3、将坩埚置于高温气氛炉中,在氮气的保护下,以10℃的升温速率加热至700℃保温1h,进行蔗糖热分解,将所得粉末冷却备用；
步骤4、将步骤3所得熔融石英粉末,置于微波反应炉中,先抽真空后,以5L/min的速度通氮气,
一段时间后,以10℃/min的升温速率加热至1050℃进行碳热还原反应,1.5h后冷却取出,然后放入马弗炉中进行加热处理,炉门不完全封闭,在600℃处理2h,去除反应剩余的碳,得到纳米熔融石英粉。
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| CN110194674A (zh) * | 2019-06-06 | 2019-09-03 | 山东工业陶瓷研究设计院有限公司 | 一种碳纤维增韧石英陶瓷基复合材料的制备方法 |
| CN111286106A (zh) * | 2020-03-20 | 2020-06-16 | 杨海青 | 一种基于碳纤维的耐磨材料及其制备方法 |
| CN111410545A (zh) * | 2020-04-11 | 2020-07-14 | 牧雅阀门有限公司 | 高性能新型陶瓷材料及其制备方法 |
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