CN109081684A - 一种碳纳米管增强氧化铝基复合材料的制备方法 - Google Patents
一种碳纳米管增强氧化铝基复合材料的制备方法 Download PDFInfo
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- 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 61
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 11
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- 238000002156 mixing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
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Abstract
本发明公开一种碳纳米管增强氧化铝基复合材料的制备方法,采用浓硫酸与浓硝酸的混合酸对碳纳米管进行预处理,经超声均匀分散于铝盐溶液中,在磁力搅拌的同时滴加碱溶液,生成的氢氧化铝沉淀以碳纳米管为形核点长大从而包覆碳纳米管,经过滤、洗涤、干燥后,低温煅烧、高温焙烧制成复合粉体,最后经SPS烧结得到高韧性的碳纳米管增强氧化铝基复合材料;碳纳米管表面被氧化铝包覆从而减少其团聚现象,并可以提高增强相与基体的界面结合强度;碳纳米管在基体中均匀分散能保证材料性能的连续性;本发明工艺简单,相对于球磨工艺可以减少制备过程对碳纳米管的破坏作用,设备要求低,适用于工业化生产。
Description
技术领域
本发明涉及一种碳纳米管增强氧化铝基复合材料的制备方法,属于复合材料制备技术领域。
背景技术
氧化铝陶瓷材料具有良好的力学性能、化学稳定性、隔热性和电绝缘性,是一种被广泛应用的材料,在高速切割、耐磨损部件等领域有着非常广泛的应用,但由于其断裂韧性较差,限制了它在许多高端领域的应用。碳纳米管具有优良的力学性能,抗拉强度达到50~200GPa是钢的100倍,是良好的增韧纤维,经常被用来增韧陶瓷,能有效的提高陶瓷的断裂韧性。但碳纳米管极易团聚,其在氧化铝中如何达到均匀分散一直是该领域很难突破的问题。
发明内容
本发明针对现有技术存在的问题,提供了一种碳纳米管增强氧化铝基复合材料的制备方法,将碳纳米管均匀分散于铝的盐溶液中,通过添加碱性溶液产生氢氧化铝沉淀并以碳纳米管为形核点,将碳纳米管包覆起来使其无法团聚,随后通过煅烧使氢氧化铝分解为氧化铝,最后采用SPS烧结成碳纳米管增强氧化铝基复合材料,该材料具有良好的力学性能。
一种碳纳米管增强氧化铝基复合材料的制备方法,具体步骤如下:
(1)碳纳米管预处理:将质量分数为98%的浓硫酸与质量分数为65%的浓硝酸按体积比3:1混合制得混酸,按照碳纳米管与浓硫酸质量体积比g:mL为1:4~6的比例,将碳纳米管加入到混酸中,封口,65℃水浴恒温4~6小时,再加入8~15倍混酸体积的去离子水,搅拌成混合均匀的混合液,抽滤并洗涤滤饼至中性,将所得产物干燥至恒重备用;
(2)配置铝盐溶液A,铝盐溶液A中铝离子浓度为0.1~1mol/L;
(3)配制碱溶液B,碱溶液B中氢氧根离子浓度为0.1~1mol/L;
(4)将步骤(1)的产物加入去离子水中,超声15~60分钟制成溶液C;
(5)按照步骤(1)的产物与根据步骤(2)铝盐溶液A中铝离子理论制得的氧化铝的质量比为1:50~1:200的比例,当碳纳米管加入太多时,碳纳米管会团聚影响性能,将铝盐溶液A与溶液C混合并超声均匀,将碱溶液B缓慢滴加到混合溶液并磁力搅拌,调节溶液pH值至9,抽滤,并用去离子水洗涤沉淀至中性,然后干燥至恒重;
(6)将步骤(5)的干燥产物置于空气中,在350~450℃煅烧1~3小时,然后置于保护气氛中,在1150~1300℃煅烧1~3小时,得到复合粉体;
(7)将步骤(6)制得的复合粉体采用SPS烧结成型,得到碳纳米管增强氧化铝基复合材料。
步骤(2)所述铝盐为硝酸铝、氯化铝、硫酸铝中的一种或几种任意比例混合。
步骤(3)所述碱溶液B为氨水、氢氧化钠溶液、氢氧化钾溶液中的一种或几种任意比例混合。
步骤(5)所述碱溶液B的滴加速度为0.1~5mL/min。
步骤(5)所述洗涤方式是抽滤滤饼加入去离子水中,搅拌分散均匀后过滤,且洗涤次数为2~4次。
步骤(5)所述干燥方式为干燥箱干燥、冷冻干燥或真空干燥。
步骤(6)所述保护气氛为氩气气氛或氮气气氛。
步骤(7)所述SPS烧结的烧结参数为:真空条件下,压力30~80MPa,烧结温度1150~1500℃,升温速度为80~150℃/min。
所述SPS烧结为放电等离子烧结的缩写。
本发明的有益效果是:
本发明的碳纳米管增强氧化铝基复合材料碳纳米管表面被氧化铝包覆从而减少其团聚现象,并可以提高增强相与基体的界面结合强度;碳纳米管在基体中均匀分散能保证材料性能的连续性;工艺简单,相对于球磨工艺可以减少制备过程对碳纳米管的破坏作用;该方法设备要求低,适用于工业化生产;采用SPS快速烧结方法使产品既能拥有较高的强度,又能显著提高其断裂韧性。
附图说明
图1为实施例1步骤(6)制备的碳纳米管表面包覆氧化铝颗粒的复合粉体FE-SEM图;
图2为实施例1步骤(6)380℃热处理后与1200℃热处理后XRD对比图;
图3为实施例1步骤(7)最后得到的碳纳米管增强氧化铝基复合材料的FE-SEM图。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1
一种碳纳米管增强氧化铝基复合材料的制备方法,具体步骤如下:
(1)碳纳米管预处理:将质量分数为98%的浓硫酸与质量分数为65%的浓硝酸按体积比3:1混合制得混酸,按照碳纳米管与浓硫酸质量体积比g:mL为1:6的比例,将碳纳米管加入到混酸中,封口,65℃水浴恒温5.5小时,再加入12倍混酸体积的去离子水,搅拌成混合均匀的混合液,抽滤并洗涤滤饼至中性,将所得产物恒温干燥箱70℃干燥至恒重备用;
(2)配置氯化铝溶液A,氯化铝溶液A中铝离子浓度为0.6mol/L;
(3)配制氢氧化钾溶液B,氢氧化钾溶液B中氢氧根离子浓度为0.6mol/L;
(4)将步骤(1)的产物加入去离子水中,超声40分钟制成溶液C;
(5)按照步骤(1)的产物与根据步骤(2)氯化铝溶液A中铝离子理论制得的氧化铝的质量比为1:100的比例,将氯化铝溶液A与溶液C混合并超声均匀,将氢氧化钾溶液B缓慢滴加到混合溶液并磁力搅拌,氢氧化钾溶液B的滴加速度为1mL/min,调节溶液pH值至9,抽滤,并用去离子水洗涤沉淀至中性,洗涤方式是抽滤滤饼加入去离子水中,搅拌分散均匀后过滤,且洗涤次数为3次,然后干燥箱干燥至恒重;
(6)将步骤(5)的干燥产物置于空气中,在380℃煅烧2.5h,然后置于氮气气氛中,在1200℃煅烧1.5小时,得到碳纳米管表面包覆氧化铝颗粒的复合粉体;
(7)将步骤(6)制得的复合粉体采用SPS烧结成型,SPS烧结的烧结参数为:真空条件下,压力60MPa,烧结温度1400℃,升温速度为120℃/min,得到碳纳米管增强氧化铝基复合材料。
本实施例所得复合材料相对密度为97.66%,抗弯强度为495.3KN/mm2,断裂韧性比纯氧化铝提高86%。
如图1所示为本实施例步骤(6)制备的碳纳米管表面包覆氧化铝颗粒的复合粉体FE-SEM图,从图中可以看出CNTs被包裹在氧化铝基体中,分散均匀且不会因后期粉末的移动而发生再次团聚,从而解决了CNTs在复合材料中的团聚问题;图2步骤(6)380℃热处理后与1200℃热处理后XRD对比图,从图中可以看出380℃预烧后所形成的为无定型氧化铝,1200℃预烧后产物变成了α-Al2O3,这么做的目的是在低温下分解氢氧化铝并保证其产生的水分子不会对碳纳米管造成破坏,然后在高温下预烧将原料预烧为稳定的α-Al2O3,有利于烧结的致密化;图3步骤(7)最后得到的碳纳米管增强氧化铝基复合材料的FE-SEM图,从图中可以看出碳纳米管均匀的嵌入氧化铝基体中,可以发挥其优良的力学性能,阻碍裂纹的扩展,从而提高陶瓷的断裂韧性及弯曲强度。
实施例2
一种碳纳米管增强氧化铝基复合材料的制备方法,具体步骤如下:
(1)碳纳米管预处理:将质量分数为98%的浓硫酸与质量分数为65%的浓硝酸按体积比3:1混合制得混酸,按照碳纳米管与浓硫酸质量体积比g:mL为1:5的比例,将碳纳米管加入到混酸中,封口,65℃水浴恒温4小时,再加入8倍混酸体积的去离子水,搅拌成混合均匀的混合液,抽滤并洗涤滤饼至中性,将所得产物冷冻干燥至恒重备用;
(2)配置硝酸铝溶液A,硝酸铝溶液A中铝离子浓度为0.1mol/L;
(3)配制氨水B,氨水B中氢氧根离子浓度为0.1mol/L;
(4)将步骤(1)的产物加入去离子水中,超声15分钟制成溶液C;
(5)按照步骤(1)的产物与根据步骤(2)硝酸铝溶液A中铝离子理论制得的氧化铝的质量比为1: 50的比例,将硝酸铝溶液A与溶液C混合并超声均匀,将氨水B缓慢滴加到混合溶液并磁力搅拌,氨水B的滴加速度为2mL/min,调节溶液pH值至9,抽滤,并用去离子水洗涤沉淀至中性,洗涤方式是抽滤滤饼加入去离子水中,搅拌分散均匀后过滤,且洗涤次数为3次,然后干燥箱干燥至恒重;
(6)将步骤(5)的干燥产物置于空气中,在450℃煅烧1h,然后置于氩气气氛中,在1300℃煅烧1小时,得到碳纳米管表面包覆氧化铝颗粒的复合粉体;
(7)将步骤(6)制得的复合粉体采用SPS烧结成型,SPS烧结的烧结参数为:真空条件下,压力30MPa,烧结温度1500℃,升温速度为150℃/min,得到碳纳米管增强氧化铝基复合材料。
所得复合材料相对密度为96.68%,抗弯强度为362.4KN/mm2,断裂韧性比纯氧化铝提高73%。
实施例3
一种碳纳米管增强氧化铝基复合材料的制备方法,具体步骤如下:
(1)碳纳米管预处理:将质量分数为98%的浓硫酸与质量分数为65%的浓硝酸按体积比3:1混合制得混酸,按照碳纳米管与浓硫酸质量体积比g:mL为1:4的比例,将碳纳米管加入到混酸中,封口,65℃水浴恒温6小时,再加入15倍混酸体积的去离子水,搅拌成混合均匀的混合液,抽滤并洗涤滤饼至中性,将所得产物于恒温干燥箱70℃干燥至恒重备用;
(2)配置硝酸铝溶液A,硝酸铝溶液A中铝离子浓度为1mol/L;
(3)配制氢氧化钠溶液B,氢氧化钠溶液B中氢氧根离子浓度为1mol/L;
(4)将步骤(1)的产物加入去离子水中,超声60分钟制成溶液C;
(5)按照步骤(1)的产物与根据步骤(2)硝酸铝溶液A中铝离子理论制得的氧化铝的质量比为1:200的比例,将硝酸铝溶液A与溶液C混合并超声均匀,将氢氧化钠溶液B缓慢滴加到混合溶液并磁力搅拌,氢氧化钠溶液B的滴加速度为5mL/min,调节溶液pH值至9,抽滤,并用去离子水洗涤沉淀至中性,洗涤方式是抽滤滤饼加入去离子水中,搅拌分散均匀后过滤,且洗涤次数为2次,然后干燥箱干燥至恒重;
(6)将步骤(5)的干燥产物置于空气中,在350℃煅烧3h,然后置于氩气气氛中,在1150℃煅烧3小时,得到碳纳米管表面包覆氧化铝颗粒的复合粉体;
(7)将步骤(6)制得的复合粉体采用SPS烧结成型,SPS烧结的烧结参数为:真空条件下,压力80MPa,烧结温度1150℃,升温速度为80℃/min,得到碳纳米管增强氧化铝基复合材料。
所得复合材料相对密度为92.6%,抗弯强度为355.7KN/mm2,断裂韧性比纯氧化铝提高64%。
实施例4
一种碳纳米管增强氧化铝基复合材料的制备方法,具体步骤如下:
(1)碳纳米管预处理:将质量分数为98%的浓硫酸与质量分数为65%的浓硝酸按体积比3:1混合制得混酸,按照碳纳米管与浓硫酸质量体积比g:mL为1:4.5的比例,将碳纳米管加入到混酸中,封口,65℃水浴恒温5小时,再加入10倍混酸体积的去离子水,搅拌成混合均匀的混合液,抽滤并洗涤滤饼至中性,将所得产物真空干燥至恒重备用;
(2)配置硝酸铝和氯化铝质量比1:2混合后加水形成的溶液A,溶液A中铝离子浓度为0.5mol/L;
(3)配制氢氧化钠和氢氧化钾质量比1:1混合后加水形成的溶液B,溶液B中氢氧根离子浓度为1mol/L;
(4)将步骤(1)的产物加入去离子水中,超声30分钟制成溶液C;
(5)按照步骤(1)的产物与根据步骤(2)溶液A中铝离子理论制得的氧化铝的质量比为1:120的比例,将溶液A与溶液C混合并搅拌均匀,将溶液B缓慢滴加到混合溶液并磁力搅拌,溶液B的滴加速度为0.1mL/min,调节溶液pH值至9,抽滤,并用去离子水洗涤沉淀至中性,洗涤方式是抽滤滤饼加入去离子水中,搅拌分散均匀后过滤,且洗涤次数为3次,然后干燥箱干燥至恒重;
(6)将步骤(5)的干燥产物置于空气中,在400℃煅烧2小时,然后置于氮气气氛中,在1250℃煅烧2小时,得到碳纳米管表面包覆氧化铝颗粒的复合粉体;
(7)将步骤(6)制得的复合粉体采用SPS烧结成型,SPS烧结的烧结参数为:真空条件下,压力50MPa,烧结温度1300℃,升温速度为100℃/min,得到碳纳米管增强氧化铝基复合材料。
所得复合材料相对密度为93.4%,抗弯强度为455.7KN/mm2,断裂韧性比纯氧化铝提高71%。
Claims (6)
1.一种碳纳米管增强氧化铝基复合材料的制备方法,其特征在于,具体步骤如下:
(1)碳纳米管预处理:将质量分数为98%的浓硫酸与质量分数为65%的浓硝酸按体积比3:1混合制得混酸,按照碳纳米管与浓硫酸质量体积比g:mL为1:4~6的比例,将碳纳米管加入到混酸中,封口,65℃水浴恒温4~6小时,再加入8-15倍混酸体积的去离子水,搅拌成混合均匀的混合液,抽滤并洗涤滤饼至中性,将所得产物干燥至恒重备用;
(2)配置铝盐溶液A,铝盐溶液A中铝离子浓度为0.1~1mol/L;
(3)配制碱溶液B,碱溶液B中氢氧根离子浓度为0.1~1mol/L;
(4)将步骤(1)的产物加入去离子水中,超声15~60分钟制成溶液C;
(5)按照步骤(1)的产物与根据步骤(2)铝盐溶液A中铝离子理论制得的氧化铝的质量比为1:50~200的比例,将铝盐溶液A与溶液C混合并超声混匀,将碱溶液B滴加到混合溶液并磁力搅拌,调节pH值至9,抽滤,并用去离子水洗涤沉淀至中性,然后干燥至恒重;
(6)将步骤(5)的干燥产物置于空气中,在350~450℃煅烧1~3小时,然后置于保护气氛中,在1150~1300℃煅烧1~3小时,得到复合粉体;
(7)将步骤(6)制得的复合粉体采用SPS烧结成型,得到碳纳米管增强氧化铝基复合材料。
2.根据权利要求1所述碳纳米管增强氧化铝基复合材料的制备方法,其特征在于,步骤(2)所述铝盐为硝酸铝、氯化铝、硫酸铝中的一种或几种任意比例混合。
3.根据权利要求1所述碳纳米管增强氧化铝基复合材料的制备方法,其特征在于,步骤(3)所述碱溶液B为氨水、氢氧化钠溶液、氢氧化钾溶液中的一种或几种任意比例混合。
4.根据权利要求1所述碳纳米管增强氧化铝基复合材料的制备方法,其特征在于,步骤(5)所述碱溶液B的滴加速度为0.1~5mL/min。
5.根据权利要求1所述碳纳米管增强氧化铝基复合材料的制备方法,其特征在于,步骤(6)所述保护气氛为氩气气氛或氮气气氛。
6.根据权利要求1所述碳纳米管增强氧化铝基复合材料的制备方法,其特征在于,步骤(7)所述SPS烧结的烧结参数为:真空条件下,压力30~80MPa,烧结温度1150~1500℃,升温速度为80~150℃/min。
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