CN107117970A - 一种新型生产低电阻高强度石墨材料的复合添加剂及该石墨材料的制备方法 - Google Patents
一种新型生产低电阻高强度石墨材料的复合添加剂及该石墨材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种新型生产低电阻高强度石墨材料的复合添加剂及该石墨材料的制备方法,其中,该复合添加剂为稀土金属粉末或稀土化合物与钛金属粉末或钛化合物的混合物,两种物质混合时的质量比为1:1~1:5;所述稀土化合物选自稀土有机化合物和稀土无机化合物中的一种或几种;所述钛化合物选自钛有机化合物和钛无机化合物中的一种或几种。
Description
技术领域
本发明涉及石墨材料技术领域,具体地说,涉及一种新型生产低电阻高强度石墨材料的复合添加剂及该低电阻高强度石墨材料的制备方法。
背景技术
石墨化过程中影响石墨产品性能的关键因素之一是气胀,焙烧品在石墨化炉中,当温度升高到1400℃以上时,氢、硫、氮等元素将以H2、H2S、N2、NH3等形式释放出来,其中氮元素主要在1400~1900℃释放出来,而硫元素集中在1700~2100℃区间释放出来,此时处于可塑状态的焦炭气孔壁受到排除气体的压力,体积产生膨胀,降低了石墨产品的物化性能。而通过添加气胀抑制剂或控制石墨化过程中1700~2100℃这一温度区间的升温速率,均能降低这一区间杂质气体的释放速率,从而有效的抑制气胀。催化石墨化可在满足性能要求的前提下,降低石墨化温度(石墨化度不降低),简化对设备的要求,减少热应力,缩短石墨化时间,实现节能降耗,降低生产制造成本。例如,在制备过程中,通过添加氧化铁,可有效降低石墨化温度并抑制气胀,添加氧化铁的方案已经在工程领域中加以应用。然而铁又是对石墨制品有害的元素,过多的加入将影响石墨制品的机械性能。
发明内容
本发明所要解决的技术问题在于克服现有技术的上述不足,提供一种在用于生产低电阻高强度石墨材料时能够有效降低石墨制品电阻率、提高石墨制品抗折强度的复合添加剂。
其所要解决的技术问题可以通过以下技术方案来实施。
一种新型生产低电阻高强度石墨材料的复合添加剂,其特点为,该复合添加剂为稀土金属粉末或稀土化合物与钛金属粉末或钛化合物的混合物,两种物质混合时的质量比为1:1~1:5;所述稀土化合物选自稀土有机化合物和稀土无机化合物中的一种或几种;所述钛化合物选自钛有机化合物和钛无机化合物中的一种或几种。
作为本发明的优选实施例之一,所述稀土金属粉末或稀土化合物与钛金属粉末或钛化合物混合时,两种物质的质量比为1:3。
作为本技术方案的进一步改进,所述稀土化合物为稀土氧化物、稀土碳化物和稀土卤化物中的一种或几种;所述镍化合物为氧化钛、碳化钛和二硼化钛中的一种或几种。
也作为本技术方案的进一步改进,所述稀土化合物为RE2O3、RE6O11和REX3中的一种或几种,所述RE为稀土元素,所述REX3中的X为Cl、Br或I;所述钛化合物为TiO2、TiC、TiB2和TiY4中的一种或几种,所述TiY4中的Y为Cl、Br或I;所选的X与Y相同或不同。
其中,所述的RE为Sc、Y、La、Ce、Pr、Nd、Pm、Sm或Eu;所述稀土金属粉末为Sc、Y、La、Ce、Pr、Nd、Pm、Sm或Eu的金属粉末。
本发明所要解决的另一种技术问题在于提供一种采用上述复合添加剂生产低电阻高强度石墨材料的制备方法,其特点为,所述石墨材料以普通石油焦、沥青焦、针状焦或炭纤维为基体,煤沥青、石油沥青或中间相沥青为粘结剂通过成型及致密化后石墨化而成。
其中,该方法中,所述复合添加剂在石墨材料生产原料中的质量百分比为0.1%~15%。优选3%~10%。
作为本方法的优选实施例,制备时先将复合添加剂球磨过200目筛(76μm),与普通石油焦、沥青焦或炭纤维均匀混合,再加上沥青粘结剂,进行混捏,成型,并经过2~4次循环焙烧与浸渍,最终石墨化制成石墨材料。
与现有技术相比,本发明的积极效果如下:
稀土化合物除了具有抑制石墨化过程由于氮硫产生的气胀作用,而且与钛的化合物对石墨制品石墨化过程中产生共催化作用,复合添加剂的共催化,体现在两种催化剂对碳材料催化作用温度范围不同,两种催化剂的复合扩展了催化作用的温度范围,同时在1700~2200℃范围内,有效抑制氮硫元素引起的碳材料制品的气胀,效果体现在石墨制品体积膨胀减小,未出现裂纹,有效降低石墨化温度,提高石墨化程度,从而降低石墨制品电阻率。
为了使稀土化合物很好的应用于石墨制品中,稀土元素以轻稀土元素为好,且为稀土氧化物最佳,钛则以金属钛或二氧化钛粉末为最佳,其中代表的复合添加剂为氧化镧和金属钛粉末、氧化铈和金属钛粉末、氧化镨和金属钛粉末。
稀土与钛的复合添加剂作为石墨添加剂主要用于低电阻、石墨材料的生产,如石墨导热材料,石墨散热材料,核石墨材料,航空用石墨材料,石墨电极,冶金石墨阳极等。
本发明技术方案中采用的稀土元素在与硫反应生成硫化物,并在高温下分解,能够降低气态氮、硫的释放速率,抑制气胀的发生。并且这里所采用的稀土氧化物等稀土化合物能够优先创造气体逃逸通道,有效抑制膨胀。稀土金属的较高蒸气压使稀土碳化物在高温下不稳定,稀土碳化物不断分解,不断生成,处于动态平衡,进而促进石墨化过程。
而钛的熔点为1675℃,钛原子在温度高于1900℃以上时,能够与碳材料中的游离碳原子发生反应生成熔点高、稳定性好的碳化钛。因此添加钛及钛的化合物能在碳材料急剧释放氮、硫等元素的温度区间内显著降低石墨化过程升温速率。
通过添加由稀土元素和钛粉末以及相关化合物组合而成的复合添加剂,既有效抑制了气胀,又催化石墨化,促进了石墨化,降低石墨制品电阻率,提高石墨制品抗折强度。
具体实施方式
以下通过具体的实例例对本发明的具体实施方式进行进一步的详细说明。
本发明涉及一种新型生产低电阻高强度石墨材料的复合添加剂,为稀土金属粉末或者稀土化合物与钛金属粉末或者钛的化合物组合成复合添加剂,所述稀土化合物为稀土氧化物、稀土碳化物、稀土卤化物以及其他稀土有机化合物和无机化合物的一种或者几种混合,所述钛的化合物为氧化钛、碳化钛、二硼化钛以及其他钛有机化合物和无机化合物的一种或者几种混合;本发明的优点:稀土和钛化合物组合成复合添加剂,作为石墨添加剂的新应用,能够有效降低石墨制品电阻率,提高石墨制品的抗折强度。
以下提供本发明一种新型生产低电阻高强度石墨材料的复合添加剂的具体实施方式。
实施例1;
采用含硫量1%、含氮量0.5%的煤系针状焦1t,改质煤沥青0.25t,金属钛粉末3kg,氧化镧1kg进行配料,其中煤系针状焦粒度配比(按质量百分比)为:1~2mm为12.5%,0.5~1mm为22.5%,0.15~0.5mm为30%,0.076~0.15mm为25%,<0.076mm为10%;改质煤沥青软化点115℃;氧化镧和金属钛粒度小于76μm。通过将以上原料采用通常的石墨制备工艺进行混捏,成型,焙烧,2次浸渍–焙烧,石墨化等工序,制成石墨材料。其中石墨材料电阻率低于4.5μΩ·m,体积密度达1.75g/cm3以上,抗折强度高达12MPa。
实施例2:
采用含硫量1%,含氮量0.5%的煤系针状焦1t,改质煤沥青0.25t,金属钛粉末3kg,氧化铈2kg进行配料,其中煤系针状焦粒度配比(按质量百分比)为:1~2mm为12.5%,0.5~1mm为22.5%,0.15~0.5mm为30%,0.076~0.15mm为25%,<0.076mm为10%;改质煤沥青软化点115℃;氧化铈和金属钛粒度小于76μm。通过将以上原料采用通常的石墨制备工艺进行混捏,成型,焙烧,2次浸渍–焙烧,石墨化等工序,制成石墨材料。其中石墨材料电阻率低于4.5μΩ·m,体积密度达1.72g/cm3以上,抗折强度高达12MPa。
实施例3:
采用含硫量1%,含氮量0.5%的煤系针状焦1t,改质煤沥青0.25t,金属钛粉末3kg,氧化镨2kg进行配料,其中煤系针状焦粒度配比(按质量百分比)为:1~2mm为12.5%,0.5~1mm为22.5%,0.15~0.5mm为30%,0.076~0.15mm为25%,<0.076mm为10%;改质煤沥青软化点115℃;氧化镨和金属钛粒度小于76μm。通过将以上原料采用通常的石墨制备工艺进行混捏,成型,焙烧,2次浸渍–焙烧,石墨化等工序,制成石墨材料。其中石墨材料电阻率低于4.1μΩ·m,体积密度达1.78g/cm3以上,抗折强度高达15MPa。
以上所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员,在不脱离本发明构思的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围内。
Claims (9)
1.一种新型生产低电阻高强度石墨材料的复合添加剂,其特征在于,该复合添加剂为稀土金属粉末或稀土化合物与钛金属粉末或钛化合物的混合物,两种物质混合时的质量比为1:1~1:5;所述稀土化合物选自稀土有机化合物和稀土无机化合物中的一种或几种;所述钛化合物选自钛有机化合物和钛无机化合物中的一种或几种。
2.根据权利要求1所述一种新型生产低电阻高强度石墨材料的复合添加剂,其特征在于,所述稀土金属粉末或稀土化合物与钛金属粉末或钛化合物混合时,两种物质的质量比为1:3。
3.根据权利要求1所述一种新型生产低电阻高强度石墨材料的复合添加剂,其特征在于,所述稀土化合物为稀土氧化物、稀土碳化物和稀土卤化物中的一种或几种;所述镍化合物为氧化钛、碳化钛和二硼化钛中的一种或几种。
4.根据权利要求1所述一种新型生产低电阻高强度石墨材料的复合添加剂,其特征在于,所述稀土化合物为RE2O3、RE6O11和REX3中的一种或几种,所述RE为稀土元素,所述REX3中的X为Cl、Br或I;所述钛化合物为TiO2、TiC、TiB2和TiY4中的一种或几种,所述TiY4中的Y为Cl、Br或I;所选的X与Y相同或不同。
5.根据权利要求4所述一种新型生产低电阻高强度石墨材料的复合添加剂,其特征在于,所述的RE为Sc、Y、La、Ce、Pr、Nd、Pm、Sm或Eu;所述稀土金属粉末为Sc、Y、La、Ce、Pr、Nd、Pm、Sm或Eu的金属粉末。
6.一种采用权利要求1-5中任一权利要求所述复合添加剂生产低电阻高强度石墨材料的制备方法,其特征在于,所述石墨材料以普通石油焦、沥青焦、针状焦或炭纤维为基体,煤沥青、石油沥青或中间相沥青为粘结剂通过成型及致密化后石墨化而成。
7.根据权利要求6所述的制备方法,其特征在于,所述复合添加剂在石墨材料生产原料中的质量百分比为0.1%~15%。
8.根据权利要求7所述的制备方法,其特征在于,所述复合添加剂在石墨材料生产原料中的质量百分比为3%~10%。
9.根据权利要求7所述的制备方法,其特征在于,制备时先将复合添加剂球磨过200目筛,与普通石油焦、沥青焦或炭纤维均匀混合,再加上沥青粘结剂,进行混捏,成型,并经过2~4次循环焙烧与浸渍,最终石墨化制成石墨材料。
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