CN106242571A - 一种碳化钛储氢材料的制备方法 - Google Patents
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Abstract
一种碳化钛储氢材料的制备方法,它根据碳含量与储氢性能的关系,经备料、混料、压制、烧结等步骤制备碳化钛储氢材料。该发明制备的碳化钛储氢材料具有优良的化学稳定性和抗氧化能力,储氢时具有高的抗杂质气体中毒能力;碳化钛储氢材料与其氢化后氢化物晶格类型一致,储放氢循环过程中体积变化小,储氢循环稳定性高;该制备方法工艺简单、原料丰富且价格低廉。
Description
技术领域:
本发明属于储氢材料技术领域,具体涉及一种碳化钛储氢材料的制备方法。
背景技术:
化石燃料燃烧释放出大量的温室气体CO2及有害气体SO2、NOx等,造成日益严重的“温室效应”和大气污染等环境问题。这一问题对于经济快速发展中的中国来说尤其突出。面对日益严重的环境污染,我国今后将逐步调整以煤为主的能源供应战略,着重改善能源利用对环境的影响。为达到这一目的,开发利用清洁的、可持续的新能源是必然选择。氢能由于具有广泛的来源、高的燃烧值及清洁无污染等,而被认为是理想的未来“绿色能源”。而要实现氢能的工业化应用,实现氢的固态存储是关键。当前研究者已开发了多种氢固态存储材料,如申请号为CN201510687910.6的中国发明专利申请公开了一种镁铝硼镍基储氢材料及其制备方法,主要是将镁粉、镍粉、硼粉及铝粉等热压成块,再用液氦快速冷却得到一种镁铝硼镍基储氢材料,该材料活化周期短,吸放氢速率快;申请号为CN201510680110.1的中国发明专利申请公开了一种复合储氢材料及其制备方法,该方法制备的储氢材料由硼化氢锂及非晶钛镁-稀土-镍-合金氢化物组成,该储氢材料具有低的放氢温度和高的放氢量;专利号为ZL02138978.0的中国发明专利发明了一种经微波等离子体刻蚀的一维纳米碳储氢材料及其制备方法,主要是采用微波等离子体刻蚀方法对一维纳米碳表面进行刻蚀,从而由表及里地增加和增大氢的扩散通道,提高一维纳米碳的储氢容量;专利号为ZL201410181654.9的中国发明专利发明了一种铝锂储氢材料及其制备方法,所发明的铝锂储氢材料具有较高的储氢容量。可以看出,当前对固态储氢材料的研究主要集中于金属氢化物如镁系、钛系、锆系、稀土系等,金属配位氢化物和碳纳米材料这几类材料。这些材料各有优势,但目前各自又有不足。如镁系储氢合金储氢容量高、成本低,但是放氢温度高;金属配位氢化物储氢容量高,但是再氢化困难等。这些不足限制了固态储氢材料的进一步推广应用。
发明内容:
本发明的目的在于提供一种碳化钛储氢材料的制备方法,所制备的储氢材料具有较高的储氢容量、良好的储氢动力学性能和循环稳定性,且制备方法简单。
本发明的制备方法如下:
(1)原料准备:准备好制备碳化钛储氢材料所需的原料钛粉和石墨粉,石墨粉的碳和钛粉的钛的原子比为0.48-0.8;或者所用的原材料为近化学计量比碳化钛粉和钛粉,碳化钛粉中的碳与碳化钛粉和钛粉中的钛之和的原子比为0.48-0.8;
(2)原料混配:将钛粉和石墨粉或者近化学计量比碳化钛粉与钛粉混合均匀;
(3)压制成型:将混合均匀的混合粉料压制成高6mm,直径12mm的圆柱体;
(4)烧结:将压制好的原料置于烧结炉中,经烧结、保温、冷却即得到所需的碳化钛储氢材料。
上述碳化钛储氢材料的制备方法,所述烧结步骤首先将首先将压块加热到400-800℃保温1-3小时,随后进一步将压块加热到1100-1550℃,保温1-4小时,使钛粉与石墨粉或者近化学计量比的碳化钛粉与钛粉反应;然后继续升高温度至1750-2000℃,保温2-4小时,使反应后的碳化钛成份均匀化,将上述烧结后的块体随炉冷却至500-850℃保温10-40小时,然后冷却到室温。
上述碳化钛储氢材料的制备方法,所制备的碳化钛储氢材料中碳钛原子比在0.48-0.8之间。
本发明与现有技术相比具有如下优点:
1、所制备的碳化钛储氢材料为陶瓷材料,具有优良的化学稳定性和抗氧化能力,储氢时具有高的抗杂质气体中毒能力;
2、碳化钛与氢化后氢化物晶格类型一致,储放氢循环过程中体积变化小,储氢循环稳定性高;
3、制备方法简单、原料丰富且价格低廉。
具体实施方式:
下面结合具体实施例,进一步阐述发明。应说明的是:以下实施例仅用以说明本发明而并非限制本发明所描述的技术方案。一切不脱离本发明的精神和范围的技术方案及其改进,其均应涵盖在本发明的权利要求范围当中。
实施例1:
(1)原料准备:准备好制备碳化钛储氢材料所需的原料钛粉和石墨粉,石墨粉的碳和钛粉的钛的原子比为0.5;
(2)原料混配:将钛粉和石墨粉混合均匀;
(3)压制成型:将混合均匀的混合粉料压制成高6mm,直径12mm的圆柱体;
(4)烧结:将压制好的原料置于烧结炉中,首先将压块加热到400℃保温3小时,随后加热到1350℃,保温2小时,使钛粉与石墨粉反应;然后继续升高温度至1900℃,保温2小时,使反应后的碳化钛成分均匀化;将上述烧结后的块体随炉冷却至700℃保温40小时,然后冷却到室温即得到化学式为TiC0.5的碳化钛储氢材料。
经电化学储氢试验测定,所得碳化钛储氢材料可在室温下实现氢的可逆存储,储氢容量约为4.0wt.%
实施例2:
(1)原料准备:准备好制备碳化钛储氢材料所需的原料钛粉和石墨粉,石墨粉的碳和钛粉的钛的原子比为0.65;
(2)原料混配:将钛粉和石墨粉混合均匀;
(3)压制成型:将混合均匀的混合粉料压制成高6mm,直径12mm的圆柱体;
(4)烧结:将压制好的原料置于烧结炉中,首先将压块加热到500℃保温2小时,随后进一步加热到1400℃,保温2小时,使钛粉与石墨粉反应;然后继续升高温度至1950℃,保温2小时,使反应后的碳化钛成分均匀化;将上述烧结后的块体随炉冷却至700℃保温30小时,然后冷却到室温即得到化学式为TiC0.65的碳化钛储氢材料。
经电化学储氢试验测定,所得碳化钛储氢材料可在室温下实现氢的可逆存储,储氢容量约为2.85wt.%
实施例3
(1)原料准备:准备好制备碳化钛储氢材料所需的原料近化学计量比的碳化钛粉和钛粉,碳化钛粉中的碳与碳化钛粉和钛粉中的钛之和的原子比为0.7;
(2)原料混配:将碳化钛粉和钛粉混合均匀;
(3)压制成型:将混合均匀的混合粉料压制成高6mm,直径12mm的圆柱体;
(4)烧结:将压制好的原料置于烧结炉中,首先将压块加热到600℃保温1.5小时,随后进一步加热到1500℃,保温3小时,使碳化钛粉与钛粉反应;然后继续升高温度至2000℃,保温2小时,使反应后的碳化钛成分均匀化;再上述烧结后的块体随炉冷却至750℃保温30小时,然后冷却到室温即得到化学式为TiC0.7的碳化钛储氢材料。
经电化学储氢试验测定,所得碳化钛储氢材料可在室温下实现氢的可逆存储,储氢容量约为2.40wt.%。
Claims (2)
1.一种碳化钛储氢材料的制备方法,其特征在于:所述制备方法由以下步骤组成:
(1)原料准备:准备好制备碳化钛储氢材料所需的原料钛粉和石墨粉,石墨粉的碳和钛粉的钛的原子比为0.48-0.8;或者所用的原材料为近化学计量比碳化钛粉和钛粉,碳化钛粉中的碳与碳化钛粉和钛粉中的钛之和的原子比为0.48-0.8;
(2)原料混配:将钛粉和石墨粉或者近化学计量比碳化钛粉与钛粉混合均匀;
(3)压制成型:将混合均匀的混合粉料压制成高6mm,直径12mm的圆柱体;
(4)烧结:将压制好的原料置于烧结炉中,经烧结、保温、冷却即得到所需的碳化钛储氢材料。
2.如权利要求1所述的一种碳化钛储氢材料的制备方法,其特征在于:首先将压块加热到400-800℃保温1-3小时,然后进一步将压块加热到1100-1550℃,保温1-4小时,使钛粉与石墨粉或者近化学计量比的碳化钛粉与钛粉反应;然后继续升高温度至1750-2000℃,保温2-4小时,使反应后的碳化钛成份均匀化,将上述烧结后的块体随炉冷却至500-850℃保温10-40小时,然后冷却到室温。
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CN111875383A (zh) * | 2020-08-13 | 2020-11-03 | 华北电力大学(保定) | 一种非化学计量比碳化钛储氢材料及其制备方法 |
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Cited By (4)
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CN108439330A (zh) * | 2018-04-20 | 2018-08-24 | 常州达奥新材料科技有限公司 | 一种复合型镁铝基储氢材料的制备方法 |
CN111620678A (zh) * | 2020-05-27 | 2020-09-04 | 新化县群华陶瓷科技有限公司 | 一种有机复合多孔陶瓷材料及其制备方法 |
CN111875383A (zh) * | 2020-08-13 | 2020-11-03 | 华北电力大学(保定) | 一种非化学计量比碳化钛储氢材料及其制备方法 |
CN111875383B (zh) * | 2020-08-13 | 2022-04-15 | 华北电力大学(保定) | 一种非化学计量比碳化钛储氢材料及其制备方法 |
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