自蔓延—热压工艺制备热电材料β-FeSi_2
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摘要
热电材料是一类能直接实现热电转换功能的材料，无需机械部件，无噪音，节约能源，因此受到人们的关注。其中β-FeSi_2作为热电材料，在世界能源危机日益显现和人们致力于绿色能源开发的今天，对其的研究开发应用有着重要的现实意义。它的特点是具有比较高的Seebeck系数，来源广泛，价格低廉，高温抗氧化性好，无毒以及高的工作温度。由于β-FeSi_2具备以上优点，它有广泛的应用前景。
本文采用自蔓延-热压工艺制备热电材料β-FeSi_2。主要从以下几个方面进行研究：1.对于自蔓延高温合成(燃烧合成)的中间产物α-Fe_2Si_5在转变为β-FeSi_2的过程中，热压时间固定为4min，探究不同的热压温度和压力对合成产物的影响，总结最合理的热压工艺参数；2.燃烧合成过程中为了使得产物只包含α-Fe_2Si_5，在配料阶段通过改变硅的含量，研究燃烧合成产物相的组成，寻找最合理的铁硅比例；3.对比分析不同的铜掺杂含量对合成产物的影响，探究最佳掺杂比例；4.通过掺杂不同含量的铝，分析不同含量下合成产物的相组成结构及形貌。
实验结果表明：1.当铁硅原子比为nFe:nSi=1:3，掺入0.50at%的Cu，热压时间定为4min，热压温度为720℃时，α-Fe_2Si_5已经基本转变为β-FeSi_2，到800℃时部分β相重新转变为α-Fe_2Si_5，且压力的提高有助于β-FeSi_2生成和致密度的提高；2.当铁、硅原子比例为1:2.5时，燃烧合成的球粒状产物只包含α-Fe_2Si_5，消除了ε-FeSi相；利用酒精在超声波清洗仪中清洗燃烧合成球粒状产物时，如果清洗不够充分，熔渣中的ε-FeSi粘附于球粒上，会导致β-FeSi_2合成过程中ε相剩余；3.在利用共析反应α→β+Si生成β-FeSi_2的过程中，少量Cu的掺入可以明显提高反应速度，并且随着Cu含量的增加，反应速度随之提高，由断口SEM形貌可见，反应生成了大小均匀的β-FeSi_2微粒，而生成的Si弥散分布于其中；4.铝的掺入可以提高原始粉料的的利用率，但铝对α-Fe_2Si_5向β-FeSi_2转变的促进作用不太明显。为了避免铝的过多的掺入，当掺入2at%Al的同时掺入0.2at%Cu，α-Fe_2Si_5完全转变为β-FeSi_2，β相的峰值达到最高。
Thermoelectric materials, which can realize thermoelectric conversion directly withoutany mechanical equipments and noise, are attractive as a kind of save-energymaterials. Withincreasing energy crisis，green energy is explored．So doing research and development ofβ-FeSi_2as a potential thermoelectric material possesses important practical significance．It hashigh Seebeck coefficient, abundance as a raw material, low cost, high oxidation resistance,non-toxicity, and high working temperature. Because β-FeSi_2with the above advantages, ithas broad application prospects, and one that fits well with the operating temperatures ofindustrial furnaces, automobile exhausts, and incinerators. However, the synthesis of β-FeSi_2is very difficulty.
In this paper, we synthesis β-FeSi_2by the way of SHS-hot pressing technology. Thispaper study the following aspects:1.In the process of Intermediate products α-Fe_2Si_5intoβ-FeSi_2, when the temperature is fixed at4min, we looked for the best hot insulation pressingtemperature and pressure through selecting different holding time and pressure, and thenconcluded the most reasonable of hot press process parameters；2.In order to make thecombustion synthesis products contain only α-Fe_2Si_5, we studied the composition of thecombustion synthesis to find the most reasonable proportion of Fe and Si in the batching stageby changing the Si content；3.The best doping ratio were explored through comparativeanalysis of different Cu doping content of synthetic products；4.By doped with differentcontent of Al, we analysis of the phase composition and morphology of the synthetic productsof the different Al content.
The experimental results include the following main points:1.The main products ofcombustion synthesis are α-Fe_2Si_5and Si when the atomic ratio of Fe to Si is1:3and0.5at%copper is doped. When the temperature is800℃, the parts of β-FeSi_2re-transformed intoα-Fe_2Si_5, pressure increased contributes to the products density increase and α-Fe_2Si_5transformed into β-FeSi_2；2.When the atomic ratio of Iron, silicon is1:2.5, the combustionsynthesis sphere products only contain α-Fe_2Si_5and eliminating ε-FeSi phase. The followingtest and analysis results have larger deviation whether combustion synthesis sphere productsare clean using ultrasonic cleaning device.when the cleaning is insufficient, the ε-FeSi in theslag buildup in the sphere, and then they will make the synthesis process of β-FeSi_2is notentirely；3.In the process of Eutectoid reaction α→β+Si to generate β-FeSi_2, a small amount ofCu doping can significantly improve the speed of response, and the reaction speed willincrease with increasing Cu content.The particles of reaction are uniform size be seen by the fracture SEM micrographs,and the Si particles dispersed in it；4.Al does not affect the phasecomposition of the combustion synthesis shere products, the sphere products of combustionsynthesis are still α-Fe_2Si_5, but Al doping can improve the utilization of the original powder，and the effect of doped Al is not obviously in the process of α→β+Si. In order to avoidexcessive Al, α-Fe_2Si_5completely transformed into β-FeSi_2while2at%Al is doped inoriginal powder adds0.2at%Cu to it. The hot pressed samples achieve the highest peak ofthe β phase.
本文采用自蔓延-热压工艺制备热电材料β-FeSi_2。主要从以下几个方面进行研究：1.对于自蔓延高温合成(燃烧合成)的中间产物α-Fe_2Si_5在转变为β-FeSi_2的过程中，热压时间固定为4min，探究不同的热压温度和压力对合成产物的影响，总结最合理的热压工艺参数；2.燃烧合成过程中为了使得产物只包含α-Fe_2Si_5，在配料阶段通过改变硅的含量，研究燃烧合成产物相的组成，寻找最合理的铁硅比例；3.对比分析不同的铜掺杂含量对合成产物的影响，探究最佳掺杂比例；4.通过掺杂不同含量的铝，分析不同含量下合成产物的相组成结构及形貌。
实验结果表明：1.当铁硅原子比为nFe:nSi=1:3，掺入0.50at%的Cu，热压时间定为4min，热压温度为720℃时，α-Fe_2Si_5已经基本转变为β-FeSi_2，到800℃时部分β相重新转变为α-Fe_2Si_5，且压力的提高有助于β-FeSi_2生成和致密度的提高；2.当铁、硅原子比例为1:2.5时，燃烧合成的球粒状产物只包含α-Fe_2Si_5，消除了ε-FeSi相；利用酒精在超声波清洗仪中清洗燃烧合成球粒状产物时，如果清洗不够充分，熔渣中的ε-FeSi粘附于球粒上，会导致β-FeSi_2合成过程中ε相剩余；3.在利用共析反应α→β+Si生成β-FeSi_2的过程中，少量Cu的掺入可以明显提高反应速度，并且随着Cu含量的增加，反应速度随之提高，由断口SEM形貌可见，反应生成了大小均匀的β-FeSi_2微粒，而生成的Si弥散分布于其中；4.铝的掺入可以提高原始粉料的的利用率，但铝对α-Fe_2Si_5向β-FeSi_2转变的促进作用不太明显。为了避免铝的过多的掺入，当掺入2at%Al的同时掺入0.2at%Cu，α-Fe_2Si_5完全转变为β-FeSi_2，β相的峰值达到最高。
Thermoelectric materials, which can realize thermoelectric conversion directly withoutany mechanical equipments and noise, are attractive as a kind of save-energymaterials. Withincreasing energy crisis，green energy is explored．So doing research and development ofβ-FeSi_2as a potential thermoelectric material possesses important practical significance．It hashigh Seebeck coefficient, abundance as a raw material, low cost, high oxidation resistance,non-toxicity, and high working temperature. Because β-FeSi_2with the above advantages, ithas broad application prospects, and one that fits well with the operating temperatures ofindustrial furnaces, automobile exhausts, and incinerators. However, the synthesis of β-FeSi_2is very difficulty.
In this paper, we synthesis β-FeSi_2by the way of SHS-hot pressing technology. Thispaper study the following aspects:1.In the process of Intermediate products α-Fe_2Si_5intoβ-FeSi_2, when the temperature is fixed at4min, we looked for the best hot insulation pressingtemperature and pressure through selecting different holding time and pressure, and thenconcluded the most reasonable of hot press process parameters；2.In order to make thecombustion synthesis products contain only α-Fe_2Si_5, we studied the composition of thecombustion synthesis to find the most reasonable proportion of Fe and Si in the batching stageby changing the Si content；3.The best doping ratio were explored through comparativeanalysis of different Cu doping content of synthetic products；4.By doped with differentcontent of Al, we analysis of the phase composition and morphology of the synthetic productsof the different Al content.
The experimental results include the following main points:1.The main products ofcombustion synthesis are α-Fe_2Si_5and Si when the atomic ratio of Fe to Si is1:3and0.5at%copper is doped. When the temperature is800℃, the parts of β-FeSi_2re-transformed intoα-Fe_2Si_5, pressure increased contributes to the products density increase and α-Fe_2Si_5transformed into β-FeSi_2；2.When the atomic ratio of Iron, silicon is1:2.5, the combustionsynthesis sphere products only contain α-Fe_2Si_5and eliminating ε-FeSi phase. The followingtest and analysis results have larger deviation whether combustion synthesis sphere productsare clean using ultrasonic cleaning device.when the cleaning is insufficient, the ε-FeSi in theslag buildup in the sphere, and then they will make the synthesis process of β-FeSi_2is notentirely；3.In the process of Eutectoid reaction α→β+Si to generate β-FeSi_2, a small amount ofCu doping can significantly improve the speed of response, and the reaction speed willincrease with increasing Cu content.The particles of reaction are uniform size be seen by the fracture SEM micrographs,and the Si particles dispersed in it；4.Al does not affect the phasecomposition of the combustion synthesis shere products, the sphere products of combustionsynthesis are still α-Fe_2Si_5, but Al doping can improve the utilization of the original powder，and the effect of doped Al is not obviously in the process of α→β+Si. In order to avoidexcessive Al, α-Fe_2Si_5completely transformed into β-FeSi_2while2at%Al is doped inoriginal powder adds0.2at%Cu to it. The hot pressed samples achieve the highest peak ofthe β phase.
引文
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[2]李伟文，赵新兵，周邦昌．β-FeSi2热电材料的研究进展[J]．材料导报，2002，16(05)：14-16
[3]张丽鹏，于先进，肖晓明．热电材料的研究进展[J]．现代技术陶瓷，2006，(109)：21-22
[4]况学成，郝恩奇．热电材料及其研究现状[J]．中国陶瓷工业，2008，15(05)：27-30．
[5]罗胜耘，曾正，路安江．一种新型环境半导体材料—β-FeSi2[J]．广西轻工业，2008，24(05)：20-21
[6] D Leong, M Harry，KJ Recscn, et al．A Silicon/Iron-Disilicide Light-Emitting Diode Operating at a Wavelength Of1.5μm[J]. Nature,1997,387(6634):686-688
[7]罗胜耘，谢泉，张晋敏等．热处理对环境半导体材料β-FeSi2形成的影响[J]．贵州大学学报(自然科学版)，2006，23(01)：81-85
[8] Ozvold M，Dubnicka M，Gasparik V．The Temperature Dependenceof the Directgap of β-FeSi2Films[J]. SolidFilms,1997,295(1-2):147-150
[9]朱铁军，赵新兵．β-FeSi2热电材料的性能优化及测试方法[J]．材料科学与工程，1999，17(04)：55-58
[10] M.Umemoto. Preparation of thermoelectric β-FeSi2doped with Al and Mn bymechanical alloying[J]. Mater Trans JIM,1995,36(02):373
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