CN108624958A - 一种掺杂大块单晶SnS的制备方法 - Google Patents

一种掺杂大块单晶SnS的制备方法 Download PDF

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CN108624958A
CN108624958A CN201810486631.7A CN201810486631A CN108624958A CN 108624958 A CN108624958 A CN 108624958A CN 201810486631 A CN201810486631 A CN 201810486631A CN 108624958 A CN108624958 A CN 108624958A
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single crystal
sns
doping
preparation
degree
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吴宏
彭坤林
周小元
王国玉
卢旭
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Chongqing University
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Chongqing University
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/46Sulfur-, selenium- or tellurium-containing compounds
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

本发明属于半导体材料掺杂技术领域,公开了一种掺杂大块单晶SnS的制备方法,将原料按化学计量比在具有氩气保护环境的手套箱中配好并真空封与石英管中,置于自制的单晶炉中,用2400分钟升温到1000度,在1000度保温800分钟来保证原料充分扩散;将炉温将至900度,利用自制单晶炉中的温度梯度,采用布里奇曼法,通过1mm/h的速率移动;共计六天时间。大块掺杂单晶SnS的生长,使用改进的布里奇曼方法;解决了生长过程中硫元素产生过大蒸汽压,这蒸汽压会导致石英管爆炸。

Description

一种掺杂大块单晶SnS的制备方法
技术领域
本发明属于半导体材料掺杂技术领域,尤其涉及一种掺杂大块单晶SnS的制备方法。
背景技术
人类社会的发展伴随着能源消耗的增加,化石燃料作为不可再生能源正日益减少,开发新的可再生能源己成为21世纪的热门问题。热电材料(温差电材料)是一种利用固体中载流子和声子的输运及其相互作用,回收废弃热能,缓解能源危机;可以将热能直接转化为电能,可以制冷,并且无噪音,无振动,无污染;是新能源技术的一种。
综上所述,现有技术存在的问题是:
(1)解决硫元素导致的过大的蒸气压引起爆炸。
(2)生长出大尺寸的SnS单晶和掺杂的SnS单晶
(3)生长质量高和效率高。
解决上述技术问题的难度和意义:对于大尺寸的单晶SnS生长,解决蒸气压过大容易引起爆炸问题。同时掺杂的SnS单晶的热电性能有了很大的提高,对于热电材料的转化效率有了很大提高。
发明内容
针对现有技术存在的问题,本发明提供了一种掺杂大块单晶SnS的制备方法。
本发明是这样实现的,一种掺杂大块单晶SnS的制备方法,所述掺杂大块单晶SnS的制备方法包括以下步骤:
步骤一,将原料按化学计量比在具有氩气保护环境的手套箱中配好并真空封与石英管中,置于自制的单晶炉中,用2400分钟升温到1000度,在1000度保温800分钟来保证原料充分扩散;
步骤二,将炉温将至900度,利用自制单晶炉中的温度梯度,采用布里奇曼法,通过1mm/h的速率移动;共计六天时间。
进一步,所述步骤一中将原料按化学计量比Sn:Na:S=98:2:100共计25g。
本发明的另一目的在于提供一种由所述掺杂大块单晶SnS的制备方法制备的掺杂大块单晶和解决蒸汽压过大的问题。
综上所述,本发明的优点及积极效果为:掺杂单晶SnS具有十分优越的热电性能,掺杂大约2%的Na可以将整体性能提高3-4倍,并且材料生长所需时间与其他传统的多晶热电材料相当(大约一周)。与很多金属硫化物热电材料相比,最高的zT(决定热电性能)或者平均zT(决定转化效率)都有很大的提高。大块掺杂单晶SnS的生长,使用改进的布里奇曼方法;解决了生长过程中硫元素产生过大蒸汽压,这蒸汽压会导致石英管爆炸。
附图说明
图1是本发明实施例提供的掺杂大块单晶SnS的制备方法流程图。
图2是本发明实施例提供的掺杂大块单晶SnS效果示意图;
图中:(a)单晶照片;(b)和(c)热电性能与其他材料对比结果。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
如图1所示,本发明实施例提供的掺杂大块单晶SnS的制备方法包括以下步骤:
S101:将原料按化学计量比(Sn:Na:S=98:2:100共计25g)在具有氩气保护环境的手套箱中配好并真空封与石英管中,置于自制的单晶炉中,用2400分钟缓慢升温到1000度,并且在1000度保温800分钟来保证原料充分扩散;
S102:将炉温将至900度,利用自制单晶炉中的温度梯度,采用布里奇曼法(Bridgeman method),通过1mm/h的速率移动;共计六天时间。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。

Claims (3)

1.一种掺杂大块单晶SnS的制备方法,其特征在于,所述掺杂大块单晶SnS的制备方法包括以下步骤:
步骤一,将原料按化学计量比在具有氩气保护环境的手套箱中配好并真空封与石英管中,置于自制的单晶炉中,用2400分钟升温到1000度,在1000度保温800分钟来保证原料充分扩散;
步骤二,将炉温将至900度,利用自制单晶炉中的温度梯度,采用布里奇曼法,通过1mm/h的速率移动;共计六天时间。
2.如权利要求1所述的掺杂大块单晶SnS的制备方法,其特征在于,所述步骤一中将原料按化学计量比Sn:Na:S=98:2:100共计25g。
3.一种由权利要求1~2任意一项所述掺杂大块单晶SnS的制备方法制备的掺杂大块单晶。
CN201810486631.7A 2018-05-21 2018-05-21 一种掺杂大块单晶SnS的制备方法 Pending CN108624958A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111416032A (zh) * 2019-01-08 2020-07-14 北京航空航天大学 一种N型SnS单晶热电材料及其制备方法
CN114908412A (zh) * 2022-05-09 2022-08-16 福州大学 一种高效生长三硫化二锡单晶热电材料的方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105908258A (zh) * 2016-06-23 2016-08-31 重庆大学 一种掺杂单晶SnSe的制备方法
CN107522489A (zh) * 2017-08-23 2017-12-29 重庆大学 一种多晶SnSe热电材料的制备方法

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN105908258A (zh) * 2016-06-23 2016-08-31 重庆大学 一种掺杂单晶SnSe的制备方法
CN107522489A (zh) * 2017-08-23 2017-12-29 重庆大学 一种多晶SnSe热电材料的制备方法

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111416032A (zh) * 2019-01-08 2020-07-14 北京航空航天大学 一种N型SnS单晶热电材料及其制备方法
CN111416032B (zh) * 2019-01-08 2022-02-18 北京航空航天大学 一种N型SnS单晶热电材料及其制备方法
CN114908412A (zh) * 2022-05-09 2022-08-16 福州大学 一种高效生长三硫化二锡单晶热电材料的方法

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Application publication date: 20181009