CN102557117A - Method of Microwave Solvothermal Synthesis of Cu2ZnSnS4 Semiconductor Material - Google Patents
Method of Microwave Solvothermal Synthesis of Cu2ZnSnS4 Semiconductor Material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 14
- 239000004065 semiconductor Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000004729 solvothermal method Methods 0.000 title abstract description 7
- 229910002475 Cu2ZnSnS4 Inorganic materials 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea group Chemical group NC(=S)N UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 6
- 150000003751 zinc Chemical class 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical group Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 235000011150 stannous chloride Nutrition 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims 3
- 150000003839 salts Chemical class 0.000 claims 2
- YMHOBZXQZVXHBM-UHFFFAOYSA-N 2,5-dimethoxy-4-bromophenethylamine Chemical compound COC1=CC(CCN)=C(OC)C=C1Br YMHOBZXQZVXHBM-UHFFFAOYSA-N 0.000 claims 1
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims 1
- 241000545067 Venus Species 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- 229960003280 cupric chloride Drugs 0.000 claims 1
- 150000004985 diamines Chemical class 0.000 claims 1
- 239000010949 copper Substances 0.000 abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 4
- 150000001879 copper Chemical class 0.000 abstract description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
本发明公开了一种微波溶剂热合成Cu2ZnSnS4(CZTS)半导体材料的方法。将铜盐、锌盐、锡盐和硫源等按预定摩尔比加入烧杯内，加入溶剂，混合均匀后倒入反应釜，密闭后放入微波场中加热，待温度上升至额定温度后保温额定时间，所得产物经过离心、洗涤、真空干燥后得Cu2ZnSnS4半导体材料。所述溶剂为水、乙二醇、乙二胺和联胺中的一种或多种；所述硫源为硫脲或硫粉。本发明利用微波辅助溶剂热合成工艺制备的Cu2ZnSnS4半导体材料纯度高，同时具有合成速度快、反应装置更简单、成本低、工艺控制容易等优点。
The invention discloses a microwave solvothermal synthesis method of Cu 2 ZnSnS 4 (CZTS) semiconductor material. Put the copper salt, zinc salt, tin salt and sulfur source into the beaker according to the predetermined molar ratio, add the solvent, mix well, pour into the reaction kettle, seal it and put it in the microwave field to heat, and keep the temperature after the temperature rises to the rated temperature. time, the obtained product is centrifuged, washed, and vacuum-dried to obtain Cu 2 ZnSnS 4 semiconductor material. The solvent is one or more of water, ethylene glycol, ethylenediamine and hydrazine; the sulfur source is thiourea or sulfur powder. The Cu 2 ZnSnS 4 semiconductor material prepared by the microwave-assisted solvothermal synthesis process has the advantages of high purity, fast synthesis speed, simpler reaction device, low cost, easy process control and the like.
Description
技术领域： Technical field:
本发明涉及一种Cu2ZnSnS4(CZTS)半导体材料的微波溶剂热合成工艺，所合成的半导体材料可被用于太阳能电池、光电传感器领域。The invention relates to a microwave solvothermal synthesis process of a Cu 2 ZnSnS 4 (CZTS) semiconductor material, and the synthesized semiconductor material can be used in the fields of solar cells and photoelectric sensors.
背景技术： Background technique:
Cu2ZnSnS4半导体材料可用于CZTS系列薄膜太阳能电池和相关光电转换器件开发生产。目前常用的Cu2ZnSnS4半导体材料的合成方法有真空热蒸发法、电子束蒸发法、溅射法、喷雾热解法、电沉积法、溶胶凝胶法及分子束外延法等，它们中的一些所需的反应条件较为苛刻，对设备的要求较高，反应成本高，工艺冗繁难控，另一些反应速度慢，需要在高温高压下进行较长时间的反应才能获得。Cu 2 ZnSnS 4 semiconductor materials can be used in the development and production of CZTS series thin film solar cells and related photoelectric conversion devices. At present, the commonly used synthesis methods of Cu 2 ZnSnS 4 semiconductor materials include vacuum thermal evaporation, electron beam evaporation, sputtering, spray pyrolysis, electrodeposition, sol-gel method and molecular beam epitaxy. Some require relatively harsh reaction conditions, high requirements for equipment, high reaction costs, cumbersome and difficult-to-control processes, and others have slow reaction speeds and require a long period of reaction at high temperature and high pressure to obtain.
发明内容 Contents of the invention
本发明的目的是以铜盐、锌盐、锡盐和硫源为原料，在微波辅助下利用溶剂热法快速合成Cu2ZnSnS4半导体材料。The object of the present invention is to use copper salt, zinc salt, tin salt and sulfur source as raw materials to rapidly synthesize Cu 2 ZnSnS 4 semiconductor material by solvothermal method under the assistance of microwave.
具体步骤为：The specific steps are:
将铜盐、锌盐、锡盐和硫源按摩尔配比(1～3)∶(0.5～1.5)∶(0.5～1.5)∶(4～6)混合，加入溶剂，溶剂用量为使上述原料完全溶解且溶剂体积不超过反应釜容积的2/3，混合均匀后倒入反应釜，密闭后放入微波场中加热，待温度上升至100～250℃后保温0.5～12小时，所得产物经过蒸馏水和无水乙醇离心洗涤2～3次，然后在70～90℃下的真空干燥箱内干燥7～9小时得Cu2ZnSnS4半导体材料；Copper salt, zinc salt, tin salt and sulfur source are mixed in molar ratio (1～3): (0.5～1.5): (0.5～1.5): (4～6), add solvent, solvent consumption is to make above-mentioned raw material Completely dissolve and the volume of the solvent does not exceed 2/3 of the volume of the reaction kettle. After mixing evenly, pour into the reaction kettle, seal it and put it in a microwave field to heat. After the temperature rises to 100-250°C, keep it warm for 0.5-12 hours. Centrifugal washing with distilled water and absolute ethanol for 2 to 3 times, and then drying in a vacuum oven at 70 to 90°C for 7 to 9 hours to obtain Cu 2 ZnSnS 4 semiconductor material;
所述溶剂为水、乙二醇、乙二胺和联胺中的一种或多种；The solvent is one or more of water, ethylene glycol, ethylenediamine and hydrazine;
所述铜盐为乙酸铜、氯化铜和硝酸铜中的一种或多种；The copper salt is one or more of copper acetate, copper chloride and copper nitrate;
所述锌盐为乙酸锌、氯化锌和硝酸锌中的一种或多种；The zinc salt is one or more of zinc acetate, zinc chloride and zinc nitrate;
所述锡盐为四氯化锡或二氯化锡；Described tin salt is tin tetrachloride or tin dichloride;
所述硫源为硫脲或硫粉。The sulfur source is thiourea or sulfur powder.
本发明具有合成速度快、产物纯净、成本低、工艺控制容易等优点。此外，微波辅助溶剂热合成工艺与常见的高压溶剂热合成工艺相比，反应装置更简单、反应速度更快、反应过程可控性更佳、目标产物纯度更高。The invention has the advantages of fast synthesis speed, pure product, low cost, easy process control and the like. In addition, compared with the common high-pressure solvothermal synthesis process, the microwave-assisted solvothermal synthesis process has simpler reaction devices, faster reaction speed, better controllability of the reaction process, and higher purity of the target product.
附图说明 Description of drawings
图1为本发明合成工艺流程图。Figure 1 is a flow chart of the synthesis process of the present invention.
图2为本发明实施例微波溶剂热合成Cu2ZnSnS4半导体材料的SEM形貌图。Fig. 2 is a SEM image of Cu 2 ZnSnS 4 semiconductor material synthesized by microwave solvothermal in the embodiment of the present invention.
图3为本发明实施例微波溶剂热合成Cu2ZnSnS4半导体材料的XRD衍射图谱。Fig. 3 is an XRD diffraction pattern of Cu 2 ZnSnS 4 semiconductor material synthesized by microwave solvothermal in the embodiment of the present invention.
具体实施方式 Detailed ways
实施例：Example:
将2.995克乙酸铜、1.642克乙酸锌、2.628克四氯化锡和硫脲2.283克倒入烧杯中，放入一个搅拌磁子，再加入30ml乙二醇溶解，转移至磁力搅拌器，待原料搅拌均匀后倒入容积为50ml的微波反应釜，安装好反应装置，设定温度为250℃，保温3小时，保温结束后自然冷却到室温，将反应液转移到烧杯中，然后分别经蒸馏水和无水乙醇离心洗涤3次，将离心洗涤后的产物在真空干燥箱内80℃下真空干燥8小时。产物经XRD分析为Cu2ZnSnS4，经电子扫描电镜分析，产物主要由不规则的颗粒状粉体组成，颗粒状粉体的粒径大小约1-2μm，通过放大的图片可以看出，颗粒状粉体由许多小的不规则片状物团聚而成。Pour 2.995 grams of copper acetate, 1.642 grams of zinc acetate, 2.628 grams of tin tetrachloride and 2.283 grams of thiourea into a beaker, put in a stirring magnet, add 30ml of ethylene glycol to dissolve, transfer to a magnetic stirrer, and wait for the raw materials to After stirring evenly, pour it into a microwave reactor with a volume of 50ml, install the reaction device, set the temperature at 250°C, and keep it warm for 3 hours. The anhydrous ethanol was centrifuged and washed 3 times, and the product after centrifuged washing was vacuum-dried in a vacuum drying oven at 80° C. for 8 hours. The product was analyzed as Cu 2 ZnSnS 4 by XRD. According to the analysis by scanning electron microscope, the product was mainly composed of irregular granular powder, and the particle size of the granular powder was about 1-2 μm. It can be seen from the enlarged picture that the particles The powder is agglomerated by many small irregular flakes.
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Cited By (9)
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|---|---|---|---|---|
| CN103011261A (en) * | 2012-12-02 | 2013-04-03 | 桂林理工大学 | Solvothermal synthesis method of wurtzite structure CZTS(Se) (Copper Zinc Tin Sulfide) semiconductor material under synergistic effect of ultrasonic waves and microwaves |
| CN103043628A (en) * | 2012-12-02 | 2013-04-17 | 桂林理工大学 | Method for thermally synthesizing sphalerite structure CZTSSe semiconductor material through solvent under synergistic action of ultrasonic microwave |
| CN103420411A (en) * | 2013-07-11 | 2013-12-04 | 南京航空航天大学 | A method of ultrasonic-assisted microwave controllable preparation of Cu2ZnSnS4 nanoparticles |
| CN103474512A (en) * | 2013-09-26 | 2013-12-25 | 南京师范大学 | Method for compounding sulfide copper zinc tin quantum dots in one-step mode through microwave method |
| CN103794373A (en) * | 2013-12-26 | 2014-05-14 | 中国矿业大学 | Cu2ZnSnS4/MWCNT nanocomposite counter electrode for dye-sensitized solar cell and preparation method thereof |
| CN104370302A (en) * | 2014-10-23 | 2015-02-25 | 上海交通大学 | Nano-pouring synthetic method of copper-zinc-tin-sulfur nano-crystal |
| US20150135994A1 (en) * | 2012-10-04 | 2015-05-21 | International Business Machines Corporation | Solution processing of kesterite semiconductors |
| CN105197985A (en) * | 2015-09-17 | 2015-12-30 | 上海大学 | One-step synthesis of superlong wurtzite structure Cu2ZnSnS4 nanorods by solvothermal method |
| CN108558202A (en) * | 2018-07-27 | 2018-09-21 | 望江县天长光学科技有限公司 | A kind of optical glass of high refractive index |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150135994A1 (en) * | 2012-10-04 | 2015-05-21 | International Business Machines Corporation | Solution processing of kesterite semiconductors |
| CN103011261A (en) * | 2012-12-02 | 2013-04-03 | 桂林理工大学 | Solvothermal synthesis method of wurtzite structure CZTS(Se) (Copper Zinc Tin Sulfide) semiconductor material under synergistic effect of ultrasonic waves and microwaves |
| CN103043628A (en) * | 2012-12-02 | 2013-04-17 | 桂林理工大学 | Method for thermally synthesizing sphalerite structure CZTSSe semiconductor material through solvent under synergistic action of ultrasonic microwave |
| CN103011261B (en) * | 2012-12-02 | 2014-08-20 | 桂林理工大学 | Solvothermal synthesis method of wurtzite structure CZTS(Se) (Copper Zinc Tin Sulfide) semiconductor material under synergistic effect of ultrasonic waves and microwaves |
| CN103043628B (en) * | 2012-12-02 | 2014-10-29 | 桂林理工大学 | Method for thermally synthesizing sphalerite structure CZTSSe semiconductor material through solvent under synergistic action of ultrasonic microwave |
| CN103420411A (en) * | 2013-07-11 | 2013-12-04 | 南京航空航天大学 | A method of ultrasonic-assisted microwave controllable preparation of Cu2ZnSnS4 nanoparticles |
| CN103474512A (en) * | 2013-09-26 | 2013-12-25 | 南京师范大学 | Method for compounding sulfide copper zinc tin quantum dots in one-step mode through microwave method |
| CN103474512B (en) * | 2013-09-26 | 2016-01-27 | 南京师范大学 | The method of microwave method one-step synthesis sulfide copper zinc tin quantum dot |
| CN103794373A (en) * | 2013-12-26 | 2014-05-14 | 中国矿业大学 | Cu2ZnSnS4/MWCNT nanocomposite counter electrode for dye-sensitized solar cell and preparation method thereof |
| CN104370302A (en) * | 2014-10-23 | 2015-02-25 | 上海交通大学 | Nano-pouring synthetic method of copper-zinc-tin-sulfur nano-crystal |
| CN105197985A (en) * | 2015-09-17 | 2015-12-30 | 上海大学 | One-step synthesis of superlong wurtzite structure Cu2ZnSnS4 nanorods by solvothermal method |
| CN108558202A (en) * | 2018-07-27 | 2018-09-21 | 望江县天长光学科技有限公司 | A kind of optical glass of high refractive index |
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Application publication date: 20120711 |