JP6127330B2 - SnS2 - Google Patents
SnS2 Download PDFInfo
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- JP6127330B2 JP6127330B2 JP2013263742A JP2013263742A JP6127330B2 JP 6127330 B2 JP6127330 B2 JP 6127330B2 JP 2013263742 A JP2013263742 A JP 2013263742A JP 2013263742 A JP2013263742 A JP 2013263742A JP 6127330 B2 JP6127330 B2 JP 6127330B2
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- tin
- sulfur
- disulfide
- sns
- diffraction
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- 238000002441 X-ray diffraction Methods 0.000 claims description 13
- 239000011135 tin Substances 0.000 description 44
- 229910052717 sulfur Inorganic materials 0.000 description 43
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 42
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 41
- 239000011593 sulfur Substances 0.000 description 41
- ALRFTTOJSPMYSY-UHFFFAOYSA-N tin disulfide Chemical class S=[Sn]=S ALRFTTOJSPMYSY-UHFFFAOYSA-N 0.000 description 41
- 229910052718 tin Inorganic materials 0.000 description 34
- 239000002184 metal Substances 0.000 description 32
- 229910052751 metal Inorganic materials 0.000 description 32
- 238000004519 manufacturing process Methods 0.000 description 26
- 238000000034 method Methods 0.000 description 15
- TUTLDIXHQPSHHQ-UHFFFAOYSA-N tin(iv) sulfide Chemical compound [S-2].[S-2].[Sn+4] TUTLDIXHQPSHHQ-UHFFFAOYSA-N 0.000 description 15
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical class [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 14
- 239000002245 particle Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000011324 bead Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000007561 laser diffraction method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
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Description
(1)金属スズと硫黄を、高圧下で加熱して反応させる方法(非特許文献1)
(2)硫黄、スズアマルガム及び塩化アンモニウムを、混合加熱する方法(非特許文献2)
(3)金属スズ1モルに対して5.5モル以上である金属スズ及び硫黄の混合物を、硫黄の沸点以上700℃以下の温度で開放系で焼成する方法(特許文献1)
(4)金属スズ塊及び硫黄塊の混合物を粉砕混合しながら加熱する方法(特許文献2)
すなわち、本発明は、CuKα線を用いたX線回折パターンにおいて、少なくとも回折角2θ=14.8〜15.0°、28.7〜28.9°、34.8〜35.0°及び50.1〜50.3°に回折ピークを有する単相のSnS2を提供するものである。
被処理物として、金属スズ(福田金属箔粉工業社製、アトマイズ品)3.25gと硫黄(細井化学社製、200メッシュ品)1.75gと秤量し、それらの被処理物を遊星ボールミル(フリッチェ社製、P7)にて、Zr製ボール(直径10mm)10個を用い、400回転で40時間、大気雰囲気で処理して、スズ硫化物を得た。このとき、遊星ボールミルにて処理した被処理物中の金属スズに対する硫黄の原子換算のモル比(S/Sn)は2であった。また、処理直後の被処理物の温度は21℃であり、装置内の圧力は0.1MPa(常圧)であった。
次いで、得られたスズ硫化物のX線回折分析を行った。その結果を表1及び図1に示す。
被処理物として、金属スズ(福田金属箔粉工業社製、アトマイズ品)5018.04gと硫黄(細井化学社製、200メッシュ品)2981.96gと秤量し、それらの被処理物をミル(ワンダーブレンダー、大阪ケミカル社製)で10秒間混合した。このとき、被処理物中の金属スズに対する硫黄の原子換算のモル比(S/Sn)は2.2であった。
次いで、ビーズミル(アシザワ・ファインテック社製、ドライスターSDA−5)に、上記混合後の被処理物を、定量フィーダ(アイシンナノテクノロジーズ社製、マイクロフィーダ)を介して、5g/分の供給速度で連続的に供給しつつ、被処理物を、ビーズミルにて950rpmで大気雰囲気で処理し、装置内での処理時間(滞留時間)が120分間となるように、装置出口から反応生成物を排出して、スズ硫化物を得た。また、処理直後の被処理物の温度は36℃であり、装置内の圧力は0.1MPa(常圧)であった。
次いで、得られたスズ硫化物のX線回折分析を行った。その結果を表1及び図1に示す。
金属スズ(福田金属箔粉工業社製、アトマイズ品)3.14gと硫黄(細井化学社製、200メッシュ品)1.86gと秤量し、それらを実施例1同様にして、遊星ボールミルにて処理して、スズ硫化物を得た。このとき、遊星ボールミルにて処理した被処理物中の金属スズに対する硫黄の原子換算のモル比(S/Sn)は2.2であった。また、処理直後の被処理物の温度は22℃であり、装置内の圧力は0.1MPa(常圧)であった。
次いで、得られたスズ硫化物のX線回折分析を行った。その結果を表1及び図1に示す。
よって、実施例1〜3の二硫化スズは、新規な結晶構造を有する単相の二硫化スズ(SnS2)である。
Claims (1)
- CuKα線を用いたX線回折パターンにおいて、少なくとも回折角2θ=14.8〜15.0°、28.7〜28.9°、34.8〜35.0°及び50.1〜50.3°に回折ピークを有する単相のSnS2。
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JP2013263742A JP6127330B2 (ja) | 2013-12-20 | 2013-12-20 | SnS2 |
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JP2013263742A JP6127330B2 (ja) | 2013-12-20 | 2013-12-20 | SnS2 |
Publications (2)
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JP2015120608A JP2015120608A (ja) | 2015-07-02 |
JP6127330B2 true JP6127330B2 (ja) | 2017-05-17 |
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JP2013263742A Active JP6127330B2 (ja) | 2013-12-20 | 2013-12-20 | SnS2 |
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JP (1) | JP6127330B2 (ja) |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AT501253B1 (de) * | 2005-01-13 | 2006-11-15 | Karl Dipl Ing Dr Rimmer | Verfahren zur herstellung von weitgehend eisenfreien metallchalkogeniden mit einer korngrössenverteilung im nanobereich |
JP4925404B2 (ja) * | 2005-09-26 | 2012-04-25 | 日本化学工業株式会社 | 二硫化スズの製造方法 |
JP4255955B2 (ja) * | 2006-04-19 | 2009-04-22 | 日本精鉱株式会社 | 金属硫化物粉末の製造方法および装置 |
KR100896656B1 (ko) * | 2007-07-25 | 2009-05-11 | 삼성전기주식회사 | 황화주석 나노입자 제조방법 및 이를 이용한 리튬이온전지제조방법 |
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