JPH0624983B2 - Method for producing chevrel compound - Google Patents
Method for producing chevrel compoundInfo
- Publication number
- JPH0624983B2 JPH0624983B2 JP63233021A JP23302188A JPH0624983B2 JP H0624983 B2 JPH0624983 B2 JP H0624983B2 JP 63233021 A JP63233021 A JP 63233021A JP 23302188 A JP23302188 A JP 23302188A JP H0624983 B2 JPH0624983 B2 JP H0624983B2
- Authority
- JP
- Japan
- Prior art keywords
- sulfide
- molybdenum
- chevrel compound
- metal
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 本発明は、ヘリウム温度域で電気抵抗がほとんどゼロに
なり高効率電力貯蔵、強磁場発生、高効率送電等に利用
できる超伝導体の材料、または、電気化学素子と電極材
料等に用いることのできるシェブレル化合物の製造法に
関する。DETAILED DESCRIPTION OF THE INVENTION Industrial Field of the Invention The present invention relates to a superconductor material which has almost zero electric resistance in the helium temperature range and can be used for high-efficiency power storage, strong magnetic field generation, high-efficiency power transmission, or the like, or The present invention relates to a method for producing a chevrel compound that can be used for electrochemical devices and electrode materials.
従来の技術 シェブレル化合物は、液体ヘリウム温度以上の臨界温度
を有し、また、極めて高い臨界磁場を有することから多
くの研究がなされている。さらに、銅シェブレル化合物
のようにシェブレル化合物のＭｏ6Ｓ8の骨格構造を壊す
ことなくシェブレル化合物中の金属元素を化学的、ある
いは、電気化学的に出し入れできるものについては電気
化学素子の電極材料への応用が期待される。しかしなが
ら、従来、シェブレル化合物の製造法としては、各種金
属元素の粉末、金属モリブデン粉末、硫黄粉末を粉砕混
合し、この混合粉末を石英ガラス管内に減圧封入し、４
００℃で１２時間焼成後、６００℃で１２時間焼成し、
さらに、１００℃で２４時間焼成して製造していた。2. Description of the Related Art Chevrel compounds have many studies because they have a critical temperature above liquid helium temperature and an extremely high critical magnetic field. Furthermore, for copper chevrel compounds that can be taken in and out chemically or electrochemically in the chevrel compound without destroying the Mo 6 S 8 skeletal structure of the chevrel compound, use the electrode material of the electrochemical device. Is expected to be applied. However, conventionally, as a method for producing a chevrel compound, powders of various metal elements, metal molybdenum powders, and sulfur powders are pulverized and mixed, and the mixed powders are sealed under reduced pressure in a quartz glass tube.
Bake at 00 ° C for 12 hours, then at 600 ° C for 12 hours,
Further, it was manufactured by firing at 100 ° C. for 24 hours.
発明が解決しようとする課題 シェブレル化合物を製造する場合、原料中に多くの金属
と反応し易い硫黄があり、また、原料を反応管に入れ減
圧封入して焼成するため、反応管は、硫黄に対して安定
で、加工が可能な石英ガラス管を用いる必要がある。ま
た、焼成後、石英ガラス反応管を開管して合成物を取り
出さなければならず石英ガラス反応管を何回も使用する
ことができない。さらに、１回の合成量を多くすると昇
温時に硫黄がガス化し、そのガス圧が高くなり過ぎると
石英ガラス反応管を破裂させるなど製造工程が煩雑であ
り工業的な生産に問題を有していた。Problems to be Solved by the Invention When a chevrel compound is produced, there is sulfur that easily reacts with many metals in the raw material, and since the raw material is put in a reaction tube and sealed under reduced pressure and fired, the reaction tube is converted to sulfur. In contrast, it is necessary to use a quartz glass tube that is stable and can be processed. Further, after firing, the quartz glass reaction tube must be opened to take out the synthetic product, and the quartz glass reaction tube cannot be used many times. Further, if the synthesis amount per one time is increased, sulfur is gasified at the time of temperature rise, and if the gas pressure becomes too high, the quartz glass reaction tube is ruptured, which complicates the manufacturing process and has a problem in industrial production. It was
課題を解決するための手段 本発明は、上記問題点を解決するため金属硫化物（金属
は、Ｌｉ，Ｎａ，Ｍｇ，Ｃａ，Ｓｃ，Ｃｒ，Ｍｎ，Ｆ
ｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚｎ，Ｓｒ，Ｙ，Ｐｄ，Ａｇ，
Ｃｄ，Ｉｎ，Ｓｎ，Ｂａ，Ｌａ，Ｐｂ，Ｃｅ，Ｐｒ，Ｎ
ｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔ
ｍ，Ｙｂ，Ｌｕのうち少なくとも一種の元素）、金属モ
リブデン、硫化モリブデンを混合し、この混合体を減圧
下または還元性ガスを含む不活性ガス（アルゴン、ヘリ
ウムまたは、窒素ガス）気流中で焼成してシェブレル化
合物を製造するものである。Means for Solving the Problems In order to solve the above problems, the present invention provides a metal sulfide (metals are Li, Na, Mg, Ca, Sc, Cr, Mn, F).
e, Co, Ni, Cu, Zn, Sr, Y, Pd, Ag,
Cd, In, Sn, Ba, La, Pb, Ce, Pr, N
d, Sm, Eu, Gd, Tb, Dy, Ho, Er, T
At least one element of m, Yb, and Lu), metallic molybdenum, and molybdenum sulfide are mixed, and this mixture is fired under reduced pressure or in an inert gas (argon, helium, or nitrogen gas) flow containing a reducing gas. To produce a chevrel compound.
作用 本発明によるシェブレル化合物の製造法において、シェ
ブレル化合物は、減圧下または還元性ガスを含む不活性
ガス（アルゴン、ヘリウム、窒素ガス）気流中で合成さ
れるため反応管を封止する必要がなく反応管を何回でも
使用することができる。また、原料中の硫黄成分は、化
合物として存在しているため昇温時にガス化せず、した
がって組成比が変化することがほとんどない。さらに、
石英ガラス反応管が開管であるため、１回の合成量を多
くしても石英ガラス反応管を破裂させることがない。Action In the method for producing a chevrel compound according to the present invention, since the chevrel compound is synthesized under reduced pressure or in an inert gas (argon, helium, nitrogen gas) flow containing a reducing gas, it is not necessary to seal the reaction tube. The reaction tube can be used any number of times. Further, since the sulfur component in the raw material exists as a compound, it is not gasified at the time of temperature rise, and therefore the composition ratio hardly changes. further,
Since the quartz glass reaction tube is an open tube, the quartz glass reaction tube does not burst even if the synthesis amount for one time is increased.
実施例 以下、本実施例について説明する。Example This example will be described below.
（実施例１） 銅シェブレル化合物Ｃｕ２Ｍｏ６Ｓ８（１００ｇ）を製
造した。以下、その製造法を述べる。Was prepared (Example 1) Copper Chevrel compound Cu 2 Mo 6 S 8 (100g ). The manufacturing method will be described below.
硫化第一銅粉末（１６．５９ｇ）、金属モリブデン粉末
（２５．００ｇ）、二硫化モリブデン粉末（５９．３５
ｇ）を秤量し、ガラス製ボールミルを用いて３時間混合
した後、この混合粉末を石英ガラス反応管に充填し、下
記の製造装置を用いて減圧下、７００℃で３０時間、さ
らに、１０００℃で４０時間焼成して銅シェブレル化合
物Ｃｕ２Ｍｏ６Ｓ８を製造した。Cuprous sulfide powder (16.59 g), metallic molybdenum powder (25.00 g), molybdenum disulfide powder (59.35)
g) was weighed and mixed using a glass ball mill for 3 hours, then the mixed powder was filled in a quartz glass reaction tube, and the temperature was reduced to 700 ° C. for 30 hours and further to 1000 ° C. using a manufacturing apparatus described below. At 40 ° C. for 40 hours to produce a copper chevrel compound Cu 2 Mo 6 S 8 .
第１図に減圧下でシェブレル化合物を製造するための製
造装置の概略図を示した。第１図において、１は原料、
２は原料を充填した石英ガラス反応管、３は電気炉、４
は熱電対、５はトラップ、６は油回転式真空ポンプであ
る。FIG. 1 shows a schematic diagram of a production apparatus for producing a chevrel compound under reduced pressure. In FIG. 1, 1 is a raw material,
2 is a quartz glass reaction tube filled with raw materials, 3 is an electric furnace, 4
Is a thermocouple, 5 is a trap, and 6 is an oil rotary vacuum pump.
得られた銅シェブレル化合物Ｃｕ2Ｍｏ6Ｓ8を粉末Ｘ線
回折で分析した結果、ほぼ単一相のものであることがわ
かった。第２図に粉末Ｘ線回折図を示した。The obtained copper chevrel compound Cu 2 Mo 6 S 8 was analyzed by powder X-ray diffraction, and as a result, it was found that it had a substantially single phase. The powder X-ray diffraction pattern is shown in FIG.
また、得られた銅シェブレル化合物Ｃｕ2Ｍｏ6Ｓ８の超
伝導特性では、約１０Ｋの臨界温度を示した。The superconducting properties of the obtained copper chevrel compound Cu 2 Mo 6 S 8 showed a critical temperature of about 10K.
（実施例２） ニッケルシェブレル化合物Ｎｉ2Ｍｏ6Ｓ８（１００ｇ）
を製造した。以下、その製造法について述べる。(Example 2) Nickel chevrel compound Ni 2 Mo 6 S 8 (100 g)
Was manufactured. The manufacturing method will be described below.
実施例１と同様に硫化ニッケル粉末（１９．１２ｇ）、
金属モリブデン（３０．３１ｇ）、二硫化モリブデン
（５０．５７ｇ）を秤量し、ガラス製ボールミルを用い
て３時間混合した後、この混合粉末を石英ガラス反応管
内に充填し、実施例１と同様の製造装置を用いて減圧
下、７００℃で３０時間、さらに、１０００℃で４０時
間焼成してニッケルシェブレル化合物Ｎｉ2Ｍｏ6Ｓ8を
製造した。Nickel sulfide powder (19.12 g) as in Example 1,
Metal molybdenum (30.31 g) and molybdenum disulfide (50.57 g) were weighed and mixed for 3 hours using a glass ball mill, and then the mixed powder was filled in a quartz glass reaction tube, and the same procedure as in Example 1 was performed. The nickel chevrel compound Ni 2 Mo 6 S 8 was manufactured by firing at 700 ° C. for 30 hours under reduced pressure and further at 1000 ° C. for 40 hours using a manufacturing apparatus.
得られたニッケルシェブレル化合物Ｎｉ2Ｍｏ6Ｓ8を粉
末Ｘ線回折で分析した結果、従来の石英ガラス管を封管
して製造したものとほぼ同様の回折パターンを示した。The obtained nickel chevrel compound Ni 2 Mo 6 S 8 was analyzed by powder X-ray diffraction, and as a result, it showed a diffraction pattern almost similar to that produced by sealing a conventional quartz glass tube.
（実施例３） 鉛シェブレル化合物ＰｂＭｏ6.2Ｓ8（１００ｇ）を製造
した。以下、その製造法について述べる。Example 3 A lead chevrel compound PbMo 6.2 S 8 (100 g) was produced. The manufacturing method will be described below.
実施例１と同様に硫化鉛粉末（２２．６０ｇ）、金属モ
リブデン粉末（２４．４７ｇ）、二硫化モリブデン粉末
（５２．９３ｇ）を秤量し、ガラス製ボールミルを用い
て３時間混合した後、この混合粉末を石英ガラス反応管
内に充填し、実施例１と同様の製造装置を用いて減圧
下、７００℃で３０時間、１０００℃で４０時間焼成し
て鉛シェブレル化合物ＰｂＭｏ6.2Ｓ8を製造した。Lead sulfide powder (22.60 g), metal molybdenum powder (24.47 g), and molybdenum disulfide powder (52.93 g) were weighed in the same manner as in Example 1, and mixed for 3 hours using a glass ball mill. The mixed powder was filled in a quartz glass reaction tube, and calcined under reduced pressure at 700 ° C. for 30 hours and at 1000 ° C. for 40 hours using the same production apparatus as in Example 1 to produce a lead chevrel compound PbMo 6.2 S 8 .
得られた鉛シェブレル化合物ＰｂＭｏ6.2Ｓ8を粉末Ｘ線
回折で分析した結果、従来の石英ガラス管を封管して製
造したものとほぼ同じＸ線回折パターンを示した。ま
た、得られた鉛シェブレル化合物ＰｂＭｏ6.2Ｓ8の超伝
導特性では、約１２Ｋの臨界温度を示した。As a result of powder X-ray diffraction analysis of the obtained lead chevrel compound PbMo 6.2 S 8 , an X-ray diffraction pattern almost the same as that produced by sealing a conventional quartz glass tube was shown. The superconducting property of the obtained lead chevrel compound PbMo 6.2 S 8 showed a critical temperature of about 12K.
（実施例４） リチウムシェブレル化合物Ｌｉ2Ｍｏ6Ｓ8（１００ｇ）
を製造した。以下、その製造法を述べる。(Example 4) Lithium chevrel compound Li 2 Mo 6 S 8 (100 g)
Was manufactured. The manufacturing method will be described below.
硫化リチウム粉末（５．６３ｇ）、金属モリブデン粉末
（２９．３９ｇ）、二硫化モリブデン粉末（６８．６５
ｇ）を秤量し、ガラス製ボールミルにて３時間混合した
後、この混合粉末を石英ガラス反応管に充填し、実施例
１同様の製造装置を用いて減圧下、７００℃で３０時
間、１０００℃で４０時間焼成してリチウムシェブレル
化合物Ｌｉ2Ｍｏ6Ｓ8を製造した。Lithium sulfide powder (5.63g), metallic molybdenum powder (29.39g), molybdenum disulfide powder (68.65)
g) was weighed and mixed in a glass ball mill for 3 hours, then the mixed powder was filled in a quartz glass reaction tube, and the same production apparatus as in Example 1 was used under reduced pressure at 700 ° C. for 30 hours at 1000 ° C. The mixture was baked at 40 ° C. for 40 hours to produce a lithium chevrel compound Li 2 Mo 6 S 8 .
得られたリチウムシェブレル化合物Ｌｉ2Ｍｏ6Ｓ8を粉
末Ｘ線回折で分析した結果、従来の石英ガラス管を封管
して製造したものとほぼ同じ回折パターンを示した。The obtained lithium chevrel compound Li 2 Mo 6 S 8 was analyzed by powder X-ray diffraction. As a result, it showed almost the same diffraction pattern as that produced by sealing a conventional quartz glass tube.
（実施例５） 銀シェブレル化合物ＡｇＭｏ6Ｓ8（１００ｇ）を製造し
た。以下、その製造法を述べる。Example 5 A silver chevrel compound AgMo 6 S 8 (100 g) was produced. The manufacturing method will be described below.
硫化銀粉末（１３．１８ｇ）、金属モリブデン粉末（２
２．９６ｇ）、二硫化モリブデン（６３．８６ｇ）を秤
量し、ガラス製ボールミルにて３時間混合した後、この
混合粉末を石英ガラス反応管に充填し、下記の製造装置
を用い、還元性ガスとして水素を１％含む窒素ガス気流
中で７００℃、３０時間、さらに、１０００℃、４０時
間焼成して銀シェブレル化合物ＡｇＭｏ6Ｓ8を製造し
た。Silver sulfide powder (13.18 g), metallic molybdenum powder (2
2.96 g) and molybdenum disulfide (63.86 g) were weighed and mixed in a glass ball mill for 3 hours, and then the mixed powder was filled in a quartz glass reaction tube and a reducing gas was produced using the following production apparatus. As a silver chevrel compound AgMo 6 S 8 was produced by firing in a nitrogen gas stream containing 1% of hydrogen at 700 ° C. for 30 hours and then at 1000 ° C. for 40 hours.
第３図に還元性ガスを含む不活性ガス気流中で製造する
ための製造装置の概略図を示した。第３図において、７
はガス流量制御機、８は石英ガラス反応管、９は電気
炉、１０は熱電対、１１は１％の水素を含む窒素ガスボ
ンベである。FIG. 3 shows a schematic view of a manufacturing apparatus for manufacturing in an inert gas flow containing a reducing gas. In FIG. 3, 7
Is a gas flow controller, 8 is a quartz glass reaction tube, 9 is an electric furnace, 10 is a thermocouple, and 11 is a nitrogen gas cylinder containing 1% hydrogen.
得られた銀シェブレル化合物ＡｇＭｏ6Ｓ8を粉末Ｘ線回
折で分析した結果、従来の石英ガラス管を封管して製造
したものとほぼ同じＸ線回折パターンを示した。また、
得られた銀シェブレル化合物の超伝導特性では、約７Ｋ
の臨界温度を示した。The obtained silver chevrel compound AgMo 6 S 8 was analyzed by powder X-ray diffraction, and as a result, it showed an X-ray diffraction pattern almost the same as that produced by sealing a conventional quartz glass tube. Also,
The superconducting property of the obtained silver chevrel compound is about 7K.
The critical temperature of
（実施例６） スズシェブレル化合物ＳｎＭｏ5Ｓ6（１００ｇ）を製造
した。以下、その製造法について述べる。硫化第一錫粉
末（１９．０６ｇ）、硫化モリブデン（１０１．２１
ｇ）を秤量し、ガラス製ボールミルにて３時間混合した
後、石英ガラス反応管に充填し、実施例５と同様の製造
装置を用い、還元性ガスとして水素５０％を含む窒素ガ
ス気流中で５００℃、３０時間、さらに、８００℃、４
０時間焼成して錫シェブレル化合物ＳｎＭｏ5Ｓ6を製造
した。Example 6 A tin chevrel compound SnMo 5 S 6 (100 g) was produced. The manufacturing method will be described below. Stannous sulfide powder (19.06 g), molybdenum sulfide (101.21)
g) was weighed and mixed in a glass ball mill for 3 hours, then charged into a quartz glass reaction tube, and using the same production apparatus as in Example 5, in a nitrogen gas stream containing 50% hydrogen as a reducing gas. 500 ℃, 30 hours, 800 ℃, 4
The tin chevrel compound SnMo 5 S 6 was produced by firing for 0 hour.
得られた錫シェブレル化合物ＳｎＭｏ5Ｓ6を粉末Ｘ線回
折で分析した結果、従来の石英ガラスを封管して製造し
たものとほぼ同様のＸ線回折パターンを示した。また、
得られた錫シェブレル化合物と超伝導特性では、約１２
Ｋの臨界温度を示した。The obtained tin chevrel compound SnMo 5 S 6 was analyzed by powder X-ray diffraction, and as a result, it showed an X-ray diffraction pattern almost similar to that produced by sealing a conventional quartz glass tube. Also,
The obtained tin chevrel compound and the superconducting property are about 12
The critical temperature of K is shown.
（実施例７） 銅シェブレル化合物Ｃｕ4Ｍｏ6Ｓ8（１００ｇ）を製造
した。以下、その製造法について述べる。(Example 7) A copper chevrel compound Cu 4 Mo 6 S 8 (100 g) was produced. The manufacturing method will be described below.
まず、酢酸銅（ＣＨ3ＣＯ2）4Ｃｕ2・２Ｈ2Ｏ（７３．
６４ｇ）を溶かした水溶液に硫化水素ガスを通じて硫化
銅を沈殿させ、生じた硫化銅を濾過、洗浄した後、乾燥
し、少量の硫黄とガラス製ボールミルを用いて３時間混
合し、水素気流中、４００℃で１０時間処理し硫化銅、
金属モリブデン粉末（２６．４９ｇ）、二硫化モリブデ
ン粉末（４４．２０ｇ）を秤量し、ガラス製ボールミル
にて３時間混合した後、石英ガラス反応管に充填し、実
施例５と同様の製造装置を用い、還元性ガスとして水素
１％を含む窒素ガス気流中で７００℃、３０時間、さら
に、１０００℃、４０時間焼成して銅シェブレル化合物
Ｃｕ4Ｍｏ6Ｓ8を製造した。First, copper acetate (CH 3 CO 2) 4 Cu 2 · 2H 2 O (73.
64 g) was dissolved in an aqueous solution of hydrogen sulfide gas to precipitate copper sulfide, and the resulting copper sulfide was filtered, washed, dried, and mixed with a small amount of sulfur for 3 hours using a glass ball mill. Copper sulfide, treated at 400 ℃ for 10 hours,
Metallic molybdenum powder (26.49 g) and molybdenum disulfide powder (44.20 g) were weighed and mixed in a glass ball mill for 3 hours, then charged into a quartz glass reaction tube, and the same production apparatus as in Example 5 was used. A copper chevrel compound Cu 4 Mo 6 S 8 was produced by firing at 700 ° C. for 30 hours and further at 1000 ° C. for 40 hours in a nitrogen gas stream containing 1% hydrogen as a reducing gas.
得られた銅シェブレル化合物Ｃｕ4Ｍｏ6Ｓ8を粉末Ｘ線
回折で分析した結果、従来の石英ガラス管を封管して製
造したものとほぼ同じ回折パターンを示した。The obtained copper chevrel compound Cu 4 Mo 6 S 8 was analyzed by powder X-ray diffraction, and as a result, it showed almost the same diffraction pattern as that produced by sealing a conventional quartz glass tube.
（実施例８） 鉄シェブレル化合物ＦｅＭｏ5Ｓ6（１００ｇ）を製造し
た。以下、その製造法について述べる。Example 8 An iron chevrel compound FeMo 5 S 6 (100 g) was produced. The manufacturing method will be described below.
まず、塩化第一鉄ＦｅＣｌ2・４Ｈ２Ｏ（２７．３１
ｇ）を溶かした水溶液に硫化アンモニウムを加えて硫化
鉄を合成した。次に、酸化モリブデンＭｏＯ３（９８．
８７ｇ）をアンモニア水に溶かした後、硫化水素を通じ
て硫化モリブデンを合成した。上記硫化鉄と硫化モリブ
デンをガラス製ボールミルを用いて３時間混合した。こ
の混合粉末を石英ガラス反応管に充填し、実施例５と同
様の製造装置を用い、還元性ガスとして水素５０％を含
む窒素ガス気流中で５００℃、３０時間、さらに、８０
０℃、４０時間焼成して鉄シェブレル化合物ＦｅＭｏ5
Ｓ6を製造した。First, ferrous chloride FeCl 2 .4H 2 O (27.31
Ammonium sulfide was added to the aqueous solution in which g) was dissolved to synthesize iron sulfide. Next, molybdenum oxide MoO 3 (98.
87 g) was dissolved in aqueous ammonia, and molybdenum sulfide was synthesized through hydrogen sulfide. The iron sulfide and molybdenum sulfide were mixed for 3 hours using a glass ball mill. This mixed powder was filled in a quartz glass reaction tube, and the same production apparatus as in Example 5 was used. In a nitrogen gas stream containing 50% hydrogen as a reducing gas, 500 ° C., 30 hours, and 80
Iron chevrel compound FeMo 5 after firing at 0 ° C for 40 hours
S 6 was manufactured.
得られた鉄シェブレル化合物ＦｅＭｏ5Ｓ6を粉末Ｘ線回
折で分析した結果、従来の石英ガラスを封管して製造し
たものとほぼ同様のＸ線回折パターンを示した。また、
製造した鉄シェブレルは、従来の硫化鉄、硫化モリブデ
ン、金属モリブデンを原料として製造したものに比べて
非常に粒径の細かいものであった。The obtained iron chevrel compound FeMo 5 S 6 was analyzed by powder X-ray diffraction, and as a result, it showed an X-ray diffraction pattern almost similar to that produced by sealing a conventional quartz glass tube. Also,
The produced iron chevrel had a very fine particle size as compared with those produced from conventional iron sulfide, molybdenum sulfide and metallic molybdenum.
実施例では、金属硫化物として銅、ニッケル、鉛、リチ
ウム、銀、錫、鉄の金属硫化物について述べたが、Ｎ
ａ，Ｍｇ，Ｃａ，Ｓｃ，Ｃｒ，Ｍｎ，Ｃｏ，Ｚｎ，Ｓ
ｒ，Ｙ，Ｐｄ，Ｃｄ，Ｉｎ，Ｂａ，Ｌａ，Ｃｅ，Ｐｒ，
Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔ
ｍ，Ｙｂ，Ｌｕの金属硫化物についても同様の方法で製
造することができる。In the examples, metal sulfides of copper, nickel, lead, lithium, silver, tin and iron were described as the metal sulfide, but N
a, Mg, Ca, Sc, Cr, Mn, Co, Zn, S
r, Y, Pd, Cd, In, Ba, La, Ce, Pr,
Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, T
The metal sulfides of m, Yb, and Lu can be manufactured by the same method.
発明の効果 以上、本発明は、金属硫化物、金属モリブデン粉末、硫
化モリブデン粉末を混合し減圧下、または、還元性ガス
を含む不活性ガス気流中で焼成することにより製造する
ことができるため従来のような煩雑な工程を必要とせ
ず、反応容器を何回でも使用することができることから
安価に大量に製造することができる。。As described above, the present invention can be produced by mixing a metal sulfide, a metal molybdenum powder, and a molybdenum sulfide powder and firing the mixture under reduced pressure or in an inert gas stream containing a reducing gas. Since the reaction container can be used any number of times without requiring such a complicated process as described above, it can be mass-produced inexpensively. .
【図面の簡単な説明】 第１図は減圧下でシェブレル化合物を製造するための焼
成装置の概略図、第２図はシェブレル化合物の粉末Ｘ線
回折図、第３図は水素を含む不活性ガス気流中でシェブ
レル化合物を製造するための焼成装置の概略図である。 １……原料、２……石英ガラス反応管、３……電気炉、
４……熱電対、５……トラップ、６……油回転式真空ポ
ンプ、７……ガス流量制御機、８……石英ガラス反応
管、９……電気炉、１０……熱電対、１１……ガスボン
ベ。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic diagram of a calcination apparatus for producing a chevrel compound under reduced pressure, FIG. 2 is a powder X-ray diffraction diagram of the chevrel compound, and FIG. 3 is an inert gas containing hydrogen. It is a schematic diagram of a calcination device for manufacturing a Chevrel compound in airflow. 1 ... Raw material, 2 ... Quartz glass reaction tube, 3 ... Electric furnace,
4 ... Thermocouple, 5 ... Trap, 6 ... Oil rotary vacuum pump, 7 ... Gas flow controller, 8 ... Quartz glass reaction tube, 9 ... Electric furnace, 10 ... Thermocouple, 11 ... … Gas cylinder.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ０１Ｇ 53/00 ＺＡＡ Ａ 55/00 ＺＡＡ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Internal reference number FI Technical display location C01G 53/00 ZAA A 55/00 ZAA
Claims (4)
Ｃａ，Ｓｃ，Ｃｒ，Ｍｎ，Ｆｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚ
ｎ，Ｓｒ，Ｙ，Ｐｄ，Ａｇ，Ｃｄ，Ｉｎ，Ｓｎ，Ｂａ，
Ｌａ，Ｐｂ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔ
ｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕのうち少なく
とも一種の元素）金属モリブデン、硫化モリブデンの混
合物を減圧下で焼成することを特徴とするシェブレル化
合物の製造法。1. A metal sulfide (metals are Li, Na, Mg,
Ca, Sc, Cr, Mn, Fe, Co, Ni, Cu, Z
n, Sr, Y, Pd, Ag, Cd, In, Sn, Ba,
La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, T
b, Dy, Ho, Er, Tm, Yb, Lu) at least one element) A method for producing a chevrel compound, which comprises firing a mixture of metallic molybdenum and molybdenum sulfide under reduced pressure.
Ｃａ，Ｓｃ，Ｃｒ，Ｍｎ，Ｆｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚ
ｎ，Ｓｒ，Ｙ，Ｐｄ，Ａｇ，Ｃｄ，Ｉｎ，Ｓｎ，Ｂａ，
Ｌａ，Ｐｂ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔ
ｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕのうち少なく
とも一種の元素）、硫化モリブデンの混合物を還元性ガ
スを含む不活性ガス気流中で焼成することを特徴とする
シェブレル化合物の製造法。2. A metal sulfide (metal is Li, Na, Mg,
Ca, Sc, Cr, Mn, Fe, Co, Ni, Cu, Z
n, Sr, Y, Pd, Ag, Cd, In, Sn, Ba,
La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, T
b, Dy, Ho, Er, Tm, Yb, Lu) and a mixture of molybdenum sulfide in an inert gas stream containing a reducing gas, and firing the mixture.
Ｃａ，Ｓｃ，Ｃｒ，Ｍｎ，Ｆｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚ
ｎ，Ｓｒ，Ｙ，Ｐｄ，Ａｇ，Ｃｄ，Ｉｎ，Ｓｎ，Ｂａ，
Ｌａ，Ｐｂ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔ
ｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕのうち少なく
とも一種の元素）、金属モリブデン、硫化モリブデンの
混合物を還元性ガスを含む不活性ガス気流中で焼成する
ことを特徴とするシェブレル化合物の製造法。3. A metal sulfide (metal is Li, Na, Mg,
Ca, Sc, Cr, Mn, Fe, Co, Ni, Cu, Z
n, Sr, Y, Pd, Ag, Cd, In, Sn, Ba,
La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, T
b, Dy, Ho, Er, Tm, Yb, Lu), a metal molybdenum, and a mixture of molybdenum sulfide in a stream of an inert gas containing a reducing gas. Manufacturing method.
ａ，Ｓｃ，Ｃｒ，Ｍｎ，Ｆｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚ
ｎ，Ｓｒ，Ｙ，Ｐｄ，Ａｇ，Ｃｄ，Ｉｎ，Ｓｎ，Ｂａ，
Ｌａ，Ｐｂ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔ
ｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕのうち少なく
とも一種の元素）を含む溶液より合成した金属硫化物、
また、モリブデン塩を含む溶液より合成した硫化モリブ
デンを用いたことを特徴とする特許請求の範囲第１項、
第２項または第３項記載のシェブレル化合物の製造法。4. Metal salt (metal is Li, Na, Mg, C
a, Sc, Cr, Mn, Fe, Co, Ni, Cu, Z
n, Sr, Y, Pd, Ag, Cd, In, Sn, Ba,
La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, T
b, Dy, Ho, Er, Tm, Yb, at least one element of Lu), a metal sulfide synthesized from a solution containing
Further, molybdenum sulfide synthesized from a solution containing a molybdenum salt is used, and claim 1
A method for producing the chevrel compound according to item 2 or 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63233021A JPH0624983B2 (en) | 1987-10-16 | 1988-09-16 | Method for producing chevrel compound |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26212087 | 1987-10-16 | ||
| JP62-262120 | 1987-10-16 | ||
| JP63233021A JPH0624983B2 (en) | 1987-10-16 | 1988-09-16 | Method for producing chevrel compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01201028A JPH01201028A (en) | 1989-08-14 |
| JPH0624983B2 true JPH0624983B2 (en) | 1994-04-06 |
Family
ID=26530797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63233021A Expired - Fee Related JPH0624983B2 (en) | 1987-10-16 | 1988-09-16 | Method for producing chevrel compound |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0624983B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2351075A (en) * | 1999-06-17 | 2000-12-20 | Secr Defence | Producing lithiated transition metal sulphides |
| US8389129B2 (en) * | 2010-07-09 | 2013-03-05 | Climax Engineered Materials, Llc | Low-friction surface coatings and methods for producing same |
| JP5825627B2 (en) * | 2011-08-05 | 2015-12-02 | 国立研究開発法人産業技術総合研究所 | Method for producing chevrel phase compound |
-
1988
- 1988-09-16 JP JP63233021A patent/JPH0624983B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01201028A (en) | 1989-08-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dev et al. | Synthesis and structure of [M (N-methylimidazole) 6] S8 (M= manganese, iron, nickel, magnesium). Polysulfide salts prepared by the reaction N-methylimidazole+ metal powder+ sulfur | |
| Bonneau et al. | Solid-state metathesis as a quick route to transition-metal mixed dichalcogenides | |
| Ferraro et al. | Infrared spectra of several hydroxy-bridged complexes of chromium (III) and iron (III) from 650 to 80 cm.-1 | |
| Schnöckel et al. | From AIX/GaX monohalide molecules to metalloid aluminum and gallium clusters | |
| US5089222A (en) | Manufacturing process of chevrel compounds | |
| US4525206A (en) | Reduction process for forming powdered alloys from mixed metal iron oxides | |
| Sivasankar et al. | Studies on bis (hydrazine) metal malonates and succinates | |
| CN1260118C (en) | Preparation for metal sulfide | |
| JPH0624983B2 (en) | Method for producing chevrel compound | |
| Reckeweg et al. | The Nitrido Borates Ln3B2N4 (Ln= La–Nd) and La5B4N9: Syntheses, Structures, and Properties | |
| US3851045A (en) | Lanthanide transition metal ternary chalcogenides | |
| Passaretti et al. | Preparation and properties of poorly crystallized cobalt disulfide and ruthenium disulfide | |
| JP2517099B2 (en) | Method for producing chevrel compound | |
| US3342591A (en) | Ferromagnetic compounds and method of preparation | |
| JPH0761866B2 (en) | Method for producing chevrel compound | |
| Michelson et al. | Synthesis and properties of some new reduced niobate compounds | |
| JPH1053414A (en) | Method for producing metal disulfides and method for further processing them to produce dimetallic trisulfides | |
| JPS6210229A (en) | Manufacture of nb3sn | |
| Zumdick et al. | Syntheses, crystal structure, and properties of Hf2Ni2In, Hf2Ni2Sn, Hf2Cu2In, and Hf2Pd2In with ordered Zr3Al2 type structure | |
| JPH0393630A (en) | Production of copper molybdenum sulfide | |
| Iyer et al. | Preparation and characterization of TIMIII (SO4) 2· 4H2O (M (III)≡ Pu, Sm to Dy) | |
| JPH0369505A (en) | Oxide superconducting material | |
| JPS63288912A (en) | Production of inorganic oxide superconductor | |
| JPH01264930A (en) | Oxide superconductor manufacturing method and applied products | |
| JPH04325420A (en) | Compound with composition NaFe3V9O19 and its synthesis method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |