JPH0761866B2 - Method for producing chevrel compound - Google Patents
Method for producing chevrel compoundInfo
- Publication number
- JPH0761866B2 JPH0761866B2 JP63087515A JP8751588A JPH0761866B2 JP H0761866 B2 JPH0761866 B2 JP H0761866B2 JP 63087515 A JP63087515 A JP 63087515A JP 8751588 A JP8751588 A JP 8751588A JP H0761866 B2 JPH0761866 B2 JP H0761866B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- chevrel compound
- powder
- reaction tube
- chevrel
- 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 - Lifetime
Links
- 150000001875 compounds Chemical class 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 238000010304 firing Methods 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 12
- 229910052802 copper Inorganic materials 0.000 claims description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052744 lithium Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910052689 Holmium Inorganic materials 0.000 claims description 4
- 229910052765 Lutetium Inorganic materials 0.000 claims description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052772 Samarium Inorganic materials 0.000 claims description 4
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052793 cadmium Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052706 scandium Inorganic materials 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- -1 A). g Inorganic materials 0.000 claims 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 26
- 239000010949 copper Substances 0.000 description 16
- 229910017267 Mo 6 S 8 Inorganic materials 0.000 description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000011133 lead Substances 0.000 description 7
- 238000000634 powder X-ray diffraction Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 229910017722 AgMo Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 101150029133 agmo gene Proteins 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (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
できる超電導体の材料、または、電気化学素子の電極材
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。TECHNICAL FIELD The present invention relates to a superconductor material which has almost zero electric resistance in a 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 as an electrode material of an electrochemical device.
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、400
℃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, as for the copper chevrel compound, the metal element in the chevrel compound can be chemically or electrochemically taken in and out without destroying the skeleton structure of Mo 6 S 8 of the chevrel compound. Expected to be applied. However,
Conventionally, as a method for producing a chevrel compound, powders of various metal elements, metal molybdenum powder, and sulfur powder are crushed and mixed, and this mixed powder is sealed under reduced pressure in a quartz glass tube.
After firing at ℃ for 12 hours, burn at 600 ℃ for 12 hours, then 100
It was manufactured by firing at ℃ 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り、し
かも、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
ることができず、また、１回の合成量を多くすると昇温
時に硫黄のガス圧が高くなり石英ガラス反応管が破裂す
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. On the other hand, it is necessary to use a stable and processable quartz glass tube, and after firing, the quartz glass reaction tube must be opened to take out the synthetic product, and the quartz glass reaction tube must be used many times. However, if the synthesis amount per one time is increased, the gas pressure of sulfur becomes high at the time of temperature rise and the quartz glass reaction tube bursts, which complicates the manufacturing process and has a problem in industrial production. .
我々は、この問題点を解決するため各種金属塩の混合溶
液より微細な各種金属硫化物の混合体を作成し、その混
合体を減圧下、または、水素を含む不活性ガス雰囲気下
で焼成してシェブレル化合物を製造する方法を提案した
（特願昭62−262120）。In order to solve this problem, we created a finer mixture of various metal sulfides than a mixed solution of various metal salts, and calcined the mixture under reduced pressure or in an inert gas atmosphere containing hydrogen. Proposed a method for producing a chevrel compound (Japanese Patent Application No. 62-262120).
しかしながら、この製造方法では、各種金属硫化物の溶
液に対する溶解度の違いや溶液で分解するものもあり、
製造可能なシェブレル化合物が限られていた。However, in this manufacturing method, there are also those that differ in solubility in various metal sulfide solutions or decompose in solution,
The number of chevrel compounds that can be produced was limited.
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モリブデン、
硫化モリブデン、金属粉末（Li,Na,Mg,Ca,Sc,Cr,Mn,Fe,
Co,Ni,Cu,Zn,Sr,Y,Pd,Ag,Cd,In,Sn,Ba,La,Pb,Ce,Pr,Nd,
Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Luのうち少なくとも一種
の元素）を混合し、この混合体を減圧下または水素を含
むアルゴン、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 metallic molybdenum,
Molybdenum sulfide, metal powder (Li, Na, Mg, Ca, Sc, Cr, Mn, Fe,
Co, Ni, Cu, Zn, Sr, Y, Pd, Ag, Cd, In, Sn, Ba, La, Pb, Ce, Pr, Nd,
Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu), and mix this mixture under reduced pressure or in an argon, helium or nitrogen gas stream containing hydrogen. It is a method of producing a chevrel compound by firing.
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、減圧下または水素を含むアルゴン、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、原料として硫黄を含まず、また、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 argon, helium, or nitrogen gas stream containing hydrogen, the reaction tube does not need to be sealed and the reaction tube can be used any number of times. can do. Further, since the raw material does not contain sulfur and the quartz glass reaction tube is an open tube, the quartz glass reaction tube will not be ruptured even if the synthesis amount per 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。(Example 1) A copper chevrel compound Cu 2 Mo 6 S 8 (100 g) was produced. The manufacturing method will be described below.
二硫化モリブデン（66.736g）、金属モリブデン粉末（2
0.004g）、金属銅粉末（13.250g）を秤量し、ガラス製
ボールミルにて30分間混合した後、石英ガラス反応管に
充填し、下記の焼成条件で焼成した。Molybdenum disulfide (66.736g), metal molybdenum powder (2
0.004 g) and metallic copper powder (13.250 g) were weighed and mixed in a glass ball mill for 30 minutes, then charged into a quartz glass reaction tube and fired under the following firing conditions.
第１図に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 view of the manufacturing apparatus. In FIG.
Reference numeral 1 is a raw material, 2 is a quartz glass reaction tube filled with the raw material, 3 is an electric furnace, 4 is a thermocouple, 5 is a trap, and 6 is an oil rotary vacuum pump.
上記石英ガラス反応管を電気炉内に配置し、石英ガラス
反応管内を油回転式真空ポンプで減圧し、上記油回転式
真空ポンプを稼働させ石英ガラス反応管内を減圧した状
態で100℃/hrの昇温速度で700℃まで昇温し、700℃で36
時間焼成した後、さらに、1000℃まで同じ昇温速度で昇
温し24時間焼成した後、室温まで冷却し、銅シェブレル
化合物Cu2Mo6S8を製造した。The quartz glass reaction tube is placed in an electric furnace, the quartz glass reaction tube is depressurized by an oil rotary vacuum pump, and the oil rotary vacuum pump is operated to depressurize the quartz glass reaction tube at 100 ° C / hr. The temperature is raised to 700 ° C and the temperature is increased to 700 ° C.
After firing for an hour, the temperature was further raised to 1000 ° C. at the same heating rate for 24 hours, and then cooled to room temperature to produce a copper chevrel compound Cu 2 Mo 6 S 8 .
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の超電導特
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） 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 2 A lead chevrel compound PbMo 6.2 S 8 (100 g) was produced. The manufacturing method will be described below.
実施例１と同様に金属鉛粉末（19.57g）、金属モリブデ
ン粉末（19.94g）、二硫化モリブデン粉末（60.49g）を
秤量し、ガラス製ボールミルで30分間混合した混合粉末
を石英ガラス反応管内に充填し、実施例１と同様に油回
転式真空ポンプを稼働させ、石英ガラス反応管内を減圧
にした状態で100℃/hrの昇温速度で700℃まで昇温し、7
00℃で36時間焼成した後、さらに、1000℃まで同じ昇温
速度で昇温し24時間焼成した後、室温まで冷却し、鉛シ
ェブレル化合物PbMo6.2S8を製造した。In the same manner as in Example 1, metallic lead powder (19.57 g), metallic molybdenum powder (19.94 g) and molybdenum disulfide powder (60.49 g) were weighed and mixed with a glass ball mill for 30 minutes to prepare a mixed powder in a quartz glass reaction tube. After filling, the oil rotary vacuum pump was operated in the same manner as in Example 1, and the temperature inside the quartz glass reaction tube was reduced to 700 ° C. at a heating rate of 100 ° C./hr.
After firing at 00 ° C. for 36 hours, the temperature was further raised to 1000 ° C. at the same heating rate for 24 hours, and after cooling to room temperature, a lead chevrel compound PbMo 6.2 S 8 was produced.
得られた鉛シェブレル化合物Pb2Mo6.2S8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の超電導特性で
は、約12Kの臨界温度を示した。The obtained lead chevrel compound Pb 2 Mo 6.2 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. The superconducting property of the obtained lead chevrel compound PbMo 6.2 S 8 showed a critical temperature of about 12K.
（実施例３） 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 3 A silver chevrel compound AgMo 6 S 8 (100 g) was produced. The manufacturing method will be described below.
実施例１と同様に金属銀粉末（11.48g）、金属モリブデ
ン粉末（20.41g）、二硫化モリブデン（68.11g）を秤量
し、ガラス製ボールミルにて30分間混合した後、石英ガ
ラス反応管に充填し、実施例１と同様の焼成条件で焼成
し製造した。Metal silver powder (11.48 g), metal molybdenum powder (20.41 g) and molybdenum disulfide (68.11 g) were weighed in the same manner as in Example 1, mixed in a glass ball mill for 30 minutes, and then filled in a quartz glass reaction tube. Then, it was fired under the same firing conditions as in Example 1 to manufacture.
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電導特性では、約7Kの臨界
温度を示した。As a result of powder X-ray diffraction analysis of the obtained silver chevrel compound AgMo 6 S 8 , an X-ray diffraction pattern almost the same as that produced by sealing a conventional quartz glass tube was shown. The superconducting properties of the obtained silver chevrel compound showed a critical temperature of about 7K.
（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 A lithium chevrel compound Li 2 Mo 6 S 8 (100 g) was produced. The manufacturing method will be described below.
金属モリブデン粉末（22.68g）、二硫化モリブデン粉末
（75.68g）を秤量し、ガラス製ボールミルにて30分間混
合した後、この混合体を400℃で24時間減圧乾燥し、ア
ルゴンガスを流したドライボックス内で、金属リチウム
（1.64g）とで混合した後、石英ガラス反応管に充填
し、石英ガラス反応管内を油回転式真空ポンプで減圧
し、油回転式真空ポンプを稼働させ石英ガラス反応管内
を減圧した状態で100℃/hrの昇温速度で700℃まで昇温
し、700℃で36時間焼成した後、さらに、1000℃まで同
じ昇温速度で昇温し24時間焼成した後、室温まで冷却
し、リチウムシェブレル化合物Li2Mo6S8を製造した。Metallic molybdenum powder (22.68g) and molybdenum disulfide powder (75.68g) were weighed and mixed in a glass ball mill for 30 minutes, and then this mixture was dried under reduced pressure at 400 ° C for 24 hours and dried by flowing argon gas. After mixing with metallic lithium (1.64g) in the box, it is filled in a quartz glass reaction tube, the quartz glass reaction tube is depressurized by an oil rotary vacuum pump, and the oil rotary vacuum pump is activated to activate the quartz glass reaction tube. Was heated to 700 ° C at a heating rate of 100 ° C / hr in a depressurized state, baked at 700 ° C for 36 hours, further heated to 1000 ° C at the same heating rate for 24 hours, and then at room temperature. The mixture was cooled to a temperature 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, and as a result, it showed almost the same diffraction pattern as that produced by sealing a conventional quartz glass tube.
（実施例５） 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 5) A copper chevrel compound Cu 4 Mo 6 S 8 (100 g) was produced. The manufacturing method will be described below.
金属銅粉末（23.40g）、金属モリブデン粉末（17.66
g）、二硫化モリブデン粉末（58.94g）を秤量し、ガラ
ス製ボールミルにて30分間混合した後、石英ガラス反応
管に充填し、石英ガラス反応管内に水素１％を含む窒素
ガス（またはアルゴン、ヘリウム）を1L/minで流した状
態で100℃/hrの昇温速度で800℃まで昇温し、800℃で36
時間焼成した後、室温まで冷却し、銅シェブレル化合物
Cu2Mo6S8を製造した。第３図に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。Metallic copper powder (23.40g), metallic molybdenum powder (17.66)
g), molybdenum disulfide powder (58.94 g) was weighed and mixed in a glass ball mill for 30 minutes, then charged into a quartz glass reaction tube, and nitrogen gas containing 1% hydrogen (or argon, in the quartz glass reaction tube). Helium) at a flow rate of 1 L / min, and the temperature is raised to 800 ° C at a heating rate of 100 ° C / hr,
After firing for hours, cool to room temperature
Cu 2 Mo 6 S 8 was manufactured. FIG. 3 shows a schematic view of the manufacturing apparatus. 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.
得られた銅シェブレル化合物Cu2Mo6S8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 2 Mo 6 S 8 was analyzed by powder X-ray diffraction. As a result, a diffraction pattern almost the same as that produced by sealing a conventional quartz glass tube was shown.
本実施例では、金属元素としてリチウム、銅、銀、鉛に
ついて述べたが、Na,Mg,Ca,Sc,Cr,Mn,Fe,Co,Ni,Zn,Sr,
Y,Pd,Cd,In,Sn,Ba,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,
Tm,Yb,Luについても同様の方法で製造することができ
る。In this embodiment, lithium, copper, silver, and lead are described as the metal elements, but Na, Mg, Ca, Sc, Cr, Mn, Fe, Co, Ni, Zn, Sr,
Y, Pd, Cd, In, Sn, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er,
Tm, Yb, and Lu can be manufactured by the same method.
発明の効果 以上、本発明は、金属モリブデン粉末、硫化モリブデン
粉末、金属元素粉末を混合し減圧下、または、水素を含
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。EFFECTS OF THE INVENTION As described above, the present invention can be produced by mixing metal molybdenum powder, molybdenum sulfide powder, and metal element powder and firing them under reduced pressure or in an inert gas stream containing hydrogen. Since the reaction container can be used any number of times without requiring complicated steps, it can be mass-produced inexpensively.
第１図は本発明の一実施例のシェブレル化合物を製造法
になる焼成装置の概略図、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。FIG. 1 is a schematic diagram of a calcination apparatus used in the method for producing a chevrel compound according to one embodiment of the present invention, FIG. 2 is a powder X-ray diffraction diagram of the chevrel compound, and FIG. 3 is an inert gas stream containing hydrogen. 1 is a schematic view of a firing apparatus for producing a chevrel compound. 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 (72)発明者 吉田 栄 埼玉県北葛飾郡鷲宮町桜田３―６―５ (56)参考文献 特開 昭61−256507（ＪＰ，Ａ) 特表 昭60−501386（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Sakae Yoshida 3-6-5 Sakurada, Washimiya Town, Kita-Katsushika-gun, Saitama Prefecture (56) References JP-A-61-256507 (JP, A) Special Table: Sho-501-501386 (JP) , A)
Claims (2)
属（Li,Na,Mg,Ca,Sc,Cr,Mn,Fe,Co,Ni,Cu,Zn,Sr,Y,Pd,A
g,Cd,In,Sn,Ba,La,Pb,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,
Tm,Yb,Luのうち少なくとも一種の元素）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. Molybdenum sulfide, molybdenum, and metals (Li, Na, Mg, Ca, Sc, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Y, Pd, A).
g, Cd, In, Sn, Ba, La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er,
A method for producing a chevrel compound, which comprises firing a mixture of at least one element of Tm, Yb, and Lu) under reduced pressure.
属（Li,Na,Mg,Ca,Sc,Cr,Mn,Fe,Co,Ni,Cu,Zn,Sr,Y,Pd,A
g,Cd,In,Sn,Ba,La,Pb,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,
Tm,Yb,Luのうち少なくとも一種の元素）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. Molybdenum sulfide, molybdenum, and metals (Li, Na, Mg, Ca, Sc, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Y, Pd, A).
g, Cd, In, Sn, Ba, La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er,
A method for producing a chevrel compound, which comprises firing a mixture of at least one element of Tm, Yb, and Lu) in an inert gas stream containing a reducing gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63087515A JPH0761866B2 (en) | 1988-04-08 | 1988-04-08 | Method for producing chevrel compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63087515A JPH0761866B2 (en) | 1988-04-08 | 1988-04-08 | Method for producing chevrel compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01261226A JPH01261226A (en) | 1989-10-18 |
| JPH0761866B2 true JPH0761866B2 (en) | 1995-07-05 |
Family
ID=13917128
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63087515A Expired - Lifetime JPH0761866B2 (en) | 1988-04-08 | 1988-04-08 | Method for producing chevrel compound |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0761866B2 (en) |
-
1988
- 1988-04-08 JP JP63087515A patent/JPH0761866B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01261226A (en) | 1989-10-18 |
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