Manufacturing process for chevrel phase compounds

Powder metallurgy processes – Powder metallurgy processes with heating or sintering – Metal and nonmetal in final product

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Details

419 57, 419 58, B22F 700

Patent

active

049667491

DESCRIPTION:

BRIEF SUMMARY
TECHNICAL FIELD

This invention relates to a manufacturing process of Chevrel phase compounds whose electric resistance in a temperature range of liquid helium becomes almost zero and which can be used as a material for a superconductor utilizable in the fields of high efficiency power storage, generation of intense magnetic fields and high efficiency power transmissions or as an electrode material for electrochemical elements.


TECHNICAL BACKGROUND

Since Chevrel phase compounds have a critical temperature higher than a temperature of liquid helium and have a very high critical magnetic field, many studies have been made. Moreover, certain Chevrel phase compounds such as, for example, copper, Chevrel phase compounds, wherein the metal element can be chemically or electrochemically released from or received in the compound without destroying the skeletal structure of Mo.sub.6 S.sub.8 of the compound, have been studied for application as electrode materials of electrochemical elements. In a conventional process of manufacturing Chevrel phase compounds, it powders of various metal elements, metallic molybdenum powder and sulfur powder were mixed after milling, the mixture was placed in a quartz glass tube and sealed under reduced pressure, and sintered at 400.degree. C. for 12 hours, then at 600.degree. C. for 12 hours and finally at 1000.degree. C. for 24 hours.
In this process, the starting materials contain sulfur which is apt to react with most metals and are sintered after placing in a reaction tube and sealing the tube under reduced pressure, so that it is necessary to use as the reactor tube, a quartz glass tube which is stable against sulfur and can be worked as desired. After the sintering, it is essential to open the quartz glass reaction tube in order to withdraw the resultant product thus making it difficult to use the quartz glass reaction tube several times. In addition, if large amounts of the product are prepared in one batch, sulfur will be gasified during the course of temperature rise. When the pressure of the resultant gas becomes too high, the quartz glass reaction tube is broken. Thus, the production process is complicated and involves a problem in the industrial production of the compound.


DISCLOSURE OF THE INVENTION

The present invention provides a manufacturing process of Chevrel phase compounds which is simple in procedure and is adapted for mass-production.
The above object of the invention is achieved by a process which comprising mixing a sulfide of a metal (which metal is at least one element selected from 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 and Lu), metallic molybdenum and molybdenum sulfide, and sintering the mixture under reduced pressure or in a stream of an inert gas (argon, helium or nitrogen gas) containing a reductive gas.


BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic illustrative view of a sintering apparatus for manufacturing Chevrel phase compounds under reduced pressure;
FIG. 2 is a powder X-ray diffraction pattern of a Chevrel phase compound; and
FIG. 3 is a schematic illustrative view of a sintering apparatus for manufacturing Chevrel phase compounds in an inert gas stream containing hydrogen.


BEST MODE OF CARRYING OUT THE INVENTION

The present invention is described by way of examples.


(EXAMPLE 1)

A copper Chevrel phase compound, Cu.sub.2 Mo.sub.6 S.sub.8 (100 g) was prepared in the following manner.
Cuprous sulfide powder (16.95 g), metallic molybdenum powder (25.00 g) and molybdenum disulfide powder (59.35 g) were weighed and mixed in a glass ball mill for 3 hours, after which the mixed powder was charged into a quartz glass reaction tube, followed by sintering by the use of the following sintering apparatus under reduced pressure at 700.degree. C. for 30 hours and then at 1000.degree. C. for 40 hours to obtain copper Chevrel phase compound, Cu.sub.2 Mo.sub.6 S.sub.8.
The sintering apparatus for manufacturing the Chevrel phase compound under r

REFERENCES:
patent: 4704249 (1987-11-01), Glatzle
patent: 4808488 (1989-02-01), Chevrel et al.

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