JPH0230624A - Production of copper molybdenum sulfide - Google Patents

Abstract

PURPOSE:To obtain the title high-purity sulfide safely and in high efficiency by charging a quartz vessel with a formulation comprising metallic copper, metallic molybdenum and simple substance sulfur and by making a reaction on heating under a vacuum so as to produce a specified compound. CONSTITUTION:A raw material (a) is prepared by formulating each powdery metallic copper, metallic molybdenum and simple substance sulfur so as to obtain the target copper molybdenum sulfide of formula I (x is 1.5-4; y is 0-0.4). A quartz vessel is then charged with the component a so as to satisfy the relationships: II (D is the total amount of the component a (g); C is inner volume of the vessel (ml)) and III (A is rate of temperature rise deg.C/hr; B is maximum pressure for the vessel kg/cm<2>-G) followed by heating under a vacuum at 500-700 deg.C for 6-24 hr to produce a precursor sulfide (b) free from unreacted simple substance sulfur. Thence, the component b is ground and put into the vessel again followed by reaction on heating under a vacuum at 900-1,100 deg.C for 24-120hr, thus obtaining the objective copper molybdenum sulfide.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing copper molybdenum sulfide. More specifically, the present invention relates to a method for producing copper molybdenum sulfide from metallic copper, metallic molybdenum, and elemental sulfur.

[Problems to be solved by conventional technology and invention] General formula 'MxMoaS*-￥ (where M is metal, y=0~
The Chevrel phase compound represented by 0.4) is a three-dimensional compound with a large oven channel synthesized by Chevrell et al. in 1971, and the third component metal M is placed in the gap formed by the arrangement of Mo1st clusters. It has an intricate structure.

This Chevrel phase compound exhibits specific properties for superconductivity, and copper molybdenum sulfide in which the metal M is Cu is
It is attracting attention as an electrode material for secondary batteries because it has the property that copper ions that enter the gaps formed by the arrangement of o1st clusters are extremely mobile. In addition, fine particles are required for use as electrode materials for secondary batteries.

General methods for producing metal sulfides include (1) direct reaction of an elemental metal or/and metal sulfide with sulfur in a sealed tube made of glass or quartz, and (2) hydrogen sulfide from an acidic solution. Or precipitation reaction method using ammonia sulfide,
(3) There is a method of reacting a metal salt or a metal element with hydrogen sulfide.

Among these methods, methods (2) and (3) have hardly been reported regarding copper molybdenum sulfide, and method (1) is common.

There are many examples of synthesis using method (1), including (a) a method in which powders of copper sulfide, molybdenum disulfide, and elemental sulfur are vacuum charged into a sealed quartz tube and heated at 1000°C for 100 hours [Toru Inoue] , Electrochemistry, ■, 812, (1986)) (bl) Each powder of metallic copper, metallic molybdenum, and elemental sulfur was vacuum charged into a sealed quartz tube, heated at 400°C overnight, and then Method of heating at 1000 °C for 2 days and then heating at 1100 °C for 3 days (K, Y, Cheung et al.
; Mat, Res, Bull,, 151717 (1
980)) (C) Copper sulfide, molybdenum disulfide, and metal molybdenum are vacuum sealed in a sealed quartz tube and heated at 400°C overnight, then heated at 1000″C for 2 days, then the contents are removed and crushed. After that, the tube is vacuum charged again into a sealed quartz tube and heated at 1000°C for 3 days (S, Yamamot
o et, al,; Mat, Res, Bull, +
ifl 1311 (1983)) (d) Metallic copper,
Powders of metallic molybdenum and elemental sulfur were vacuum charged into a sealed quartz tube and heated at 440'C for 4 hours without shaking every 4 to 6 hours.
A method of heating for 8 hours and then heating at 1000°C for 24 hours (J, Mizusaki et al,; 5olid
5tate Ionics, 11293 (198
4)) etc. have been reported.

However, all of these methods have the following problems. That is, in methods (a) and (C), there is a problem that the purity of the product is low because it is difficult to obtain high purity copper sulfide and molybdenum disulfide as raw materials.
With methods b) and (d), it is easy to obtain high-purity raw materials,
Although the resulting product has high purity, it takes too long to produce and is unsuitable for industrial production.Also, when heating in a sealed quartz tube using methods (b) and (b), unreacted sulfur is produced. If the temperature increase rate is too high, there is a risk that the sealed tube will burst, and if the temperature increase rate is too low, the manufacturing time will take longer.

As a result of various studies to solve the above problems, the present inventors have developed a method for producing copper molybdenum sulfide using a quartz container. It was discovered that the above problem could be solved by specifying the heating time to the desired temperature, and copper molybdenum sulfide could be produced safely and economically.
The application was filed as No. 20.

[Means to solve the problem]

However, according to subsequent studies by the present inventors,
The copper molybdenum sulfide obtained by the method of No.-145820 is
Analysis with an X-ray diffractometer reveals that the material has a single phase, but in some cases it may contain a considerable amount of coarse particles that do not pass through a 115-mesh sieve. And this 115
When only coarse particles larger than mesh were analyzed using an X491 diffractometer, it was found that they contained a considerable amount of molybdenum disulfide as an impurity.

Therefore, the inventors of the present invention continued to conduct extensive studies on a method for producing high-purity copper molybdenum sulfide that does not contain impurities such as molybdenum disulfide. By heating at a relatively low temperature to obtain a precursor sulfide that does not contain elemental sulfur, and then pulverizing and mixing this precursor sulfide and heating it again in a quartz container, fine and highly pure copper molybdenum sulfide can be obtained. The present invention was completed based on the discovery that the present invention can be obtained.

That is, in the present invention, metallic copper, metallic molybdenum, and elemental sulfur are charged into a quartz container, evacuated, and then the quartz container is heated in a sealed state to form a compound with a compound formula of CuxMo*5s-y.
(However, x = 1.5 to 4, V = O to 0.4) When producing copper molybdenum sulfide, metal copper, metal molybdenum, and elemental sulfur are charged into a quartz container, evacuated, and then sealed. Then, the quartz container is heated at a temperature of 500 to 700°C for 6 to 24 hours to obtain a precursor sulfide free of unreacted elemental sulfur.Then, the precursor sulfide is taken out from the quartz container and pulverized and mixed. A method for producing copper molybdenum sulfide, which is characterized in that the mixed precursor sulfide is charged into a quartz container again, the container is evacuated, the container is sealed, and the quartz container is reacted by heating at a temperature of 900 to 1100'C for 24 to 120 hours. A manufacturing method is provided.

[Detailed disclosure of the invention]

The present invention will be explained in more detail.

The copper molybdenum sulfide of the present invention is a compound represented by the above chemical formula, and is a type of what is commonly called a Chevrel type compound, and has a structure in which copper enters the gaps formed by the arrangement of Mo, S, and clusters. Therefore, the CuO value in the above chemical formula can take any value between 1.5 and 4. Further, the value of S is basically 8, but when the value of Cu is 3.5 or less, it is easier to form a uniform compound by setting the value of S to less than 8.

Therefore, taking these things into consideration, Cu, Mo
, The molar ratio of S may be changed within the range indicated by the proviso to the above chemical formula.

In the present invention, first, a precursor sulfide is produced, which will be described below.

The raw materials, metal copper, metal molybdenum, and elemental sulfur, are charged into a quartz container. In this case, it is preferable to uniformly mix these raw materials in powder form beforehand and charge them into a quartz container in order to obtain a precursor sulfide with a uniform composition, and also to shorten the reaction time as much as possible. Preferably, however, since elemental sulfur is in a gaseous state at the reaction temperature of the precursor sulfide, it does not necessarily have to be in the form of powder and may be in the form of granules or lumps, but a quartz container with a seal made of quartz as described later may be used. When using a tube, powdered material is preferred because it can be easily loaded into the sealed tube.

The particle size of these powders is not particularly limited, but it is preferable that the particle size is smaller than 50 mesh.

There are no particular limitations on the respective purity of metallic copper, metallic molybdenum, and elemental sulfur, but the purity may be selected depending on the purity of the required product copper molybdenum sulfide.

In the present invention, each of the above raw materials is charged into a quartz container in the same amount as the molar ratio of the product copper molybdenum sulfide to be obtained.

The quartz container charged with each raw material is heated, the air inside is evacuated, and then the container is sealed. The above heating temperature is not particularly limited, but if the heating temperature is low, gases such as air adsorbed by the raw materials will not be completely exhausted and will remain partially, which is undesirable. If it is too high, volatilization of elemental sulfur will occur, which is also not preferable. Therefore, this heating temperature is preferably about 50 to 100°C.

Regarding vacuum evacuation of the quartz container, it is preferable that the inside of the quartz container be in a high vacuum after evacuation.
The vacuum is evacuated to below orr.

In the present invention, elemental sulfur as a raw material is heated and gasified at the reaction temperature of the precursor sulfide, so the quartz container used has all parts that may come into contact with this gasified elemental sulfur made of quartz. Although any type of tube can be used as long as it is made of quartz, a sealed tube made of quartz is generally used. In addition, even containers that can be divided, such as separable flasks and bell-shaped containers (pell jars) with removable bottom plates, have a structure that has a vacuum exhaust port and can be sealed at high temperatures. If so, it can be suitably used.

Thus, metallic copper, metallic molybdenum and elemental sulfur (hereinafter referred to as
After charging the raw materials (collectively referred to as raw materials), the sealed quartz container is heated to 500 to 700
℃ and then reacted at this temperature for 6 to 24 hours to obtain a precursor sulfide. 63-14
The heating rate described in No. 5820 is preferred.

In other words, the total amount D (g) of raw materials charged into the quartz container satisfies the relationship of equation 1) below, and the temperature increase rate A ("C
/h) is carried out within the range of formula 2) below.

D≦0.70 −・ −−・−・−・−−i >(0
, 5X B x C) /D≦A≦(1,5xBxC)
/D. d) D: Total charge amount (g) of metallic copper, metallic molybdenum, and elemental sulfur If the total amount D (g) of the raw materials charged into the quartz container is 0.0% of the internal volume C (Id) of the quartz container. If it exceeds 7, there is a very high possibility that the quartz container will burst during heating up to the reaction temperature of the precursor sulfide, so it must be avoided.

Furthermore, even if the total charge ID (g) satisfies formula 1) above, if the heating rate A exceeds the upper limit of the range shown in formula 2> above, the quartz container may burst during temperature rise. This is undesirable because the temperature increase becomes very large and it is dangerous to curl it.On the other hand, if the heating rate A is less than the lower limit of the range shown in equation 2), it takes too long to raise the temperature and it is not practical.

In addition, in the above equation 2), the pressure resistance B (kg/c
d-G) is the maximum stress in the strength calculation of 70kg/c+J-
The value calculated as G (safety factor 3 to 5 times).

The reaction temperature and reaction time are as described above, but within the above range the reaction time varies in relation to the reaction temperature.
When the reaction temperature is low, a long reaction time is required, and when the reaction temperature is high, a relatively short reaction time is sufficient6.Therefore, the reaction time depends on the selected reaction temperature, and when analyzed with an X-ray diffraction device, elemental sulfur can be detected. It is sufficient that the time is longer than the time when it is no longer recognized.

When the reaction is completed, the quartz container is cooled and the contents are taken out, but the cooling rate is not particularly limited and may be cooled slowly or rapidly.

The precursor sulfide thus obtained is taken out from the quartz container and then pulverized and mixed. Although there are no particular limitations on the crushing device, the precursor sulfide is crushed until the particle size of the precursor sulfide becomes smaller than 115 mesh.

Next, the production of copper molybdenum sulfide will be explained.

The pulverized and mixed precursor sulfide obtained above is charged into a quartz container similar to that used for the production of the precursor sulfide, and then processed in exactly the same manner as in the production of the precursor sulfide. After vacuum evacuation, seal.

That is, the quartz container is heated to about 50 to 100° C., evacuated to below I Torr, and then sealed.

The sealed quartz container is heated to 900℃ using a heating device such as an electric furnace.
The temperature was raised to ~1100℃, and at this temperature 24~1
Copper molybdenum sulfide is obtained by reacting for 20 hours. In this case, there is no particular restriction on the rate of temperature rise to the reaction temperature, and the temperature may be raised within a range that does not cause any adverse effects such as distortion or cracking on the quartz container.

The relationship between reaction temperature and reaction time is similar to that in the production of precursor sulfides. Therefore, depending on the reaction temperature selected, the reaction time may be longer than the time required to generate a single Chevrel phase when analyzed with an X-ray diffraction device.

When the reaction is completed, the quartz container is cooled and the contents are taken out, but the cooling rate is not particularly limited and may be cooled slowly or rapidly.

〔Example〕

EXAMPLES Hereinafter, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to these Examples.

Example 1 13°3g of electrolytic copper powder with a purity of 99.7% and a particle size of 50 mesh pass as gold N steel, a purity of 99.9% and a particle size of 50
60.0 g of mesh pass metallic molybdenum powder and 26.1 g of elemental sulfur powder having a purity of 99.9% and a particle size of 50 mesh pass were weighed and mixed. (Molar ratio Cu:Mo:S = 2:6:7.8) The above mixture was charged into a sealed tube with an internal volume of 150 d, which was made from a quartz tube with an outer diameter of 3411 Il and an inner diameter of 28 m5+, as a quartz container, and then, With this sealed tube heated to 60°C using a heater, the air inside the sealed tube is pumped out using a vacuum pump.
It was evacuated to a pressure of Torr or less and melt-sealed.

The pressure resistance B of this sealed tube was 13.4 kg/cd-G, the internal volume C was 150 d, and the total charged amount was 99
．． 4g, the upper limit of the temperature increase rate A in equation 2) is (1,
5x B x C)/D = 30.3, the lower limit is (0,5
x B x C)/D=10.1. Therefore, the temperature increase rate may be 10.1 to 30.3°C/h, and the amount of raw material charged into the sealed tube also satisfies the conditions of formula 1) as shown in Table 1.

This sealed tube was heated to 60°C in an electric furnace at a heating rate of 20°C/h.
The temperature was raised to 0°C, and the reaction was carried out at this temperature for 12 hours to produce a precursor sulfide. After the reaction, the sealed tube was allowed to cool naturally, the contents were taken out, and analyzed with an X-ray diffraction device. No sulfur peak was detected.

Next, this precursor sulfide was ground in a mortar so that the total amount was 115 menshupas.

This pulverized precursor sulfide was charged into a sealed quartz tube that was the same as that used for producing the precursor sulfide, and then this sealed tube was heated to a temperature of 60"C with a heater. ,
The air in the sealed tube was evacuated to a pressure of ITorr or less using a vacuum pump, and the tube was fused and sealed.

This sealed tube was placed in an electric furnace at 100'C/min as shown in Table 2.
The temperature was raised to 1000°C at a heating rate of 24 h, and at this temperature
After 0 hours of reaction, the sealed tube was allowed to cool naturally and the contents were taken out and analyzed using an X-ray diffraction device. As shown in Figure 1, only a single-phase Chevrel-type compound was detected.
It was confirmed to be CuaMobSq,s from the raw material molar ratio.

When this product was sieved using a 115-mesh sieve, it was found that the under-sieve fraction was as fine as 95%. Further, the sieved underfield was also analyzed using an X-ray diffraction device, but only single-phase Chevrel-type compounds were detected in this undersieve.

From the above, it can be seen that the copper molybdenum sulfide produced by the method of the present invention has extremely high purity and is fine.

Comparative Example 1 The electrolytic copper, metal molybdenum, and elemental sulfur powders used in Example 1 were mixed in the same amounts as in Example 1, and this was charged into the same quartz sealed tube as used in Example 1. ,I Tor
The sealed tube was evacuated to a pressure of r or less and melt-sealed in the same manner as in Example 1. After that, this sealed tube was heated at 20℃/h in an electric furnace.
The temperature was raised to 1000"C at a heating rate of Only one-phase Chevrel-type compound was detected. However, when this product was sieved using a 115-mesh sieve, the percentage of undersieve was 38%, which was significantly increased compared to Example 1. As a result of analyzing this undersieve field using an X-ray diffraction device, a peak for molybdenum disulfide was also observed, indicating that a considerable amount of molybdenum disulfide was present.

Comparative Example 2 Copper molybdenum sulfide was produced under the same conditions as Comparative Example 1 except that the reaction time was changed to 48 hours. When the obtained product was sieved using a 115-mesh sieve in the same manner as in Comparative Example 1, the under-sieve ratio was 17%, which was lower than in Comparative Example 1 but significantly increased compared to Example 1. Was.

As a result of analyzing this undersieve field using an X-ray diffraction apparatus in the same manner as in Comparative Example 1, a peak of molybdenum disulfide was also observed, indicating that a considerable amount of molybdenum disulfide was present.

Example 2 Copper molybdenum was produced in exactly the same manner as in Example 1, except that the reaction temperature for obtaining copper molybdenum sulfide from the precursor sulfide was changed to 950'C1 reaction time to 90 hours as shown in Table 2. Sulfide was obtained.

The obtained copper molybdenum sulfide was added to 115 in the same manner as in Example 1.
When sieved with a mesh sieve, the percentage of undersieve was 97%.
It was minute. Furthermore, the undersieve field sieved here was also analyzed using an X-ray diffraction device, and only single-phase Chevrel-type compounds were detected in this undersieve field, and based on the raw material molar ratio, copper molybdenum with the composition shown in Table 2 was detected. The fact that 0 or more sulfides were confirmed indicates that the copper molybdenum sulfide produced by the method of the present invention has extremely high purity and is fine as in Example 1.

Example 3 A sealed tube made of the same quartz tube as that used in Example 1 was used, and the same electrolytic copper as used in Example 1 was added to the sealed tube.
The amounts of metal molybdenum and elemental sulfur powders shown in Table 1 were weighed and mixed.

Thereafter, this mixture was charged into a sealed tube in the same manner as in Example 1, and after this was evacuated under the same conditions as in Example 1, the sealed tube was melt-sealed, heated, reacted, and cooled to form a precursor. Sulfide was obtained.

The heating rate, reaction temperature, and reaction time were as shown in Table 1.

When this precursor sulfide was analyzed using an X-ray diffraction apparatus in the same manner as in Example 1, no peak of elemental sulfur was detected.

Next, in the same manner as in Example 1, this precursor sulfide was mixed with a total of 1115
The pulverized precursor sulfide was pulverized to the particle size of a mesh bath, and the pulverized precursor sulfide was charged into the same quartz tube type sealed tube as above, and after vacuum evacuation in the same manner as in Example 1, the sealed tube was fused and sealed, and the temperature was increased. , reacted and cooled to obtain copper molybdenum sulfide having the composition shown in Table 2. The heating rate, reaction temperature, and reaction time were as shown in Table 2.

The obtained copper molybdenum sulfide was added to 115 in the same manner as in Example 1.
When sifted with a mesh sieve, the percentage of unsifted material was 97%.
It was a fine powder. Furthermore, the sieve material sieved here was also analyzed using an X-ray diffraction device, and since only single-phase Chevrel type compounds were detected in this sieve material, it was found that the sieve material was manufactured by the method of the present invention. It can be seen that the copper molybdenum sulfide has extremely high purity and is fine as in Example 1.

Comparative Example 3 In exactly the same manner as in Example 3, a mixture of electrolytic copper, metal molybdenum, and elemental sulfur powder was charged into a sealed quartz tube, evacuated, and the sealed tube was melt-sealed. Increase heating rate to 30°
The temperature was raised to a temperature of 1000'C at a heating rate of C/h, and the reaction was carried out at this rate for 48 hours.

After the reaction was completed, the sealed tube was allowed to cool naturally and the contents were taken out and analyzed using an X-ray diffraction apparatus, and only a single-phase Chevrel type compound was detected. However, when this product was sieved using a 115-mesh sieve, the proportion of the sieved product was 15%, which was significantly increased compared to Example 3. Furthermore, as a result of analyzing this sieve material with an X-ray diffraction device, a peak of molybdenum disulfide was also observed, indicating that molybdenum disulfide was present.

Example 4 As a quartz container, the inner diameter is 400 mm and the height is 550 IIll.
A Pelger-type quartz container with an internal volume of 651 cm was used.

This quartz container can be sealed using a slotted joint, so that the sulfur gas generated after sealing does not come into contact with metal, and it can be sealed after the air inside the quartz container is evacuated. There is. Also, the calculated pressure resistance of this quartz container is 7.0 kg/c+! -G.

2394 g each of the same electrolytic copper powder, metal molybdenum powder, and elemental sulfur powder as used in Example 1,
After weighing and mixing 10,800 g and 4,698 g, they were placed in a quartz tray, and the quartz tray was placed in the Pelger-type quartz container. (Preparation molar ratio Cu:Mo
:S = 2:6:7.8) Then, while heating the Pelger-type quartz container to a temperature of 60°C using an external heater, the air inside the quartz container is pumped with a vacuum pump. The chamber was evacuated to a pressure below lτorr and then sealed.

Note that the pressure resistance B of this quartz container is 7.0 kg/cd, the internal volume C is 65000 mg, and the amount of raw material charged is 17892 g, so the upper limit to the temperature increase rate in equation 2) is (1.5x B
x C)/D-38,1, the lower limit is (0,5x B x
C)/D = 12.7, and the amount of raw material charged into the quartz container also satisfies the condition of formula l) as shown in Table 1.

This quartz container was heated to 600°C at a heating rate of 20°C/h using a heater, and then reacted at this temperature for 12 hours. After the reaction was completed, the quartz container was allowed to cool naturally to sulfurize the precursor. When the sample was taken out and the precursor sulfide was analyzed using an X-ray diffraction apparatus in the same manner as in Example 1, no peak of elemental sulfur was detected.

Next, in the same manner as in Example 1, this precursor sulfide was mixed with a total of 1115
The pulverized precursor sulfide was pulverized to the particle size of a mesh bath, and the pulverized precursor sulfide was charged again into the above-mentioned quartz container, vacuum evacuated, and the sealed tube was melt-sealed.
The temperature was raised to 1000''C at a heating rate of 'c/h, and the reaction was carried out at this temperature for 24 hours.After the reaction was completed, the copper molybdenum sulfide having the composition shown in Table 2 was cooled by natural cooling. Obtained.

The obtained copper molybdenum sulfide was added to 115 in the same manner as in Example 1.
When sieved using a mesh sieve, the percentage of unsifted products was 96%.
It was minute. Furthermore, the sieve material sieved here was also analyzed using an X-ray diffraction device, and since only single-phase Chevrel-type compounds were detected in this sieve material as well, it was found that the sieve material was manufactured by the method of the present invention. It can be seen that the copper molybdenum sulfide has extremely high purity and is fine as in Example 1.

Table 1 [Effects of the Invention] As explained in detail above, the present invention uses metallic copper, metallic molybdenum, and elemental sulfur as raw materials, heats these raw materials in a sealed quartz container, causes them to react, and produces copper. In a method for producing molybdenum sulfide, raw materials are heated in a sealed quartz container at a temperature of 500 to 700"C for 6 to 24 hours to obtain a precursor sulfide free of unreacted elemental sulfur, and this precursor sulfide is 900-1100° in a resealed quartz container
This is a method of carrying out a heating reaction at a temperature of C for 24 to 120 hours, and by employing the method of the present invention, highly pure and fine copper molybdenum sulfide can be obtained.

In the conventional method of producing copper molybdenum sulfide, it has been investigated whether the produced copper molybdenum sulfide has a homogeneous phase by analyzing it with an X-ray diffraction device, etc., but the particle size and purity have not been determined. Nothing was known about their relationship.

The present inventors clarified the relationship between the particle size and purity of the produced copper molybdenum sulfide, and also found a method to reduce the particle size, and thereby succeeded in obtaining highly pure and fine copper molybdenum sulfide. .

When copper molybdenum sulfide is used as an electrode material for a secondary battery, it is extremely important that it be highly pure and fine, and the effects of the present invention are extremely significant.

Furthermore, in carrying out the present invention, the rate of temperature rise described in Japanese Patent Application No. 145820/1988, previously filed by the present inventors, should be adopted for raising the temperature up to the reaction temperature when obtaining the precursor sulfide. For example, copper molybdenum sulfide can be produced safely and efficiently without the conventional problem of sealing tubes often bursting during temperature rise, which is very dangerous and hinders productivity.

[Brief explanation of the drawing]

FIG. 1 is an X-ray diffraction diagram of the copper molybdenum sulfide of the present invention obtained in Example 1. Patent applicant Mitsui Toatsu Chemical Co., Ltd.

Claims (1)

[Claims] (1) Metallic copper, metallic molybdenum, and elemental sulfur are charged into a quartz container and evacuated, and then the quartz container is heated in a sealed state so that the compound formula Cu_xMo_6S_8_-_y(
However, in producing copper molybdenum sulfide represented by The quartz container was heated at a temperature of 500 to 700°C.
Heating for ~24 hours to obtain a precursor sulfide free of unreacted elemental sulfur, then taking out the precursor sulfide from the quartz container, pulverizing and mixing, and charging the pulverized and mixed precursor sulfide into the quartz container again. After vacuum evacuation, the quartz container was sealed and heated to 90°C.
A method for producing copper molybdenum sulfide, which comprises carrying out a heating reaction at a temperature of 0 to 1100°C for 24 to 120 hours.