WO2025109872A1 - 二硫化モリブデン微粒子の製造方法 - Google Patents

二硫化モリブデン微粒子の製造方法 Download PDF

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WO2025109872A1
WO2025109872A1 PCT/JP2024/035059 JP2024035059W WO2025109872A1 WO 2025109872 A1 WO2025109872 A1 WO 2025109872A1 JP 2024035059 W JP2024035059 W JP 2024035059W WO 2025109872 A1 WO2025109872 A1 WO 2025109872A1
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molybdenum disulfide
molybdenum
sulfur
molybdenum trioxide
trioxide
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French (fr)
Japanese (ja)
Inventor
秀之 村田
滉生 平林
直人 矢木
建軍 袁
彰志 今村
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DIC Corp
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DIC Corp
Dainippon Ink and Chemicals Co Ltd
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Priority to JP2025559070A priority Critical patent/JP7846470B2/ja
Priority to CN202480053711.7A priority patent/CN121773074A/zh
Publication of WO2025109872A1 publication Critical patent/WO2025109872A1/ja
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides

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  • the present invention relates to a method for producing fine molybdenum disulfide particles.
  • Molybdenum sulfide is known as a lubricant for reducing friction and wear, mainly in the automotive industry, and is used in various countries, particularly as a liquid lubricant for engine oil, etc.
  • Molybdenum sulfide represented by molybdenum disulfide (MoS 2 )
  • MoS 2 molybdenum disulfide
  • a method is known in which molybdenum trioxide powder, which consists of fine particles of molybdenum trioxide, is heated at a temperature of 200 to 1000°C in the presence of a sulfur source to produce molybdenum disulfide powder (see Patent Document 4).
  • molybdenum trioxide absorbs electromagnetic waves well and its temperature rises quickly, while sulfur has poor electromagnetic wave absorption, and therefore sulfur itself is not easily heated by electromagnetic wave irradiation. Therefore, when molybdenum trioxide and sulfur are mixed and irradiated with electromagnetic waves, molybdenum trioxide is heated preferentially and its reaction activity is increased. Some of the high-temperature molybdenum trioxide with increased reaction activity reacts with the surrounding sulfur and is immediately converted to molybdenum disulfide.
  • This heating by electromagnetic wave irradiation activates the reaction of molybdenum trioxide and suppresses the evaporation and distillation of sulfur, making it possible to efficiently produce molybdenum disulfide microparticles with low energy consumption and high conversion rate. That is, in this embodiment, heating by electromagnetic wave irradiation is easy to control ON/OFF and irradiation intensity, and selective heating to molybdenum trioxide is possible without heating the atmosphere. Therefore, the objective is to provide a method for producing molybdenum disulfide that can efficiently produce molybdenum disulfide fine particles with a high conversion rate even with low energy consumption.
  • a method for producing a molybdenum trioxide comprising the steps of: irradiating molybdenum trioxide with electromagnetic waves in the presence of sulfur to heat the molybdenum trioxide; and reacting the heated molybdenum trioxide with the sulfur;
  • [3] The method for producing molybdenum disulfide microparticles according to [1] or [2], wherein the average particle size of the molybdenum disulfide microparticles is 10 nm to 10 ⁇ m.
  • [4] The method for producing molybdenum disulfide fine particles according to any one of [1] to [3], wherein the molybdenum disulfide fine particles have a BET specific surface area of 0.01 m 2 /g to 500 m 2 /g.
  • [5] The method for producing molybdenum disulfide fine particles according to any one of [1] to [4], wherein the molybdenum disulfide fine particles contain a 2H crystal structure.
  • [6] The method for producing molybdenum disulfide fine particles according to any one of [1] to [5], wherein the molybdenum disulfide fine particles contain a 3R crystal structure.
  • [7] The method for producing molybdenum disulfide fine particles according to any one of [1] to [6], wherein the average particle size of the molybdenum trioxide is 10 ⁇ m or less.
  • [8] The method for producing molybdenum disulfide fine particles according to any one of [1] to [7], wherein the molybdenum trioxide has a BET specific surface area of 0.1 m 2 /g or more.
  • a method for producing molybdenum disulfide microparticles can be provided that can efficiently produce molybdenum disulfide microparticles with low energy consumption and high conversion rate.
  • FIG. 1 is a schematic diagram of an example of an apparatus used for producing molybdenum disulfide fine particles according to one embodiment of the present invention.
  • a method for producing molybdenum disulfide fine particles includes a step of heating molybdenum trioxide by irradiating the molybdenum trioxide with electromagnetic waves in the presence of sulfur, and reacting the heated molybdenum trioxide with the sulfur.
  • the frequency of the electromagnetic waves is in the range of 300 to 30,000 MHz.
  • the frequency of the electromagnetic waves is preferably in the range of 900 to 2,450 MHz.
  • the method for producing molybdenum disulfide fine particles of the present embodiment may involve mixing molybdenum trioxide and sulfur, and irradiating the mixture with electromagnetic waves to react the heated molybdenum trioxide with the sulfur.
  • the reaction between the molybdenum trioxide and the sulfur is preferably carried out, for example, according to the reaction formula shown in the following formula (1). This is because the sulfide is released from the reaction system, and only molybdenum disulfide remains in the system as a product, and the sulfide can be easily captured with an alkali or the like without being released into the atmosphere.
  • the method for producing molybdenum disulfide microparticles according to this embodiment can be suitably carried out, for example, using the molybdenum disulfide microparticle production apparatus 10 shown in FIG. 1.
  • FIG. 1 is a schematic diagram of an example of an apparatus used to manufacture molybdenum disulfide microparticles according to this embodiment.
  • An apparatus capable of irradiating electromagnetic waves (sometimes referred to as an "electromagnetic wave irradiating apparatus"; not shown) is disposed above the chamber 1.
  • the molybdenum disulfide microparticle manufacturing apparatus 10 has a chamber 1 in which electromagnetic waves generated by the electromagnetic wave irradiating apparatus are irradiated to a mixture of the molybdenum trioxide and sulfur placed in a container 2 to heat the molybdenum trioxide (hereinafter sometimes referred to as "electromagnetic wave heating") and react the heated molybdenum trioxide with sulfur.
  • the chamber 1 has an outside air intake 6 disposed at the left end and an exhaust 8 disposed at the right end.
  • An exhaust device (not shown), which is a blowing means, is connected to the intake 6.
  • the molybdenum disulfide microparticle manufacturing apparatus 10 may have an external cooling device (not shown), which allows the reaction conditions in the chamber 1 to be controlled as desired.
  • the product obtained by the method for producing molybdenum disulfide fine particles of this embodiment is fine particles composed of molybdenum disulfide (MoS 2 ). It has a certain preferred average particle size range described below.
  • the molybdenum disulfide fine particles according to the production method of this embodiment may contain molybdenum sulfides other than molybdenum disulfide (MoS 2 ).
  • the obtained fine particles of molybdenum disulfide may also contain a certain amount of other molybdenum sulfides.
  • Atoms other than molybdenum atoms and sulfur atoms may be included in molybdenum disulfide to the extent that the effects of this embodiment are not impaired.
  • Specific examples include silicon, aluminum, sodium, iron, titanium, potassium, calcium, yttrium, etc. These other atoms may be included alone or in a mixture of two or more.
  • the content of other atoms in molybdenum disulfide is preferably 10 mol % or less, more preferably 5 mol % or less, and most preferably 2 mol % or less.
  • the molybdenum disulfide microparticles obtained by the manufacturing method of this embodiment can be used appropriately based on the surface and internal structures depending on the purpose for which they are used. For example, when they are used as a catalyst themselves, it is effective to increase the contact area with the molecules of the reaction raw materials as much as possible in order to more effectively proceed with the intended chemical reaction.
  • molybdenum disulfide having a structure with a pore entrance facing the inside of the surface on the surface and independent pores and/or pores communicating with other surfaces inside, such as a porous structure can exhibit catalytic activity compared to that of a medium-dense structure.
  • the size and number of pores inside the hexahedron of molybdenum sulfide can be measured by a known and commonly used method as appropriate, corresponding to each of micropores, mesopores, and macropores.
  • Japanese Industrial Standards (JIS) Z8831 and Japanese Industrial Standards (JIS) Z8830 can be mentioned as measurement methods.
  • JIS Z8831 is a method for measuring the pore size distribution and pore characteristics of powders (solids) using the mercury intrusion method, with respect to pore distribution and pore volume, mainly focusing on mesopores and macropores.
  • Japanese Industrial Standard (JIS) Z8830 is a method for measuring the BET specific surface area using the nitrogen gas adsorption method, with respect to the surface size inside pores, mainly focusing on micropores. Of course, these can be combined for measurement if necessary.
  • the specific surface area of the molybdenum disulfide fine particles of this embodiment is preferably 0.01 m 2 /g to 500 m 2 /g. It is more preferably 1 m 2 /g or more, more preferably 10 m 2 /g or more, and even more preferably 20 m 2 /g or more. It may be 500 m 2 /g or less, 200 m 2 /g or less, or 100 m 2 /g or less. It is most preferably 20 to 200 m 2 /g.
  • the average particle diameter of the molybdenum disulfide microparticles of this embodiment is preferably 10 nm to 100 ⁇ m.
  • the average particle diameter of the molybdenum disulfide microparticles of this embodiment can be measured, for example, by a known particle size distribution measurement method.
  • the average particle diameter of the molybdenum disulfide microparticles of this embodiment is more preferably 10 nm or more, more preferably 20 nm or more, and even more preferably 50 nm or more. It may also be 100 ⁇ m or less, 10 ⁇ m or less, or 1 ⁇ m or less.
  • the molybdenum disulfide fine particles according to this embodiment preferably contain a 2H crystal structure.
  • the "2H crystal structure” is a hexagonal crystal structure, which is the most stable crystal structure of molybdenum disulfide. The inclusion of the 2H crystal structure has the effect of improving the stability of the structure.
  • molybdenum disulfide fine particles containing a 2H crystal structure can be produced efficiently.
  • the "2H crystal structure” can be confirmed by a conventional XRD (X-ray diffraction) method.
  • the molybdenum disulfide fine particles may include a 3R crystal structure.
  • the "3R crystal structure” is a rhombohedral crystal with a three-layer unit cell. The inclusion of the 3R crystal structure provides excellent catalytic effects.
  • molybdenum disulfide fine particles containing a 3R crystal structure can be produced efficiently.
  • the "3R crystal structure” can be confirmed by a conventional XRD (X-ray diffraction) method.
  • the molybdenum trioxide used in the method for producing molybdenum disulfide microparticles of this embodiment may be used alone or in combination with other molybdenum oxides such as molybdenum dioxide.
  • the sulfur may be used alone or in combination with a sulfur compound other than sulfur, such as hydrogen sulfide. Sulfur may also be used in the reaction as a solid, or may be used in the form of a liquid or gas at high temperatures.
  • Molybdenum trioxide may be used in the reaction as a solid, or may be used in the form of a liquid or gas at high temperatures.
  • molybdenum disulfide can be obtained quantitatively in accordance with the stoichiometry, and high-purity molybdenum disulfide can be obtained with a smaller content of by-products.
  • inorganic fillers such as alumina, spinel, and other metal composite oxides, and gemstones such as ruby, sapphire, and red spinel
  • gas mainly composed of molybdenum trioxide evaporates from the reaction system during the process.
  • this vapor can be recovered and reused in the production of molybdenum disulfide microparticles of this embodiment, either as gas or liquid, or as solidified by cooling as necessary.
  • the above-mentioned inorganic fillers and gemstones can be produced in parallel with molybdenum disulfide, which is useful as a catalyst, for example.
  • molybdenum disulfide which is useful as a catalyst, for example.
  • there is no need for equipment for recovering molybdenum trioxide which is required for the production of only the former.
  • the productivity of both can be significantly increased while suppressing the environmental load, equipment costs, and installation space.
  • the molybdenum trioxide used in the production of the molybdenum disulfide microparticles of this embodiment may have any properties, but when used as a solid raw material in the above reaction, the average particle size of the molybdenum trioxide is preferably 10 ⁇ m or less.
  • the average primary particle size of 50 molybdenum trioxide particles in the field of view of a two-dimensional image of a transmission electron microscope (TEM) photograph is more preferably 5 to 5000 nm, and more preferably 5 to 1000 nm.
  • the magnification of the TEM may be such that at least 50 molybdenum trioxide particles are included in one field of view in visual observation or image photography, but it is preferable to select an appropriate magnification from the range of 1000 to 200000 times based on the average range of vertical (length) x horizontal (width) x thickness described later.
  • a SEM may be used instead of the TEM.
  • the molybdenum trioxide preferably has a BET specific surface area of 0.1 m 2 /g or more.
  • molybdenum trioxide having the above-mentioned specific average primary particle diameter range Any of the publicly known and commonly used commercial products can be used as molybdenum trioxide having the above-mentioned specific average primary particle diameter range. Furthermore, molybdenum trioxide powder having the above-mentioned specific average primary particle diameter range can be easily obtained from molybdenum trioxide having a larger average primary particle diameter.
  • molybdenum trioxide which is a relatively inexpensive, commercially available, room temperature solid having a larger average primary particle diameter
  • molybdenum trioxide gas by heating and vaporizing molybdenum trioxide, which is a relatively inexpensive, commercially available, room temperature solid having a larger average primary particle diameter, and then rapidly cooling the resulting molybdenum trioxide gas, it is possible to easily obtain molybdenum trioxide powder having the above-mentioned specific average primary particle diameter range and which is an excellent raw material for obtaining molybdenum disulfide of this embodiment.
  • the above-mentioned powder of molybdenum trioxide which is a suitable raw material, can be obtained by contacting the molecular molybdenum trioxide gas with a large amount of refrigerant that is in large excess compared to the amount of the molybdenum trioxide gas, and cooling it.
  • This principle itself is well known, and can be realized with known, conventional equipment. If the amount of molybdenum trioxide gas is very small, the molybdenum trioxide gas is diluted by the refrigerant by contacting it with a large excess of the refrigerant, and the molybdenum trioxide is cooled in an extremely short time with a phase change from gas to solid.
  • Cooling can be performed by introducing a large amount of refrigerant into the system from the outside (outside the system) all at once, or by dividing a large amount of refrigerant, intermittently or continuously.
  • the frequency of the electromagnetic waves used in the method for producing molybdenum disulfide microparticles of the present embodiment is in the range of 300 to 30,000 MHz.
  • the frequency of the electromagnetic waves is preferably in the range of 900 to 3,000 MHz.
  • the electromagnetic waves according to this embodiment can be, for example, an electromagnetic wave generator used in a known electromagnetic wave heating device.
  • the electromagnetic wave generator may include, for example, a mechanism for ventilating a purge gas or the like, a sensor for measuring the temperature inside the furnace, and an exhaust pump for evacuating the inside of the furnace.
  • Examples of commercially available electromagnetic wave generators include MRK-3050 manufactured by Kyoei Electric Furnace Manufacturing Co., Ltd. and microwave heating device AMU-RUSH manufactured by Motoyama Corporation.
  • the method for producing molybdenum disulfide microparticles of the present embodiment may involve using an electromagnetic wave heating device to irradiate molybdenum trioxide with electromagnetic waves, thereby heating the molybdenum trioxide and reacting the heated molybdenum trioxide with sulfur.
  • the electromagnetic wave heating device may include an electromagnetic wave generator and a reaction section, in which molybdenum trioxide and sulfur as raw materials may be placed.
  • the intensity of the electromagnetic waves to be irradiated can be appropriately selected according to the form, composition (mixture ratio of molybdenum trioxide and sulfur), weight, arrangement, installation location, etc. of the raw material to be irradiated.
  • the intensity of the electromagnetic waves to be irradiated can be adjusted, for example, by the temperature of the raw material to be irradiated.
  • the (surface or internal) temperature of the raw material (sometimes referred to as the electromagnetic wave heating temperature) can be measured while the electromagnetic waves are being irradiated.
  • duration of the electromagnetic wave there are no particular limitations on the duration of the electromagnetic wave, so long as the time is sufficient to supply the heating energy required for the reaction; for example, it can be 10 minutes or more, 10 minutes to 10 hours, 20 minutes to 5 hours, or 30 minutes to 3 hours.
  • the electromagnetic waves may be irradiated continuously for a fixed period of time, or may be irradiated intermittently by turning on and off.
  • the intensity of the electromagnetic waves may be constant, or the electromagnetic heating temperature may be changed at a constant rate.
  • the manufacturing method of this embodiment is characterized by the ability to control the ON/OFF setting, compared to conventional heating methods using electric furnaces, etc.
  • the reaction between molybdenum trioxide and sulfur can be carried out by determining the molar ratio of each component stoichiometrically according to the reaction formula (1) above.
  • the sulfur/molybdenum trioxide (molar ratio) is in the range of 3.0 to 10.
  • the production method of this embodiment uses the above-mentioned electromagnetic heating, it is possible to suppress the presence of unreacted molybdenum trioxide even with a smaller blend amount of sulfur than when conventional electric furnace heating is used, as proven by a comparison between the Examples and Comparative Examples described later.
  • the reaction between molybdenum trioxide and sulfur can be carried out, for example, by uniformly mixing the two in advance to obtain a powder, and heating the powder by irradiating it with electromagnetic waves at a temperature of 200 to 1000° C.
  • the electromagnetic wave irradiation (heating) time can be selected, for example, from the range of 2 to 10 hours.
  • the reaction is preferably carried out at a temperature of 300 to 600° C. for an electromagnetic wave irradiation (heating) time of 2 to 7 hours.
  • the above-mentioned electromagnetic wave irradiation (heating) can be performed according to any electromagnetic wave irradiation (heating) profile.
  • the temperature may be increased at a constant rate from room temperature and maintained at a constant temperature within the above-mentioned heating temperature range for a certain period of time, or the heating temperature may be changed by increasing or decreasing the temperature stepwise within the above-mentioned temperature range and each temperature may be maintained for a certain period of time. Heating is preferably performed for a time until the amount of molybdenum disulfide produced does not increase and the amount produced does not change (it becomes saturated).
  • the extent to which molybdenum disulfide microparticles containing molybdenum disulfide are produced based on the above-mentioned reaction can be determined by quantifying molybdenum disulfide.
  • One method for quantifying molybdenum disulfide is to fix conditions other than time in a given heating profile, sample the product at each heating time, and quantify molybdenum disulfide using inductively coupled plasma (ICP) atomic emission spectrometry for the cooled product. In this way, if the relationship between time and molybdenum disulfide is understood, the reaction end point can be determined based only on the heating time when implementing the manufacturing method of this embodiment industrially.
  • ICP inductively coupled plasma
  • the above reaction can be carried out while ventilating. Specifically, the reaction can be carried out while ventilating a heat-resistant container with an inert gas such as helium or argon, or nitrogen or air.
  • an inert gas such as helium or argon, or nitrogen or air.
  • the electromagnetic wave irradiation (heating) conditions may be within the above-mentioned range.
  • the electromagnetic wave irradiation (heating) rate, ON/OFF control, etc. it is possible to suppress the reaction with molybdenum trioxide from being sufficiently carried out and the remaining of more unreacted molybdenum trioxide. If the electromagnetic wave irradiation (heating) rate, ON/OFF control, etc. are not appropriately selected, the temperature rise rate is slow and sulfur volatilizes out of the system before the reaction.
  • Examples of the method of measuring the temperature of the mixture include a method of measuring the temperature by inserting a thermocouple into the mixture, and a method of measuring the temperature of the mixture by thermography.
  • the temperature of the mixture can be measured by the above-mentioned temperature measurement method, and the ON/OFF or irradiation intensity of the electromagnetic wave irradiation can be controlled so as to maintain the temperature.
  • MoS2 Conversion Rate In the method for producing molybdenum disulfide microparticles according to the present embodiment, as described above, the reaction is stoichiometrically carried out according to the reaction formula (1) above. Therefore, when the molar ratio of molybdenum trioxide and sulfur is within a range in which sulfur is in excess, the presence of unreacted molybdenum trioxide can be suppressed. This can be evaluated by checking the conversion rate of MoS2 .
  • MoS2 conversion rate (unit %) refers to the number of moles of molybdenum disulfide contained in the generated molybdenum disulfide fine particles per 100 moles of molybdenum trioxide blended as a raw material.
  • the conversion rate of MoS2 is 80%.
  • the conversion rate of MoS2 in the produced molybdenum disulfide fine particles is related to the molar ratio of molybdenum trioxide and sulfur.
  • the conversion rate of MoS2 is high.
  • the method for producing molybdenum disulfide fine particles of this embodiment can directly heat only molybdenum trioxide using electromagnetic waves. Therefore, compared to the conventional electric furnace heating method, even if the molar ratio of molybdenum trioxide and sulfur charged is the same, a high conversion rate of MoS2 can be obtained. In addition, since the conversion rate of MoS2 is high, the excess amount of sulfur in the production method of this embodiment may be lower than that in the conventional electric furnace heating method. The method for evaluating the MoS2 conversion rate will be described in detail in the Examples.
  • the conversion rate R C of molybdenum disulfide particles to MoS 2 can be obtained by the RIR (reference intensity ratio) method from profile data obtained by measuring molybdenum disulfide particles by X-ray diffraction (XRD).
  • the conversion rate R C to MoS 2 can be obtained from the following formula (2).
  • K A is the RIR value of molybdenum disulfide (MoS 2 );
  • K B is the RIR value of each molybdenum oxide (the raw material MoO 3 and the reaction intermediates Mo 9 O 25 , Mo 4 O 11 , MoO 2 , etc.),
  • IB is the integrated intensity of the strongest peak of each molybdenum oxide (the raw material MoO 3 , and the reaction intermediates Mo 9 O 25 , Mo 4 O 11 , MoO 2 , etc.).
  • the RIR value can be any value listed in the Inorganic Crystal Structure Database (ICSD) (manufactured by the Japan Chemical Information
  • Example 1 1.00 g of molybdenum trioxide (manufactured by Taiyo Koko Co., Ltd., 5 ⁇ m) and 1.57 g of sulfur (manufactured by Kanto Chemical Co., Ltd.) were mixed with a stirring rod. The mixed raw material was then placed in an alumina crucible. The mixture was then placed in a stainless steel chamber equipped with an electromagnetic wave irradiation port, a gas inlet, and a gas exhaust port. Nitrogen was then supplied to the chamber at a flow rate of 0.5 L per minute using a nitrogen gas cylinder, and the chamber was completely replaced with nitrogen.
  • an electromagnetic wave having a frequency of 2450 MHz was irradiated from the electromagnetic wave irradiation port at the top of the chamber with an intensity of 100 W to the mixed raw material in the crucible, and the mixed raw material was heated until the temperature of the mixed raw material reached 450°C.
  • the temperature of the mixed raw material was observed non-contact from the electromagnetic field irradiation port using a radiation thermometer.
  • the irradiation intensity of the electromagnetic wave was adjusted so as to maintain 450°C.
  • the electromagnetic wave irradiation was stopped, and after waiting until the internal temperature of the crucible reached 50° C.
  • Example 2 Synthesis of molybdenum sulfide fine particles was carried out in the same manner as in Example 1, except that the molybdenum trioxide obtained in Synthesis Example 1 was used. XRD measurement showed a characteristic peak derived from MoS2 , confirming the formation of MoS2 fine particles. It was confirmed that the conversion rate of MoS2 was 80% or more.
  • Example 1 and Example 2 a higher conversion rate of MoS2 was obtained compared to Comparative Example 1.
  • Example 1 and Example 2 since electromagnetic wave heating was used, molybdenum trioxide absorbed electromagnetic waves (microwaves) well and the temperature rose quickly.
  • sulfur has poor electromagnetic wave absorption, so sulfur itself is not easily heated even by electromagnetic wave irradiation. Therefore, the vaporization of sulfur is suppressed.
  • molybdenum trioxide and sulfur were mixed and irradiated with electromagnetic waves, molybdenum trioxide was heated preferentially and its reaction activity was increased.
  • Example 2 the fine particles of molybdenum trioxide obtained in Synthesis Example 1 were used, and thus the reaction efficiency with sulfur was further increased compared to Example 1. As a result, a higher conversion rate of MoS2 was obtained in Example 2 than in Example 1.

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WO2019181723A1 (ja) * 2018-03-19 2019-09-26 Dic株式会社 モリブデン硫化物、その製造方法及び水素発生触媒
JP6614471B1 (ja) 2018-03-19 2019-12-04 Dic株式会社 モリブデン硫化物、その製造方法及び水素発生触媒
WO2021059325A1 (ja) * 2019-09-24 2021-04-01 Dic株式会社 硫化モリブデン粉体及びその製造方法
JP7060170B2 (ja) 2019-09-24 2022-04-26 Dic株式会社 硫化モリブデン粉体及びその製造方法、重金属吸着剤、光熱変換材料、蒸留方法、酸素還元触媒、並びに触媒インク

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