CN102616855A - Method for preparing nanometer molybdenum disulfide by aid of microemulsion system - Google Patents
Method for preparing nanometer molybdenum disulfide by aid of microemulsion system Download PDFInfo
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- CN102616855A CN102616855A CN2012100975182A CN201210097518A CN102616855A CN 102616855 A CN102616855 A CN 102616855A CN 2012100975182 A CN2012100975182 A CN 2012100975182A CN 201210097518 A CN201210097518 A CN 201210097518A CN 102616855 A CN102616855 A CN 102616855A
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Abstract
The invention provides a method for preparing nanometer molybdenum disulfide by the aid of a microemulsion system. The method includes steps of chemically reducing hexamolybdate, then adding sulfide into the hexamolybdate to perform sulfidation reaction so as to generate thiomolybdate sulfite; adding the thiomolybdate sulfite into TritonX100, isoamyl alcohol, normal heptane and secondary deionized water to form microemulsion a; adding hydrochloric acid into TritonX100, soamyl alcohol, normal heptane and secondary deionized water to form microemulsion b; adding the microemulsion b into the microemulsion a; fast mixing and stirring; leading acid sinking reaction to be thorough to obtain a product; and obtaining the nanometer molybdenum disulfide after the product is separated centrifugally, washed and dried in a vacuum manner. The preparation method is simple, reaction conditions are easy to be controlled, stability is good, generated particles are uniform, appearances are neat, and the nanometer molybdenum disulfide is expectably prepared on a large scale.
Description
Technical field
The invention belongs to molybdenum is the inorganic nano material preparing technical field, is specifically related to a kind of method that adopts microemulsion system to prepare nano molybdenum disulfide.
Background technology
Nano molybdenum disulfide is because specific surface area is big, high adsorption capacity, and advantage such as reactive behavior is high, and catalytic performance is strong has a wide range of applications in fields such as catalysis, Chu Qing, lubricated, semi-conductor and electrode materialss.The nano molybdenum disulfide preparation method who has reported at present generally can be divided into chemical method, physics method and materialization synthetic method; If the state according to the preparation system is different, can also be divided into solid phase method, liquid phase method and vapor phase process.Chemical method is to prepare MoS through chemical reaction
2, and in the preparation process, reach the purpose that reduces particle diameter through the control reaction conditions, divide according to reaction type mainly to comprise reduction method, decomposition method, oxidation style and electrochemical process etc.The physics method is to MoS by means such as mechanical mill, high energy physics
2Thereby pulverize, cut or spray the purpose that reaches refinement or obtain coating.The short decomposition method of high energy physics means also is preparation nanometer MoS
2Effective ways, this method is in the chemical preparation process, to obtain nanoparticle by high energy physics means such as gamma-rays, UW, is the physics method and the combining of chemical method.At existing nano molybdenum disulfide preparing technical field, though chemical precipitation method can be prepared the less nano molybdenum disulfide of particle diameter, particles dispersed property is relatively poor, and can't definitely control the size of particle diameter; Though mechanical milling method is simple to operate, the product particle diameter is bigger; The extreme condition synthesis method can be prepared the molybdenumdisulphide of different shapes and size, but high to equipment requirements.
Microemulsion method is produced nanoparticle and is had that easy control of reaction, granularity are little, uniform particles, particle diameter are controlled, particle is difficult for advantages such as reunion, can more accurately control the particle diameter and the pattern of institute's synthetic nanoparticle, is nano material synthetic ecotopia.The existing nano metal powders such as successfully synthesizing nano-silver powder, nanometer bronze, Pt, Bi, Pb in the microemulsion system, nano level calcium phosphate, Ba of being reported in
0.7Sr
0.3TiO
3Nano metal compounds such as nanotube, and Au/Fe, Au/Ag, CeO
2/ CeLnO
x, SiO
2/ TiO
2In the inorganic composite nano powder.
Up to the present, yet there are no the report that utilizes microemulsion system to prepare nano molybdenum disulfide.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art, the object of the present invention is to provide a kind of method that adopts microemulsion system to prepare nano molybdenum disulfide, have simple efficient, good stability, uniform particles, the controlled characteristics of particle diameter.
To achieve these goals, the technical scheme of the present invention's employing is:
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide comprises the steps:
Step 1; In concentration is to add reductive agent in the molybdate solution of 0.03～0.05mo l/L it is reduced to the inferior molybdate of tetravalence; Molybdate is 1: 1～1: 1.3 with the ratio of reductive agent amount of substance, and temperature of reaction is 65 ℃～75 ℃, reaction times 75min～85min;
Step 2 is added sulfide and is made its sulfuration in step 1 gained solution, the ratio of the amount of substance of molybdate is 3: 1～4: 1 in sulfide and the step 1, and temperature of reaction is 75 ℃～85 ℃, reaction times 90min～100min;
Step 3 is configured to microemulsion a with TritonX100, primary isoamyl alcohol, normal heptane, above-mentioned steps two gained solution and secondary deionized water; Hydrochloric acid and secondary deionized water with TritonX100, primary isoamyl alcohol, normal heptane, 1mol/L are configured to microemulsion b; Then microemulsion b is all joined microemulsion a; Under 40 ℃～60 ℃, carry out the heavy reaction of acid; Reaction times 55min～65min finally obtains nano molybdenum disulfide after centrifugal, washing, vacuum-drying;
Wherein, The concrete steps of said configuration microemulsion a are: under the normal temperature; TritonX100 and primary isoamyl alcohol are pressed mass ratio mixing in 1: 1, and then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution, slowly splashes into step 2 gained solution and secondary deionized water; Guarantee that the molybdate starting point concentration is 0.03～0.05mol/L; The mol ratio of water and TritonX100 is 25～30 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends;
The concrete steps of said configuration microemulsion b are: under the normal temperature; Is mixing in 1: 1 with TritonX100 and primary isoamyl alcohol by mass ratio; And then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution; Slowly splash into hydrochloric acid and the secondary deionized water of 1mol/L, adding the acid amount is 2: 1～2.5: 1 with the molybdate mol ratio, and the mol ratio of water and tensio-active agent is 25～30 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end by muddiness.
Compared with prior art, the present invention has simple efficient, good stability, uniform particles, the controlled characteristics of particle diameter.
Description of drawings
Fig. 1 is the process flow sheet that the inventive method prepares nano molybdenum disulfide.
Fig. 2 is nano molybdenum disulfide X-ray diffraction (XRD) spectrogram that makes with the inventive method.
Fig. 3 is nano molybdenum disulfide field emission scanning electron microscope (SEM) photo that makes with the inventive method.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is explained further details.
Embodiment one
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide comprises the steps:
Step 1 is to add oxalic acid in the sodium molybdate solution of 0.05mol/L it is reduced to the inferior Sodium orthomolybdate of tetravalence in concentration, and Sodium orthomolybdate is 1: 1 with the ratio of oxalic acid amount of substance, and temperature of reaction is 65 ℃, reaction times 75min;
Step 2 is added sodium sulphite and is made its sulfuration in step 1 gained solution, the ratio of the amount of substance of Sodium orthomolybdate is 3: 1 in sodium sulphite and the step 1, and temperature of reaction is 75 ℃, reaction times 90min;
Step 3 is configured to microemulsion a with TritonX100, primary isoamyl alcohol, normal heptane, above-mentioned steps two gained solution and secondary deionized water; Hydrochloric acid and secondary deionized water with TritonX100, primary isoamyl alcohol, normal heptane, 1mol/L are configured to microemulsion b; Then microemulsion b is all joined microemulsion a; Under 60 ℃, carry out the heavy reaction of acid; Reaction times 55min washs the heavy precipitated product that reacts of said acid respectively more than three times with ethanol, acetone and deionized water; Finally after centrifugal, washing, vacuum-drying, obtain nano molybdenum disulfide:
Wherein, the concrete steps of said configuration microemulsion a are: under the normal temperature, TritonX100 and primary isoamyl alcohol are pressed mass ratio mixing in 1: 1; And then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution; Slowly splash into step 2 gained solution and secondary deionized water, guarantee that the Sodium orthomolybdate starting point concentration is 0.05mol/L, the mol ratio of water and TritonX100 is 25 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end by muddiness;
The concrete steps of said configuration microemulsion b are: under the normal temperature; Is mixing in 1: 1 with TritonX100 and primary isoamyl alcohol by mass ratio, and then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution, slowly splashes into hydrochloric acid and the secondary deionized water of 1mol/L; Adding the acid amount is 2.3: 1 with the Sodium orthomolybdate mol ratio; The mol ratio of water and tensio-active agent is 25 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends.
Embodiment two
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide comprises the steps:
Step 1 is to add oxammonium hydrochloride in the Potassium orthomolybdate solution of 0.03mol/L it is reduced to the inferior Potassium orthomolybdate of tetravalence in concentration, and Potassium orthomolybdate is 1: 1.3 with the ratio of oxammonium hydrochloride amount of substance, and temperature of reaction is 75 ℃, reaction times 85min;
Step 2 is added potassium sulphide and is made its sulfuration in step 1 gained solution, the ratio of the amount of substance of Potassium orthomolybdate is 4: 1 in potassium sulphide and the step 1, and temperature of reaction is 85 ℃, reaction times 100min;
Step 3 is configured to microemulsion a with TritonX100, primary isoamyl alcohol, normal heptane, above-mentioned steps two gained solution and secondary deionized water; Hydrochloric acid and secondary deionized water with TritonX100, primary isoamyl alcohol, normal heptane, 1mol/L are configured to microemulsion b; Then microemulsion b is all joined microemulsion a; Under 40 ℃, carry out the heavy reaction of acid; Reaction times 65min washs the heavy precipitated product that reacts of said acid respectively more than three times with ethanol, acetone and deionized water; Finally after centrifugal, washing, vacuum-drying, obtain nano molybdenum disulfide:
Wherein, the concrete steps of said configuration microemulsion a are: under the normal temperature, TritonX100 and primary isoamyl alcohol are pressed mass ratio mixing in 1: 1; And then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution; Slowly splash into step 2 gained solution and secondary deionized water, guarantee that the Potassium orthomolybdate starting point concentration is 0.03mol/L, the mol ratio of water and TritonX100 is 30 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end by muddiness;
The concrete steps of said configuration microemulsion b are: under the normal temperature; Is mixing in 1: 1 with TritonX100 and primary isoamyl alcohol by mass ratio, and then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution, slowly splashes into hydrochloric acid and the secondary deionized water of 1mol/L; Adding the acid amount is 2.5: 1 with the Potassium orthomolybdate mol ratio; The mol ratio of water and tensio-active agent is 30 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends.
Embodiment three
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide comprises the steps:
Step 1 is to add oxammonium hydrochloride in the ammonium molybdate solution of 0.04mol/L it is reduced to the inferior ammonium molybdate of tetravalence in concentration, and ammonium molybdate is 1: 1.2 with the ratio of oxammonium hydrochloride amount of substance, and temperature of reaction is 70 ℃, reaction times 80min;
Step 2 is added sodium sulphite and is made its sulfuration in step 1 gained solution, the ratio of the amount of substance of ammonium molybdate is 3: 1 in sodium sulphite and the step 1, and temperature of reaction is 80 ℃, reaction times 95min;
Step 3 is configured to microemulsion a with TritonX100, primary isoamyl alcohol, normal heptane, above-mentioned steps two gained solution and secondary deionized water; Hydrochloric acid and secondary deionized water with TritonX100, primary isoamyl alcohol, normal heptane, 1mol/L are configured to microemulsion b; Then microemulsion b is all joined microemulsion a; Under 50 ℃, carry out the heavy reaction of acid; Reaction times 60min washs the heavy precipitated product that reacts of said acid respectively more than three times with ethanol, acetone and deionized water; Finally after centrifugal, washing, vacuum-drying, obtain nano molybdenum disulfide;
Wherein, the concrete steps of said configuration microemulsion a are: under the normal temperature, TritonX100 and primary isoamyl alcohol are pressed mass ratio mixing in 1: 1; And then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution; Slowly splash into step 2 gained solution and secondary deionized water, guarantee that the ammonium molybdate starting point concentration is 0.04mol/L, the mol ratio of water and TritonX100 is 28 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end by muddiness;
The concrete steps of said configuration microemulsion b are: under the normal temperature; Is mixing in 1: 1 with TritonX100 and primary isoamyl alcohol by mass ratio, and then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution, slowly splashes into hydrochloric acid and the secondary deionized water of 1mol/L; Adding the acid amount is 2.2: 1 with the ammonium molybdate mol ratio; The mol ratio of water and tensio-active agent is 28 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends.
Embodiment four
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide, technical process as shown in Figure 1:
Step 1 is poured 4mmo l Sodium orthomolybdate in the beaker into, adds the 100ml deionized water, and stirring and dissolving adds 4mmol oxalic acid again, puts into thermostat water bath (temperature is 70 ℃), reduction 75min;
Step 2 takes by weighing 12mmol sulfuration and receives and add after the above-mentioned reaction in the solution, and changing the water-bath temperature is 80 ℃, and reaction 90min obtains mixing solutions.
Step 3 under the normal temperature, is to mix at 1: 1 by mass ratio respectively with TritonX100 and primary isoamyl alcohol, and then in mixed solution, is to add normal heptane at 4: 1 with (TritonX100+ primary isoamyl alcohol) and normal heptane mass ratio, is divided into two parts.A copy of it slowly splashes into the solution 20mL and the secondary deionized water of two of above-mentioned steps, and the mol ratio of water and tensio-active agent is 25 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends, and obtains microemulsion a.Another part slowly splashes into hydrochloric acid and the secondary deionized water of 1mol/L, and guaranteeing to add the acid amount is 2.5: 1 with the Sodium orthomolybdate mol ratio; The mol ratio of water and tensio-active agent is 25 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end, obtain microemulsion b by muddiness.Microemulsion a is placed water bath with thermostatic control (temperature is 60 ℃), short mix, stirring are wherein carried out in the whole addings of microemulsion b, through the high speed spinning, throw out washs respectively more than three times with ethanol, acetone and deionized water behind the reaction 60min.The gained throw out places 60 ℃ of vacuum drying ovens dry, obtains black powder shape product.This powdery product is directly carried out XRD and sem analysis characterize, the result is shown in Fig. 2 and 3.According to Fig. 2, confirm that this product is the MoS with hexagonal system
2(with reference to card JCPDS37-1492).It is that size is even, the spheroidal particle of mean diameter 60nm～90nm that Fig. 3 can demonstrate products therefrom fully aware ofly.
Embodiment five
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide, technical process as shown in Figure 1:
Step 1 is poured the 4mmol Potassium orthomolybdate in the beaker into, adds the 100ml deionized water, and stirring and dissolving adds 4mmol oxalic acid again, puts into thermostat water bath (temperature is 65 ℃), reduction 85min;
Step 2 takes by weighing 12mmol sulfuration and receives and add after the above-mentioned reaction in the solution, and changing the water-bath temperature is 80 ℃, and reaction 90min obtains mixing solutions;
Step 3 under the normal temperature, is to mix at 1: 1 by mass ratio respectively with TritonX100 and primary isoamyl alcohol, and then in mixed solution, is to add normal heptane at 4: 1 with (TritonX100+ primary isoamyl alcohol) and normal heptane mass ratio, is divided into two parts; A copy of it slowly splashes into above-mentioned steps two solution 20mL and secondary deionized water, and the mol ratio of water and tensio-active agent is 25 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends, and obtains microemulsion a; Another part slowly splashes into hydrochloric acid and the secondary deionized water of 1mol/L, and guaranteeing to add the acid amount is 2.5: 1 with the Sodium orthomolybdate mol ratio; The mol ratio of water and tensio-active agent is 25 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end, obtain microemulsion b by muddiness.Microemulsion a is placed water bath with thermostatic control (temperature is 60 ℃), short mix, stirring are wherein carried out in the whole addings of microemulsion b, through the high speed spinning, throw out washs respectively more than three times with ethanol, acetone and deionized water behind the reaction 60min.The gained throw out places 60 ℃ of vacuum drying ovens dry, obtains black powder shape nano molybdenum disulfide.
Embodiment six
A kind of method that adopts microemulsion system to prepare nano molybdenum disulfide, technical process as shown in Figure 1:
Step 1 is poured the 4mmol Sodium orthomolybdate in the beaker into, adds the 100ml deionized water, and stirring and dissolving adds 4mmol oxalic acid again, puts into thermostat water bath (temperature is 70 ℃), reduction 75min;
Step 2 takes by weighing 13mmol sulfuration and receives and add after the above-mentioned reaction in the solution, and changing the water-bath temperature is 75 ℃, and reaction 100min obtains mixing solutions;
Step 3 under the normal temperature, is to mix at 1: 1 by mass ratio respectively with TritonX100 and primary isoamyl alcohol, and then in mixed solution, is to add normal heptane at 4: 1 with (TritonX100+ primary isoamyl alcohol) and normal heptane mass ratio, is divided into two parts; A copy of it slowly splashes into above-mentioned steps two gained solution 20mL and secondary deionized water, and the mol ratio of water and tensio-active agent is 30 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends, and obtains microemulsion a; Another part slowly splashes into hydrochloric acid and the secondary deionized water of 1mol/L, and guaranteeing to add the acid amount is 2.5: 1 with the Sodium orthomolybdate mol ratio; The mol ratio of water and tensio-active agent is 30 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end, obtain microemulsion b by muddiness.Microemulsion a is placed water bath with thermostatic control (temperature is 60 ℃), short mix, stirring are wherein carried out in the whole addings of microemulsion b, through the high speed spinning, throw out washs respectively more than three times with ethanol, acetone and deionized water behind the reaction 60min.The gained throw out places 60 ℃ of vacuum drying ovens dry, obtains black powder shape nano molybdenum disulfide.
Claims (5)
1. a method that adopts microemulsion system to prepare nano molybdenum disulfide is characterized in that, comprises the steps:
Step 1; In concentration is to add reductive agent in the molybdate solution of 0.03～0.05mol/L it is reduced to the inferior molybdate of tetravalence; Molybdate is 1: 1～1: 1.3 with the ratio of reductive agent amount of substance, and temperature of reaction is 65 ℃～75 ℃, reaction times 75min～85min;
Step 2 is added sulfide and is made its sulfuration in step 1 gained solution, the ratio of the amount of substance of molybdate is 3: 1～4: 1 in sulfide and the step 1, and temperature of reaction is 75 ℃～85 ℃, reaction times 90min～100min;
Step 3 is configured to microemulsion a with TritonX100, primary isoamyl alcohol, normal heptane, above-mentioned steps two gained solution and secondary deionized water; Hydrochloric acid and secondary deionized water with TritonX100, primary isoamyl alcohol, normal heptane, 1mol/L are configured to microemulsion b; Then microemulsion b is all joined microemulsion a; Under 40 ℃～60 ℃, carry out the heavy reaction of acid; Reaction times 55min～65min finally obtains nano molybdenum disulfide after centrifugal, washing, vacuum-drying;
Wherein, The concrete steps of said configuration microemulsion a are: under the normal temperature; TritonX100 and primary isoamyl alcohol are pressed mass ratio mixing in 1: 1, and then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution, slowly splashes into step 2 gained solution and secondary deionized water; Guarantee that the molybdate starting point concentration is 0.03～0.05mol/L; The mol ratio of water and TritonX100 is 25～30 in the hierarchy of control, observes solution and becomes clarification by muddiness, becomes muddy by clarification again and ends;
The concrete steps of said configuration microemulsion b are: under the normal temperature; Is mixing in 1: 1 with TritonX100 and primary isoamyl alcohol by mass ratio; And then total mass and the normal heptane mass ratio with TritonX100 and primary isoamyl alcohol is 4: 1 adding normal heptanes in mixed solution; Slowly splash into hydrochloric acid and the secondary deionized water of 1mol/L, adding the acid amount is 2: 1～2.5: 1 with the molybdate mol ratio, and the mol ratio of water and tensio-active agent is 25～30 in the hierarchy of control; Observe solution and become clarification, become muddy by clarification again and end by muddiness.
2. the method for preparing nano molybdenum disulfide according to claim 1 is characterized in that, said molybdate is Sodium orthomolybdate, Potassium orthomolybdate or ammonium molybdate.
3. the method for preparing nano molybdenum disulfide according to claim 1 is characterized in that, said reductive agent is oxalic acid or oxammonium hydrochloride.
4. the method for preparing nano molybdenum disulfide according to claim 1 is characterized in that, said sulfide is sodium sulphite or potassium sulphide.
5. the method for preparing nano molybdenum disulfide according to claim 1 is characterized in that, the heavy precipitated product that reacts of said acid is washed respectively more than three times with ethanol, acetone and deionized water.
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| WO2016065890A1 (en) * | 2014-05-19 | 2016-05-06 | Baoshan Iron & Steel Co., Ltd. | Method of producing a catalyst |
| CN106492844A (en) * | 2016-11-24 | 2017-03-15 | 青岛大学 | A kind of preparation method and application of amorphous nano molybdenum disulfide catalyst |
| CN107913641A (en) * | 2017-12-01 | 2018-04-17 | 中国计量大学 | A kind of preparation method of microemulsion |
| CN108083337A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of method that hollow mos2 microsphere is prepared in reverse micro emulsion |
| CN108083338A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of ion liquid microemulsion thermal synthesis MoS2The preparation method of sub-micron bouquet |
| CN114843109A (en) * | 2022-05-13 | 2022-08-02 | 福州大学 | Sea urchin shaped MoS 2 Foamed nickel composite capacitor electrode material and preparation method thereof |
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| WO2016065890A1 (en) * | 2014-05-19 | 2016-05-06 | Baoshan Iron & Steel Co., Ltd. | Method of producing a catalyst |
| CN106470759A (en) * | 2014-05-19 | 2017-03-01 | 宝山钢铁股份有限公司 | The method preparing catalyst |
| CN106470759B (en) * | 2014-05-19 | 2019-11-01 | 宝山钢铁股份有限公司 | The method for preparing catalyst |
| US10286385B2 (en) | 2014-05-19 | 2019-05-14 | Baoshan Iron & Steel Co., Ltd. | Method for producing a catalyst |
| CN105032596A (en) * | 2015-08-05 | 2015-11-11 | 哈尔滨工业大学 | Method for grading particle sizes of nanoscaled molybdenum disulfide by adjusting pH value |
| CN108083338A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of ion liquid microemulsion thermal synthesis MoS2The preparation method of sub-micron bouquet |
| CN108083337A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of method that hollow mos2 microsphere is prepared in reverse micro emulsion |
| CN108083338B (en) * | 2016-11-23 | 2019-11-12 | 中国科学院大连化学物理研究所 | A kind of ion liquid microemulsion thermal synthesis MoS2The preparation method of sub-micron bouquet |
| CN106492844B (en) * | 2016-11-24 | 2018-12-11 | 青岛大学 | A kind of preparation method and application of amorphous nano molybdenum disulfide catalyst |
| CN106492844A (en) * | 2016-11-24 | 2017-03-15 | 青岛大学 | A kind of preparation method and application of amorphous nano molybdenum disulfide catalyst |
| CN107913641A (en) * | 2017-12-01 | 2018-04-17 | 中国计量大学 | A kind of preparation method of microemulsion |
| CN114843109A (en) * | 2022-05-13 | 2022-08-02 | 福州大学 | Sea urchin shaped MoS 2 Foamed nickel composite capacitor electrode material and preparation method thereof |
| CN114843109B (en) * | 2022-05-13 | 2023-09-29 | 福州大学 | Sea urchin-shaped MoS 2 Foam nickel composite capacitor electrode material and preparation method thereof |
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