CN113772731A - Method for synthesizing molybdenum disulfide in vacuum - Google Patents
Method for synthesizing molybdenum disulfide in vacuum Download PDFInfo
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- CN113772731A CN113772731A CN202110952049.7A CN202110952049A CN113772731A CN 113772731 A CN113772731 A CN 113772731A CN 202110952049 A CN202110952049 A CN 202110952049A CN 113772731 A CN113772731 A CN 113772731A
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 35
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- 239000010453 quartz Substances 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 32
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000007789 sealing Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 17
- 239000000314 lubricant Substances 0.000 abstract description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 abstract description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 19
- 239000000047 product Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 13
- 238000005303 weighing Methods 0.000 description 8
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 238000004073 vulcanization Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910016003 MoS3 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- -1 transition metal sulfide Chemical class 0.000 description 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The invention discloses a method for synthesizing molybdenum disulfide in vacuum, which is to mix MoO3Uniformly mixing the powder and the S powder, placing the mixture into a quartz tube, sealing the quartz tube by using a tube sealing machine under the condition that the vacuum degree is 2-20 Pa, carrying out heat treatment on the sealed quartz tube, cooling and taking out the quartz tube, wherein the product in the quartz tube is MoS2The yield can reach 91.89% at most, and the product can be directly used as lubricant; the method adopts a vacuum synthesis mode to sulfurize molybdenum oxide into molybdenum disulfide, can be used for sulfurizing transition metal oxides, and has the advantages of low cost, short flow, simple and convenient operation, high yield and small environmental pollution.
Description
Technical Field
The invention relates to a method for synthesizing molybdenum disulfide in vacuum, belonging to the technical field of vacuum metallurgy.
Background
The transition metal sulfide has a crystal structure similar to that of graphene and a band gap structure which is not contained in graphene, so that the transition metal sulfide has unique physical, chemical and photoelectric properties and becomes a research hotspot in new materials. Molybdenum disulfide can still keep better lubricating property under the environmental conditions of high temperature, high pressure and high-speed rotation, is known as lubricant king, and is widely applied to high and new technical fields of aerospace, military industry, nuclear industry and the like. The industrial production of molybdenum disulfide is mainly a chemical synthesis method, the raw materials used are different, generally ammonium molybdate is used as raw material, the ammonium molybdate is vulcanized and converted into ammonium thiomolybdate, and then MoS is prepared by thermal decomposition of the ammonium thiomolybdate2In addition, molybdenum trioxide can be directly reacted with industrial sulfur powder to generate MoS2And the like.
The patent with application number 201410314766.7 takes ammonium molybdate as a raw material and thiourea as a sulfur source to carry out vulcanization to generate MoS3Precipitating, centrifuging, and thermally decomposing to obtain MoS2The production process is long, the preparation conditions are severe, and the size and the shape of the product are difficult to regulate and control, so that the method is not suitable for large-scale production and application.
HL A et al utilize molybdenum trioxide to directly react with industrial sulfur powder, and free MoO in the product3With incompletely vulcanised MoO2Becomes main impurities, and the sulfur content is unstable, so that the content ratio of Mo and S is unstable, and the subsequent use of the product is influenced to a certain extent. Meanwhile, no matter what method, the method can cause a great amount of loss of raw materials, doping of components in the product,Low yield, complex collection process, great environmental pollution, high production cost and the like.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a method for synthesizing molybdenum disulfide in vacuum, which takes molybdenum oxide (99.95%) and industrial sulfur powder as raw materials, uniformly mixes the raw materials according to a certain proportion, then puts the raw materials into a quartz tube, seals the quartz tube under the vacuum condition, and then heats the quartz tube to directly obtain the product molybdenum disulfide.
A method for synthesizing molybdenum disulfide in vacuum comprises the following specific steps:
(1) adding MoO3Uniformly mixing the powder and the S powder;
(2) putting the powder obtained in the step (1) into a quartz tube, and sealing the quartz tube by using a tube sealing machine under the condition that the vacuum degree is 2-20 Pa;
(3) carrying out heat treatment on the sample obtained in the step (2), cooling and taking out the quartz tube, wherein the product in the quartz tube is MoS2。
The MoO3The purity of the powder is 99.95 percent; the S powder is industrial sulfur powder.
The MoO3The mass ratio of the powder to the S powder is 1: 1-3.
When the quartz tube is sealed, the pressure is 2-20 Pa, and the inner diameter of the quartz tube is 10-30 mm.
The heat treatment is carried out by heating to 500-600 ℃ and then preserving the heat for 10-30 min.
According to the formula of vapor pressure and temperature of a substance: lg (P/kPa) ═ a 103*T-1+B*lgT+c*10-3+ D, calculating the volatilization temperature of molybdenum trioxide under the condition of 1-120 Pa, as shown in FIG. 1, it is known that the temperature required for the molybdenum trioxide to volatilize increases significantly with the increase of the saturated vapor pressure, and when the pressure is 2-20 Pa, the corresponding volatilization temperature is: 890K to 950K; it is known that vacuum conditions can significantly reduce the temperature required for the reaction.
Utilizing Factsage to calculate MoO under the condition of 10Pa3The binary equilibrium phase diagram-S, as shown in FIG. 2, shows the reaction temperature for producing molybdenum disulfide at 10PaAbout 700K to 1490K, and is required to participate in the reaction MoO3The mass ratio of S to S is: the ratio of the molybdenum disulfide to the water is 1: 0.125-9, so that gas-solid reaction is carried out to generate molybdenum disulfide under the condition of setting the pressure to be 2-20 Pa, and the reaction temperature can be set to be 500-600 ℃.
Meanwhile, according to the binary equilibrium phase diagram, under the condition that S participates in less reaction, MoO is generated2、MoS3The intermediate products are stored under vacuum condition, the reaction temperature is set to be 500-600 ℃, and MoO is controlled3The mass ratio of the powder to the S powder is 1: 1-3, and the reaction under the conditions is as follows: MoO3+3.5S(g)＝MoS2+1.5SO2(g) The sulfur powder is quickly volatilized to be changed into gas under the vacuum condition, so that the reaction heat preservation time can be controlled within 10-30 min, the molybdenum trioxide is completely vulcanized into the molybdenum disulfide, no intermediate product is generated, and the vacuum sealing can obtain higher yield at lower temperature and shorter heat preservation time.
The invention has the advantages that the process flow is simple, the operation is convenient, the vulcanization process is carried out in a closed quartz tube, the process can realize the full reaction of molybdenum oxide and sulfur, the use amount of industrial sulfur powder is greatly reduced, and MoS is generated2No new impurity is generated in the process, and the product quality is high. Because the reaction is carried out under the vacuum condition, the reaction temperature of the raw materials is obviously reduced, and the method has the advantages of economy, environmental protection, high reaction speed, low energy consumption and the like; from the analysis of the principle of vulcanization, the raw material used in this method is not limited to molybdenum trioxide, but can be used for the vulcanization of transition metal oxides such as tungsten trioxide.
Drawings
FIG. 1 is MoO3The relationship of saturated vapor pressure to temperature;
FIG. 2 shows MoO3And a binary equilibrium phase diagram of S under the condition of 10 Pa;
figure 3 is the XRD pattern of the product of example 1.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1
A method for synthesizing molybdenum disulfide in vacuum comprises the following specific steps:
(1) mixing raw materials: weighing MoO according to the mass ratio of 1:13Weighing the powder and S powder, uniformly mixing the weighed raw materials to prepare a plurality of parts of mixed powder; wherein MoO3The purity of the powder is 99.95 percent, and the sulfur powder is industrial sulfur powder;
(2) vacuum tube sealing: respectively putting a plurality of parts of powder obtained in the step (1) into a plurality of quartz tubes, wherein the inner diameter of each quartz tube is 10mm, and sealing the quartz tubes by using a tube sealing machine under the condition of 10Pa of vacuum degree;
(3) putting the sample obtained in the step (2) into an internal heating type vacuum furnace, heating to 500 ℃ under the pressure of 10Pa, preserving the heat for 30min, and taking out a quartz tube after cooling; the MoS obtained2The product mass was 0.89g, and the yield was 80.18%.
FIG. 3 is the XRD pattern of the product of step (3) in this example, from which the characteristic peaks and MoS of the product can be seen2Complete match, which indicates MoO in the vacuum vulcanization process3All converted into MoS2. The prepared molybdenum disulfide is widely used for lubricants, lithium battery super capacitors, photocatalysts, synthetic nano composite materials and the like.
Example 2
A method for synthesizing molybdenum disulfide in vacuum comprises the following specific steps:
(1) mixing raw materials: weighing MoO according to the mass ratio of 1:23Weighing the raw materials and uniformly mixing the raw materials with the S powder to prepare a plurality of parts of mixed powder; wherein MoO3The purity of the powder is 99.95 percent, and the sulfur powder is industrial sulfur powder;
(2) vacuum tube sealing: respectively putting a plurality of parts of powder obtained in the step (1) into a plurality of quartz tubes, wherein the inner diameter of each quartz tube is 30mm, and sealing the quartz tubes by using a tube sealing machine under the condition of vacuum degree of 2 Pa;
(3) putting the sample obtained in the step (2) into an internal heating type vacuum furnace, heating to 550 ℃ under the pressure of 2Pa, preserving the heat for 20min, and taking out a quartz tube after cooling; the resulting condensate MoS2The product mass was 0.96g, and the yield was 86.48%.
Example 3
A method for synthesizing molybdenum disulfide in vacuum comprises the following specific steps:
(1) mixing raw materials: weighing MoO according to the mass ratio of 1:33Weighing the raw materials and uniformly mixing the raw materials with the S powder to prepare a plurality of parts of mixed powder; wherein MoO3The purity of the powder is 99.95 percent, and the sulfur powder is industrial sulfur powder;
(2) vacuum tube sealing: respectively putting a plurality of parts of powder obtained in the step (1) into a plurality of quartz tubes, wherein the inner diameter of each quartz tube is 20mm, and sealing by using a tube sealing machine; wherein the quartz tube is sealed under the condition of vacuum degree of 20 Pa;
(3) putting the sample obtained in the step (2) into an internal heating type vacuum furnace, heating to 600 ℃ under the pressure of 20Pa, preserving the heat for 10min, and taking out a quartz tube after cooling; the resulting condensate MoS2The product mass was 1.02g, and the yield was 91.89%.
Comparative example 1
Now will MoO3Weighing raw material MoO and S powder according to the mass ratio of 1:53Mixing with S powder, directly placing into an open graphite crucible, placing the graphite crucible into a vacuum furnace at 10Pa, heating to 800 deg.C, and keeping the temperature for 60min to obtain MoO powder2And MoS2The mixture weighed 0.55g, and the yield was 49.54%.
Comparative example 2
Preparation of MoS by traditional vapor deposition method2Adding MoO3Weighing the powder and S powder according to the mass ratio of 1:10, respectively placing the raw materials in two temperature regions of 800 ℃ and 180 ℃, and simultaneously introducing H2Ar creates reducing atmosphere, and the temperature is kept for 90min at the set temperature to generate MoS2The mass of the product was 0.76g, and the yield was 68.46%.
In summary, the yields of the products of examples 1-3 of the present invention are higher than those of comparative examples 1 and 2, and MoO is used in the present invention3After being uniformly mixed with S, the mixture is placed in a quartz tube for vacuum sealing and is roasted in a resistance furnace, the reaction temperature is effectively reduced under the vacuum condition, the raw materials are all reacted without adding excessive sulfur powder, and the product of the embodiment is MoS2High purity and impurityLess, fine in granularity and without further impurity removal treatment.
Claims (5)
1. A method for synthesizing molybdenum disulfide in vacuum is characterized by comprising the following specific steps:
adding MoO3Uniformly mixing the powder and the S powder, placing the mixture into a quartz tube, sealing the quartz tube by using a tube sealing machine under the condition that the vacuum degree is 2-20 Pa, carrying out heat treatment on the sealed quartz tube, cooling and taking out the quartz tube, wherein the product in the quartz tube is MoS2。
2. The method for vacuum synthesis of molybdenum disulfide as claimed in claim 1, wherein MoO3The purity of the powder is 99.95 percent, and the S powder is industrial sulfur powder.
3. The method for vacuum synthesis of molybdenum disulfide as claimed in claim 1, wherein MoO3The mass ratio of the powder to the S powder is 1: 1-3.
4. The method for synthesizing molybdenum disulfide under vacuum according to claim 1, wherein the sealing pressure of the quartz tube is 2-20 Pa, and the inner diameter of the quartz tube is 10-30 mm.
5. The method for synthesizing molybdenum disulfide in vacuum according to claim 1, wherein the heat treatment is carried out by heating to 500-600 ℃ and then holding for 10-30 min.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224905A (en) * | 2007-12-17 | 2008-07-23 | 金堆城钼业股份有限公司 | Method for preparing molybdenum disulfide with spheroidal structure |
| CN103952682A (en) * | 2014-04-22 | 2014-07-30 | 中国科学院上海光学精密机械研究所 | Method for growing single-layer molybdenum disulfide by chemical vapor deposition |
| CN108588674A (en) * | 2018-05-03 | 2018-09-28 | 昆明理工大学 | A kind of synthetic method of single layered porous molybdenum disulfide |
| CN108677162A (en) * | 2018-05-03 | 2018-10-19 | 昆明理工大学 | A kind of method that a step prepares multilayer molybdenum disulfide |
| CN110357162A (en) * | 2019-07-22 | 2019-10-22 | 金堆城钼业股份有限公司 | A method of efficiently synthesizing high pure alcohol |
| CN110436525A (en) * | 2019-07-22 | 2019-11-12 | 金堆城钼业股份有限公司 | A kind of preparation method of micro-/ nano molybdenum disulfide |
| US20210053037A1 (en) * | 2018-03-19 | 2021-02-25 | Dic Corporation | Molybdenum sulfide, method for producing same, and hydrogen generation catalyst |
-
2021
- 2021-08-18 CN CN202110952049.7A patent/CN113772731A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224905A (en) * | 2007-12-17 | 2008-07-23 | 金堆城钼业股份有限公司 | Method for preparing molybdenum disulfide with spheroidal structure |
| CN103952682A (en) * | 2014-04-22 | 2014-07-30 | 中国科学院上海光学精密机械研究所 | Method for growing single-layer molybdenum disulfide by chemical vapor deposition |
| US20210053037A1 (en) * | 2018-03-19 | 2021-02-25 | Dic Corporation | Molybdenum sulfide, method for producing same, and hydrogen generation catalyst |
| CN108588674A (en) * | 2018-05-03 | 2018-09-28 | 昆明理工大学 | A kind of synthetic method of single layered porous molybdenum disulfide |
| CN108677162A (en) * | 2018-05-03 | 2018-10-19 | 昆明理工大学 | A kind of method that a step prepares multilayer molybdenum disulfide |
| CN110357162A (en) * | 2019-07-22 | 2019-10-22 | 金堆城钼业股份有限公司 | A method of efficiently synthesizing high pure alcohol |
| CN110436525A (en) * | 2019-07-22 | 2019-11-12 | 金堆城钼业股份有限公司 | A kind of preparation method of micro-/ nano molybdenum disulfide |
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