CN107055615B - A kind of two-dimensional nanostructure MoS2The preparation method of nanometer sheet - Google Patents
A kind of two-dimensional nanostructure MoS2The preparation method of nanometer sheet Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
A kind of two-dimensional nanostructure MoS2The preparation method of nanometer sheet, it is related to the preparing technical field of nano material, the present invention is using powdery halloysite nanotubes as template, by the mixed solution for adding in molybdenum source and sulphur source, molybdenum source is made to be deposited with sulphur source in template outer surface and interlayer, molybdenum source can be reacted rapidly with sulphur source, generate molybdenum disulfide nucleus in a template, and the nucleus of generation quickly grows into curling sheet；Removing template is removed, obtains curly molybdenum disulfide crude product；It is unfolded again through curly molybdenum disulfide own tension, forms the two-dimensional layered structure MoS of multilayer chip2Nanometer sheet.Manufacturing cost of the present invention is low, and stability is good, and preparing nanometer sheet using template, to have taken into account step simultaneously simple, and the nanometer sheet number of plies is controllable and the advantages of large-scale production.
Description
Technical field
The present invention relates to the preparing technical fields of nano material, particularly lubriation material technical field.
Background technology
Transition-metal dichalcogenide, especially molybdenum disulfide have laminar structured, the model of interlayer similar to graphite
De Huali is very weak, easily peelable between layers, therefore its friction coefficient is very low, easily slides；Covalent bond in layer is very
By force, illustrate that it is freely hanged with good mechanical strength, with good thermal stability in inert environments and with surface
The features such as key, can prevent from being pierced in metal surface protruding parts lubricating film, and the sulphur atom for being exposed to plane of crystal can be right
Metal surface generates very strong adhesion, forms very firm film so that its greasy property is superior to graphite.
Compared with common molybdenum disulfide, MoS2Nanometer sheet is because of great specific surface area, table the features such as stronger adsorption capacity
Reveal more excellent greasy property.MoS2Nanometer sheet is used as lubriation material can significantly reduce its friction coefficient and carry
High-wearing feature has good application prospect in tribology.Vattikuti et al. successfully synthesizes MoS2Nanometer sheet is made
Excellent wear-resistant and reduction frictional behaviour is shown for lubricating additive, is seen《Use solvent structure MoS2Nanosphere and
The structural characterization of nanometer sheet》（Material science journal, 2015,50:5024-5038.）.
MoS2Nanometer sheet can be by mechanically pulling off method, electrochemical stripping method, embedding lithium stripping method, hydro-thermal method, solvent-thermal method,
Hummer methods, CVD method, ultrasonic water bath method, hydrodynamic, ball-milling method, steam blow etc..However the above method can not
Meet that step is simple simultaneously, the nanometer sheet number of plies is controllable and the requirement of large-scale production.
Invention content
It is simple, controllable with good friction performance, the nanometer sheet number of plies based on method the purpose of the present invention is to provide one kind,
And conducive to the two-dimensional nanostructure MoS of industrialized production2The preparation method of nanometer sheet.
The present invention includes the following steps：
1）Under magnetic stirring, molybdenum source and sulphur source are dissolved in deionized water, obtain the mixed solution of molybdenum source and sulphur source；
2）By 60~100 DEG C of dry powdery halloysite nanotubes（HNTs）It is mixed with the mixed solution of above-mentioned molybdenum source and sulphur source
It is reacted after conjunction；
3）It is cooled to room temperature after reaction, galapectite is successively removed using hydrofluoric acid aqueous solution and aqueous hydrochloric acid solution washing
Nanotube（HNTs）, obtain MoS2Crude product；
4）Using deionized water, absolute ethyl alcohol washing MoS2After crude product, centrifuging and taking obtains solid phase, through drying, grinding, obtains two
Dimension nanometer construction MoS2Nanometer sheet.
The present invention is with powdery halloysite nanotubes（HNTs）For template, by step 2）, the mixed solution of molybdenum source and sulphur source
Middle molybdenum source is deposited with sulphur source in template outer surface and interlayer, and molybdenum source can be reacted rapidly with sulphur source, generate molybdenum disulfide in a template
Nucleus, the nucleus of generation quickly grow into curling sheet；By step 3）Removing template is removed, curly molybdenum disulfide is obtained and slightly produces
Product；By step 3）After processing, curly molybdenum disulfide own tension is unfolded, and forms the two-dimensional nanostructure of multilayer chip
MoS2Nanometer sheet.
The step 2）In, halloysite nanotubes during for mixing（HNTs）Temperature be 60~100 DEG C.HNTs
Enough solution can be absorbed after removal intermediary water, makes full use of interlayer template action.
The present invention is with halloysite nanotubes（HNTs）It is carrier by controlling solid-liquid volume ratio, utilizes pipe outer wall template and layer
Between the method for intercalation template prepare two-dimensional nanostructure MoS2Nanometer sheet, compared with prior art, technical advantage body of the invention
Now：
1st, the template that the present invention uses is natural halloysite nanotubes, and at low cost, stability is good.
2nd, the present invention using template prepares nanometer sheet to have taken into account step simultaneously simple, and the nanometer sheet number of plies is controllable and scale
The advantages of metaplasia is produced.
Further, step 1 of the present invention）In, the molybdenum source is ammonium molybdate or sodium molybdate.Ammonium molybdate and sodium molybdate are all
It for the principle that is easy to get, can decompose in a heated condition, generate MoS2。
The step 1）In, the sulphur source is thiocarbamide or thioacetamide or vulcanized sodium.In a heated condition, these sulphur sources
It is reacted with water and generates H2S, generated hydrogen sulfide are very strong reducing agents, can be by Mo+6It is reduced to Mo+4.In addition, hydrogen sulfide is also
Vulcanizing agent is served as, sulphur source is provided for generation molybdenum disulfide.
The step 1）In, in the mixed solution of the molybdenum source and sulphur source the molar ratio of molybdenum atom and sulphur atom for 1: 2~
4.Using the dosage of above each material convenient for control solid-liquid volume ratio, if sulphur source is very few, then MoS2Easily aoxidized；Such as sulphur source mistake
It is more, then it wastes raw material.
The step 1）In, the temperature condition of the dissolving is 30~60 DEG C.The special meaning dissolved using the temperature
Justice：Dissolution of raw material does not react between two kinds of raw materials.
The step 2）In, the powdery halloysite nanotubes（HNTs）For 1-dimention nano tubular structure, length for 200~
500 nm, a diameter of 50~100nm, interlayer structure are 7~10.Tool is used to use the material of more than characteristic as possessed by carrier
Special Significance：With larger external surface area, surface active groups are more, molybdenum disulfide can using outside surface area as template,
The more MoS of the number of plies is prepared2Nanometer sheet, and nanometer interlayer structure is 7~10, it can be as template contral MoS2Nanometer
The number of plies of piece, the number of plies that nanometer sheet is made are 2~3 layers.
The step 2）In, the halloysite nanotubes are 100 mL: 3.8~215 g with the mixing ratio of molybdenum source and sulphur source:
3.2~330 g.Using Special Significance possessed by the amount ratio：
1st, solid-liquid volume ratio is 1:When 40, molybdenum source, sulphur source are mainly in template outside deposition；
2nd, solid-liquid volume ratio is 1：When 0.2, molybdenum source, sulphur source are first filled with HNTs interlayers；
3rd, solid-liquid volume ratio therebetween when, either way will appear；
4th, achieved the purpose that the nanometer sheet number of plies is controllable, the number of plies that can control preparation nanometer sheet is 2~8 layers.
The step 2）In, the reaction the temperature of mixed system be 180~240 DEG C, the conditions of 5~15 rpm rotating speeds
Lower progress.Using more than reaction condition for Special Significance possessed by present invention process：
1st, rotating speed is slower, HNTs powder is caused to deposit, it is impossible to preferably play template action；
2nd, under cryogenic, the crystallinity of the molybdenum disulfide of synthesis is poor；
3rd, with the raising of temperature, the crystallinity of the nanometer sheet of synthesis is preferable；
4th, the crystallinity of nanometer sheet further rises high temperature increases rotating speed after having reached requirement, leads to the waste of the energy；
The step 3）In, the mass percent of HF is 20~40% in the hydrofluoric acid aqueous solution, in aqueous hydrochloric acid solution
The mass percent of HCl is 20~38%.Using Special Significance possessed by the concentration of above each material：
1st, because template HNTs is mainly by alumino-silicate, so selecting hydrofluoric acid and hydrochloric acid that can remove template；
2nd, the concentration of acid solution is too low, and template cannot be removed thoroughly totally；
3rd, it is easy to buy, facilitates reduction production cost.
Description of the drawings
Fig. 1 is the flow chart of the method for the present invention preparation process.
Fig. 2 is 1 gained MoS of example2The SEM photograph of nanometer sheet.
Fig. 3 is 2 gained MoS of example2The TEM photos of nanometer sheet.
Fig. 4 is 3 gained MoS of example2The HRTEM photos of nanometer sheet.
Specific embodiment
Present invention process is illustrated with reference to Fig. 1.
The powdery halloysite nanotubes used in following technique（HNTs）For 1-dimention nano tubular structure, length for 200~
500 nm, a diameter of 50~100nm, interlayer structure are 7~10.First HNTs powder is put into 60~100 DEG C of insulating box and is done
Dry 12~24 h, and heat preservation for standby use.
Example 1：
1st, MoS is prepared2Nanometer sheet：
3.8 g ammonium molybdates and 6.6 g thiocarbamides are placed in 70 mL distilled water, magnetic agitation is allowed to dissolve at 30 DEG C, obtains
To a concentration of 0.05 g/ mL of ammonium molybdate, thiourea concentration is 0.09 g/ mL and the molar ratio of molybdenum atom and sulphur atom is 1:4
Solution adds in the HNTs powder of 60 DEG C of 2 mL into above-mentioned mixed system, continues stirring so that solid-liquid is uniformly mixed, is transferred to
Polytetrafluoroethylene (PTFE) is in the stainless steel autoclave of liner, reacts 48 h under 180 DEG C, 5 rpm rotating speeds.
System naturally cools to room temperature after reaction, respectively with the hydrofluoric acid aqueous solution and matter that mass percent is 20%
It measures the aqueous hydrochloric acid solution that percentage is 20% and washs product, to remove template HNTs, then with deionized water, absolute ethyl alcohol washing 3
It~5 times, centrifuges, filtering, dry 12 h, black product is collected after grinding at 50 DEG C.
As shown in the SEM photograph of Fig. 2, the MoS that is prepared2Laminated structure together is stacked above, the number of plies is 2 layers.
2nd, it applies：
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery friction
Coefficient has dropped 24.2% compared to base oil.
Example 2：
1st, MoS is prepared2Nanometer sheet：
3.8 g ammonium molybdates and 4.7 g thioacetamides are placed in 70 mL distilled water, magnetic agitation is allowed at 40 DEG C
Dissolving obtains a concentration of 0.05 g/ mL of ammonium molybdate, a concentration of 0.07 g/ mL of thioacetamide and molybdenum atom and sulphur atom
Molar ratio is 1:3 solution adds in the HNTs powder of 80 DEG C of 2 mL into above-mentioned mixed system, continues stirring so that solid-liquid mixes
It closes and uniformly, is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, react 24 under 220 DEG C, 10 rpm rotating speeds
h。
System naturally cools to room temperature after reaction, respectively with the hydrofluoric acid aqueous solution and matter that mass percent is 30%
It measures the aqueous hydrochloric acid solution that percentage is 30% and washs product, to remove template, then with deionized water, absolute ethyl alcohol washing 3~5
It is secondary, it centrifuges, filtering, dry 18 h, product is collected after grinding at 60 DEG C.
As shown in the TEM photos of Fig. 3, the MoS that is prepared2Laminated structure together is stacked above, the number of plies is 8 layers.
2nd, it applies：
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery friction
Coefficient has dropped 19.7% compared to base oil.
Example 3：
1st, MoS is prepared2Nanometer sheet：
4.3 g sodium molybdates and 3.3 g vulcanized sodium are placed in 70 mL distilled water, magnetic agitation is allowed to molten at 60 DEG C
Solution, obtains a concentration of 0.06 g/ mL of sodium molybdate, a concentration of 0.05 g/ mL of vulcanized sodium and the molar ratio of molybdenum atom and sulphur atom
It is 1:2 solution adds in the HNTs powder of 100 DEG C of 2 mL into above-mentioned mixed system, continues stirring so that solid-liquid mixing is equal
It is even, it is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, reacts 12 h under 240 DEG C, 15 rpm rotating speeds.
System naturally cools to room temperature after reaction, respectively with the hydrofluoric acid aqueous solution and matter that mass percent is 40%
It measures the aqueous hydrochloric acid solution that percentage is 38% and washs product, to remove template, then with deionized water, absolute ethyl alcohol washing 3~5
It is secondary, it centrifuges, filtering, dry 24 h, product is collected after grinding at 80 DEG C.
As shown in the HRTEM photos of Fig. 4, the MoS that is prepared2Laminated structure together is stacked above, the number of plies is 5 layers.
2nd, it applies：
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery friction
Coefficient has dropped 19.7% compared to base oil.
Example 4：
1st, MoS is prepared2Nanometer sheet：
3.8 g ammonium molybdates and 6.6 g thiocarbamides are placed in 20 mL distilled water, magnetic agitation is allowed to dissolve at 30 DEG C,
A concentration of 0.19 g/ mL of ammonium molybdate are obtained, thiourea concentration is 0.33 g/ mL and the molar ratio of molybdenum atom and sulphur atom is 1:4
Solution, above-mentioned mixed solution is added in the HNTs powder of 60 DEG C of 100 mL, is continuously agitated so that solid-liquid mixing is equal
It is even, it is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, reacts 48 h under 180 DEG C, 5 rpm rotating speeds.
System naturally cools to room temperature after reaction, respectively with the hydrofluoric acid aqueous solution and matter that mass percent is 20%
It measures the aqueous hydrochloric acid solution that percentage is 20% and washs product, to remove template, then with deionized water, absolute ethyl alcohol washing 3~5
It is secondary, it centrifuges, filtering, dry 12 h, collect product, the MoS being prepared after grinding at 50 DEG C2It is stacked above piece together
Shape structure, the number of plies are 2 layers.
2nd, it applies：
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery friction
Coefficient has dropped 36.8% compared to base oil.
Example 5：
1st, MoS is prepared2Nanometer sheet：
3.8 g ammonium molybdates and 4.7 g thioacetamides are placed in 20 mL distilled water, magnetic agitation is allowed at 40 DEG C
Dissolving obtains a concentration of 0.19 g/ mL of ammonium molybdate, a concentration of 0.24 g/ mL of thioacetamide and molybdenum atom and sulphur atom
Molar ratio is 1:Above-mentioned mixed solution is added in the HNTs powder of 80 DEG C of 100 mL by 3 solution, be continuously agitated so that
Solid-liquid is uniformly mixed, and is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, under 220 DEG C, 10 rpm rotating speeds
React 24 h.
System naturally cools to room temperature after reaction, is distinguished respectively with 30% hydrofluoric acid aqueous solution and 30% aqueous hydrochloric acid solution
Product is washed, to remove template, then with deionized water, absolute ethyl alcohol is washed 3~5 times, centrifuged, and filtering is dry at 60 DEG C
18 h collect product after grinding, the MoS being prepared2Laminated structure together is stacked above, the number of plies is 3 layers.
2nd, it applies：
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery friction
Coefficient has dropped 19.6% compared to base oil.
Example 6：
1st, MoS is prepared2Nanometer sheet：
4.3g sodium molybdates and 3.3 g vulcanized sodium are placed in 20 mL distilled water, magnetic agitation is allowed to dissolve at 60 DEG C,
A concentration of 0.22 g/ mL of ammonium molybdate are obtained, thiourea concentration is 0.17 g/ mL and the molar ratio of molybdenum atom and sulphur atom is 1:2
Solution, above-mentioned mixed solution is added in the HNTs powder of 100 DEG C of 100 mL, is continuously agitated so that solid-liquid mixing is equal
It is even, it is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, reacts 12 h under 240 DEG C, 15 rpm rotating speeds.
System naturally cools to room temperature after reaction, is washed respectively with 40% hydrofluoric acid aqueous solution and 38% aqueous hydrochloric acid solution
Product, to remove template, then with deionized water, absolute ethyl alcohol is washed 3~5 times, is centrifuged, filtering, dry 24 at 80 DEG C
H collects product after grinding, the MoS being prepared2Laminated structure together is stacked above, the number of plies is 5 layers.
2nd, it applies：
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery friction
Coefficient has dropped 19.6% compared to base oil.
The present invention is prepared for the uniform MoS of the number of plies using a kind of simple template2Nanometer sheet, oil adds based on research
Add the greasy property of agent.
Claims (4)
1. a kind of two-dimensional nanostructure MoS2The preparation method of nanometer sheet, it is characterised in that include the following steps：
1）Under magnetic stirring, molybdenum source and sulphur source are dissolved in deionized water, obtain the mixed solution of molybdenum source and sulphur source；It is described
Molybdenum source is ammonium molybdate or sodium molybdate, and the sulphur source is thiocarbamide or thioacetamide or vulcanized sodium；The mixing of the molybdenum source and sulphur source
The molar ratio of Molybdenum in Solution atom and sulphur atom is 1: 2~4；
2）It is carried out after 60~100 DEG C of dry powdery halloysite nanotubes are mixed with the mixed solution of above-mentioned molybdenum source and sulphur source anti-
It should；The powdery halloysite nanotubes be 1-dimention nano tubular structure, length be 200~500 nm, a diameter of 50~100nm,
Interlayer structure is 7~10；The halloysite nanotubes are 100 mL: 3.8~215 g: 3.2 with the mixing ratio of molybdenum source and sulphur source
~330 g；
3）It is cooled to room temperature after reaction, galapectite nanometer is successively removed using hydrofluoric acid aqueous solution and aqueous hydrochloric acid solution washing
Pipe, obtains MoS2Crude product；
4）Using deionized water, absolute ethyl alcohol washing MoS2After crude product, centrifuging and taking obtains solid phase, through drying, grinding, obtains two wieners
Rice structure MoS2Nanometer sheet.
2. preparation method according to claim 1, it is characterised in that the step 1）In, the temperature condition of the dissolving is
30~60 DEG C.
3. preparation method according to claim 1, it is characterised in that the step 2）In, the reaction is in mixed system
Temperature is 180~240 DEG C, is carried out under conditions of 5~15 rpm rotating speeds.
4. preparation method according to claim 1, it is characterised in that the step 3）In, HF in the hydrofluoric acid aqueous solution
Mass percent for 20~40%, the mass percent of HCl is 20~38% in aqueous hydrochloric acid solution.
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| CN108554424A (en) * | 2018-04-20 | 2018-09-21 | 河北工业大学 | The preparation method of molybdenum disulfide-tourmaline composite |
| CN108557889A (en) * | 2018-04-20 | 2018-09-21 | 河北工业大学 | The preparation method of molybdenum disulfide-halloysite nanotubes composite material |
| CN108525680A (en) * | 2018-04-20 | 2018-09-14 | 河北工业大学 | The preparation method of molybdenum disulfide-sepiolite nano-fiber composite material |
| CN108394936A (en) * | 2018-04-20 | 2018-08-14 | 河北工业大学 | The preparation method of molybdenum disulfide-Palygorskite Nanometer rod composite material |
| CN108893974B (en) * | 2018-06-05 | 2020-07-24 | 湖北大学 | Petal-like molybdenum disulfide film and preparation method and application thereof |
| CN110871051A (en) * | 2018-08-30 | 2020-03-10 | 中国科学院理化技术研究所 | Fe3O4@MoS2Superparamagnetic nano material and preparation method and application thereof |
| CN108929742B (en) * | 2018-08-31 | 2020-12-15 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
| CN110452677B (en) * | 2019-08-08 | 2021-10-15 | 河南郸城顺兴石油助剂有限公司 | MoS based on modification2Process for preparing drag reducing agents |
| CN112259733A (en) * | 2020-10-21 | 2021-01-22 | 湘潭大学 | Nanotube-shaped magnesium ion battery positive electrode material and preparation method thereof |
| CN113800568B (en) * | 2021-10-18 | 2023-03-17 | 上海交通大学 | Preparation method of two-dimensional laminated transition metal sulfide material |
| CN114084876B (en) * | 2021-11-22 | 2023-09-01 | 乌海瑞森新能源材料有限公司 | One-dimensional multilayer nano-chain composite material, preparation method thereof and application thereof in lithium ion battery |
| CN114477287B (en) * | 2022-03-11 | 2024-01-26 | 合肥学院 | Method for enhancing lubricating property of flaky nano molybdenum disulfide by improving curvature rate of flaky layers |
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