CN107055615A - 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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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 molybdenum source and sulphur source, molybdenum source is set to be deposited with sulphur source in template outer surface and interlayer, molybdenum source can be reacted rapidly with sulphur source, and molybdenum disulfide nucleus is produced in a template, and the nucleus of generation quickly grows into curling sheet;Removing template is removed, curly molybdenum disulfide crude product is obtained;Deploy again through curly molybdenum disulfide own tension, form the two-dimensional layered structure MoS of multilayer chip2Nanometer sheet.The present invention prepares that cost 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 advantage of large-scale production.
Description
Technical field
The present invention relates to the preparing technical field 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 coefficient of friction is very low, easily slides;Covalent bond in layer is very
By force, illustrate that it has good mechanical strength, has good heat endurance in inert environments and freely hanged with surface
The features such as key, it can prevent from being pierced in metal surface protruding parts lubricating film, and can be right exposed to the sulphur atom of plane of crystal
Metal surface produces 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 coefficient of friction and carry
High-wearing feature, has good application prospect in tribology.Vattikuti et al. successfully synthesizes MoS2Nanometer sheet, it 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, ultrasonic water bath method, hydrodynamic, ball-milling method, steam blow etc..But the above method can not
Meet that step is simple simultaneously, the nanometer sheet number of plies is controllable and requirement of large-scale production.
The content of the invention
It is simple, controllable with good friction performance, the nanometer sheet number of plies based on method it is an object of the invention to provide one kind,
And beneficial to the two-dimensional nanostructure MoS of industrialized production2The preparation method of nanometer sheet.
The present invention comprises 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)After being mixed with the mixed solution of above-mentioned molybdenum source and sulphur source
Reacted;
3)Reaction is cooled to room temperature after terminating, and successively removes galapectite nanometer using hydrofluoric acid aqueous solution and aqueous hydrochloric acid solution washing
Pipe(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 wieners
Rice structure 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, and molybdenum disulfide is produced in a template
Nucleus, the nucleus of generation quickly grows 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 expansion 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 removing intermediary water, interlayer template action is made full use of.
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 is used is natural halloysite nanotubes, and cost is low, and stability is good.
2nd, the present invention prepares nanometer sheet using template to have taken into account step simultaneously simple, and the nanometer sheet number of plies is controllable and scale
The advantage of metaplasia production.
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, produce MoS2。
The step 1)In, the sulphur source is thiocarbamide or thioacetamide or vulcanized sodium.In a heated condition, these sulphur sources
H is produced with water reaction2S, produced hydrogen sulfide is very strong reducing agent, 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 mol ratio of molybdenum atom and sulphur atom be 1: 2~
4.The consumption of each material is easy to control solid-liquid volume ratio more than, and such as sulphur source is very few, then MoS2Easily it is oxidized;Such as sulphur source mistake
It is many, then waste raw material.
The step 1)In, the temperature conditionss of the dissolving are 30~60 DEG C.The special meaning dissolved using the temperature
Justice:Do not reacted between dissolution of raw material, two kinds of raw materials.
The step 2)In, the powdery halloysite nanotubes(HNTs)For 1-dimention nano tubular structure, length is 200~
500 nm, a diameter of 50~100nm, interlayer structure are 7~10.Use what the material of tool above characteristic was had by carrier
Special Significance:With larger external surface area, surface active groups are more, molybdenum disulfide can using outside surface area as template,
Prepare the more MoS of the number of plies2Nanometer sheet, and nanometer interlayer structure is 7~10, can be as template contral MoS2Nanometer
The number of plies of piece, the number of plies that nanometer sheet is made is 2~3 layers.
The step 2)In, the halloysite nanotubes and the mixing ratio of molybdenum source and sulphur source are 100 mL: 3.8~215 g:
3.2~330 g.The Special Significance being had using 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 occur;
4th, the controllable purpose of the nanometer sheet number of plies has been reached, the number of plies that can control to prepare 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
It is lower to carry out.The Special Significance being had using above reaction condition for present invention process:
1st, rotating speed is slower, causes HNTs powder to deposit, it is impossible to preferably to play template action;
2nd, under cryogenic, the crystallinity of the molybdenum disulfide of synthesis is poor;
3rd, with the rise of temperature, the crystallinity of the nanometer sheet of synthesis is preferable;
4th, the crystallinity of nanometer sheet, which has reached, further rises high temperature increases rotating speed after requirement, cause the waste of the energy;
The step 3)In, HF mass percent is HCl in 20~40%, aqueous hydrochloric acid solution in the hydrofluoric acid aqueous solution
Mass percent is 20~38%.The Special Significance that the concentration of each material has more than:
1st, because template HNTs is mainly by alumino-silicate, so template can be removed from hydrofluoric acid and hydrochloric acid;
2nd, the concentration of acid solution is too low, and template can not be removed thoroughly totally;
3rd, it is easy to purchase, convenient reduction production cost.
Brief description of the drawings
Fig. 1 is the flow chart of the inventive method preparation technology.
Fig. 2 is the gained MoS of example 12The SEM photograph of nanometer sheet.
Fig. 3 is the gained MoS of example 22The TEM photos of nanometer sheet.
Fig. 4 is the gained MoS of example 32The HRTEM photos of nanometer sheet.
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 is 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 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 molybdenum
Sour ammonium concentration is 0.05 g/ mL, and thiourea concentration is 0.09 g/ mL and the mol ratio of molybdenum atom and sulphur atom is 1:4 solution,
60 DEG C of 2 mL HNTs powder is added into above-mentioned mixed system, continues stirring and solid-liquid is well mixed, be transferred to poly- four
PVF for liner stainless steel autoclave in, react 48 h under 180 DEG C, 5 rpm rotating speeds.
Reaction terminates rear system and naturally cools to room temperature, respectively the hydrofluoric acid aqueous solution and matter with mass percent for 20%
It is 20% aqueous hydrochloric acid solution washing product to measure percentage, to remove template HNTs, then with deionized water, absolute ethyl alcohol washing 3
~5 times, centrifuge, filtering dries 12 h at 50 DEG C, black product is collected after grinding.
As shown in Fig. 2 SEM photograph, the MoS prepared2Laminated structure together is stacked above, the number of plies is 2 layers.
2nd, apply:
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery coefficient of friction
24.2% is have dropped 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 to molten at 40 DEG C
Solution, obtains molybdic acid ammonium concentration for 0.05 g/ mL, and thioacetamide concentration is 0.07 g/ mL and molybdenum atom and sulphur atom rub
You are than being 1:3 solution, 80 DEG C of 2 mL HNTs powder is added into above-mentioned mixed system, continues to stir so that solid-liquid mixing
Uniformly, it is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 24 h is reacted under 220 DEG C, 10 rpm rotating speeds.
Reaction terminates rear system and naturally cools to room temperature, respectively the hydrofluoric acid aqueous solution and matter with mass percent for 30%
It is 30% aqueous hydrochloric acid solution washing product to measure percentage, to remove template, then with deionized water, absolute ethyl alcohol washing 3~5
It is secondary, centrifuge, filtering dries 18 h at 60 DEG C, product is collected after grinding.
As shown in Fig. 3 TEM photos, the MoS prepared2Laminated structure together is stacked above, the number of plies is 8 layers.
2nd, apply:
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery coefficient of friction
19.7% is have dropped 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 dissolve at 60 DEG C, obtains
It is 0.06 g/ mL to molybdic acid na concn, vulcanization na concn is 0.05 g/ mL and the mol ratio of molybdenum atom and sulphur atom is 1:2
Solution, add 100 DEG C of 2 mL HNTs powder into above-mentioned mixed system, continue to stir solid-liquid is well mixed, turn
Move in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 12 h are reacted under 240 DEG C, 15 rpm rotating speeds.
Reaction terminates rear system and naturally cools to room temperature, respectively the hydrofluoric acid aqueous solution and matter with mass percent for 40%
It is 38% aqueous hydrochloric acid solution washing product to measure percentage, to remove template, then with deionized water, absolute ethyl alcohol washing 3~5
It is secondary, centrifuge, filtering dries 24 h at 80 DEG C, product is collected after grinding.
As shown in Fig. 4 HRTEM photos, the MoS prepared2Laminated structure together is stacked above, the number of plies is 5 layers.
2nd, apply:
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery coefficient of friction
19.7% is have dropped 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, obtains
Molybdic acid ammonium concentration is 0.19 g/ mL, and thiourea concentration is 0.33 g/ mL and the mol ratio of molybdenum atom and sulphur atom is 1:4 it is molten
In liquid, the HNTs powder that above-mentioned mixed solution is added to 60 DEG C of 100 mL, it is continuously agitated so that solid-liquid is well mixed,
It is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 48 h is reacted under 180 DEG C, 5 rpm rotating speeds.
Reaction terminates rear system and naturally cools to room temperature, respectively the hydrofluoric acid aqueous solution and matter with mass percent for 20%
It is 20% aqueous hydrochloric acid solution washing product to measure percentage, to remove template, then with deionized water, absolute ethyl alcohol washing 3~5
It is secondary, centrifuge, filtering dries 12 h at 50 DEG C, collects product after grinding, the MoS prepared2It is stacked above piece together
Shape structure, the number of plies is 2 layers.
2nd, apply:
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery coefficient of friction
36.8% is have dropped 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 to molten at 40 DEG C
Solution, obtains molybdic acid ammonium concentration for 0.19 g/ mL, and thioacetamide concentration is 0.24 g/ mL and molybdenum atom and sulphur atom rub
You are than being 1:In 3 solution, the HNTs powder that above-mentioned mixed solution is added to 80 DEG C of 100 mL, it is continuously agitated so that solid
Liquid is well mixed, and is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, anti-under 220 DEG C, 10 rpm rotating speeds
Answer 24 h.
Reaction terminates rear system and naturally cools to room temperature, 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 dried at 60 DEG C
Product is collected after 18 h, grinding, the MoS prepared2Laminated structure together is stacked above, the number of plies is 3 layers.
2nd, apply:
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery coefficient of friction
19.6% is have dropped 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, obtains
Molybdic acid ammonium concentration is 0.22 g/ mL, and thiourea concentration is 0.17 g/ mL and the mol ratio of molybdenum atom and sulphur atom is 1:2 it is molten
In liquid, the HNTs powder that above-mentioned mixed solution is added to 100 DEG C of 100 mL, it is continuously agitated so that solid-liquid is well mixed,
It is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 12 h is reacted under 240 DEG C, 15 rpm rotating speeds.
Reaction terminates rear system and naturally cools to room temperature, 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, centrifuged, and filtering dries 24 at 80 DEG C
Product is collected after h, grinding, the MoS prepared2Laminated structure together is stacked above, the number of plies is 5 layers.
2nd, apply:
Weigh the above-mentioned MoS of 16 mg2Nanometer sheet is dispersed in 500 SN base oils, rubbed to learn test discovery coefficient of friction
19.6% is have dropped compared to base oil.
The present invention is prepared for the homogeneous MoS of the number of plies using a kind of simple template2Oil adds based on nanometer sheet, research
Plus the greasy property of agent.
Claims (8)
1. a kind of two-dimensional nanostructure MoS2The preparation method of nanometer sheet, it is characterised in that comprise 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)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-
Should;
3)Reaction is cooled to room temperature after terminating, and successively removes galapectite nanometer 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 molybdenum source is ammonium molybdate or molybdenum
Sour sodium, the sulphur source is thiocarbamide or thioacetamide or vulcanized sodium.
3. preparation method according to claim 2, it is characterised in that the step 1)In, the mixing of the molybdenum source and sulphur source
The mol ratio of Molybdenum in Solution atom and sulphur atom is 1: 2~4.
4. the preparation method according to claim 1 or 2 or 3, it is characterised in that the step 1)In, the temperature of the dissolving
Condition is 30~60 DEG C.
5. preparation method according to claim 1, it is characterised in that the step 2)In, the powdery halloysite nanotubes
For 1-dimention nano tubular structure, length is 200~500 nm, and a diameter of 50~100nm, interlayer structure is 7~10.
6. preparation method according to claim 3, it is characterised in that the step 2)In, the halloysite nanotubes and molybdenum
The mixing ratio of source and sulphur source is 100 mL: 3.8~215 g: 3.2~330 g.
7. the preparation method according to claim 1 or 6, it is characterised in that the step 2)In, the reaction is in mixture
The temperature of system is 180~240 DEG C, carried out under conditions of 5~15 rpm rotating speeds.
8. preparation method according to claim 1, it is characterised in that the step 3)In, HF in the hydrofluoric acid aqueous solution
Mass percent be 20~40%, HCl mass percent is 20~38% in aqueous hydrochloric acid solution.
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Cited By (12)
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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 |
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 |
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 |
CN108893974A (en) * | 2018-06-05 | 2018-11-27 | 湖北大学 | One type petal molybdenum disulfide film and its preparation method and application |
CN108929742A (en) * | 2018-08-31 | 2018-12-04 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
CN110452677A (en) * | 2019-08-08 | 2019-11-15 | 河南郸城顺兴石油助剂有限公司 | One kind is based on modified MoS2The method for preparing drag reducer |
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CN114084876A (en) * | 2021-11-22 | 2022-02-25 | 安徽师范大学 | One-dimensional multilayer nano-chain composite material, preparation method thereof and application thereof in lithium ion battery |
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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 |
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 |
CN108893974B (en) * | 2018-06-05 | 2020-07-24 | 湖北大学 | Petal-like molybdenum disulfide film and preparation method and application thereof |
CN108893974A (en) * | 2018-06-05 | 2018-11-27 | 湖北大学 | One type petal molybdenum disulfide film and its preparation method and application |
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 |
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CN108929742B (en) * | 2018-08-31 | 2020-12-15 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
CN110452677A (en) * | 2019-08-08 | 2019-11-15 | 河南郸城顺兴石油助剂有限公司 | One kind is based on modified MoS2The method for preparing drag reducer |
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 |
CN113800568A (en) * | 2021-10-18 | 2021-12-17 | 上海交通大学 | Preparation method of two-dimensional laminated transition metal sulfide material |
CN114084876A (en) * | 2021-11-22 | 2022-02-25 | 安徽师范大学 | One-dimensional multilayer nano-chain composite material, preparation method thereof and application thereof in lithium ion battery |
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 |
CN114477287A (en) * | 2022-03-11 | 2022-05-13 | 合肥学院 | Method for enhancing lubricating property of flaky nano molybdenum disulfide by improving sheet layer bending rate |
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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