CN106145065B - Transition metal chalcogenide MX2Ultrathin nanometer piece, preparation method and its usage - Google Patents
Transition metal chalcogenide MX2Ultrathin nanometer piece, preparation method and its usage Download PDFInfo
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- CN106145065B CN106145065B CN201610524016.1A CN201610524016A CN106145065B CN 106145065 B CN106145065 B CN 106145065B CN 201610524016 A CN201610524016 A CN 201610524016A CN 106145065 B CN106145065 B CN 106145065B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The present invention provides a kind of transition metal chalcogenide MX2Ultrathin nanometer piece, preparation method and its usage, with MX2Element simple substance powder be raw material, will carry out ball milling activation with planetary ball mill after the two solid phase mixing, then fill this blend into stainless steel reaction container and synthesize MX using high temperature solid-state method under protective atmosphere2Precursor Powder；Then, by MX2Precursor Powder is encapsulated into vacuum ball grinder together with suitable absolute ethyl alcohol and surfactant, and under certain rotating speed and uses planetary ball mill ball milling in the regular hour, finally by washing, dry obtained MX2Ultrathin nanometer piece.The method of the present invention raw material is easy to get, technique is simple, parameter is easily-controllable, safety and environmental protection, and the product purity being prepared is high, yield is high, and has important application in the fields such as tribology, thermoelectricity, semiconductor, is expected to be used for large-scale industrial production.
Description
Technical field
The present invention relates to nano-lubricating material field, specifically a kind of transition metal chalcogenide MX2Ultrathin nanometer
Piece, preparation method and its usage.
Background technology
Transition metal chalcogenide, abbreviation TMDCs, commonly uses MX2Represent (M=Mo, W, Nb etc., X=S, Se, Te).Due to
Its unique structure and excellent physicochemical property, it has also become one of research hotspot of Nanotribology.Recently, nano material is made
For lube oil additive, in friction, educational circles has been obtained for widely studying, and some researches show that many nanometer sheets are as lubricating oil
Additive is respectively provided with good antiwear and antifriction effect, it might even be possible to plays repair to wear surface.Have in TMDCs similar
The piece laminate of graphite, is very strong covalent bond in layer, interlayer is then very weak Van der Waals Er Sili, between layers very
Easily it is stripped, and there is good anisotropy and relatively low friction coefficient.Therefore, MX is peeled off2Obtain ultra-thin nanometer
Piece has broad prospects in tribological field.
So far, people have carried out numerous studies in the synthesis of transition metal chalcogenide nano material, mainly
There are hydro-thermal method, thermal decomposition method, high-temperature gas-solid reaction, vapour deposition process, solid phase reaction etc..Wherein solid phase synthesis technique is applied to nothing
The synthesis of machine micro Nano material has the advantages that simple technique, easy to operate, temperature-controllable, reaction time are short.But solid phase method
The thickness of the nanometer sheet of preparation is larger, generally special using the typical structure of transition metal chalcogenide in 800nm or so, the present invention
Property, using the method for ball milling induction mechanical stripping, successfully by large-sized MX2Peel off into ultrathin nanometer piece.It is used as lubricating
Oil additive, when be subject to shearing force interlayer easily occurs is slided, while ultra-thin nanometer sheet can be more easily entered and rubbed
Wipe interface and form lubrication transfer membrane, the direct contact between avoiding friction secondary, so as to play the wear-resistant effect of anti-attrition.At present, ball
Mill stripping prepares transition metal chalcogenide MX2Ultrathin nanometer piece and based on oil additive be applied to tribological field and grinding
Study carefully it is relatively fewer, therefore, the present invention propose ball milling induction stripping method prepare MX2Ultrathin nanometer piece is of great significance.
The content of the invention
It is easy to get it is an object of the invention to provide a kind of raw material, technique is simple, yield is high and the ultra-thin MX of safety and environmental protection2Receive
The preparation method of rice piece and based on oil additive show preferable lubricity and wearability.
Above-mentioned purpose is achieved by the following technical solution：First, MX2Element powder pass through Solid phase synthesis for raw material
MX2Precursor Powder, then, is induced by ball milling and peels off MX2Ultra-thin nanometer sheet is made in Precursor Powder.
Transition metal chalcogenide MX2The preparation method of ultrathin nanometer piece, it is characterised in that comprise the following steps：
(1) according to 1：2.2 molar ratio weighs the powder of transition metal M and the powder of chalcogen X, wherein X powder mistake
Amount 10%；The two is mixed and is encapsulated into vacuum ball grinder together with abrading-ball, argon gas is passed through after vacuumizing, is made under an argon atmosphere
15h is dry grinded with planetary ball mill to reach activated sample and mixed uniformly purpose；
(2) ball milling material in (1) is positioned in vacuum drying chamber, after 60 DEG C of vacuum drying 2h, remains to react；
(3) question response thing in (2) is loaded into quartz ampoule, and vacuum sealing is carried out using tube sealing machine, then, by good seal
Quartz ampoule is placed in stainless steel hydrothermal reaction kettle, then kettle is placed in high temperature box type resistance furnace, according to the heating of 5~15 DEG C/min
In-furnace temperature is increased to 600~900 DEG C by speed, is kept the temperature furnace cooling after 0.5~2h, is obtained MX2Precursor Powder；
(4) MX in (3) is weighed2Precursor Powder, adds it in absolute ethyl alcohol, magnetic agitation 30min, is made
The suspended nitride of 50mg/mL, and suitable surfactant Arlacel-80 is added, play the role of stable dispersion；
(5) by the MX in (4)2Slurry is transferred to vacuum ball grinder, and ball milling induction machinery is carried out using planetary ball mill
Peel off, treat that ball milling is completed, the product of secondary ball milling is filtered, is washed, and 4h is dried in vacuo at 60 DEG C, finally obtain institute
MX processed2Ultrathin nanometer piece.
Further, the ratio of grinding media to material of planetary ball mill ball milling is 12 in the step (1)：1~8：1, rotating speed is
300rpm, sphere diameter 8mm.
Further, step (1) Central Plains feed powder specification is≤300 mesh, and purity is >=99.5%.
Further, the step (3) if in MX2For MS2Or MSe2, sintering temperature is 600~800 DEG C；If MX2For MTe2
Sintering temperature is 800 DEG C~900 DEG C.
Further, heat up in step (3) the high temperature chamber type electric resistance furnace according to the heating rate of 10 DEG C/min, insulation
1h。
Further, the quartz glass tube a diameter of 15mm, length 10cm sealed in the step (3).
Further, the volume fraction of surfactant Arlacel-80 used is 5% in the step (4).
Further, secondary ball milling carries out in argon gas atmosphere in the step (5), ratio of grinding media to material 10：1, sphere diameter 8mm,
Ball mill runs 10~20h under 250rpm rotating speeds.
The transition metal chalcogenide MX2Transition metal chalcogenide prepared by the preparation method of ultrathin nanometer piece is ultra-thin
Nanometer sheet, it is characterised in that the thickness of the ultrathin nanometer piece is 2~50nm.
The transition metal chalcogenide MX2Nano material prepared by the preparation method of ultrathin nanometer piece adds as lubricating oil
Add agent.
Using ball milling induction stripping method method, raw material is easy to get preparation method of the present invention, technique is simple, yield is high and pacifies
The ultra-thin MX that loopful is protected2Nanometer sheet, the product purity being prepared is high, yield is high, and in tribology, thermoelectricity, semiconductor etc.
There is important application in field, be expected to be used for large-scale industrial production.Prepared MX2Ultrathin nanometer piece can be used as lubricating oil
The use of additive simultaneously shows preferable lubricity and wearability.
Brief description of the drawings
Fig. 1 is NbTe produced by the present invention2Front and rear XRD spectra and NbTe are peeled off in the induction of sample ball milling2Ultrathin nanometer piece
EDS energy spectrum diagrams.
Fig. 2 is NbTe produced by the present invention2Front and rear scanning electron microscope (SEM) photo is peeled off in the induction of sample ball milling.
Fig. 3 is NbTe produced by the present invention2Atomic force microscope (AFM) picture of ultrathin nanometer piece.
Fig. 4 is WS produced by the present invention2Front and rear scanning electron microscope (SEM) photo is peeled off in the induction of sample ball milling.
Fig. 5 is NbSe produced by the present invention2Front and rear scanning electron microscope (SEM) photo is peeled off in the induction of sample ball milling.
Fig. 6 is that front and rear NbTe is peeled off in the ball milling induction obtained by the present invention2Sample is added in saxol not
With the fretting wear block diagram under load.
Fig. 7 is that front and rear WS is peeled off in the ball milling induction obtained by the present invention2Sample is added to what is measured in saxol
Friction coefficient curve figure.
Fig. 8 is that front and rear NbSe is peeled off in the ball milling induction obtained by the present invention2Sample, which is added in saxol, to be measured
Friction coefficient curve figure.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention can also pass through it
Its scheme for not departing from the technology of the present invention feature describes, therefore all within the scope of the present invention or in the equivalent scope of the invention
Change be included in the invention.
Embodiment 1：
NbTe is prepared in accordance with the following steps2Ultrathin nanometer piece：
(1) according to 1：The molar ratio of 2.2 (Te powder excessive 10%) weigh a certain amount of granularity be 300 mesh, purity be
The Te powder that 99.95% Nb powder and granularity is 300 mesh, purity is 99.95%, after the two is mixed, according still further to 10：1 ball material
Than the stainless steel abrading-ball for weighing 8mm, ball material is encapsulated into vacuum ball grinder together, argon gas is passed through after vacuumizing, in argon gas atmosphere
It is lower that 15h is dry grinded with the rotating speed of 300rpm to reach activated sample and mixed uniformly purpose using planetary ball mill；Then, will
Ball milling mixing material is positioned in vacuum drying chamber, after 60 DEG C of vacuum drying 2h, remains to react；
(2) question response thing is loaded to the quartz ampoule of a diameter of 15mm, and vacuum sealing is carried out using tube sealing machine, then, will
The quartz ampoule of good seal is placed in stainless steel hydrothermal reaction kettle, pays attention to preventing from exploding, then kettle is placed in high temperature box type resistance furnace,
In-furnace temperature is increased to 850 DEG C according to the heating rate of 10 DEG C/min, furnace cooling after 1h is kept the temperature, obtains NbTe2Front axle shell
End；
(3) NbTe is weighed2Precursor Powder 5g, adds it in 100mL absolute ethyl alcohols, and adds 5mL Arlacel-80s, magnetic
Power stirring 30min is modulated into NbTe2Suspended nitride；Then, by NbTe2Suspended nitride is transferred to vacuum ball grinder, in Ar atmosphere
It is lower that ball milling induction mechanical stripping 20h, ratio of grinding media to material 10 are carried out with the rotating speed of 250rpm using planetary ball mill：1, sphere diameter 8mm,
Treat that ball milling is completed, the product of secondary ball milling is filtered, is washed, and 4h is dried in vacuo at 60 DEG C, finally obtain made
NbTe2Ultrathin nanometer piece.
NbTe prepared by the XRD spectrum explanation of Fig. 1 a2XRD peak positions provided with standard diffraction figure (PDF No.21-0605)
Diffraction data it is consistent, find out that product only has two kinds of elements of Nb and Te and both atomic molar ratio from the EDS energy spectrum diagrams of Fig. 1 b
Close to NbTe2Stoichiometric ratio 1：2, it is two telluride niobiums to illustrate product.From the XRD spectrum of Fig. 1 a it is also seen that by ball
After mill induction mechanical stripping, diffraction maximum, which broadens, to die down, especially (002) peak, and product thickness substantially reduces after illustrating ball milling stripping.
Fig. 2 a are the NbTe peeled off without ball milling2The SEM figures of Precursor Powder, Fig. 2 b are the NbTe peeled off by ball milling2It is ultra-thin to receive
The SEM figures of rice piece, are clear that from figure and induce mechanical stripping, NbTe by ball milling2Lamellar spacing occur it is very bright
It is aobvious to reduce, the Nano grade of very little is dropped to from micron level.Fig. 3 be product AFM figure, from figure can with it is further seen that
NbTe2Ultrathin nanometer piece thickness is most of between 2~10nm.
Embodiment 2：
(1) according to 1：2.2 molar ratio weigh the W powder that granularity is 200 mesh, purity is 99.8% and granularity be 100 mesh, it is pure
Spend the S powder for 99.5%, S powder excessive 10%, after the two is mixed, according still further to 12：1 ratio of grinding media to material weighs the stainless steel mill of 8mm
Ball, is encapsulated into vacuum ball grinder by ball material, argon gas is passed through after vacuumizing together, under an argon atmosphere using planetary ball mill with
The rotating speed of 300rpm dry grinds 15h to reach activated sample and mixed uniformly purpose；Then, ball milling mixing material is positioned over vacuum
In drying box, after 60 DEG C of vacuum drying 2h, remain to react；
(2) question response thing is loaded to the quartz ampoule of a diameter of 15mm, and vacuum sealing is carried out using tube sealing machine, then, will
The quartz ampoule of good seal is placed in stainless steel hydrothermal reaction kettle, pays attention to preventing from exploding, then kettle is placed in high temperature box type resistance furnace,
In-furnace temperature is increased to 800 DEG C according to the heating rate of 5 DEG C/min, furnace cooling after 2h is kept the temperature, obtains WS2Precursor Powder；
(3) WS is weighed2Precursor Powder 5g, adds it in 100mL absolute ethyl alcohols, and adds 5mL Arlacel-80s, magnetic force
Stirring 30min is modulated into WS2Suspended nitride；Then, by WS2Suspended nitride is transferred to vacuum ball grinder, under an ar atmosphere using row
Planetary ball mill carries out ball milling induction mechanical stripping 15h, ratio of grinding media to material 10 with the rotating speed of 250rpm：1, sphere diameter 8mm, treats that ball milling is complete
Into, the product of secondary ball milling is filtered, is washed, and 4h is dried in vacuo at 60 DEG C, finally obtain made WS2It is ultra-thin to receive
Rice piece.
Fig. 4 a are the WS peeled off without ball milling2The SEM figures of Precursor Powder, Fig. 4 b are the WS peeled off by ball milling2It is ultra-thin
The SEM figures of nanometer sheet, are clear that from figure and induce mechanical stripping, WS by ball milling2Lamellar spacing occur it is very bright
It is aobvious to reduce, the Nano grade of very little is dropped to from micron level.
Embodiment 3：
(1) according to 1：2.2 molar ratio weigh the niobium powder that granularity is 300 mesh, purity is 99.95% and granularity be 200 mesh,
Purity is 99.9% Se powder, Se powder excessive 10%, after the two is mixed, according still further to 8：1 ratio of grinding media to material weighs the stainless steel of 8mm
Abrading-ball, is encapsulated into vacuum ball grinder by ball material, argon gas is passed through after vacuumizing, under an argon atmosphere using planetary ball mill together
15h is dry grinded with the rotating speed of 300rpm to reach activated sample and mixed uniformly purpose；Then, ball milling mixing material is positioned over very
In empty drying box, after 60 DEG C of vacuum drying 2h, remain to react；
(2) question response thing is loaded to the quartz ampoule of a diameter of 15mm, and vacuum sealing is carried out using tube sealing machine, then, will
The quartz ampoule of good seal is placed in stainless steel hydrothermal reaction kettle, pays attention to preventing from exploding, then kettle is placed in high temperature box type resistance furnace,
In-furnace temperature is increased to 750 DEG C according to the heating rate of 15 DEG C/min, furnace cooling after 1h is kept the temperature, obtains NbSe2Front axle shell
End；
(3) NbSe is weighed2Precursor Powder 5g, adds it in 100mL absolute ethyl alcohols, and adds 5mL Arlacel-80s, magnetic
Power stirring 30min is modulated into NbSe2Suspended nitride；Then, by NbSe2Suspended nitride is transferred to vacuum ball grinder, in Ar atmosphere
It is lower that ball milling induction mechanical stripping 10h, ratio of grinding media to material 10 are carried out with the rotating speed of 250rpm using planetary ball mill：1, sphere diameter 8mm,
Treat that ball milling is completed, the product of secondary ball milling is filtered, is washed, and 4h is dried in vacuo at 60 DEG C, finally obtain made
NbSe2Ultrathin nanometer piece.
Fig. 5 a and Fig. 5 b are that ball milling peels off front and rear NbSe respectively2SEM figure, be clear that from figure by ball milling
Induce mechanical stripping, NbSe2Lamellar spacing occur clearly reduce, the Nano grade of very little, ruler are dropped to from micron level
Very little about 50nm.
Embodiment 4：
By NbTe in embodiment 12Precursor Powder and NbTe2Ultrathin nanometer piece is added to atoleine base by 2% mass ratio
In plinth oil, and appropriate span-80 dispersants are added, ultrasonic wave disperses 30min, is configured to lubricating oil oil sample.In UMT-2 type frictions
Neat liquid paraffin base oil is investigated on abrasion tester and makes the tribological property of lubricating oil oil sample by oneself.45 are used in experiment#Steel
The GCr15 bearing steel balls of disk and a diameter of 4mm carry out ball-disc type revolution and rub, and load be 5~40N, rotating speed 100rpm, in fact
Test time 20min.
Neat liquid paraffin base oil is with containing 2wt%NbTe2Friction coefficient of the lubricating oil oil sample under different loads, mill
The results are shown in Figure 6 for loss rate, it is seen that NbTe prepared by the present invention2Ultrathin nanometer piece and initial NbTe2Compare, based on oil
Additive has more preferable friction and wear behavior, while also significantly improves the performance indicator of lubricating oil.
Embodiment 5：
By WS in embodiment 22Precursor Powder and WS2Ultrathin nanometer piece is added to liquid paraffin base oil by 2% mass ratio
In, and appropriate span-80 dispersants are added, ultrasonic wave disperses 30min, is configured to lubricating oil oil sample.In UMT-2 type fretting wears
Neat liquid paraffin base oil is investigated on testing machine and makes the tribological property of lubricating oil oil sample by oneself.45 are used in experiment#Steel disk with
The GCr15 bearing steel balls of a diameter of 4mm carry out ball-disc type revolution friction, load 10N, rotating speed 100rpm, experimental period
20min。
Neat liquid paraffin base oil is with containing 2wt%WS2Friction coefficient of lubricating oil curve it is as shown in Figure 7, it is seen that this hair
The WS of bright preparation2Ultrathin nanometer piece and initial WS2Compare, based on oil additive there is lower friction coefficient.
Embodiment 6：
By NbSe in embodiment 32Precursor Powder and NbSe2Ultrathin nanometer piece is added to atoleine base by 2% mass ratio
In plinth oil, and appropriate span-80 dispersants are added, ultrasonic wave disperses 30min, is configured to lubricating oil oil sample.In UMT-2 type frictions
Neat liquid paraffin base oil is investigated on abrasion tester and makes the tribological property of lubricating oil oil sample by oneself.45 are used in experiment#Steel
The GCr15 bearing steel balls of disk and a diameter of 4mm carry out ball-disc type revolution and rub, load 10N, rotating speed 100rpm, during experiment
Between 20min.
Neat liquid paraffin base oil is with containing 2wt%NbSe2Friction coefficient of lubricating oil curve it is as shown in Figure 8, it is seen that this
Invent the NbSe prepared2Ultrathin nanometer piece and initial NbSe2Compare, based on oil additive there is lower friction coefficient.
The embodiment is preferred embodiment of the invention, but present invention is not limited to the embodiments described above, not
Away from the present invention substantive content in the case of, those skilled in the art can make it is any it is conspicuously improved, replace
Or modification belongs to protection scope of the present invention.
Claims (8)
1. transition metal chalcogenide MX2The preparation method of ultrathin nanometer piece, it is characterised in that comprise the following steps：
(1) according to 1：2.2 molar ratio weighs the powder of transition metal M and the powder of chalcogen X, and wherein X powder is excessive
10%；The two is mixed and is encapsulated into vacuum ball grinder together with abrading-ball, argon gas is passed through after vacuumizing, is used under an argon atmosphere
Planetary ball mill dry grinds 15h to reach activated sample and mixed uniformly purpose；
(2) ball milling material in (1) is positioned in vacuum drying chamber, after 60 DEG C of vacuum drying 2h, remains to react；
(3) question response thing in (2) is loaded into quartz ampoule, and vacuum sealing is carried out using tube sealing machine, then, by the quartz of good seal
Pipe is placed in stainless steel hydrothermal reaction kettle, then kettle is placed in high temperature box type resistance furnace, according to the heating rate of 5~15 DEG C/min
In-furnace temperature is increased to 600~900 DEG C, furnace cooling after 0.5h~2h is kept the temperature, obtains MX2Precursor Powder；
(4) MX in (3) is weighed2Precursor Powder, adds it in absolute ethyl alcohol, magnetic agitation 30min, is made 50mg/mL's
Suspended nitride, and suitable surfactant Arlacel-80 is added, play the role of stable dispersion；
(5) by the MX in (4)2Slurry is transferred to vacuum ball grinder, and ball milling induction mechanical stripping is carried out using planetary ball mill,
Treat that ball milling is completed, the product of secondary ball milling is filtered, is washed, and 4h is dried in vacuo at 60 DEG C, finally obtain made MX2
Ultrathin nanometer piece.
2. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
The ratio of grinding media to material for stating planetary ball mill ball milling in step (1) is 12：1~8：1, rotating speed 300rpm, sphere diameter 8mm.
3. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
It is≤300 mesh to state step (1) Central Plains feed powder specification, and purity is >=99.5%.
4. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
State step (3) if in MX2For MS2Or MSe2, sintering temperature is 600~800 DEG C；If MX2For MTe2Sintering temperature is 800~900
℃。
5. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
State in step (3) high temperature chamber type electric resistance furnace and heat up according to the heating rate of 10 DEG C/min, keep the temperature 1h.
6. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
State the quartz glass tube a diameter of 15mm, length 10cm of sealing in step (3).
7. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
The volume fraction for stating surfactant Arlacel-80 used in step (4) is 5%.
8. transition metal chalcogenide MX according to claim 12The preparation method of ultrathin nanometer piece, it is characterised in that institute
State secondary ball milling in step (5) to carry out in argon gas atmosphere, ratio of grinding media to material 10：1, sphere diameter 8mm, ball mill is under 250rpm rotating speeds
Run 10~20h.
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