CN107539964A - A kind of selenizing molybdenum powder body material of hexagonal flake two and preparation method thereof - Google Patents
A kind of selenizing molybdenum powder body material of hexagonal flake two and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to a kind of artificial crystal growth new technology, more particularly to selenizing molybdenum powder body material of a kind of hexagonal flake two and preparation method thereof.The preparation method of the selenizing molybdenum powder body material of hexagonal flake two specifically comprises the following steps：Using simple substance molybdenum powder and simple substance selenium powder as raw material, absolute ethyl alcohol is first added into raw material, mixes, after first time ball milling, then adds cosolvent, cosolvent includes NaCl and KCl, adds absolute ethyl alcohol again, then carry out second of ball milling；Material after ball milling terminates is dried in 60~80 DEG C of drying box, and drying time is 18~24h, forms material；Material is ground into fine powder, fine powder is then pressed into tabletting；Tabletting is put into crucible, fluxing agent NaCl and KCl are then added into crucible；Crucible is put and calcined under nitrogen atmosphere；By the material cooling after calcining, washing, dry.
Description
Technical field
The invention belongs to a kind of artificial crystal growth new technology, more particularly to a kind of selenizing molybdenum powder body material of hexagonal flake two
And preparation method thereof.
Background technology
In recent years, two-dimension nano materials are drawn due to its unique structure and performance and in the application of micro-nano person in electronics
The extensive concern of people is played.Representative two-dimension nano materials are graphenes, and it has strong toughness, good conduction
The performances such as property, high electron mobility, have extensive potential application in fields such as nanoelectronics, photonic propulsion, sensors.So
And limit its application in microelectronics and optoelectronic areas because graphene lacks band gap.Two-dimentional Transition Metal Sulfur selenizing is closed
Thing (MoS2、MoSe2、WS2、WSe2) there is the two-dimension plane structure similar with graphene, and compared with graphene, two-dimentional mistake
Crossing metal sulphur selenium compound has less energy gap (1.1-1.9eV), compensate for graphene due to lacking direct band gap not
The defects of electricity device can be applied individually to any, so as to widely be studied.Two selenizing molybdenums are as magnesium-yttrium-transition metal disulphide
One kind in material family, not only possess all characteristics of above-mentioned magnesium-yttrium-transition metal disulphide, in addition with other disulphide
Compare, two selenizing molybdenums also possess the performances such as back-gate effect, solid lubrication, therefore become the focus studied now.At present, with
Society and economic fast development, country increasingly pay attention to environmental problem, and in the synthesis in chemical plant, energy-saving and emission-reduction are that enterprise can
The vital task and target of sustainable development.
But the hydrogen selenide gas of severe toxicity can be produced in the preparation process on two selenizing molybdenum nano materials, and after reaction
Waste material also have very big harm to environment.
The content of the invention
The selenizing hydrogen of severe toxicity can be produced in preparation process it is an object of the invention to overcome the selenizing molybdenum of prior art two
Body, and reacted waste material also has the defects of very big to environment, there is provided a kind of preparation of the selenizing molybdenum powder body material of hexagonal flake two
Method.
The invention provides a kind of preparation method of the selenizing molybdenum powder body material of hexagonal flake two to specifically comprise the following steps：
(1) using simple substance molybdenum powder and simple substance selenium powder as raw material, absolute ethyl alcohol, mixing, first time ball milling are first added into raw material
Afterwards, cosolvent is then added, cosolvent includes NaCl and KCl, adds absolute ethyl alcohol again, then carry out second of ball milling；
(2) raw material after second of the ball milling of step (1) is terminated is dried in 60~80 DEG C of drying box, drying time 18
~24h, form material；
(3) material that step (2) obtains is ground into fine powder, fine powder is then pressed into tabletting；
(4) tabletting that step (3) obtains is put into crucible, fluxing agent NaCl and KCl is then added into crucible；
(5) crucible is put and calcined under nitrogen atmosphere, calcining heat is 600~700 DEG C；
(6) material cooling, washing, dry, grinding after step (5) is calcined.
Specifically, in step (1), the mol ratio of simple substance molybdenum powder and simple substance selenium powder is 1:2.5~3.5, first add anhydrous
The volume of ethanol is that raw material is completely covered and is higher by 3~5mm of raw material surface by absolute ethyl alcohol.
Specifically, in step (1), cosolvent quality and raw material total mass ratio are 1:1~2；In step (1) and step
(4) in, fluxing agent NaCl and KCl mol ratio is 1:1, cosolvent quality and raw material total mass ratio are 1:1~2.
Specifically, in step (1), ball milling is carried out with steel ball, the total mass ratio of steel ball quality and raw material is 20~30:1.
Specifically, in step (1), the rotating speed of first time ball milling ball mill is 200~250 revs/min, first time ball milling ball
To consume time as 10-15h, the rotating speed of second of ball milling ball mill is 100~150 revs/min, second of Ball-milling Time be 30~
60min。
Specifically, in step (3), tabletting is rounded, a diameter of 20mm of round tablet.
Specifically, in step (4), fluxing agent NaCl and KCl mol ratio are 1:1, the mass ratio of fluxing agent and tabletting
For 1~3:1.
Specifically, 200 DEG C first are heated to 5~10 DEG C/min heating rate in step (5), during calcining, Ran Houbao
20~30min of temperature, then be heated to 600~700 DEG C with 5~10 DEG C/min heating rate and calcined, 2~3h is incubated again.
Specifically, in step (6), in washing, it is washed with deionized successively, absolute ethyl alcohol is washed, dry
When dry, drying temperature is 70 DEG C, and drying time is 24h.
In addition, present invention also offers six made from a kind of preparation method using the selenizing molybdenum powder body material of hexagonal flake two
The selenizing molybdenum powder body material of square piece shape two, the diameter of the selenizing molybdenum powder body material of hexagonal flake two is 1~3 μm, and thickness is 30nm.
Beneficial effects of the present invention：(1) preparation method of two selenizing molybdenum powder body materials of the invention belongs to environmentally friendly, instead
The hydrogen selenide gas and waste material of severe toxicity will not be produced during answering, not only energy-saving and emission-reduction, reduction environmental pollution, can also hold for China
Supervention exhibition lays the foundation, and has great importance to creating friendly environment society；(2) prior art prepares two selenium with solid phase method
When changing molybdenum, it is at 800 DEG C, two selenizing molybdenums is synthesized in vacuum or protective atmosphere, two selenizing molybdenum sizes of gained are larger, pattern
Heterogeneity, and when utilizing the preparation method of two selenizing molybdenum powder body materials of the invention, is calcined under nitrogen atmosphere, it is heated to 600~
700 DEG C, reaction temperature is greatly reduced, and the two selenizing molybdenum powder body materials prepared are in hexagonal flake, form is than more uniform, product
Yield be 90~95%；(3) when preparing two selenizing molybdenums with vapor phase method, its principle is first in SiO2One layer is coated in/Si substrates
MoO3, the substrate and selenium powder are placed in tube-type atmosphere furnace, substrate is placed on tube furnace central thermal zone position, and selenium powder, which is placed on, to be leaned on
Nearly air inlet area, the selenium steam and MoO generated after being gasified using selenium powder3Reaction two selenizing molybdenums of production, the preparation technology is more complicated, and
Simple, convieniently synthesized, the used low in raw material price of the preparation methods of two selenizing molybdenum powder body materials of the invention, has good business
Industry prospect, it is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the selenizing molybdenum powder body material of six side two prepared by the embodiment of the present invention 1；
Fig. 2 is the EDS collection of illustrative plates of the selenizing molybdenum powder body material of six side two prepared by the embodiment of the present invention 1；
Fig. 3 is field emission scanning electron microscope (SEM) figure of the selenizing molybdenum powder body material of six side two prepared by the embodiment of the present invention 1；
Fig. 4 is in the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, in step (4) plus
The step of entering cosolvent removes field emission scanning electron microscope (SEM) figure of rear prepared product；
Fig. 5 is in (3) step of the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, is not had
Have and fine powder is pressed into tabletting, but fine powder is directly placed into field emission scanning electron microscope (SEM) figure of the product prepared by crucible；
Fig. 6 is in (5) step of the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, is forged
Finally heated to 550 DEG C during burning, field emission scanning electron microscope (SEM) figure of the constant prepared product of other steps；
Fig. 7 is in (5) step of the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, is forged
Finally heated to 800 DEG C during burning, field emission scanning electron microscope (SEM) figure of the constant prepared product of other steps.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
First using simple substance molybdenum powder and simple substance selenium powder as raw material, the mol ratio of simple substance molybdenum powder and simple substance selenium powder is 1:2.5 pour into
In ball grinder, 15mL absolute ethyl alcohols are added into tank, then steel ball is added into tank, the total mass ratio of steel ball quality and raw material is
20:1, drum's speed of rotation is arranged to 200 revs/min, ball milling 10 hours.Ball grinder is opened after ball mill stopping, into slurry
Cosolvent is added, cosolvent quality and raw material total mass ratio are 1:1, cosolvent includes NaCl and KCl, NaCl and KCl mol ratios
It is 1:1,8mL absolute ethyl alcohols are added, drum's speed of rotation are arranged to 100 revs/min, again ball milling 30min.After ball milling
Slurry pours into beaker, is put into drying box drying, and drying box temperature is set to 60 DEG C, drying time 18h.Dried material is poured into
Fine powder is pressed into a diameter of 20mm disk into fine powder by mortar, hand lapping.Disk is put into crucible, then added into crucible
Enter cosolvent, cosolvent quality and raw material total mass ratio are 1:1, cosolvent includes NaCl and KCl, NaCl and KCl mol ratios are equal
For 1:1.Crucible is put into tube-type atmosphere furnace central thermal zone position, N is passed through into tube furnace2, it is warming up to 5 DEG C/min speed
200 DEG C and 20min is incubated, is then warming up to 600 DEG C with 5 DEG C/min speed again and is incubated 2h, furnace cooling to normal temperature.Will
Crucible after cooling is taken out from tube furnace, and powder therein is poured out, and is first cleaned once with the deionized water for being heated to 70 DEG C,
Cleaned twice with deionized water at normal temperature again, the material after cleaning is put into drying box 70 finally washes of absolute alcohol with twice
24h is dried at a temperature of DEG C, finally dried material is taken out and wears into fine powder by hand with mortar, just obtains six required sides two
Selenizing molybdenum powder body material, the yield of the selenizing molybdenum powder body material of six side two is 93%.
Embodiment 2
First using simple substance molybdenum powder and simple substance selenium powder as raw material, the mol ratio of simple substance molybdenum powder and simple substance selenium powder is 1:3 pour into ball
In grinding jar, 15mL absolute ethyl alcohols are added into tank, then steel ball is added into tank, the total mass ratio of steel ball quality and raw material is 25:
1, drum's speed of rotation is arranged to 225 revs/min, ball milling 13 hours.Ball grinder is opened after ball mill stopping, being added into slurry
Cosolvent, cosolvent quality and raw material total mass ratio are 1:1.5, cosolvent includes NaCl and KCl, NaCl and KCl mol ratios are equal
For 1:1,8mL absolute ethyl alcohols are added, drum's speed of rotation are arranged to 125 revs/min, again ball milling 45min.By the slurry after ball milling
Material pours into beaker, is put into drying box drying, and drying box temperature is set to 70 DEG C, drying time 21h.Dried material is poured into and ground
Fine powder is pressed into a diameter of 20mm disk into fine powder by alms bowl, hand lapping.Disk is put into crucible, then added into crucible
Cosolvent, cosolvent quality and raw material total mass ratio are 1:1.5, cosolvent includes NaCl and KCl, NaCl and KCl mol ratios are equal
For 1:1.Crucible is put into tube-type atmosphere furnace central thermal zone position, N is passed through into tube furnace2, it is warming up to 8 DEG C/min speed
200 DEG C and 25min is incubated, is then warming up to 650 DEG C with 8 DEG C/min speed again and is incubated 2.5h, furnace cooling to normal temperature.
Crucible after cooling is taken out from tube furnace, powder therein is poured out, first cleans one with the deionized water for being heated to 70 DEG C
It is secondary, then cleaned twice with deionized water at normal temperature, the material after cleaning is put into drying box and existed washes of absolute alcohol with twice finally
24h is dried at a temperature of 70 DEG C, finally dried material is taken out and wears into fine powder by hand with mortar, just obtains six required sides
Two selenizing molybdenum powder body materials, the yield of the selenizing molybdenum powder body material of six side two is 91%.
Embodiment 3
First using simple substance molybdenum powder and simple substance selenium powder as raw material, the mol ratio of simple substance molybdenum powder and simple substance selenium powder is 1:3.5 pour into
In ball grinder, 15mL absolute ethyl alcohols are added into tank, then steel ball is added into tank, the total mass ratio of steel ball quality and raw material is
30:1, drum's speed of rotation is arranged to 250 revs/min, ball milling 15 hours.Ball grinder is opened after ball mill stopping, into slurry
Cosolvent is added, cosolvent quality and raw material total mass ratio are 1:2, cosolvent includes NaCl and KCl, NaCl and KCl mol ratios
It is 1:1,8mL absolute ethyl alcohols are added, drum's speed of rotation are arranged to 150 revs/min, again ball milling 60min.After ball milling
Slurry pours into beaker, is put into drying box drying, and drying box temperature is set to 80 DEG C, drying time 24h.Dried material is poured into
Fine powder is pressed into a diameter of 20mm disk into fine powder by mortar, hand lapping.Disk is put into crucible, then added into crucible
Enter cosolvent, cosolvent quality and raw material total mass ratio are 1:2, cosolvent includes NaCl and KCl, NaCl and KCl mol ratios are equal
For 1:1.Crucible is put into tube-type atmosphere furnace central thermal zone position, N is passed through into tube furnace2, heated up with 10 DEG C/min speed
To 200 DEG C and 30min is incubated, then 700 DEG C is warming up to 10 DEG C/min speed again and is incubated 3h, furnace cooling is to often
Temperature.Crucible after cooling is taken out from tube furnace, powder therein is poured out, is first cleaned with the deionized water for being heated to 70 DEG C
Once, then with deionized water at normal temperature clean twice, the material after cleaning is put into drying box finally washes of absolute alcohol with twice
24h is dried at a temperature of 70 DEG C, finally dried material is taken out and wears into fine powder by hand with mortar, just obtains required six
Two selenizing molybdenum powder body materials of side, the yield of the selenizing molybdenum powder body material of six side two is 92%.
Fig. 1 is the XRD spectrum of the selenizing molybdenum powder body material of six side two prepared by the embodiment of the present invention 1, as can be seen from the figure
That prepared is pure MoSe2；Fig. 2 is the EDS collection of illustrative plates of the selenizing molybdenum powder body material of six side two prepared by the embodiment of the present invention 1,
Only Se elements and Mo elements are found out in figure, the atomic ratio of two elements is 1.98:1, it is pure to illustrate prepared product
MoSe2；Fig. 3 is field emission scanning electron microscope (SEM) figure of the selenizing molybdenum powder body material of six side two prepared by the embodiment of the present invention 1, from
It can be seen that the prepared selenizing molybdenum powder shape of six side two is in six square pieces in Fig. 3, six square piece diameters are about in 1~3 μm, thickness
30nm。
Fig. 4 is in the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, in step (4) plus
The step of entering cosolvent removes field emission scanning electron microscope (SEM) figure of rear prepared product.
Fig. 5 is in (3) step of the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, is not had
Have and tabletting is made in fine powder, but fine powder is directly placed into field emission scanning electron microscope (SEM) figure of the product prepared by crucible.
Fig. 6 is in (5) step of the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, is forged
Finally heated to 550 DEG C during burning, field emission scanning electron microscope (SEM) figure of the constant prepared product of other steps.
Fig. 7 is in (5) step of the preparation method of the selenizing molybdenum powder body material of 1 hexagonal flake of the embodiment of the present invention two, is forged
Finally heated to 800 DEG C during burning, field emission scanning electron microscope (SEM) figure of the constant prepared product of other steps.
If the step of can be seen that addition cosolvent that step (4) is middle in the preparation from Fig. 4~Fig. 7 is removed；Preparation method
(3) step in, tabletting is not made in fine powder, but fine powder is directly placed into crucible；(5) step of preparation method
In, it is finally heated into 550 DEG C or (5) step of preparation method during calcining, during calcining prepared by finally heated to 800 DEG C
The size of product differs, pattern heterogeneity, and shape is not hexagonal flake, but shows substandard shape, and product is not
It is the selenizing molybdenum powder body material of hexagonal flake two.Therefore the step of adding cosolvent the preparation process the step of in (4), preparation method
(3) step in tabletting is made in fine powder, be then placed in crucible, preparation method (5) step in, it is finally heated during calcining
To 550 DEG C or finally heated to 800 DEG C are all the necessary conditions for preparing the selenizing molybdenum powder body material of hexagonal flake two of the present invention.
The above is only the section Example of the present invention, any formal limitation not done to the present invention, it is every according to
Any simple modification made according to the technical spirit of the present invention to above-described embodiment, equivalent variations and modification, belong to the present invention
In the range of technical scheme.
Claims (10)
1. a kind of preparation method of the selenizing molybdenum powder body material of hexagonal flake two, it is characterised in that specifically comprise the following steps：
(1) using simple substance molybdenum powder and simple substance selenium powder as raw material, absolute ethyl alcohol is first added into raw material, is mixed, after first time ball milling, so
After add cosolvent, cosolvent includes NaCl and KCl, adds absolute ethyl alcohol again, then carry out second of ball milling；
(2) raw material after second of the ball milling of step (1) is terminated is dried in 60~80 DEG C of drying box, and drying time is 18~
24h, form material；
(3) material that step (2) obtains is ground into fine powder, fine powder is then pressed into tabletting；
(4) tabletting that step (3) obtains is put into crucible, fluxing agent NaCl and KCl is then added into crucible；
(5) crucible is put and calcined under nitrogen atmosphere, calcining heat is 600~700 DEG C；
(6) material cooling, washing, dry, grinding after step (5) is calcined.
2. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(1) in, the mol ratio of simple substance molybdenum powder and simple substance selenium powder is 1:2.5~3.5, the volume for first adding absolute ethyl alcohol is that absolute ethyl alcohol will
Raw material is completely covered and is higher by 3~5mm of raw material surface.
3. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(1) in, cosolvent quality and raw material total mass ratio are 1:1~2；In step (1) and step (4), fluxing agent NaCl and KCl rub
Your ratio is 1:1, cosolvent quality and raw material total mass ratio are 1:1~2.
4. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(1) in, ball milling is carried out with steel ball, the total mass ratio of steel ball quality and raw material is 20~30:1.
5. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(1) in, the rotating speed of first time ball milling ball mill is 200~250 revs/min, and first time ball milling Ball-milling Time is 10~15h, second
The rotating speed of secondary ball milling ball mill is 100~150 revs/min, and second of Ball-milling Time is 30~60min.
6. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(3) in, tabletting is rounded, a diameter of 20mm of round tablet.
7. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(4) in, fluxing agent NaCl and KCl mol ratio are 1:1, the mass ratio of fluxing agent and tabletting is 1~3:1.
8. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(5) 200 DEG C first are heated to 5~10 DEG C/min heating rate in, during calcining, is then incubated 20~30min, then with 5~10
DEG C/min heating rate is heated to 600~700 DEG C and calcined, 2~3h is incubated again.
9. the preparation method of the selenizing molybdenum powder body material of hexagonal flake two according to claim 1, it is characterised in that：In step
(6) in, in washing, it is washed with deionized successively, absolute ethyl alcohol is washed, when drying, drying temperature is 70 DEG C, is done
The dry time is 24h.
10. made from a kind of preparation method using the selenizing molybdenum powder body material of hexagonal flake two according to claims 1 to 9
The selenizing molybdenum powder body material of hexagonal flake two, it is characterised in that：The shape of the selenizing molybdenum powder body material of hexagonal flake two is in six square pieces, and six
The diameter of square piece is 1~3 μm, and thickness is 30nm.
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| CN113292322A (en) * | 2021-05-18 | 2021-08-24 | 重庆科技学院 | Method for preparing graphene reinforced non-metal-based composite material by adopting step-by-step feeding ball milling and hot-pressing sintering |
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