CN106623980A - Preparation method of metal molybdenum nanosheet - Google Patents
Preparation method of metal molybdenum nanosheet Download PDFInfo
- Publication number
- CN106623980A CN106623980A CN201610828412.3A CN201610828412A CN106623980A CN 106623980 A CN106623980 A CN 106623980A CN 201610828412 A CN201610828412 A CN 201610828412A CN 106623980 A CN106623980 A CN 106623980A
- Authority
- CN
- China
- Prior art keywords
- nanometer sheet
- preparation
- metal molybdenum
- molybdenum
- molybdenum nanometer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 102
- 239000011733 molybdenum Substances 0.000 title claims abstract description 102
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 71
- 239000002184 metal Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002135 nanosheet Substances 0.000 title abstract 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000012159 carrier gas Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000009413 insulation Methods 0.000 claims abstract description 9
- 239000010453 quartz Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 239000003708 ampul Substances 0.000 claims description 7
- 239000008246 gaseous mixture Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 239000005078 molybdenum compound Substances 0.000 claims description 3
- 150000002752 molybdenum compounds Chemical group 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 27
- 230000008569 process Effects 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 230000001788 irregular Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000033228 biological regulation Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 206010054949 Metaplasia Diseases 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000015689 metaplastic ossification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a metal molybdenum nanosheet. The method comprises the following steps: a molybdenum source is put in a tubular furnace; air in a quartz pipe is all exhausted; then, carrier gas is introduced for reaction in an insulation state after heating; and the metal molybdenum nanosheet is obtained by cooling to the room temperature after reaction. The prepared metal molybdenum nanosheet is sheet-shaped, macroscopically takes the shape of fluffy-accumulated sponges, and microscopically has irregular edges; the size is 0.1-2 microns; and the thickness is lower than 100 nm. The preparation method is simple in process, convenient to operate, cheap in raw materials, easy to obtain the raw materials, excellent in repeatability, high in efficiency, easy to realize large-scale preparation and production, lower in requirements on the preparation environments and excellent in application and industrial propsect.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to the preparation method of metal molybdenum nanometer sheet.
Background technology
In field of nanometer technology, in recent years two-dimensional material is developed rapidly so that nano lamellar material becomes again people
The focus of research.Because nano material often has the functional performances such as its unexistent light of correspondence block materials, electricity, magnetic, catalysis
And special mechanical mechanics property, so nano material has very wide potential application.For the preparation of nano material, one
As have two approach：" from bottom to top " prepare with " from top to bottom "." from bottom to top " preparation method has chemical vapour deposition technique,
For this method, nanocrystalline growth is substantially its growth with the atom comprising object element or molecular substance as presoma
Process can be classified as " nucleation-growth " mechanism.The method can grow multielement, complex structure, morphology controllable it is nanocrystalline, but
High to growing state modulator required precision, reappearance is poor, which greatly limits the scale of nano structural material
Metaplasia is produced, and relatively costly.The present invention proposes a kind of operation letter based on the complex art of molybdenum compound distillation and hydrogen reducing
Just, control accuracy is low for folk prescription, reproducible, the method that can prepare the molybdenum nanometer sheet of a large amount of high volumes.At present, because molybdenum is received
The property of ground rice body, its application development is very fast, has been widely used in industrial or agricultural field at present, such as rubber, plastics, make
The aspects such as paper, coating, food, water process.In recent years, because lightweight molybdenum powder can strengthen the performance of some materials, have very
Big application prospect.
The content of the invention
It is an object of the invention to provide a kind of preparation method of metal molybdenum nanometer sheet.The main feature of the preparation method exists
In including molybdenum source distillation and the balanced reaction of hydrogen reducing：Molybdenum source distils obtain molybdenum source steam at high temperature, in carrier gas gaseous mixture
By hydrogen reducing in atmosphere, and then obtain molybdenum nanometer sheet.Obtained molybdenum nanometer sheet is molybdenum simple substance, and pattern is sheet.
Based on above-mentioned purpose, following technical scheme is this invention takes.
A kind of preparation method of metal molybdenum nanometer sheet, comprises the steps：Effective heating that molybdenum source is placed in tube furnace
Region, the air in quartz ampoule is drained using vavuum pump, then passes to carrier gas, is reacted under keeping warm mode after intensification, reaction
After be cooled to room temperature, obtain the metal molybdenum nanometer sheet.
Further, the molybdenum source is molybdenum compound, including molybdenum trioxide or molybdate.
Further, the carrier gas is argon hydrogen gaseous mixture or nitrogen and hydrogen mixture, preferably 5-20vol%H2/ Ar gaseous mixtures,
More preferably 10vol%H2/ Ar gaseous mixtures.
Further, gas of carrier gas flow is 10～50sccm, preferably 10sccm during intensification.
Further, gas of carrier gas flow is 100～200sccm, preferably 100sccm during insulation.
Further, the speed of the intensification is 5～20 DEG C/min, preferably 20 DEG C/min.
Further, the temperature of the insulation is 790 DEG C～1000 DEG C, preferably 900 DEG C；The time of insulation be 60～
240min。
Obtained metal molybdenum nanometer sheet is macroscopically fluffy spongy to pile up, and has random edge shape on microcosmic
Looks, and size is at 0.1～2 μm, thickness<100nm.
Compared with prior art, the invention has the advantages that and beneficial effect：
（1）The method that the present invention prepares metal molybdenum nanometer sheet, process is simple, short preparation period is easy to operate, reproducible, effect
Rate is high, it is easy to accomplish large-scale production, relatively low to preparing environmental requirement, contributes to practical application and the industry of metal molybdenum nanometer sheet
Metaplasia is produced.
Description of the drawings
Fig. 1 is the TG-DTA analysis curve map of the molybdenum trioxide that the present invention is used；
Fig. 2 is the SEM of the molybdenum trioxide that the present invention is used（SEM）Figure；
Fig. 3 prepares metal molybdenum nanometer sheet process flow diagram for the present invention；
Fig. 4 is the X-ray diffractogram of metal molybdenum nanometer sheet obtained in embodiments of the invention 1；
Fig. 5 is the SEM of metal molybdenum nanometer sheet prepared by embodiments of the invention 1（SEM）Photo；
Fig. 6 is the high power SEM of metal molybdenum nanometer sheet prepared by embodiments of the invention 1（SEM）Photo；
Fig. 7 is the transmission electron microscope of metal molybdenum nanometer sheet prepared by the embodiment of the present invention 1（TEM）Photo；
Fig. 8 is the high resolution transmission electron microscopy of molybdenum nanometer sheet prepared by the embodiment of the present invention 1（TEM）Photo；
Fig. 9 is the SEAD spectrogram of metal molybdenum nanometer sheet obtained in the embodiment of the present invention 1；
Figure 10 is the SEM of metal molybdenum nanometer sheet prepared by embodiments of the invention 2（SEM）Photo；
Figure 11 is the SEM of metal molybdenum nanometer sheet prepared by embodiments of the invention 3（SEM）Photo；
Figure 12 is the SEM of metal molybdenum nanometer sheet prepared by embodiments of the invention 4（SEM）Photo；
Specific embodiment
By the following examples the present invention is further elaborated, but the invention is not restricted to following examples.
The TG-DTA analysis curve of the molybdenum trioxide that the present invention is used is as shown in figure 1, by TG-DTA result, sentence
The sublimation temperature of disconnected molybdenum oxide is 790 DEG C.At 790～1000 DEG C, molybdenum trioxide distils, three oxygen of the hydrogen being passed through and generation
Changing molybdenum steam carries out reduction reaction, forms molybdenum sheet.
The SEM figures of the molybdenum trioxide that the present invention is adopted are as shown in Figure 2.
It is as shown in Figure 3 that the present invention prepares molybdenum nanometer sheet process flow diagram.
Embodiment 1
Using the TG-DTA analysis curve of molybdenum trioxide as shown in Figure 1, the distillation rule of molybdenum trioxide is analyzed；And adopt Fig. 3
Shown process flow diagram prepares metal molybdenum nanometer sheet.
To be placed in porcelain boat without the molybdenum trioxide powder of any process, effective heating area porcelain boat being put into tube furnace
In the quartz ampoule of domain, the air in quartz ampoule is drained using vavuum pump, then pass to 10vol%H2/ Ar gases, 10 in heating process
vol% H2/ Ar gas flow rates are maintained at 10sccm, control heating rate for 20 DEG C/min；
When tubular type furnace temperature reaches 900 DEG C, regulation is passed through 10vol%H2The amount of/Ar is flow 100sccm, is incubated 2 hours, instead
Should after be cooled to room temperature, obtain metal molybdenum nanometer sheet.
By XRD results（Fig. 4）The product that sign the present embodiment is obtained is simple metal molybdenum.
As shown in Figure 5, Figure 6, the metal molybdenum nano flake for obtaining is macroscopically to pile up fluffy sponge to stereoscan photograph
Shape, size uniform and size are 0.1 ~ 2 μm on microcosmic, thickness<100nm, edge has a large amount of dendritic morphologies.
Transmission electron microscope photo shows that nanometer molybdenum sheet has ultra-thin thickness（Fig. 7）With good mono-crystalline structures（Figure
8）.
SEAD spectrogram（Fig. 9）Analysis show that the molybdenum nanometer sheet is cube phase structure.
Embodiment 2
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, reaction temperature is 790 DEG C, when tubular type furnace temperature reaches
During to 790 DEG C, regulation is passed through 10vol%H2The flow of/Ar is 100sccm, after reaction, closes tube furnace, is cooled to room temperature, is obtained
To metal molybdenum nanometer sheet.
The product that the present embodiment is obtained is similar to the result of embodiment 1, has equally grown metal molybdenum nanometer sheet；Obtained metal
The SEM figures of molybdenum nanometer sheet such as Figure 10, size uniform and size is 0.1 ~ 2 μm, thickness on microcosmic<100nm, edge has a large amount of branches
Shape structure.
Embodiment 3
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, reaction temperature is 1000 DEG C, when tubular type furnace temperature
When reaching 1000 DEG C, regulation is passed through 10vol%H2The flow of/Ar is 100sccm, after reaction, closes tube furnace, is cooled to room temperature,
Obtain metal molybdenum nanometer sheet.
The product that the present embodiment is obtained is similar to the result of embodiment 1, has equally grown metal molybdenum nanometer sheet；The metal for obtaining
The SEM figures of molybdenum nanometer sheet are as shown in figure 11, are to pile up fluffy spongy.
Embodiment 4
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, react heating rate and be set to 10 DEG C/min, react
Afterwards, tube furnace is closed, is cooled to room temperature, obtain metal molybdenum nanometer sheet.
The product that the present embodiment is obtained is similar to the result of embodiment 1, has equally grown metal molybdenum nanometer sheet；The metal for obtaining
The SEM figures of molybdenum nanometer sheet referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μ on microcosmic
M, thickness<100nm, edge has a large amount of dendritic morphologies.
Embodiment 5
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, react temperature retention time and be set to 60min, after reaction,
Tube furnace is closed, room temperature is cooled to, metal molybdenum nanometer sheet is obtained.
The product that the present embodiment is obtained is similar to the result of embodiment 1, has equally grown metal molybdenum nanometer sheet；The metal for obtaining
The SEM figures of molybdenum nanometer sheet referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μ on microcosmic
M, thickness<100nm, edge has a large amount of dendritic morphologies.
Embodiment 6
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, react temperature retention time and be set to 240min, after reaction,
Tube furnace is closed, room temperature is cooled to, metal molybdenum nanometer sheet is obtained.
The product that the present embodiment is obtained is similar to the result of embodiment 1, has equally grown metal molybdenum nanometer sheet；The metal for obtaining
The SEM figures of molybdenum nanometer sheet referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μ on microcosmic
M, thickness<100nm, edge has a large amount of dendritic morphologies.
Embodiment 7
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, when tubular type furnace temperature reaches 900 DEG C, regulation is passed through
10vol%H2The flow of/Ar is 200sccm, after reaction terminates, closes tube furnace, is cooled to room temperature, that is, obtain metal molybdenum nanometer
Piece.
The present embodiment result is similar to the result of embodiment 1, has equally prepared metal molybdenum nanometer sheet；The metal molybdenum for obtaining
The SEM figures of nanometer sheet referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μm on microcosmic,
Thickness<100nm, edge has a large amount of dendritic morphologies.
Embodiment 8
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, when tubular type furnace temperature reaches 900 DEG C, regulation is passed through
H2The volume fraction of/Ar is 5vol%H2/ Ar, after reaction terminates, closes tube furnace, is cooled to room temperature, that is, obtain metal molybdenum nanometer
Piece.
The present embodiment result is similar to the result of embodiment 1, has equally prepared metal molybdenum nanometer sheet；The metal molybdenum for obtaining
The SEM figures of nanometer sheet referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μm on microcosmic,
Thickness<100nm, edge has a large amount of dendritic morphologies.
Embodiment 9
According to molybdenum nanometer sheet prepared by the method in embodiment 1.Except for the difference that, when tubular type furnace temperature reaches 900 DEG C, regulation is passed through
H2The volume fraction of/Ar is 20vol%H2/ Ar, after reaction terminates, closes tube furnace, is cooled to room temperature, that is, obtain metal molybdenum nanometer
Piece.
The present embodiment result is similar to the result of embodiment 1, has equally prepared metal molybdenum nanometer sheet；The metal molybdenum for obtaining
The SEM figures of nanometer sheet referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μm on microcosmic,
Thickness<100nm, edge has a large amount of dendritic morphologies.
Embodiment 10
Molybdenum nanometer sheet is prepared according to the method in embodiment 1.Except for the difference that, heating rate is 5 DEG C/min, adjusts and is passed through when heating up
10vol%H2The flow of/Ar is 50sccm, after reaction terminates, closes tube furnace, is cooled to room temperature, that is, obtain metal molybdenum nanometer
Piece.
The present embodiment result is similar to 1 result is implemented, and has equally prepared metal molybdenum nanometer sheet；Obtained metal molybdenum nanometer
The SEM figures of piece referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μm, thickness on microcosmic<
100nm, edge has a large amount of dendritic morphologies.
Embodiment 11
Molybdenum nanometer sheet is prepared according to the method in embodiment 1.Except for the difference that, molybdenum trioxide nano band is adopted for molybdenum source, tube furnace
When temperature reaches 900 DEG C, regulation is passed through 10vol%H2The flow of/Ar is 100sccm, after reaction 120min, closes tube furnace, cold
But to room temperature, that is, metal molybdenum nanometer sheet is obtained.
The present embodiment result is similar to 1 result is implemented, and has equally prepared metal molybdenum nanometer sheet；Obtained metal molybdenum nanometer
The SEM figures of piece referring to shown in Fig. 5,6, being to pile up fluffy spongy, size uniform and size is 0.1 ~ 2 μm, thickness on microcosmic<
100nm, edge has a large amount of dendritic morphologies.
Embodiment 12
（1）To be positioned in porcelain boat as molybdenum source without the molybdenum trioxide powder of any process, porcelain boat is put into quartz ampoule, make
Molybdenum source is placed on diamond heating region, and the air in quartz ampoule is drained using vavuum pump, then passes to 10vol%H2/N2Gas
Body, the oxygen that so circulation is discharged in quartz ampoule for 3 times as far as possible.Then begin to heating, 10vol%H in heating process2/N2Gas stream
Speed is maintained at 10sccm, controls heating rate for 20 DEG C/min；
（2）When tubular type furnace temperature reaches 900 DEG C, by 10vol%H2/N2Flow is adjusted to 100sccm；The carrier gas flux passes through
Flowmeter is monitored；
（3）After 240min, after reaction terminates, tube furnace is closed, until temperature drops to room temperature.Obtain metal molybdenum nanometer sheet.
The present embodiment result is similar to the result of embodiment 1, has equally prepared metal molybdenum nanometer sheet.Obtained metal molybdenum is received
The SEM figures of rice piece are as shown in figure 12, are to pile up fluffy spongy.
The present invention being can be seen that from the result of embodiment, metal molybdenum nanometer sheet has been grown by simple method.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
In addition can also be combined between a variety of embodiments of the invention, as long as it is without prejudice to this
Bright thought, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of metal molybdenum nanometer sheet, it is characterised in that comprise the steps：Molybdenum source is placed in tube furnace
Effective heating area domain, the air in quartz ampoule is drained using vavuum pump, then passes to carrier gas, is carried out under keeping warm mode after intensification anti-
Should, room temperature is cooled to after reaction, obtain the metal molybdenum nanometer sheet.
2. the preparation method of a kind of metal molybdenum nanometer sheet according to claim 1, it is characterised in that obtained metal molybdenum is received
Rice piece is molybdenum simple substance, and pattern is sheet, macroscopically fluffy spongy to pile up, and has random edge shape on microcosmic
Looks, and size is 0.1～2 μm, thickness<100nm.
3. the preparation method of a kind of metal molybdenum nanometer sheet according to claim 1, it is characterised in that the molybdenum source is molybdenum
Compound, including molybdenum trioxide or molybdate.
4. the preparation method of a kind of metal molybdenum nanometer sheet according to claim 1, it is characterised in that the carrier gas is argon hydrogen
Gaseous mixture or nitrogen and hydrogen mixture.
5. the preparation method of a kind of metal molybdenum nanometer sheet according to claim 1, it is characterised in that the carrier gas is 5-
20vol% H2/ Ar gaseous mixtures.
6. a kind of preparation method of metal molybdenum nanometer sheet according to claim 1, it is characterised in that gas of carrier gas during intensification
Flow is 10～50sccm；Gas of carrier gas flow is 100～200sccm during insulation.
7. a kind of preparation method of metal molybdenum nanometer sheet according to claim 1, it is characterised in that gas of carrier gas during intensification
Flow is 10sccm；Gas of carrier gas flow is 100sccm during insulation.
8. a kind of preparation method of metal molybdenum nanometer sheet according to claim 1, it is characterised in that the speed of the intensification
For 5 ~ 20 DEG C/min.
9. a kind of preparation method of metal molybdenum nanometer sheet according to claim 1, it is characterised in that the temperature of the insulation
For 790 DEG C～1000 DEG C, the time of insulation is 60～240min.
10. a kind of preparation method of metal molybdenum nanometer sheet according to claim 1, it is characterised in that the temperature of the insulation
Spend for 900 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610828412.3A CN106623980B (en) | 2016-09-18 | 2016-09-18 | A kind of preparation method of metal molybdenum nanometer sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610828412.3A CN106623980B (en) | 2016-09-18 | 2016-09-18 | A kind of preparation method of metal molybdenum nanometer sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106623980A true CN106623980A (en) | 2017-05-10 |
| CN106623980B CN106623980B (en) | 2019-06-18 |
Family
ID=58851994
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610828412.3A Expired - Fee Related CN106623980B (en) | 2016-09-18 | 2016-09-18 | A kind of preparation method of metal molybdenum nanometer sheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106623980B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162058A (en) * | 2017-06-30 | 2017-09-15 | 华南理工大学 | A kind of molybdenum dioxide hexagonal nano-flake and preparation method thereof |
| CN114632943A (en) * | 2022-03-21 | 2022-06-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional metal nanosheet and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2398114A (en) * | 1942-09-12 | 1946-04-09 | Westinghouse Electric Corp | Reduction of molybdenum trioxide |
| CN101778683A (en) * | 2007-08-16 | 2010-07-14 | H.C.施塔克有限公司 | Nanostructured of forming by valve metal and valve metal protoxide and preparation method thereof |
| CN103801706A (en) * | 2012-11-09 | 2014-05-21 | 北京有色金属研究总院 | Molybdenum powder for ceramic metallizing and preparing method of molybdenum powder |
| CN104722771A (en) * | 2015-04-16 | 2015-06-24 | 柳州豪祥特科技有限公司 | Preparation method of molybdenum powder |
| CN105458280A (en) * | 2016-01-12 | 2016-04-06 | 金堆城钼业股份有限公司 | Preparation method for highly-dispersed ultrafine molybdenum powder with narrow particle size distribution |
-
2016
- 2016-09-18 CN CN201610828412.3A patent/CN106623980B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2398114A (en) * | 1942-09-12 | 1946-04-09 | Westinghouse Electric Corp | Reduction of molybdenum trioxide |
| CN101778683A (en) * | 2007-08-16 | 2010-07-14 | H.C.施塔克有限公司 | Nanostructured of forming by valve metal and valve metal protoxide and preparation method thereof |
| CN104889381A (en) * | 2007-08-16 | 2015-09-09 | H.C.施塔克有限公司 | Nanosize structures composed of valve metals and valve metal suboxides and process for producing them |
| CN103801706A (en) * | 2012-11-09 | 2014-05-21 | 北京有色金属研究总院 | Molybdenum powder for ceramic metallizing and preparing method of molybdenum powder |
| CN104722771A (en) * | 2015-04-16 | 2015-06-24 | 柳州豪祥特科技有限公司 | Preparation method of molybdenum powder |
| CN105458280A (en) * | 2016-01-12 | 2016-04-06 | 金堆城钼业股份有限公司 | Preparation method for highly-dispersed ultrafine molybdenum powder with narrow particle size distribution |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162058A (en) * | 2017-06-30 | 2017-09-15 | 华南理工大学 | A kind of molybdenum dioxide hexagonal nano-flake and preparation method thereof |
| CN114632943A (en) * | 2022-03-21 | 2022-06-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional metal nanosheet and preparation method and application thereof |
| CN114632943B (en) * | 2022-03-21 | 2023-10-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional metal nano sheet and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106623980B (en) | 2019-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108273541B (en) | Green and efficient preparation method and application of graphite-phase carbon nitride nanosheets | |
| CN102001650B (en) | Method for preparing graphene through chemical vapor deposition under cold cavity wall condition | |
| CN105668555B (en) | A kind of method for preparing three-dimensional grapheme | |
| CN106430128A (en) | Compounding method for nanometer ultrathin boron carbon nitrogen sheet | |
| CN106245001B (en) | The method that plasma enhanced chemical vapor deposition prepares hexagonal boron nitride and its hybrid structure | |
| CN107964680A (en) | A kind of method for preparing individual layer hexagonal boron nitride large single crystal | |
| CN102424375A (en) | Preparation method for vertical carbon nanotube array | |
| CN105821383A (en) | Method for preparing rhenium disulfide film | |
| Xu et al. | CTAB-assisted synthesis of unique 3D ZnO and the acetone sensing performances | |
| CN109437124A (en) | A method of synthesis single layer Transition-metal dichalcogenide | |
| CN106623980A (en) | Preparation method of metal molybdenum nanosheet | |
| CN105036096A (en) | Method for preparing high-purity boron nitride nanotubes through reaction gas vortexes | |
| CN106830081B (en) | A kind of MoO2The preparation method of nanometer rods | |
| CN107162058A (en) | A kind of molybdenum dioxide hexagonal nano-flake and preparation method thereof | |
| CN105543972B (en) | High-purity high-density MoO2The preparation method of lamellar nanostructured | |
| CN103160929B (en) | The preparation method of a kind of monocrystal AIN nano cone and nanometer sheet | |
| CN105810530B (en) | Nitrogen-doped graphene@SiO2The preparation method and application of Coaxial Nanotubes | |
| Cheng | Synthesis and characterisation of CuO nanorods via a hydrothermal method | |
| CN109095494B (en) | Preparation method of cuprous oxide nanowire material | |
| CN102815698A (en) | Method for synthesizing two-dimensional carbide through template restriction | |
| CN108408788B (en) | Preparation method of octahedral poly-crystal with directionally attached and grown pyrite nanosheets | |
| CN106115771A (en) | A kind of In2o3the preparation method that polyhedron micron is brilliant | |
| CN104419894B (en) | Controllable one-dimensional tellurium micro-nano structure film of wellability and preparation method thereof | |
| CN106702352B (en) | A kind of pulse laser assistant chemical vapor deposition growth system device and the method for preparing low-dimensional materials with it | |
| CN109336180B (en) | Method for growing ultra-long molybdenum oxide nanobelts |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190618 |