CN104846428B - A kind of method that metal fusing agent method grows transient metal chalcogenide compound crystal - Google Patents
A kind of method that metal fusing agent method grows transient metal chalcogenide compound crystal Download PDFInfo
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Abstract
The present invention relates to a kind of method that metal fusing agent method grows transient metal chalcogenide compound crystal, including step is as follows：(1) simple substance M, simple substance X and simple substance Sn are mixed, in 1 × 10‑3‑1×10‑4Under the vacuum degree condition of Pa, 1,100 1150 DEG C are warming up to, are incubated 20 40h；M is Cr, Mo or W, and X is S, Se or Te；(2) first stage cooling is carried out with the rate of temperature fall of 16 DEG C/h, makes crystal spontaneous crystallization, when temperature is down to 900 1000 DEG C, be incubated 20 40h；Then quench, room temperature is cooled in 5 10min, is obtained final product.Operating condition of the present invention is easily realized, controllable, raw material are easy to get, low price, and the crystal mass for obtaining is high, has very big application prospect in terms of photon, photoelectricity and electronic device.
Description
Technical field
The present invention relates to a kind of method that metal fusing agent method grows transient metal chalcogenide compound crystal, belongs to crystal life
Long technical field.
Background technology
With science and technology and expanding economy, the base support material silicon of information-intensive society will reach its physics pole
Limit, the substitution material for finding silicon are extremely urgent.In recent years, it has been found that transient metal chalcogenide compound is due to excellent quasiconductor
Performance, it is possible to which surmounting Graphene becomes the substitution material of silicon.And, this kind of material also has important in fields such as photon, photoelectricity
Application prospect.Transient metal chalcogenide compound (TMDCs) chemical formula is MX2(M=Cr, Mo, W；X=S, Se, Te), belong to six
Prismatic crystal system, is layered semiconductor material, is combined by weak Van der Waals force between layers, it is possible to peel off into and Graphene
Similar monolayer or a few layer films.This kind of thin film is by the scale down of existing semiconductor technology to atom magnitude.People utilize this
Plant monolayer or which floor TMDCs thin film produces various functions device, for example：MoS2、MoSe2、WS2、WSe2Etc. can be fabricated to
Field-effect transistor, can obtain higher carrier mobility and current on/off ratio；Using MoS2Heliosensitivity and gas sensing property,
Photoresponse device and various gas detectors can be fabricated to；Use MoS2As saturated absorbing body with the laser；MoS2、WS2Deng
Material as lithium ion battery and the anode material of Magnesium ion battery, can improve the charge and discharge capacitance amount of battery；In addition, organic
The research of the aspects such as light emitting diode, memorizer is all underway.Generally speaking, transient metal chalcogenide compound is in photon, electricity
There is good application prospect in terms of the micro-nano electronic device such as son, photoelectricity, and how to prepare high-quality transient metal chalcogenide
Solvate crystal, becomes the emphasis of research.
The method for preparing transient metal chalcogenide compound at present mainly has hydro-thermal method, chemical vapour deposition technique, thermal decomposition method
Deng, the synthesis nanometer sheet of transient metal chalcogenide compound, thin film or small crystalss can be grown by these methods, but at present
The large-sized crystal of high-quality is obtained by these methods are more difficult.
The content of the invention
For the deficiencies in the prior art, the present invention proposes that a kind of metal fusing agent method growth transient metal chalcogenide compound is brilliant
The method of body, the method can grow and obtain the large-sized crystal of high-quality, can be used in the various devices in the fields such as making information, photoelectricity
Part.
Term explanation：
Transient metal chalcogenide compound according to the present invention, formula are MX2, wherein M is Cr, Mo or W, and X is S, Se or Te.
Technical solution of the present invention is as follows：
A kind of method that metal fusing agent method grows transient metal chalcogenide compound crystal, including step is as follows：
(1) by M, X, Sn atomic molar ratio be 1：2：(5-20), simple substance M, simple substance X and simple substance Sn are mixed, in 1 × 10-3-
1×10-4Under the vacuum degree condition of Pa, 1100-1150 DEG C is warming up to, is incubated 20-40h；
Described M is Cr, Mo or W, and described X is S, Se or Te；
(2) first stage cooling is carried out with the rate of temperature fall of 1-6 DEG C/h, makes crystal spontaneous crystallization, when temperature is down to 900-
When 1000 DEG C, 20-40h is incubated；Then quench, room temperature is cooled in 5-10min, obtains MX2Crystal.
, according to the invention it is preferred to, in step (1), M, X, Sn atomic molar ratio is 1：2：(7.5-10), temperature retention time is
20-40h；
Preferably, described M is Mo or W；Described X is S.
, according to the invention it is preferred to, in step (2), the rate of temperature fall of first stage cooling is 2-4 DEG C/h.
, according to the invention it is preferred to, in step (2), the mode of quenching is centrifugal quenching, or, remove the Sn of molten condition
Deca water afterwards.
, according to the invention it is preferred to embodiment it is as follows：
(1) by M, X, Sn atomic molar ratio be 1：2：(5-20), simple substance M, simple substance X and simple substance Sn are mixed, quartz is put into
Guan Zhong, makes vacuum in quartz ampoule reach 1 × 10 using vacuum pump evacuation-3-1×10-4Pa, then using oxyhydrogen flame by stone
The sintering sealing of English pipe；Quartz ampoule is put in shaft furnace, 1100-1150 DEG C is warming up to, 20-40h is incubated；
Described M is Cr, Mo or W, and described X is S, Se or Te；
(2) first stage cooling is carried out with the rate of temperature fall of 1-6 DEG C/h, makes crystal spontaneous crystallization, when temperature is down to 900-
When 1000 DEG C, 20-40h is incubated；
Then quartz ampoule is taken out from shaft furnace rapidly, then quenched, be allowed to room temperature is cooled in 5-10min, obtain MX2
Crystal.
The inventive method can obtain the high-quality MX of 0.5-9mm2Crystal.
, according to the invention it is preferred to, the MX2Crystal is MoS2、MoSe2、MoTe2、WS2、WSe2、WTe2Or CrSe2。
The principle of the present invention：
The metal method of fluxing is a kind of conventional method of field of crystal growth, but is directed to the not all metal of Cr, Mo or W
Flux is can serve as, if flux metal selects improper, other compounds will be produced in crystal growing process, from
And cannot get monocrystalline, have a strong impact on the quality of crystal.The present invention is explored and is tested through long-time, and selection uses metal Sn conducts
Flux；The fusing point of Sn is relatively low, and molten condition is constantly in crystal growing process, using the side being centrifuged in quenching process
Sn centrifugations under molten condition can be come by formula, and Sn is dissolved in acid, can thoroughly be gone with acid solution immersion crystal
Except metal fusing agent Sn, high-quality monocrystalline MX is obtained2；Also can be in Deca water flexible modulation quenching process in quenching process
Rate of temperature fall.
In the present invention, the first stage speed of cooling is most important, and rate of temperature fall is too fast, the crystal very little for obtaining, and affects
Using rate of temperature fall is excessively slow, and the crystal for obtaining is polycrystalline, has a strong impact on crystal mass.The present invention is explored through long-time and real
Test, select the rate of temperature fall of 1-6 DEG C/h interval, obtain that quality is good, the suitable monocrystalline MX of crystal size2。
Beneficial effects of the present invention are as follows：
1st, condition needed for the inventive method is simple, and growth cycle is 4-20 days, you can obtain millimetre-sized high-quality
Transient metal chalcogenide compound crystal, growth cycle are short, can be used in the various devices in the fields such as making information, photoelectricity.
2nd, the inventive method operating condition is easily realized, controllable, raw material are easy to get, low price, and crystal is easily divided with flux
From without other by-products.
3rd, the grade MX that the inventive method is obtained2Monocrystalline it is superior in quality, it is steady with very high chemical stability and heat
It is qualitative.
Description of the drawings
Fig. 1 is the MoS that the embodiment of the present invention 1 is obtained2The X-ray diffractogram of crystal.
Fig. 2 obtains MoS for the embodiment of the present invention 12The crystal structure figure of crystal.
Fig. 3 is the MoS that the embodiment of the present invention 2 is obtained2The photo in kind of crystal.
Fig. 4 is the MoS that comparative example of the present invention 1 is obtained2The photo in kind of crystal.
Fig. 5 is the MoSe that the embodiment of the present invention 5 is obtained2The photo in kind of crystal.
Specific embodiment
Below by specific embodiment and combine accompanying drawing the present invention will be further described, but not limited to this.
Embodiment 1：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoS2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance S, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the speed cooling of 6 DEG C/h, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C
When, after 20h being incubated at 900 DEG C, take out quartz ampoule rapidly from shaft furnace, be then centrifuged for quenching, be allowed to room is cooled in 10min
Temperature, that is, obtain the MoS of silver gray shape 0.5mm × 1mm2Crystal.
The MoS that test the present embodiment is obtained2The X-ray diffractogram of monocrystalline, as shown in Figure 1.As shown in Figure 1, X-ray diffraction
Figure is consistent with Theoretical Calculation, and only shows the diffraction maximum in [00L] direction, illustrates the MoS for obtaining2The natural-surface of crystal is crystallization
Learn ab planes.
Embodiment 2：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoS2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance S, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 2 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 10min,
Silver gray 3mm × 4mm lamellars MoS are obtained2Crystal, under this rate of temperature fall, crystal structure is best in quality.
Comparative example 1：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoS2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance S, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 0.5 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C
When, after 20h being incubated at 900 DEG C, take out quartz ampoule rapidly from shaft furnace, be then centrifuged for quenching, be allowed to be cooled to room in 10min
Temperature, that is, obtain silver gray 7mm × 8mm lamellars MoS2Crystal.
The crystal thickness that this comparative example is obtained is significantly increased compared with the crystal that embodiment 1 and embodiment 2 are obtained, crystallogram
As shown in figure 4, as shown in Figure 4, crystal is evident as polycrystalline, and crystalline quality is poor.
Embodiment 3：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoS2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance S, simple substance Sn according to mol ratio 1：2：5 carry out dispensing, uniform to mix, and are put into clean
High purity quartz pipe in, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using oxyhydrogen flame
Quartz ampoule sintering is sealed；Quartz ampoule is put in shaft furnace, 1100 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 6 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 5min,
Silver gray grade lamellar MoS is obtained2Crystal.
Embodiment 4：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoS2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance S, simple substance Sn according to mol ratio 1：2：20 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1100 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 6 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, remove Deca water after the Sn of molten condition, be allowed in 8min
Room temperature is cooled to, that is, obtains silver gray grade lamellar MoS2Crystal.
Embodiment 5：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoSe2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance Se, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 4 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 10min,
Silver gray MoSe is obtained2Crystal.
Embodiment 6：
A kind of metal fusing agent method grows transient metal chalcogenide compound MoTe2The method of crystal, including step is as follows：
(1) by raw material simple substance Mo, simple substance Te, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1100 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 3 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 1000 DEG C,
After 20h is incubated at 1000 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 7min,
Silver gray MoTe is obtained2Crystal.
Embodiment 7：
A kind of metal fusing agent method grows transient metal chalcogenide compound WS2The method of crystal, including step is as follows：
(1) by raw material simple substance W, simple substance S, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into clean
High purity quartz pipe in, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using oxyhydrogen flame
Quartz ampoule sintering is sealed；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 4 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 5min,
Silver gray WS is obtained2Crystal.
Embodiment 8：
A kind of metal fusing agent method grows transient metal chalcogenide compound WSe2The method of crystal, including step is as follows：
(1) by raw material simple substance W, simple substance Se, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 2 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 9min,
Silver gray WSe is obtained2Crystal.
Embodiment 9：
A kind of metal fusing agent method grows transient metal chalcogenide compound WTe2The method of crystal, including step is as follows：
(1) by raw material simple substance W, simple substance Te, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 1 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 6min,
Silver gray WTe is obtained2Crystal.
Embodiment 10：
A kind of metal fusing agent method grows transient metal chalcogenide compound CrSe2The method of crystal, including step is as follows：
(1) by raw material simple substance Cr, simple substance Se, simple substance Sn according to mol ratio 1：2：10 carry out dispensing, uniform to mix, and are put into dry
In net high purity quartz pipe, make in quartz ampoule, to reach 1 × 10 using vacuum pump evacuation-3The vacuum of Pa, then using hydrogen-oxygen
Quartz ampoule sintering is sealed by flame；Quartz ampoule is put in shaft furnace, 1150 DEG C are warming up to, 20h is incubated；
(2) first stage cooling is carried out with the cooling of 4 DEG C/h speed, makes crystal spontaneous crystallization, when temperature is down to 900 DEG C,
After 20h is incubated at 900 DEG C, quartz ampoule is taken out from shaft furnace rapidly, be then centrifuged for quenching, be allowed to be cooled to room temperature in 7min,
Black CrSe is obtained2Crystal.
Claims (7)
1. a kind of method of metal fusing agent method growth transient metal chalcogenide compound crystal, including step is as follows：
（1）It is 1 by M, X, Sn atomic molar ratio：2：（5-20）, simple substance M, simple substance X and simple substance Sn are mixed, in 1 × 10-3 -1×
10-4Under the vacuum degree condition of Pa, 1100-1150 DEG C is warming up to, is incubated 20-40 h；
Described M is Cr, Mo or W, and described X is S, Se or Te；
（2）First stage cooling is carried out with the rate of temperature fall of 1-6 DEG C/h, crystal spontaneous crystallization is made, when temperature is down to 900-1000
DEG C when, be incubated 20-40 h；Then quench, room temperature is cooled in 5-10 min, obtains MX2Crystal；
The MX2Crystal is MoS2 、MoSe2、MoTe2 、WS2 、WSe2 、WTe2Or CrSe2。
2. method according to claim 1, it is characterised in that step（1）Middle M, X, Sn atomic molar ratio is 1：2：（7.5-
10）.
3. method according to claim 1, it is characterised in that step（1）Described in M be Mo or W.
4. method according to claim 1, it is characterised in that step（1）Middle X is S.
5. method according to claim 1, it is characterised in that step（2）The rate of temperature fall of middle first stage cooling is 2-4
℃/h。
6. method according to claim 1, it is characterised in that step（2）The mode of middle quenching is centrifugal quenching, or,
Remove Deca water after the Sn of molten condition.
7. a kind of method of metal fusing agent method growth transient metal chalcogenide compound crystal, including step is as follows：
（1）It is 1 by M, X, Sn atomic molar ratio：2：（5-20）, simple substance M, simple substance X and simple substance Sn are mixed, are put in quartz ampoule,
Vacuum in quartz ampoule is made to reach 1 × 10 using vacuum pump evacuation-3 -1×10-4Then quartz ampoule is burnt by Pa using oxyhydrogen flame
Knot sealing；Quartz ampoule is put in shaft furnace, 1100-1150 DEG C is warming up to, 20-40 h are incubated；
Described M is Cr, Mo or W, and described X is S, Se or Te；
（2）First stage cooling is carried out with the rate of temperature fall of 1-6 DEG C/h, crystal spontaneous crystallization is made, when temperature is down to 900-1000
DEG C when, be incubated 20-40 h；
Then quartz ampoule is taken out from shaft furnace rapidly, then quenched, be allowed to be cooled to room temperature in 5-10 min, obtain MX2It is brilliant
Body；
The MX2Crystal is MoS2 、MoSe2、MoTe2 、WS2 、WSe2 、WTe2Or CrSe2。
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