CN104846428A - Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method - Google Patents
Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method Download PDFInfo
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Abstract
The invention relates to a method used for growth of transition metal chalcogenide crystals via metal fluxing agent method. The method comprises following steps: (1) elementary substance M, elementary substance X, and elementary substance Sn are mixed, an obtained mixture is heated to 1100 to 1150 DEG C at a vacuum degree of 1*10<-3> to 1*10<-4>Pa, and thermal prevention is carried out for 20 to 40h, wherein M is used for representing Cr, Mo, or W, and X is used for representing S, Se, or Te; and (2) the mixture is subjected to first stage temperature reducing at a temperature reducing speed of 1-6 DEG C/h so as to realize crystal spontaneous crystallization, when the temperature is reduced to 900 to 1000 DEG C, thermal preservation is carried out for 20 to 40h, quenching is carried out, and an obtained product is cooled to room temperature in 5 to 10min so as to obtain the transition metal chalcogenide crystals. Operation conditions of the method are easy to realize, and controllable; raw materials are easily available, and are cheap; the obtained transition metal chalcogenide crystals are high in quality; and application prospect in the fields of photon, photoelectric, and electronic devices is promising.
Description
Technical field
The present invention relates to the method for a kind of metal fusing agent method growth transient metal chalcogenide compound crystal, belong to technical field of crystal growth.
Background technology
Along with science and technology and expanding economy, the base support material silicon of information society will arrive its physics limit, and the equivalent material finding silicon is extremely urgent.In recent years, it is found that the semiconducting behavior of transient metal chalcogenide compound due to excellence, likely surmount the equivalent material that Graphene becomes silicon.And this kind of material also has important application prospect in the field such as photon, photoelectricity.Transient metal chalcogenide compound (TMDCs) chemical formula is MX
2(M=Cr, Mo, W; X=S, Se, Te), belong to hexagonal system, be layered semiconductor material, combined by weak Van der Waals force between layers, so the individual layer similar with Graphene or a few layer film can be peeled off into.This kind of film by the scale down of existing semiconductor technology to atom magnitude.People utilize this individual layer or which floor TMDCs film to produce various functional device, such as: MoS
2, MoSe
2, WS
2, WSe
2etc. field-effect transistor can be made into, higher carrier mobility and current on/off ratio can be obtained; Utilize MoS
2photosensitivity and gas sensing property, photoresponse device and various gas detector can be made into; Use MoS
2use in the laser as saturated absorbing body; MoS
2, WS
2as the anode material of lithium ion battery and Magnesium ion battery, the charge and discharge capacitance amount of battery can be improved Deng material; In addition, the research of the aspect such as Organic Light Emitting Diode, storer is all underway.Generally speaking, transient metal chalcogenide compound has good application prospect in the micro-nano electron devices such as photon, electronics, photoelectricity, and how to prepare high-quality transient metal chalcogenide compound crystal, becomes the emphasis of research.
The method preparing transient metal chalcogenide compound at present mainly contains hydrothermal method, chemical Vapor deposition process, thermal decomposition method etc., the nanometer sheet, film or the small-crystalline that synthesize transient metal chalcogenide compound can be grown by these methods, but at present by the large-sized crystal of these methods more difficult acquisition high quality.
Summary of the invention
For the deficiencies in the prior art, the present invention proposes the method for a kind of metal fusing agent method growth transient metal chalcogenide compound crystal, and the method can grow and obtain the large-sized crystal of high quality, can be used in the various devices in field such as making information, photoelectricity.
Term illustrates:
The transient metal chalcogenide compound that the present invention relates to, general formula is MX
2, wherein M is Cr, Mo or W, and X is S, Se or Te.
Technical solution of the present invention is as follows:
A method for metal fusing agent method growth transient metal chalcogenide compound crystal, comprises step as follows:
(1) compare for 1:2:(5-20 by M, X, Sn atomic molar), 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, be warming up to 1100-1150 DEG C, insulation 20-40h;
Described M is Cr, Mo or W, and described X is S, Se or Te;
(2) carry out first stage cooling with the rate of temperature fall of 1-6 DEG C/h, make crystal spontaneous crystallization, when temperature is down to 900-1000 DEG C, insulation 20-40h; Then quench, in 5-10min, be cooled to room temperature, obtain MX
2crystal.
According to the present invention, preferably, in step (1), M, X, Sn atomic molar is than being 1:2:(7.5-10), soaking time is 20-40h;
Preferably, described M is Mo or W; Described X is S.
According to the present invention, preferably, in step (2), the rate of temperature fall of first stage cooling is 2-4 DEG C/h.
According to the present invention, preferably, in step (2), the mode of quenching is centrifugal quenching, or, drip water after removing the Sn of molten state.
According to the present invention, preferred embodiment is as follows:
(1) compare for 1:2:(5-20 by M, X, Sn atomic molar), simple substance M, simple substance X and simple substance Sn are mixed, puts into silica tube, use vacuum pump evacuation to make vacuum tightness in silica tube reach 1 × 10
-3-1 × 10
-4pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1100-1150 DEG C, insulation 20-40h;
Described M is Cr, Mo or W, and described X is S, Se or Te;
(2) carry out first stage cooling with the rate of temperature fall of 1-6 DEG C/h, make crystal spontaneous crystallization, when temperature is down to 900-1000 DEG C, insulation 20-40h;
Then rapidly from pit furnace, take out silica tube, then quench, make it to be cooled to room temperature in 5-10min, obtain MX
2crystal.
The inventive method can obtain the high-quality MX of 0.5-9mm
2crystal.
According to the present invention, preferably, described MX
2crystal is MoS
2, MoSe
2, MoTe
2, WS
2, WSe
2, WTe
2or CrSe
2.
Principle of the present invention:
The metal method of fluxing is a kind of conventional method of field of crystal growth, but can as fusing assistant for the not all metal of Cr, Mo or W, if it is improper that fusing assistant metal is selected, other compounds will be produced in crystal growing process, thus can not get monocrystalline, have a strong impact on the quality of crystal.The present invention explores and experiment through long-time, and choice for use metal Sn is as fusing assistant; The fusing point of Sn is lower, in crystal growing process, be in molten state always, in quenching process, adopt centrifugal mode the Sn centrifugation under molten state can be come, and Sn be dissolved in acid, crystal can be soaked with acid solution and thoroughly remove metal fusing agent Sn, obtain high-quality monocrystalline MX
2; Also the rate of temperature fall in water flexible modulation quenching process can be dripped in quenching process.
In the present invention, the first stage speed of cooling is most important, and rate of temperature fall is too fast, and the crystal obtained is very little, and impact application, rate of temperature fall is excessively slow, and the crystal obtained is polycrystalline, has a strong impact on crystal mass.The present invention explores and experiment through long-time, selects the rate of temperature fall of 1-6 DEG C/h interval, obtains the monocrystalline MX that quality is good, crystallographic dimension is suitable
2.
Beneficial effect of the present invention is as follows:
1, needed for the inventive method, condition is simple, and growth cycle is 4-20 days, and can obtain millimetre-sized high quality transient metal chalcogenide compound crystal, growth cycle is short, can be used in the various devices in field such as making information, photoelectricity.
2, the inventive method operational condition easily realizes, controllable, raw material be easy to get, and low price, crystal is easily separated with fusing assistant, without other by products.
3, the grade MX that obtains of the inventive method
2monocrystalline superior in quality, has very high chemical stability and thermostability.
Accompanying drawing explanation
Fig. 1 is the MoS that the embodiment of the present invention 1 obtains
2the X-ray diffractogram of crystal.
Fig. 2 is that the embodiment of the present invention 1 obtains MoS
2the crystalline structure figure of crystal.
Fig. 3 is the MoS that the embodiment of the present invention 2 obtains
2the photo in kind of crystal.
Fig. 4 is the MoS that comparative example 1 of the present invention obtains
2the photo in kind of crystal.
Fig. 5 is the MoSe that the embodiment of the present invention 5 obtains
2the photo in kind of crystal.
Embodiment
Below by specific embodiment, also the present invention will be further described by reference to the accompanying drawings, but be not limited thereto.
Embodiment 1:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoS
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance S, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) first stage cooling is carried out with the cooling of the speed of 6 DEG C/h, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, silica tube is taken out rapidly from pit furnace, then centrifugal quenching, makes it to be cooled to room temperature in 10min, namely obtains the MoS of silver gray shape 0.5mm × 1mm
2crystal.
The MoS that test the present embodiment obtains
2the X-ray diffractogram of monocrystalline, as shown in Figure 1.As shown in Figure 1, X-ray diffractogram is consistent with Theoretical Calculation, and only shows the diffraction peak in [00L] direction, and the MoS obtained is described
2the natural-surface of crystal is crystallography ab plane.
Embodiment 2:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoS
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance S, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 2 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 10min, namely obtain silver gray 3mm × 4mm sheet MoS
2crystal, under this rate of temperature fall, crystal structure is best in quality.
Comparative example 1:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoS
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance S, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) first stage cooling is carried out with the cooling of 0.5 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, silica tube is taken out rapidly from pit furnace, then centrifugal quenching, makes it to be cooled to room temperature at 10min, namely obtains silver gray 7mm × 8mm sheet MoS
2crystal.
The crystal that the crystal thickness that this comparative example obtains obtains compared with embodiment 1 and embodiment 2 is significantly increased, and as shown in Figure 4, as shown in Figure 4, crystal is evident as polycrystalline to crystallogram, and crystalline quality is poor.
Embodiment 3:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoS
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance S, simple substance Sn are prepared burden according to mol ratio 1:2:5, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1100 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 6 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 5min, namely obtain silver gray grade sheet MoS
2crystal.
Embodiment 4:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoS
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance S, simple substance Sn are prepared burden according to mol ratio 1:2:20, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1100 DEG C, insulation 20h;
(2) first stage cooling is carried out with the cooling of 6 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, silica tube is taken out rapidly from pit furnace, drip water after removing the Sn of molten state, make it to be cooled to room temperature at 8min, namely obtain silver gray grade sheet MoS
2crystal.
Embodiment 5:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoSe
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance Se, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 4 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 10min, namely obtain silver gray MoSe
2crystal.
Embodiment 6:
A kind of metal fusing agent method growth transient metal chalcogenide compound MoTe
2the method of crystal, comprises step as follows:
(1) raw material simple substance Mo, simple substance Te, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1100 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 3 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 1000 DEG C, after 1000 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 7min, namely obtain silver gray MoTe
2crystal.
Embodiment 7:
A kind of metal fusing agent method growth transient metal chalcogenide compound WS
2the method of crystal, comprises step as follows:
(1) raw material simple substance W, simple substance S, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 4 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 5min, namely obtain silver gray WS
2crystal.
Embodiment 8:
A kind of metal fusing agent method growth transient metal chalcogenide compound WSe
2the method of crystal, comprises step as follows:
(1) raw material simple substance W, simple substance Se, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 2 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 9min, namely obtain silver gray WSe
2crystal.
Embodiment 9:
A kind of metal fusing agent method growth transient metal chalcogenide compound WTe
2the method of crystal, comprises step as follows:
(1) raw material simple substance W, simple substance Te, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 1 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 6min, namely obtain silver gray WTe
2crystal.
Embodiment 10:
A kind of metal fusing agent method growth transient metal chalcogenide compound CrSe
2the method of crystal, comprises step as follows:
(1) raw material simple substance Cr, simple substance Se, simple substance Sn are prepared burden according to mol ratio 1:2:10, Homogeneous phase mixing, puts into clean high purity quartz pipe, uses vacuum pump evacuation to make to reach 1 × 10 in silica tube
-3the vacuum tightness of Pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1150 DEG C, insulation 20h;
(2) carry out first stage cooling with the cooling of 4 DEG C/h speed, make crystal spontaneous crystallization, when temperature is down to 900 DEG C, after 900 DEG C of insulation 20h, from pit furnace, take out silica tube rapidly, then centrifugal quenching, make it to be cooled to room temperature at 7min, namely obtain black CrSe
2crystal.
Claims (8)
1. a method for metal fusing agent method growth transient metal chalcogenide compound crystal, comprises step as follows:
(1) compare for 1:2:(5-20 by M, X, Sn atomic molar), 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, be warming up to 1100-1150 DEG C, insulation 20-40h;
Described M is Cr, Mo or W, and described X is S, Se or Te;
(2) carry out first stage cooling with the rate of temperature fall of 1-6 DEG C/h, make crystal spontaneous crystallization, when temperature is down to 900-1000 DEG C, insulation 20-40h; Then quench, in 5-10min, be cooled to room temperature, obtain MX
2crystal.
2. method according to claim 1, is characterized in that, in step (1), M, X, Sn atomic molar is than being 1:2:(7.5-10).
3. method according to claim 1, is characterized in that, the M described in step (1) is Mo or W.
4. method according to claim 1, is characterized in that, in step (1), X is S.
5. method according to claim 1, is characterized in that, in step (2), the rate of temperature fall of first stage cooling is 2-4 DEG C/h.
6. method according to claim 1, is characterized in that, in step (2), the mode of quenching is centrifugal quenching, or, drip water after removing the Sn of molten state.
7. a method for metal fusing agent method growth transient metal chalcogenide compound crystal, comprises step as follows:
(1) compare for 1:2:(5-20 by M, X, Sn atomic molar), simple substance M, simple substance X and simple substance Sn are mixed, puts into silica tube, use vacuum pump evacuation to make vacuum tightness in silica tube reach 1 × 10
-3-1 × 10
-4pa, then uses oxyhydrogen flame by the sealing of silica tube sintering; Silica tube is put into pit furnace, is warming up to 1100-1150 DEG C, insulation 20-40h;
Described M is Cr, Mo or W, and described X is S, Se or Te;
(2) carry out first stage cooling with the rate of temperature fall of 1-6 DEG C/h, make crystal spontaneous crystallization, when temperature is down to 900-1000 DEG C, insulation 20-40h;
Then rapidly from pit furnace, take out silica tube, then quench, make it to be cooled to room temperature in 5-10min, obtain MX
2crystal.
8. method according to claim 1, is characterized in that, described MX
2crystal is MoS
2, MoSe
2, MoTe
2, WS
2, WSe
2, WTe
2or CrSe
2.
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