CN107400917A - A kind of SnSe2Crystalline compounds and its preparation method and application - Google Patents
A kind of SnSe2Crystalline compounds and its preparation method and application Download PDFInfo
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- CN107400917A CN107400917A CN201710617019.4A CN201710617019A CN107400917A CN 107400917 A CN107400917 A CN 107400917A CN 201710617019 A CN201710617019 A CN 201710617019A CN 107400917 A CN107400917 A CN 107400917A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
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Abstract
The invention discloses a kind of SnSe2The preparation method of crystalline compounds, first with Sn particles, Se particles and SnCl2Powder is raw material, carries out heating melting, cools down to obtain ingot body material；It is subsequently placed in zone melting furnace, growth is oriented using area's process of smelting, obtains the SnSe2Crystalline compounds.Present invention firstly provides prepare SnSe using melt binding area process of smelting2The quasi- monocrystal material of compound, products therefrom have preferable single phase property, compactness, and with preferable quasi- mono-crystalline structures；To SnSe2Sill is doped improvement, can significantly lift the thermoelectricity capability of gained doped samples；In addition, preparation time of the present invention is short, simple to operate, equipment requirement is low, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to new energy materialses field, and in particular to a kind of SnSe2Crystalline compounds and preparation method thereof and should
With.
Background technology
70% is there are about in the energy that the whole world consumes every year to be wasted in the form of used heat, if these used heat can be carried out
It is effective to recycle, it will greatly alleviate the problem of energy shortage.Thermoelectric generation technology utilizes semi-conductor thermoelectric material
The technology that match Bake (Seebeck) effect and Peltier (Peltier) effect are directly changed heat energy and electric energy, including heat
Electricity generates electricity and thermoelectric cooling two ways.This technology has that system bulk is small, reliability is high, operating cost is low, long lifespan, system
The features such as technique is simple, environment-friendly, Applicable temperature scope is wide is made, as particular power source and accurate temperature controlling device in space skill
The high-technology fields such as art, military equipment have been obtained for more application.Turn as a kind of new, environmental harmony type clear energy sources
Technology is changed, thermoelectric generation technology is attracted attention in the world in the past 20 years.The core of thermoelectric conversion element is thermoelectric material, its turn
Change the dimensionless figure of merit ZT that efficiency depends primarily on thermoelectric material.
SnSe2It is a kind of broadband based semiconductor, component rich content, nontoxic pollution-free, shows excellent electricity
And photoelectric property, there is important application prospect in photovoltaic and energy storing device.In recent years on SnSe2Semiconductor is ground
Study carefully more and more, but so far, single-phase SnSe is synthesized using solid state process2A greatly challenge is still, due to SnSe poles
High stability causes SnSe2SnSe in material always be present2With SnSe eutectic phase.Therefore, at present mainly using solvent method, change
Learn vapour deposition process and machine-alloying prepares SnSe2.And solvent method synthesis SnSe2It is complex, use containing Sn's and Se
Precursor solution is sufficiently expensive, and the requirement in whole experiment flow to instrument and equipment is also higher, and SnSe2Limits throughput；
Chemical vapor deposition is under medium temperature or high temperature, is consolidated by the gas-phase chemical reaction between gaseous precursor compound and what is formed
For body electrodeposition substance on matrix, required time is longer, and equipment is very expensive, is unfavorable for commercial introduction application.And mechanical alloy
Although method requires relatively low to instrument and equipment, and the time used is shorter, the SnSe of generation2In many dephasigns be present, be unfavorable for protecting
Demonstrate,prove SnSe2The performance of compound.
Therefore a kind of short preparation period, SnSe simple to operate, the low and suitable industrialized production of equipment requirement are developed2Chemical combination
Thing technology of preparing, and its thermoelectricity capability is further lifted, it is SnSe2The important topic faced in compound research field.
The content of the invention
The purpose of the present invention is to be directed to above-mentioned the shortcomings of the prior art, there is provided a kind of SnSe2Crystalline compounds and its
Preparation technology, the SnSe2Crystalline compounds possess quasi- mono-crystalline structures, and the preparation technology being related to is simple, preparation time is short, operation
Simply, equipment requirement is low, suitable for scale production；Simultaneously by SnSe2Crystalline compounds are doped modification, can effectively carry
The mechanical property of gained crystalline material is risen, to SnSe2There is important propulsion to make for application of the sill in thermoelectric material field
With.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of SnSe2The preparation method of crystalline compounds, it is characterised in that comprise the following steps：
1) with Sn particles, Se particles and SnCl2Powder is raw material, then carries out heating melting, furnace cooling obtains ingot body material；
2) ingot body material obtained by step 1) is placed in zone melting furnace, growth is oriented using area's process of smelting, obtained described
SnSe2Crystalline compounds.
In such scheme, the Sn particles, Se particles and SnCl2Powder is according to chemical formula SnSe2-xClxThe chemistry of middle each element
Metering ratio is weighed, and wherein x span is：0≤x≤0.07.
Preferably, the span of the x is：0 ＜ x≤0.07.
It is furthermore preferred that the span of the x is：0.01≤x≤0.02.
In such scheme, smelting process is described in step 1)：700-800 DEG C is heated to, is incubated 24-36h.
In such scheme, step 2) area's process of smelting is that middle ingot body material is placed in glass tube, and the bottom of glass tube is put
In the medium position (glass bottom of the tube is placed in the middle part of heating collar plane) of heating collar, and central axis of the glass tube along heating collar
Place, length direction of the heating collar along glass tube at the uniform velocity moves.
In such scheme, in area's process of smelting：Zone-melting temperature is 973-1073K, and the translational speed of heating collar is 1.2-
1.8mm h-1。
In such scheme, the heating collar is moved in parallel through the height position of ingot body material along quartz glass tube axial direction
Put, that is, complete area's process of smelting.
The SnSe prepared according to such scheme2Crystalline compounds, it has quasi- mono-crystalline structures (quasi- monocrystalline knot of the present invention
Structure is：The relatively orderly polycrystalline structure of atomic arrangement, products therefrom of the present invention is similar to monocrystalline, but the atomic arrangement degree of order is than single
It is brilliant weaker), thermoelectric material is used as, dimensionless thermoelectric figure of merit ZT is up to 0.35 in 773K, significantly larger than existing research
Level, to SnSe2Application of the sill in thermoelectric material field has important progradation.
The present invention principle be：The present invention prepares quasi- mono-crystalline structures using zone-melting process, products therefrom with respect to polycrystalline material and
Speech reduces a large amount of crystal boundaries, carrier moving is reduced along melting the obstruction that direction is subject to parallel to area, and carrier mobility improves,
Be advantageous to lift electrical conductivity；In addition, the application is further to SnSe2Sill carries out chlorine doping vario-property, effectively controls chlorine element
It is doped into SnSe2In lattice, the thermoelectricity capability of gained doped samples is significantly lifted, to SnSe2The thermoelectricity capability research of sill
With important progradation.
Beneficial effects of the present invention are：
1) present invention firstly provides prepare SnSe using melt binding area process of smelting2The quasi- monocrystal material of compound, gained production
Thing has preferable single phase property and consistency, and the preparation time being related to is short, simple to operate, and equipment requirement is low, is adapted to extensive
Industrialized production.
2) present invention firstly provides prepare SnSe using area's process of smelting2Compound, the quasi- mono-crystalline structures of formation are advantageous to carry
The thermoelectricity capability of material is risen, to SnSe2Application of the sill in thermoelectric material field has important progradation.
3) present invention is further to SnSe2Sill is doped modification, can significantly lift the heat of gained doped samples
Electrical property, SnSe1.98Cl0.02Material dimensionless thermoelectric figure of merit ZT is 0.35 in 773K, significantly larger than existing research level.
Brief description of the drawings
Fig. 1 is the gained SnSe of embodiment 12The shape appearance figure of crystalline compounds.
Fig. 2 is the gained SnSe of embodiment 12The XRD of crystalline compounds, test surfaces melt direction parallel to area.
Fig. 3 is the gained SnSe of embodiment 12The FESEM of crystalline compounds.
Fig. 4 is the gained SnSe of embodiment 12The DSC figures of crystalline compounds.
Fig. 5 is the gained SnSe of embodiment 12The EPMA results of crystalline compounds burnishing surface, including backscattered electron image and member
Vegetarian noodles is distributed.
Fig. 6 is the gained SnSe of embodiment 22The EPMA results of crystalline compounds burnishing surface, including backscattered electron image and member
Vegetarian noodles is distributed.
Fig. 7 is the gained SnSe of embodiment 22The XRD spectrum of crystalline compounds powder.
Fig. 8 is embodiment 1 and the gained SnSe of embodiment 22Crystalline compounds (are respectively SnSe2And SnSe1.98Cl0.02)
The graph of a relation that direction electrical conductivity varies with temperature is melted parallel to area.
Fig. 9 is embodiment 1 and the gained SnSe of embodiment 22Crystalline compounds (are respectively SnSe2And SnSe1.98Cl0.02)
The graph of a relation that direction Seebeck coefficients vary with temperature is melted parallel to area.
Figure 10 is embodiment 1 and the gained SnSe of embodiment 22Crystalline compounds (are respectively SnSe2And SnSe1.98Cl0.02)
The graph of a relation that direction thermal conductivity varies with temperature is melted parallel to area.
Figure 11 is embodiment 1 and the gained SnSe of embodiment 22Crystalline compounds (are respectively SnSe2And SnSe1.98Cl0.02)
The graph of a relation that direction ZT values vary with temperature is melted parallel to area.
Embodiment
For a better understanding of the present invention, with reference to the specific embodiment content that the present invention is furture elucidated, but this hair
Bright content is not limited solely to the following examples.
In following examples, Sn particles, Se particles and the SnCl of use2Powder is commercially available prod, and its purity is
99.99%.
Embodiment 1
A kind of SnSe2The preparation method of crystalline compounds, comprises the following steps：
1) using Sn particles and Se particles as raw material, Sn grains and Se grains are pressed 1:2 mol ratio is weighed, and is weighed total amount and is
30g, the raw material after weighing is well mixed and is put into the special quartz glass tube of area's process of smelting rear vacuum sealing, is then placed in
24h, melting temperature 923K are melted in melting furnace, furnace cooling is carried out and obtains ingot body material；
2) quartz glass tube that ingot body material is housed in step 1) is put in zone melting furnace and be oriented using area's process of smelting
Growth, is comprised the following steps that：By the quartz glass tube equipped with ingot body material along the axially placed of heating collar, and its bottom is placed in
The middle of heating collar, it is 1073K to control zone-melting temperature, and with 1.8mm h-1Speed by heating collar along quartz glass tube axial direction
Direction moves in parallel the height and position through ingot body material, is then shut off zone melting furnace, is taken out after being down to room temperature, produces with good
The SnSe of Forming Quality2Crystalline compounds (quasi- monocrystalline).
Fig. 1 is SnSe obtained by the present embodiment2The shape appearance figure of crystalline compounds, as can be seen from the figure products therefrom shaping matter
Amount is preferable, and its consistency is 98%；By SnSe obtained by the present embodiment2Crystalline compounds cut into 3mm × 3mm × 15mm strips and
A diameter of 6mm disks carry out thermoelectricity capability test, remaining leftover pieces carry out phase composition, micro-structural etc. characterize, it is as a result as follows：
Fig. 2 is SnSe obtained by the present embodiment2The XRD of crystalline compounds, test surfaces melt direction parallel to area, can see
Go out, the SnSe prepared using zone-melting process2In extraordinary single-phase, and it is basic grown along (00l) crystal plane orientation, be shown to be preferable
Quasi- monocrystal material.
Fig. 3 is SnSe obtained by the present embodiment2The FESEM figures of crystalline compounds, as can be seen from the figure products therefrom is layer
Shape structure, and be in oriented alignment, coarse grains, essentially monocrystal material.
Fig. 4 is SnSe obtained by the present embodiment2The high temperature DSC figures of crystalline compounds, it can be seen that in products therefrom
It is SnSe without other dephasigns2Endothermic peak caused by melting.
Fig. 5 is SnSe obtained by the present embodiment2The burnishing surface EPMA results of crystalline compounds, including backscattered electron image and member
Vegetarian noodles is distributed, Sn and Se Elemental redistributions are highly uniform as can be seen from Fig., and is generated without obvious second phase.
SnSe obtained by the present embodiment2Crystalline compounds are melting the electrical conductivity in direction, Seebeck coefficients, thermal conductivity parallel to area
The graph of a relation that rate and ZT values vary with temperature is shown in Fig. 8-11 respectively.Dimensionless thermoelectric figure of merit ZT during the present embodiment products therefrom 773K
Up to 0.08.
Embodiment 2
A kind of SnSe2The preparation method of crystalline compounds, comprises the following steps：
1) with Sn particles, Se particles and SnCl2Powder is raw material, by chemical formula SnSe1.98Cl0.02The chemistry of middle each element
Metering ratio is weighed, and weighing total amount is 30g, is well mixed and is put into area the raw material after weighing and melt special quartz glass tube
In after vacuum sealing, be then placed in melting furnace and melt 24h, melting temperature 923K, carry out furnace cooling obtain ingot body material；
2) quartz glass tube that ingot body material is housed in step 1) is put in zone melting furnace and be oriented using area's process of smelting
Growth, is comprised the following steps that：By the quartz glass tube equipped with ingot body material along the axially placed of heating collar, and its bottom is placed in
The middle of heating collar, it is 1073K to control zone-melting temperature, and with 1.8mm h-1Speed by heating collar along quartz glass tube axial direction
Direction moves through the height and position of ingot body material, is then shut off zone melting furnace, is taken out after being down to room temperature, produces with good shaping
The SnSe of quality2Crystalline compounds (SnSe1.98Cl0.02Quasi- monocrystal material, consistency 98%).
By SnSe obtained by the present embodiment2Crystalline compounds cut into 3mm × 3mm × 15mm strips and a diameter of 6mm disks
Carry out thermoelectricity capability test, remaining leftover pieces carry out phase composition, micro-structural etc. characterize：The EPMA of the present embodiment products therefrom
As a result it is as shown in Figure 6, the results showed that Sn, Se, Cl Elemental redistribution are highly uniform after doping；The XRD of the present embodiment products therefrom
Compose and see Fig. 7, surface products therefrom of the present invention is in extraordinary SnSe in figure2It is single-phase, no SnCl2Deng dephasign, illustrate that Cl elements are effective
It is doped into SnCl2In lattice.
SnSe obtained by the present embodiment2Crystalline compounds are melting the electrical conductivity in direction, Seebeck coefficients, thermal conductivity parallel to area
The graph of a relation that rate and ZT values vary with temperature is shown in Fig. 7-10 respectively, is as can be seen from the figure doped modified products therefrom
Electrical conductivity and dimensionless thermoelectric figure of merit are largely increased.When final product room temperature ZT values are 0.08,773K obtained by the present embodiment
Dimensionless thermoelectric figure of merit is up to 0.35.
Embodiment 3
A kind of SnSe2The preparation method of crystalline compounds, comprises the following steps：
1) with Sn particles, Se particles and SnCl2Powder is raw material, by chemical formula SnSe1.99Cl0.01The chemistry of middle each element
Metering ratio is weighed, and weighing total amount is 30g, is well mixed and is put into area the raw material after weighing and melt special quartz glass tube
In after vacuum sealing, be then placed in melting furnace and melt 24h, melting temperature 873K, carry out furnace cooling obtain ingot body material；
2) quartz glass tube that ingot body material is housed in step 1) is put in zone melting furnace and be oriented using area's process of smelting
Growth, is comprised the following steps that：By the quartz glass tube equipped with ingot body material along the axially placed of heating collar, and its bottom is placed in
The middle of heating collar, it is 1073K to control zone-melting temperature, and with 1.8mm h-1Speed by heating collar along quartz glass tube axial direction
Direction moves through the height and position of ingot body material, is then shut off zone melting furnace, is taken out after being down to room temperature, produces with good shaping
The SnSe of quality2Crystalline compounds (SnSe1.99Cl0.01Quasi- monocrystal material, consistency 98%).
SnSe obtained by the present embodiment2Dimensionless thermoelectric figure of merit ZT can when crystalline compounds its room temperature ZT values are 0.06,773K
Up to 0.3.
Embodiment 4
A kind of SnSe2The preparation method of crystalline compounds, comprises the following steps：
1) with Sn particles, Se particles and SnCl2Powder is raw material, by chemical formula SnSe1.96Cl0.04The chemistry of middle each element
Metering ratio is weighed, and weighing total amount is 30g, is well mixed and is put into area the raw material after weighing and melt special quartz glass tube
In after vacuum sealing, be then placed in melting furnace and melt 24h, melting temperature 873K, carry out furnace cooling obtain ingot body material；
2) quartz glass tube that ingot body material is housed in step 1) is put in zone melting furnace and be oriented using area's process of smelting
Growth, is comprised the following steps that：By the quartz glass tube equipped with ingot body material along the axially placed of heating collar, and its bottom is placed in
The middle of heating collar, it is 1073K to control zone-melting temperature, and with 1.8mm h-1Speed by heating collar along quartz glass tube axial direction
Direction moves through the height and position of ingot body material, is then shut off zone melting furnace, is taken out after being down to room temperature, produces with good shaping
The SnSe of quality2Crystalline compounds (SnSe1.96Cl0.04Quasi- monocrystal material, consistency 98%).
SnSe obtained by the present embodiment2Dimensionless thermoelectric figure of merit ZT can when crystalline compounds its room temperature ZT values are 0.07,773K
Up to 0.32.
Comparative example 1
Z.V.Borges et al. (Materials Chemistry and Physics, 2016,169,47-54) uses machine
Tool alloyage combination discharge plasma sintering prepares SnSe2Polycrystalline material, the ZT values of gained sample are 0.0125 in room temperature.
Its preparation technology is as follows：
1) first stoichiometrically SnSe2Weigh Sn and Se powder (quality purity 99.999%), the raw material that will be weighed
Be well mixed and be put into vacuumized in ball grinder after carry out ball milling, ball milling speed 400r/min, Ball-milling Time 2h, obtain powder
Material；
2) a small amount of gained powder body material test XRD is taken, XRD results show a small amount of SnSe and SeO2Dephasign；
3) gained powder body material is subjected to discharge plasma sintering, sintering temperature 773K, sintering time 10min, burnt
Knot pressure power is 10MPa, obtains the block materials that consistency is 98%, and its room temperature ZT values are 0.015.
The above results show that the present invention prepares SnSe using melt binding area process of smelting2The quasi- monocrystal material of compound, gained
Product has preferable single phase property and consistency, and the quasi- mono-crystalline structures of formation are advantageous to be lifted the thermoelectricity capability of material, and pass through
To SnSe2Sill carries out chlorine doping, the thermoelectricity capability of gained doped samples can be further obviously improved, to SnSe2Sill exists
Application in thermoelectric material field has important progradation.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (8)
- A kind of 1. SnSe2The preparation method of crystalline compounds, it is characterised in that comprise the following steps：1) with Sn particles, Se particles and SnCl2Powder is raw material, then carries out heating melting, furnace cooling obtains ingot body material；2) ingot body material obtained by step 1) is placed in zone melting furnace, growth is oriented using area's process of smelting, obtains the SnSe2It is brilliant Body compound.
- 2. preparation method according to claim 1, it is characterised in that the Sn particles, Se particles and SnCl2Powder is according to change Formula SnSe2-xClxThe stoichiometric proportion of middle each element is weighed, and wherein x span is 0≤x≤0.06.
- 3. preparation method according to claim 1, it is characterised in that the span of the x is 0.01≤x≤0.02.
- 4. preparation method according to claim 1, it is characterised in that smelting process is described in step 1)：It is heated to 700-750 DEG C, it is incubated 24-36h.
- 5. preparation method according to claim 1, it is characterised in that during step 2) area's process of smelting is, ingot body material It is placed in glass tube, the bottom of glass tube is placed in the medium position of heating collar, and central axis of the glass tube along heating collar is placed, Length direction of the heating collar along glass tube at the uniform velocity moves.
- 6. preparation method according to claim 1, peculiar to be, in area's process of smelting：Zone-melting temperature is 973- 1073K, the translational speed of heating collar is 1.2-1.8mm h-1。
- 7. SnSe prepared by any one of claim 1~6 preparation method2Crystalline compounds.
- 8. SnSe described in claim 72Application of the crystalline compounds in thermoelectric material field.
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| CN108330543A (en) * | 2018-02-10 | 2018-07-27 | 北京航空航天大学 | A kind of N-type SnSe monocrystalline and preparation method thereof |
| CN108615806A (en) * | 2018-04-26 | 2018-10-02 | 北京航空航天大学 | A kind of N-type SnSe thermoelectric materials and preparation method thereof |
| CN110344120A (en) * | 2019-08-16 | 2019-10-18 | 河南理工大学 | A kind of SnSe2Base monocrystal material and preparation method thereof |
| CN110344120B (en) * | 2019-08-16 | 2020-12-08 | 河南理工大学 | SnSe2Base single crystal material and method for producing same |
| CN113113531A (en) * | 2021-03-16 | 2021-07-13 | 西北工业大学 | Preparation method of high ZT value pure SnSe polycrystalline block thermoelectric material |
| CN113113531B (en) * | 2021-03-16 | 2023-09-08 | 西北工业大学 | Preparation method of high ZT value pure SnSe polycrystal block thermoelectric material |
| CN114481290A (en) * | 2022-02-15 | 2022-05-13 | 深圳热电新能源科技有限公司 | Vertical zone melting furnace and preparation method for preparing magnesium bismuthate-based thermoelectric crystal by using same |
| CN114686986A (en) * | 2022-04-02 | 2022-07-01 | 齐齐哈尔大学 | SnSe2Method for producing single crystal |
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