CN109371468A - A kind of high quality Cu2Se(1-x)AxThe growing method of crystal - Google Patents
A kind of high quality Cu2Se(1-x)AxThe growing method of crystal Download PDFInfo
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- CN109371468A CN109371468A CN201811225006.3A CN201811225006A CN109371468A CN 109371468 A CN109371468 A CN 109371468A CN 201811225006 A CN201811225006 A CN 201811225006A CN 109371468 A CN109371468 A CN 109371468A
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- 239000013078 crystal Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000010453 quartz Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000003708 ampul Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 9
- SWLJJEFSPJCUBD-UHFFFAOYSA-N tellurium tetrachloride Chemical compound Cl[Te](Cl)(Cl)Cl SWLJJEFSPJCUBD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 230000032258 transport Effects 0.000 claims description 14
- 229910052740 iodine Inorganic materials 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002019 doping agent Substances 0.000 abstract description 3
- 239000003034 coal gas Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 46
- 239000000126 substance Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000005619 thermoelectricity Effects 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910002688 Ag2Te Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of high quality Cu2Se(1‑x)AxThe growing method of crystal.This method comprises the following steps: (1) raw material is prepared: weighing a certain amount of Cu2Se powder, is then added TeCl4、TeBr4Or I2Powder by raw material as in clean high temperature resistant quartz ampoule after being mixed with mortar grinder, then in the state of vacuumizing, is sealed spare using coal gas flame as transporting agent and dopant；(2) crystal growth: the quartz ampoule that step (1) is sealed is placed in two warm areas or the tube furnace of multi-temperature zone, and growth temperature is arranged, can get the Cu by the growth of some cycles2Se(1‑x)AxCrystal, wherein A=Cl, Br or I.Cu provided in the present invention2Se(1‑x)AxGrowing method has many advantages, such as that growth apparatus crystal quality that is simple, low in cost, being grown is high, size is big.
Description
Technical field
The invention belongs to technical field of crystal growth, in particular to a kind of growth high quality Cu2Se(1-x)Ax(A=Cl, Br,
I) the method for crystal.
Background technique
Berzeline (Cu2Se) belong to Transition-metal dichalcogenide.In recent years, in thermoelectric material, solar energy materials, open up
It flutters in the research of material, giant magnetic resistance, Transition-metal dichalcogenide is due to physical property abundant and application value
Cause the very big concern of material and community of physicists.It is well known that increase of the transition metal element with atomic number Z, electronics-
Electron correlation (U) effect can weaken, but Effect of Spin-orbit Coupling enhances.The variation of both effects is increased to material property
A possibility that regulation, to produce physical phenomenon abundant.Wherein silver-colored chalcogenide (such as Ag2Te) there is giant magnetoresistance effect
It answers, has recently been identified as a new class of binary topological insulator of the dirac cone with high anisotropy.And selenizing is sub-
Copper (Cu2Se) as an important member of Transition-metal dichalcogenide, in recent years, development and light with thermoelectricity electronics
The development of electronics has also obtained more and more concerns due to its unique transmission characteristic and preferable thermoelectricity capability.Shanghai
Silicate research institute Chen Li east study group experiment discovery Cu2-xThe thermoelectric figure of merit (ZT) of Se reaches 1.5 in 1000K, then right
Cu2Se has carried out iodine doping research, has experimentally obtained the Cu that ZT value is up to 2.3 in 400K2Se(1-x)IxSample [Huili
Liu,Xun Yuan,Ping Lu,Xun Shi,Fangfang Xu,Ying He,Yunshan Tang,Shengqiang Bai,
Wenqing Zhang,Lidong Chen,Yue Lin,Lei Shi,He Lin,Xingyu Gao,Xingmin Zhang,
Hang Chi, and Ctirad Uher.Adv.Mater.25 (45): 6607 (2013)], this is that exploitation has practical value
Thermoelectric material device provides possibility.
However at present about Cu2Se(1-x)IxExperimental report, also only polycrystalline ceramics, and polycrystalline ceramics contain it is more
Defect, therefore it is difficult the mechanism of the high thermoelectricity capability behind of analysis of material, while there is also very big difficulties for practical application exploitation.Therefore
Grow the large-sized Cu of high quality2Se(1-x)AxBefore (A=Cl, Br, I) crystal has great learning value and potential application
Scape.
Chemical vapor transportation method is one of important method of crystal growth.It is raw that chemical vapor transportation mainly applies to monocrystalline
Long, synthesis of novel substance etc..When preparing the crystal of solid matter A a kind of using chemical vapor transportation method, Ke Yi
It is added in system and transports agent B, substance A reacts the volatile product C of generation with agent B is transported, and sets up following chemical balance: xA
(s)+yB(g)←→zC(g).Reactant is enclosed in the higher quartz ampoule of vacuum degree, and is placed on that there are certain temperature gradients
High temperature process furnances in.Under the action of temperature gradient, above-mentioned reaction has the different equilibrium constants, the gaseous substance C of generation
When being transported to the other end from one end of quartz ampoule, balance moves round about, deposits substance A.In this way not
Can only substance A be made to be purified, the crystal of large scale, high quality can also be obtained.The advantages of chemical vapor transportation method is to hold
Easily grow uniformity and the good high quality crystal of integrality, and strong applicability, it is desirable that temperature it is low, therefore equipment is relatively simple
It is single, be conducive to industrialized production.
Summary of the invention
The purpose of the present invention is to provide one kind to prepare high quality Cu based on chemical vapor transportation method2Se(1-x)Ax(A=Cl,
Br, I) crystal effective ways.This method transports the quality of agent by regulation growing end-feed end temperature gradient and change,
Obtain that serial high quality, uniformity be good, large-sized Cu2Se(1-x)Ax(A=Cl, Br, I) crystal.
The technical scheme is that
A kind of high quality Cu2Se(1-x)AxThe growing method of crystal, this method comprises the following steps:
(1) raw material is prepared: weighing a certain amount of Cu2Se powder, is then added TeCl4、TeBr4Or I2Powder is used as and transports
Agent and dopant, by raw material as in clean high temperature resistant quartz ampoule after being mixed with mortar grinder, then in the state of vacuumizing,
It is sealed using coal gas flame spare；
(2) crystal growth: the quartz ampoule that step (1) is sealed is placed in two warm areas or the tube furnace of multi-temperature zone,
Growth temperature is set, can get the Cu by the growth of some cycles2Se(1-x)AxCrystal, wherein A=Cl, Br or I.
Further, the Cu2The quality of Se powder is 1.0~1.5g.
Further, the TeCl4、TeBr4Or I2The quality of powder is 100~200mg, and concentration is 5~10mg/
cm3。
Further, the length of the quartz ampoule is 10~20cm, and diameter is 1~3cm.
Further, in the step (1), 10 are evacuated to-5~10-3Sealed silica envelope after pa.
Further, in the step (2), growth temperature setting are as follows: 450-550 DEG C of growing end, feed end 550-650
℃。
Further, in the step (2), the Cu of acquisition2Se(1-x)AxThe size of crystal is about 1.0~1.5mm.
Further, in the step (2), the Cu of acquisition2Se(1-x)AxThe value of the x of crystal is 0.01~0.10.
The present invention use chemical vapor transportation method technology path, by adjust special ratios transport agent/dopant and
Its growth temperature section etc. successfully solves the problem of the prior art, obtains the Cu of high quality2Se(1-x)Ax(A=Cl,
Br, I) monocrystal.The present invention has the advantages that
(1) agent TeCl is transported in addition4、TeBr4Or I2Under the conditions of, growth raw material, which has, preferably transports rate, grows out
Crystal perfection it is uniform, quality is high, size is big, while also effectively being adulterated to crystal, obtain higher thermoelectricity capability
Cu2Se(1-x)Ax(A=Cl, Br, I) crystal prototype.
(2) preparation method provided by the invention, Cu are used2Se(1-x)Ax(A=Cl, Br, I) monocrystal can be compared with low temperature
The lower growth for realizing high quality crystal of degree, and device is simple and easy, low in cost, used to transport agent relatively stable, transports
Property is good, therefore is conducive to industrialized production.
(3) the innovation of the invention consists in that by improved chemical vapor transportation method, never someone grows before solving
Cu out2Se(1-x)AxThe problem of (A=Cl, Br, I) crystal provides a kind of simple and effective growing method.
Detailed description of the invention
Fig. 1 (a) is Cu2Se0.98Cl0.02The X-ray energy dispersion spectrum of crystal；It (b) is Cu2Se0.95Cl0.05The X of crystal is penetrated
Heat input dispersion spectrum；It (c) is Cu2Se0.97Br0.03The X-ray energy dispersion spectrum of crystal；It (d) is Cu2Se0.96Br0.04The X of crystal
Ray energy dispersion spectroscopy；It (e) is Cu2Se0.95I0.05The X-ray energy dispersion spectrum of crystal；It (f) is Cu2Se0.94I0.06The X of crystal
Ray energy dispersion spectroscopy；
Fig. 2 (a) is Cu2Se0.98Cl0.02The optical photograph of crystal；It (b) is Cu2Se0.95Cl0.05The optical photograph of crystal；
It (c) is Cu2Se0.97Br0.03The optical photograph of crystal；It (d) is Cu2Se0.96Br0.04The optical photograph of crystal；(e) it is
Cu2Se0.95I0.05The optical photograph of crystal；It (f) is Cu2Se0.94I0.06The optical photograph of crystal；
Specific embodiment
Further illustrate how the present invention realizes below with reference to specific preferred embodiment of implementing:
The Cu of 4N grades of purity is used in experiment2Se、TeCl4、TeBr4And I2As growth raw material.
Embodiment 1
Weigh the Cu of 1.1g2The TeCl of Se and 100mg4Powder mixes the stone for being placed on pickling and drying with mortar grinder
Ying Guanzhong is placed in two warm area high temperature process furnances after the quartz ampoule vacuum sealing equipped with the above growth raw material using chemical gas
Phase transport method carries out crystal growth, and growing end temperature is 500 DEG C, and feed end temperature is 600 DEG C, grows 10 under this temperature gradient
It, finally naturally cools to room temperature, can be obtained the Cu of high quality2Se0.98Cl0.02Monocrystal, maximum size about 1.5mm.
Embodiment 2
Weigh the Cu of 1.1g2The TeCl of Se and 150mg4Powder mixes the stone for being placed on pickling and drying with mortar grinder
Ying Guanzhong is placed in two warm area high temperature process furnances after the quartz ampoule vacuum sealing equipped with the above growth raw material using chemical gas
Phase transport method carries out crystal growth, and growing end temperature is 500 DEG C, and feed end temperature is 600 DEG C, grows 10 under this temperature gradient
It, finally naturally cools to room temperature, can be obtained the Cu of high quality2Se0.95Cl0.05Crystal, maximum size about 1.5mm.
Embodiment 3
Weigh the Cu of 1.1g2The TeBr of Se and 100mg4Powder mixes the stone for being placed on pickling and drying with mortar grinder
Ying Guanzhong is placed in two warm area high temperature process furnances after the quartz ampoule vacuum sealing equipped with the above growth raw material using chemical gas
Phase transport method carries out crystal growth, and growing end temperature is 550 DEG C, and feed end temperature is 650 DEG C, grows 10 under this temperature gradient
It, finally naturally cools to room temperature, can be obtained the Cu of high quality2Se0.97Br0.03Monocrystal, maximum size about 1.5mm.
Embodiment 4
Weigh the Cu of 1.1g2The TeBr of Se and 150mg4Powder mixes the stone for being placed on pickling and drying with mortar grinder
Ying Guanzhong is placed in two warm area high temperature process furnances after the quartz ampoule vacuum sealing equipped with the above growth raw material using chemical gas
Phase transport method carries out crystal growth, and growing end temperature is 550 DEG C, and feed end temperature is 650 DEG C, grows 10 under this temperature gradient
It, finally naturally cools to room temperature, can be obtained the Cu of high quality2Se0.96Br0.04Crystal, maximum size about 1.5mm.
Embodiment 5
Weigh the Cu of 1.1g2The I of Se and 150mg2Powder mixes the quartz for being placed on pickling and drying with mortar grinder
Guan Zhong is placed in two warm area high temperature process furnances after the quartz ampoule vacuum sealing equipped with the above growth raw material using chemical gaseous phase
Transport method carries out crystal growth, and growing end temperature is 500 DEG C, and feed end temperature is 600 DEG C, grows 10 under this temperature gradient
It, finally naturally cools to room temperature, can be obtained the Cu of high quality2Se0.95I0.05Monocrystal, maximum size about 1.5mm.
Embodiment 6
Weigh the Cu of 1.1g2The I of Se and 200mg2Powder mixes the quartz for being placed on pickling and drying with mortar grinder
Guan Zhong is placed in two warm area high temperature process furnances after the quartz ampoule vacuum sealing equipped with the above growth raw material using chemical gaseous phase
Transport method carries out crystal growth, and growing end temperature is 500 DEG C, and feed end temperature is 600 DEG C, grows 10 under this temperature gradient
It, finally naturally cools to room temperature, can be obtained the Cu of high quality2Se0.94I0.06Crystal, maximum size about 1.5mm.
Wen Zhongyi general explanation, specific embodiment and experiment, the present invention is described in detail, but in this hair
On the basis of bright, it can be modified or is improved, this is easy to those skilled in the art.Therefore exist
It without departing from these modifications made on the basis of spirit of that invention or improves, falls within the scope of the claimed invention.
Claims (8)
1. a kind of high quality Cu2Se(1-x)AxThe growing method of crystal, which is characterized in that this method comprises the following steps:
(1) raw material is prepared: weighing a certain amount of Cu2Se powder, is then added TeCl4、TeBr4Or I2Powder is used as and transports agent and mix
Miscellaneous dose, by raw material as in clean high temperature resistant quartz ampoule after being mixed with mortar grinder, then in the state of vacuumizing, using coal
Bluster sealing is spare；
(2) crystal growth: the quartz ampoule that step (1) is sealed is placed in two warm areas or the tube furnace of multi-temperature zone, setting
Growth temperature can get the Cu by the growth of some cycles2Se(1-x)AxCrystal, wherein A=Cl, Br or I.
2. a kind of high quality Cu according to claim 12Se(1-x)AxThe growing method of crystal, which is characterized in that described
Cu2The quality of Se powder is 1.0~1.5g.
3. a kind of high quality Cu according to claim 1 or 22Se(1-x)AxThe growing method of crystal, which is characterized in that described
TeCl4、TeBr4Or I2The quality of powder is 100~200mg, and concentration is 5~10mg/cm3。
4. a kind of high quality Cu according to claim 12Se(1-x)AxThe growing method of crystal, which is characterized in that the stone
The length of English pipe is 10~20cm, and diameter is 1~3cm.
5. a kind of high quality Cu according to claim 12Se(1-x)AxThe growing method of crystal, which is characterized in that the step
Suddenly in (1), 10 are evacuated to-5~10-3Sealed silica envelope after pa.
6. a kind of high quality Cu according to claim 12Se(1-x)AxThe growing method of crystal, which is characterized in that the step
Suddenly in (2), growth temperature setting are as follows: 450-550 DEG C of growing end, 550-650 DEG C of feed end.
7. a kind of high quality Cu according to claim 12Se(1-x)AxThe growing method of crystal, which is characterized in that the step
Suddenly in (2), the Cu of acquisition2Se(1-x)AxThe size of crystal is about 1.0~1.5mm.
8. a kind of high quality Cu according to claim 12Se(1-x)AxThe growing method of crystal, which is characterized in that the step
Suddenly in (2), the Cu of acquisition2Se(1-x)AxThe value of the x of crystal is 0.01~0.10.
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Citations (7)
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|---|---|---|---|---|
| JPS61222910A (en) * | 1985-03-28 | 1986-10-03 | Mitsubishi Metal Corp | Production of copper selenide |
| CN102674270A (en) * | 2012-05-25 | 2012-09-19 | 武汉理工大学 | Method for preparing Cu2Se thermoelectric material by low-temperature solid-phase reaction |
| CN103165809A (en) * | 2013-03-19 | 2013-06-19 | 武汉理工大学 | Self-propagating high-temperature rapid one-step synthesis thermoelectric material powder with nanostructure Cu2Se method |
| CN103803511A (en) * | 2014-02-24 | 2014-05-21 | 南京工业大学 | Copper selenide fluorescent quantum dot and preparation method and application thereof |
| CN104211024A (en) * | 2013-06-04 | 2014-12-17 | 中国科学院上海硅酸盐研究所 | P-type reversible phase transformation high-performance thermoelectric material and preparation method thereof |
| CN104630892A (en) * | 2015-02-28 | 2015-05-20 | 安庆美晶新材料有限公司 | Method for growing molybdenum disulfide single crystal by vapor phase transportation method |
| CN107324292A (en) * | 2017-02-27 | 2017-11-07 | 武汉理工大学 | A kind of supper-fast preparation high-performance Cu2The method of Se block thermoelectric materials |
-
2018
- 2018-10-20 CN CN201811225006.3A patent/CN109371468B/en active Active
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|---|---|---|---|---|
| JPS61222910A (en) * | 1985-03-28 | 1986-10-03 | Mitsubishi Metal Corp | Production of copper selenide |
| CN102674270A (en) * | 2012-05-25 | 2012-09-19 | 武汉理工大学 | Method for preparing Cu2Se thermoelectric material by low-temperature solid-phase reaction |
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Non-Patent Citations (4)
| Title |
|---|
| HUILI LIU，ET AL.: "Ultrahigh Thermoelectric Performance by Electron and Phonon Critical Scattering in Cu2Se1-xIx", 《ADV. MATER.》 * |
| JINGYI WANG，ET AL.: "I-doped Cu2Se nanocrystals for high-performance thermoelectric applications", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| LAN-LING ZHAO，ET AL.: "Superior intrinsic thermoelectric performance with zT of 1.8 in single-crystal and melt-quenched highly dense Cu2-xSe bulks", 《SCIENTIFIC REPORTS》 * |
| TRISTAN W. DAY,ET AL.: "Influence of Compensating Defect Formation on the Doping Efficiency and Thermoelectric Properties of Cu2-ySe1-xBrx", 《CHEM. MATER.》 * |
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