CN105603532A - Preparation method of antimony selenide monocrystal microparticles - Google Patents
Preparation method of antimony selenide monocrystal microparticles Download PDFInfo
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- CN105603532A CN105603532A CN201610168330.0A CN201610168330A CN105603532A CN 105603532 A CN105603532 A CN 105603532A CN 201610168330 A CN201610168330 A CN 201610168330A CN 105603532 A CN105603532 A CN 105603532A
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- single crystal
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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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- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
Abstract
The invention discloses a preparation method of antimony selenide monocrystal microparticles. The method comprises the following steps: grinding and mixing a simple substance antimony, a simple substance selenium and a fluxing agent, encapsulating the mixture in a quartz reaction vessel in a vacuum, keeping the temperature at 600-750 DEG C for 48-120 hours, and quickly cooling the quartz reaction vessel; and taking out the sample, washing and drying to obtain the antimony selenide monocrystal particles. The size of the monocrystal particles can be regulated by utilizing the recrystallization temperature and time; the particle components can be effectively regulated within a certain range through the mole ratio of the elements in the precursor; and the prepared monocrystal particles have the advantages of high uniformity, controllable size and better properties than the monocrystal particles prepared by the traditional method.
Description
Technical field
The present invention relates to photoelectric semiconductor material and device technology field, more specifically, relate to a kind of preparation method of antimony selenide micron single crystal grain.
Background technology
Solar cell is all a study hotspot all the time, current compound film battery mainly contains cadmium telluride (CdTe) and CIGS (CIGS) solar cell, these two kinds of batteries have severe toxicity and also have Partial Elements scarcity of resources because of contained Partial Elements, expensive, be difficult to large-scale application; And copper-zinc-tin-sulfur (CZTS) based solar battery rising in recent years utilizes large, the cheap Zn of reserves and Sn to replace the In in CIGS, and obtain 12.7% photoelectric transformation efficiency record, but CZTS be all multicomponent system the same as CIGS, Thermodynamically stable interval is little, the control of component and lattice defect is too complicated, cause in material impurity and defect too much, the further lifting difficulty of efficiency. Than above-mentioned different materials, antimony selenide (Sb2Se3) be the single-phase compound of a kind of binary, because its raw material reserves are large, toxicity is low, low price, bandwidth suitable (～1.15eV), large (> 10 of absorptivity5cm-1), crystal growth temperature is low, is very applicable to making the solar cell of novel low-cost low toxicity.
At present, all had about Sb both at home and abroad2Se3The application of material aspect solar cell, Sb2Se3Preparation mainly contain the techniques such as the hot note method of solution, solvent-thermal method, hydro-thermal method, electrodeposition process, hot spray process, and to prepare nanotube, nano wire and nano thin-film as main, and Sb2Se3Large-particle monocrystal preparation remain a technical barrier; In the time preparing solar cell, the performance of single crystal battery is better than the performance of hull cell again, and still, traditional Crystal Growth Technique (gas phase transmission technology, fusion technology) is difficult to grow the large size single crystal that meets solar battery obsorbing layer performance requirement.
Summary of the invention
Technical problem to be solved by this invention is to overcome existing preparation large scale Sb2Se3The existing above-mentioned defect of particle, provides a kind of Sb2Se3The preparation method of micron single crystal grain.
Second object of the present invention is to provide the Sb that above-mentioned preparation method obtains2Se3Micron single crystal grain.
The 3rd object of the present invention is to provide and contains above-mentioned Sb2Se3The solar cell of single crystal grain.
The 4th object of the present invention is to provide above-mentioned Sb2Se3Single crystal grain is in the application of preparing aspect solar cell.
The object of the invention is to be achieved by the following technical programs:
1. a preparation method for antimony selenide micron single crystal grain, comprises the following steps:
S1. reaction raw materials simple substance antimony, simple substance selenium are mixed by a certain percentage, add flux, ground and mixed is evenly mixed with presoma;
S2. presoma is packed in quartz reaction container, vacuumize or pass into inert gas after and seal quartz reaction container;
S3. the quartz reaction container after sealing is kept to 48～120h at 600～750 DEG C, quartz reaction container fast cooling, to room temperature, is taken out to the sample in quartz reaction container, after washing, being dried, obtain antimony selenide single crystal grain; Wherein, described in S1, simple substance antimony and simple substance selenium mol ratio are 1:1.5～3.
The present invention mixes simple substance antimony (Sb), simple substance selenium (Se) according to the ratio designing, and adds flux, and fully ground and mixed is made presoma, and under high temperature fused state, crystallization generates Sb2Se3Single crystal grain; In fused salt, crystal grain is grown under equilibrium state, in the time that grain shape and size reach requirement, reaction vessel is carried out to fast cooling, suppresses the nonequilibrium state growth of crystal in temperature-fall period, thereby has controlled the pattern of single crystal grain; The composition of single crystal grain can be by the effectively allotment within the specific limits of the mol ratio of element in presoma, and the size of single crystal grain can utilize crystallization temperature and time to regulate and control.
For different elements, different structure compositions, the parameter that it need to be controlled, as element ratio, crystallization temperature, crystallization time, inventor need to constantly grope in this process, thereby makes satisfactory single crystal grain.
Can be able to make each single crystal grain form a battery unit owing to utilizing pattern rule, the uniform single crystal grain of component to prepare solar cell, effectively reduce absorbed layer defect and the impact of interface impurity on device performance, and single crystal grain formation matte can effectively improve the utilization rate of incident light, there is advanced optical characteristics, can significantly promote in theory Sb2Se3The conversion efficiency of battery, therefore, single crystal grain has the performance more excellent than thin-film material and obtained people to be paid close attention to widely. It is uncontrollable that prior art utilizes molten-salt growth method to prepare the pattern of single crystal grain, component is inhomogeneous, and the time that forms single crystal grain is oversize, be unfavorable for industrial production, the invention reaction raw materials and flux are ground, obtain pattern by vacuum seal, high-temperature fusion crystallization controlled, the single crystal grain that component is controlled.
In fact, it is very difficult that preparation meets the single crystal grain of solar battery obsorbing layer, is only control element composition, raw material proportioning or the growth technique of only controlling monocrystalline, all likely causes single crystal grain to be prepared unsuccessfully; To, in conjunction with the growth technique of element composition, raw material proportioning and the monocrystalline of the actual single crystal grain that will prepare, could finally obtain qualified single crystal grain. The present invention is taking molten-salt growth method as prototype, by reaction raw materials and flux are ground and evenly vacuumize sealing according to certain ratio, it is reacted to certain hour at a certain temperature, when reaction generates desirable size pattern, suppress the further growth of crystal by fast cooling, cooling and suitable temperature can effectively be prepared the micron single crystal grain of ideal dimensions size timely.
When after completion of the reaction, need to lower the temperature to quartz reaction container, first be cooled to 450 DEG C, interior crystal growing process is still in equilibrium state growth during this period of time, be conducive to reduce the blemish of crystal, carrying out fast cooling, is the nonequilibrium state growth in order to suppress crystal again, and effectively prevents the generation of other impurity phases.
In addition, flux kind and consumption are prepared tool to single crystal grain and are had a certain impact, in suitable fused salt kind and molten salt system, suitable flux consumption contributes to the growth of molten salt system crystal, and preferably, flux is one or more in KI, CsCl, CsI described in S1.
Preferably, described flux is 1～10:1 with the mol ratio of mixing of reaction raw materials.
Preferably, the vacuum vacuumizing described in S2 in rear quartz reaction container is 10～102Pa。
The antimony selenide micron single crystal grain that the present invention also provides any one method to obtain.
The solar cell that contains described single crystal grain is provided simultaneously.
Also provide described single crystal grain in the application of preparing aspect solar cell.
Compared with prior art, the present invention has following beneficial effect:
The invention provides a kind of preparation method of antimony selenide micron single crystal grain, according to the formula reaction raw material of design, then add the abundant ground and mixed of flux to prepare presoma, by precursor powder Vacuum Package, in quartz reaction container, at the temperature of setting, melting recrystallization generates Sb2Se3Single crystal grain; The size of prepared single crystal grain can utilize the temperature and time of recrystallization to regulate and control, the composition of particle can be by the effectively allotment within the specific limits of the mol ratio of each element in presoma, preparation-obtained single crystal grain composition is even, regular shape, big or small controlled, performance is better than the single crystal grain that conventional method prepares, and concrete advantage is as follows:
(1) high-temperature fusion crystallization can obtain the uniform single crystal grain of component, and fast cooling suppresses the nonequilibrium state growth of monocrystalline in temperature-fall period, thereby has controlled pattern and the component of single crystal grain.
(2) combination of different fused salt and proportioning can be passed through the phase mutual friction of the phase mutual friction of crystal grain and crystal grain and fused salt in single crystal growth process, effectively eliminate the crystal face corner angle of grain surface, thereby control the form of grain surface, obtain the comparatively bright and clean single crystal grain in surface.
(3) reaction raw materials aboundresources used, cheap, Preparation equipment is simple, pollutes littlely in preparation process, is easy to suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the Sb that in embodiment 1 prepared by molten-salt growth method2Se3Single crystal grain.
Fig. 2 is the surface topography of the sample of preparation in comparative example 1.
Fig. 3 is the surface topography of the sample of preparation in comparative example 2.
Detailed description of the invention
Further illustrate content of the present invention below in conjunction with Figure of description and specific embodiment, but should not be construed as limitation of the present invention. Without departing from the spirit and substance of the case in the present invention, the simple modification that the inventive method, step or condition are done or replacement, all belong to scope of the present invention; If do not specialize, the conventional means that in embodiment, technological means used is well known to those skilled in the art.
Embodiment 1
Take reaction raw materials 2mmolSb, 3mmolSe and flux 10mmolCsCl, after mixing, obtain presoma, presoma is fully ground, it is mixed; Mixed sample is packed in quartz bottle, utilize vavuum pump unit to vacuumize and reach 10～102Pa(also can blanketing with inert gas), thus the impact of deaeration on molten salt react ion, with oxyhydrogen flame by quartzy bottle closure; The quartz bottle that biased sample is housed after sealing is placed in common heating furnace and is heated to 700 DEG C of maintenance 72h from normal temperature, then cool to 450 DEG C of taking-up quartz bottles fast cooling to room temperature (putting into water); Finally the sample in quartz bottle is taken out, flux CsCl is repeatedly removed in ultrasonic washing, afterwards sample is placed in to 80 DEG C of dry 2h of drying box, obtains surface and have the micron-scale Sb of crystal gloss2Se3Single crystal grain, approximately 55 microns.
To the Sb obtaining2Se3Single crystal grain carries out Performance Detection, and result shows, the Sb of embodiment 12Se3Single crystal grain is all grain of rice shape strip, and resistance value is 3.22K Ω, and band gap width is about 1.27eV.
Embodiment 2
Take reaction raw materials 2mmolSb, 4mmolSe and flux 30mmolCsI, after mixing, obtain presoma, presoma is fully ground, it is mixed; Mixed sample is packed in quartz bottle, utilize vavuum pump unit to vacuumize and reach 10～102Pa(also can blanketing with inert gas), thus the impact of deaeration on molten salt react ion, with oxyhydrogen flame by quartzy bottle closure; The quartz bottle that biased sample is housed after sealing is placed in common heating furnace and is heated to 650 DEG C of maintenance 96h from normal temperature, then cool to 450 DEG C of taking-up quartz bottles fast cooling to room temperature (putting into water); Finally the sample in quartz bottle is taken out, flux CsI is repeatedly removed in ultrasonic washing, afterwards sample is placed in to 80 DEG C of dry 2h of drying box, obtains surface and have the micron-scale Sb of crystal gloss2Se3Single crystal grain, approximately 60 microns.
To the Sb obtaining2Se3Single crystal grain carries out Performance Detection, and result shows, the Sb of embodiment 22Se3Single crystal grain is all grain of rice shape strip, and resistance value is 3.02K Ω, and band gap width is about 1.21eV.
Embodiment 3
Take reaction raw materials 2mmolSb, 6mmolSe and flux 64mmolKI, after mixing, obtain presoma, presoma is fully ground, it is mixed; Mixed sample is packed in quartz bottle, utilize vavuum pump unit to vacuumize and reach 10～102Pa(also can blanketing with inert gas), thus the impact of deaeration on molten salt react ion, with oxyhydrogen flame by quartzy bottle closure; The quartz bottle that biased sample is housed after sealing is placed in common heating furnace and is heated to 600 DEG C of maintenance 120h from normal temperature, then cool to 450 DEG C of taking-up quartz bottles fast cooling to room temperature (putting into water); Finally the sample in quartz bottle is taken out, flux KI is repeatedly removed in ultrasonic washing, afterwards sample is placed in to 80 DEG C of dry 2h of drying box, obtains surface and have the micron-scale Sb of crystal gloss2Se3Single crystal grain, approximately 50 microns.
To the Sb obtaining2Se3Single crystal grain carries out Performance Detection, and result shows, the Sb of embodiment 32Se3Single crystal grain is all grain of rice shape strip, and resistance value is 3.54K Ω, and band gap width is about 1.31eV.
Comparative example 1
Experimental technique is with embodiment 1, unique different, and reaction raw materials is not containing flux, to the Sb finally obtaining2Se3Single crystal grain carries out nature examination, and result shows: cannot prepare pattern rule, the uniform Sb of component2Se3Micron single crystal grain.
Comparative example 2
Experimental technique is with embodiment 1, and unique different, presoma does not grind, and directly puts into the reaction of quartz bottle, to the Sb finally obtaining2Se3Single crystal grain carries out nature examination, and result shows: the sample composition obtaining is inhomogeneous, and grain shape is irregular, and the particle of micron-scale is less.
Comparative example 3
Experimental technique is with embodiment 1, uniquely different be, the quartz bottle that biased sample is housed after sealing is placed in common heating furnace and is heated to 900 DEG C of maintenance 96h from normal temperature, then cool to 650 DEG C of taking-up quartz bottles fast cooling to room temperature, the particle finally obtaining is carried out to nature examination, result shows: particle surface fineness is poor, has obvious simple substance Se, simple substance Sb cluster body, does not meet the absorbed layer material as solar cell.
Claims (8)
1. a preparation method for antimony selenide micron single crystal grain, is characterized in that, comprises the following steps:
S1. reaction raw materials simple substance antimony, simple substance selenium are mixed by a certain percentage, add flux, ground and mixed is evenly mixed with presoma;
S2. presoma is packed in quartz reaction container, vacuumize or pass into inert gas after and seal quartz reaction container;
S3. the quartz reaction container after sealing is kept to 48～120h at 600～750 DEG C, quartz reaction container fast cooling, to room temperature, is taken out to the sample in quartz reaction container, after washing, being dried, obtain antimony selenide single crystal grain; Wherein, described in S1, simple substance antimony and simple substance selenium mol ratio are 1:1.5～3.
2. preparation method according to claim 1, is characterized in that, S3 is first cooled to 450 DEG C to quartz reaction container, then fast cooling is to room temperature.
3. preparation method according to claim 1, is characterized in that, flux is one or more in KI, CsCl, CsI described in S1.
4. preparation method according to claim 1, is characterized in that, described flux is 1～10:1 with the mol ratio of mixing of reaction raw materials.
5. preparation method according to claim 1, is characterized in that, the vacuum vacuumizing in rear quartz reaction container described in S2 is 10～102Pa。
6. the antimony selenide micron single crystal grain that described in claim 1 to 5 any one, preparation method obtains.
7. contain the solar cell of single crystal grain described in claim 6.
Described in claim 6 single crystal grain in the application of preparing aspect solar cell.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106477534B (en) * | 2016-09-29 | 2018-08-31 | 广东先导稀材股份有限公司 | A kind of preparation method of selenium arsenic alloy |
| CN113235166A (en) * | 2021-05-13 | 2021-08-10 | 重庆文理学院 | Preparation method of large-size antimony selenide single crystal material |
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Cited By (2)
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| CN113235166A (en) * | 2021-05-13 | 2021-08-10 | 重庆文理学院 | Preparation method of large-size antimony selenide single crystal material |
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