WO2019085679A1 - 一种制备多元合金化合物的装置 - Google Patents

一种制备多元合金化合物的装置 Download PDF

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WO2019085679A1
WO2019085679A1 PCT/CN2018/107005 CN2018107005W WO2019085679A1 WO 2019085679 A1 WO2019085679 A1 WO 2019085679A1 CN 2018107005 W CN2018107005 W CN 2018107005W WO 2019085679 A1 WO2019085679 A1 WO 2019085679A1
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reactor
zone
alloy compound
producing
compound according
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PCT/CN2018/107005
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English (en)
French (fr)
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陈腾
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北京铂阳顶荣光伏科技有限公司
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Publication of WO2019085679A1 publication Critical patent/WO2019085679A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J12/00—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor
    • B01J12/005—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor carried out at high temperatures, e.g. by pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0073—Sealings
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/541—Heating or cooling of the substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/305—Sulfides, selenides, or tellurides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264—Inorganic materials
    • H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00331—Details of the reactor vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00594—Gas-phase processes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • H01L31/042—PV modules or arrays of single PV cells
    • H01L31/0445—PV modules or arrays of single PV cells including thin film solar cells, e.g. single thin film a-Si, CIS or CdTe solar cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/541—CuInSe2 material PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • This application relates to, but is not limited to, a device for preparing a multi-alloy compound.
  • the heating device is disposed around the reactor, configured to heat the reactor and form a temperature gradient
  • the reactor has an opening and the sealing device is configured to seal the opening.
  • the low temperature evaporation zone may be a quartz boat, crucible or a pit formed in the reactor.
  • the high temperature synthesis zone may be located at one end of the long side of the L-shaped reaction tube, and the low temperature evaporation zone may be located at one end of the short side of the L-shaped reaction tube.
  • the length of the long side of the L-shaped reaction tube may be 1100 mm to 1600 mm
  • the length of the short side may be 400 mm to 700 mm
  • the diameter of the L-shaped reaction tube may be 60 mm to 80 mm.
  • the reactor may be a quartz tube or a ceramic tube.
  • the L-shaped reaction tube may be closed at one end and open at the other end and provided with an opening.
  • multi-alloy compound is defined as a compound which is made of a plurality of simple substances, and whose sublimation temperature of one element is lower than the melting temperature of a mixture composed of other simple substances.
  • the apparatus for preparing a multi-component compound of the present application can control the content of each element in the multi-alloy compound, it is possible to prepare a multi-element alloy compound having different element contents, for example, a copper indium gallium selenide compound having a different indium gallium ratio, thereby preparing the prepared The distribution of each element in the alloy compound is more uniform and the quality is more controllable.
  • FIG. 1 is a schematic view of an apparatus for preparing a copper indium gallium selenide compound according to an embodiment of the present application.
  • the present embodiment provides an apparatus for preparing a multi-component alloy compound, the apparatus comprising a reactor 1, a low temperature evaporation zone 2, a high temperature synthesis zone 3, a sealing device 4, and a heating device 5, wherein: the high temperature synthesis zone 3 and the Low temperature evaporation zones 2 are respectively disposed at both ends of the reactor 1; the heating device 5 is disposed around the reactor 1 and configured to heat the reactor 1 and form a temperature gradient; the reaction The device 1 has an opening, and the sealing device 4 is configured to be able to seal the opening.
  • the high temperature synthesis zone 3 may be a quartz boat, crucible or a pit formed in the reactor 1.
  • the low temperature evaporation zone 2 may be a quartz boat, crucible or a pit formed in the reactor 1.
  • the reactor 1 may be an L-shaped reaction tube; the reactor 1 may be a quartz tube, a ceramic tube or a tube having a certain rigidity prepared by using other high temperature resistant materials.
  • the high temperature synthesis zone 3 may be located at one end of the long side of the L-shaped reaction tube, and the low temperature evaporation zone 2 may be located at one end of the short side of the L-shaped reaction tube.
  • the high temperature synthesis zone 3 and the low temperature evaporation zone 2 are respectively disposed at both ends of the reactor 1, so that the high temperature synthesis zone 3 and the low temperature evaporation zone 2 are spaced apart by a set distance, so that they can be heated to different temperatures. In the case where the distance requirement is satisfied, the positions of the high temperature synthesis zone 3 and the low temperature evaporation zone 2 can be adjusted as needed.
  • the length of the long side of the L-shaped reaction tube may be 1100 mm to 1600 mm, the length of the short side may be 400 mm to 700 mm, and the diameter of the L-shaped reaction tube may be 60 mm to 80 mm.
  • the heating device 5 can be configured to enable zone heating of the reactor 1 so that the temperature of each zone can be individually controlled and form a temperature gradient.
  • the heating device 5 may be an electric heating coil that may surround the outer surface of the L-shaped quartz tube or may be disposed adjacent to the outer surface of the L-shaped quartz tube as shown.
  • An electric heating coil corresponding to the low temperature evaporation zone 2 and the high temperature synthesis zone 3 may have a length of 300 mm, and is located between the electric heating coils corresponding to the low temperature evaporation zone 2 and the electric heating coil of the high temperature synthesis zone 3.
  • the length can be 200mm and can be set at intervals of 100mm.
  • the L-shaped reaction tube may be disposed to be closed at one end, open at the other end and having an opening, or may be provided with an opening at both ends.
  • the opening may be located at one end of the long side of the L-shaped reaction tube.
  • the opening may be a constriction
  • the sealing device 4 may be a bubble
  • the encapsulation may match the shape of the constriction to enable sealing of the constriction.
  • the vacuum container comprises a high temperature synthesis zone 3 and a low temperature evaporation zone 2;
  • the quartz boat containing the Se element corresponds to the low temperature zone corresponding to the low temperature evaporation zone 2 in the electric furnace
  • the quartz boat containing the CuInGa element corresponds to the high temperature zone corresponding to the high temperature synthesis zone 3 in the electric furnace.
  • the reactor of the apparatus for preparing a multi-alloy compound of the present embodiment may be used to form a vacuum vessel, and the reactor may be evacuated to other pressures of 10 -1 Pa or below, for example, 10 -1 . Pa, 10 -2 Pa, 10 -3 Pa or 10 -4 Pa. It is also possible to use other high-temperature-resistant containers without using a quartz boat to hold the materials, for example, using enamel materials.
  • the composition of the above copper indium gallium selenide compound is not limited to the formation of the composition of the copper indium gallium selenide compound prepared in the present embodiment.
  • a copper indium gallium selenide compound of the following composition may also be prepared: CuIn 0.85 Ga 0.15 Se 2.05 , CuIn 0.9 Ga 0.1 Se 2 , CuIn 0.8 Ga 0.2 Se 2 , CuIn 0.75 Ga 0.25 Se 2 ; during the preparation of the above copper indium gallium selenide compound, the sum of the molar fraction of indium and gallium and the molar fraction of copper may be used for weighing The numbers are substantially equal to calculate the mass of elemental copper, indium, and gallium.
  • the ratio of the mole fraction of copper, indium, and gallium can be substantially equal to the ratio of the number of atoms of copper, indium, and gallium in the compound to be prepared.
  • the molar fraction of selenium can be calculated by more than twice the molar fraction of copper.
  • the ratio of the molar fraction of selenium to copper can be slightly larger than the atomic ratio of selenium to copper in the compound to be prepared;
  • the molar fraction of selenium may be 2.1 times, 2.2 times, 2.3 times, 2.4 times or 2.5 times that of copper. Excess selenium is placed in the low temperature evaporation zone 2, so that the reaction can be maintained in an atmosphere of selenium vapor throughout the entire reaction process because selenium is excessive.
  • a linear temperature gradient interval from a low temperature to a high temperature can be formed by adjusting the temperature control power between the high temperature synthesis zone 3 and the low temperature evaporation zone 2.
  • the high temperature synthesis zone 3 can be set to rise from 1100 ° C to 1150 ° C from 85 min to 90 min.
  • the temperature of the high temperature synthesis zone 3 can be raised to 700 ° C to 750 ° C.
  • the temperature rise of the low temperature evaporation zone 2 can be started, and the low temperature evaporation zone 2 can be set to be heated from 55 min to 60 min. To 550 ° C to 600 ° C.
  • the temperature gradient from the low temperature to the high temperature can be formed from the low temperature evaporation zone 2 to the high temperature synthesis zone 3 by separately adjusting the heating power of the heating device corresponding to each region between the high temperature synthesis zone 3 and the low temperature evaporation zone 2.
  • a linear temperature gradient interval can be formed.
  • the power of the heating device can be set such that the temperature of the high temperature synthesis zone 3 is raised to between 1100 ° C and 1150 ° C in the range of 85 min to 90 min.
  • the power of the heating device can be set such that the temperature of the low temperature evaporation zone 2 is raised to between 550 ° C and 600 ° C in 55 min to 60 min.
  • the time at which the selenium in the low temperature evaporation zone 2 begins to change to the gaseous state no earlier than the time in which the copper indium gallium is melted may be that the time at which the selenium in the low temperature evaporation zone 2 begins to change to the gaseous state is not earlier than the time in which the copper indium gallium is completely melted.
  • the mass of each element is weighed according to the composition CuIn 0.7 Ga 0.3 Se 2.05 in step S2, and the composition of the obtained CIGS compound is CuIn 0.7 Ga 0.3 Se 2 , that is, to obtain the compound CuIn 0.7 Ga 0.3 Se 2 can calculate the molar ratio of each element to be weighed according to the atomic ratio of each element in CuIn 0.7 Ga 0.3 Se 2.05 .
  • a method of preparing a copper indium gallium selenide compound comprising the steps of:
  • the vacuum container comprises a high temperature synthesis zone 3 and a low temperature evaporation zone 2;
  • a vacuum container is provided, and the vacuum container may be an L-shaped quartz tube.
  • the vacuum container includes a high temperature synthesis zone 3 and a low temperature evaporation zone 2, and the portions having a certain interval in the vacuum vessel are respectively used as the high temperature synthesis zone 3 and In the low temperature evaporation zone 2, the two ends of the L-shaped quartz tube are respectively a high temperature synthesis zone 3 and a low temperature evaporation zone 2, and a high temperature synthesis zone 3 is placed with a quartz boat containing a copper indium selenium element, and a selenium is placed in the low temperature evaporation zone 2 Simple quartz boat;
  • step S2 Cu, In, Ga, and Se simple substances having a purity greater than 99.999% can be used as raw materials, and the mass of each element can be weighed according to the composition CuIn 0.8 Ga 0.2 Se 2.05 , and the Se element is placed in the L-shaped quartz tube.
  • the Cu, In, Ga element is placed in the quartz boat at the end of the long side of the L-shaped quartz tube.
  • the quartz tube can be vacuumed to below 10 -3 Pa, and the L-shaped quartz tube is sealed and placed in the electric heating.
  • a linear temperature gradient interval from a low temperature to a high temperature can be formed by adjusting the temperature control power between the high temperature synthesis zone and the low temperature synthesis zone.
  • the high temperature synthesis zone 3 can be set to a temperature of 1125 ° C for 88 minutes.
  • the temperature of the high temperature synthesis zone 3 can be raised to 725 ° C.
  • the temperature rise of the low temperature evaporation zone 2 can be started, and the low temperature evaporation zone 2 can be set to rise to 575 ° C in 56 minutes.
  • step S4 after the low temperature evaporation zone 2 reaches 575 ° C, the temperature of the high temperature synthesis zone and the temperature of the low temperature evaporation zone can be maintained for 6 hours.
  • the mass of each element is weighed according to the composition CuIn 0.8 Ga 0.2 Se 2.05 in step S2, and the composition of the obtained CIGS compound is CuIn 0.8 Ga 0.2 Se 2 , that is, to obtain the compound CuIn 0.8 Ga 0.2 Se 2 can calculate the molar ratio of each element to be weighed according to the atomic ratio of each element in CuIn 0.8 Ga 0.2 Se 2.05 .
  • a positive temperature gradient from the low temperature evaporation zone 2 to the high temperature synthesis zone 3 can be achieved, in order to ensure the stability of the selenium vapor transport rate. It is possible to control a linear temperature gradient between the low temperature evaporation zone 2 of the entire quartz tube and the high temperature synthesis zone 3.
  • the preparation method of the copper indium gallium selenide alloy of the present application can precisely control the composition of the copper indium gallium selenide alloy during the preparation process, the copper indium gallium selenide of each absorption layer can be controlled when preparing the progressive band gap light absorbing layer.
  • the composition can control the band gap width of each of the absorbing layers, thereby enabling the printing method to produce a progressive bandgap light absorbing layer.

Abstract

一种制备多元合金化合物的装置，所述装置包括反应器(1)、低温蒸发区(2)、高温合成区(3)、封口装置(4)和加热装置(5)，其中：所述高温合成区(3)和低温蒸发区(2)分别设置在所述反应器(1)的两端；所述加热装置(5)间隔设置在所述反应器(1)的周围，配置为对所述反应器(1)加热，并形成温度梯度；所述反应器(1)具有开口，所述封口装置(4)配置为能够对所述开口进行密封。

Description

一种制备多元合金化合物的装置 技术领域
本申请涉及但不限于一种制备多元合金化合物的装置。
背景技术
众所周知，CIGS(CuIn xGa (1-x)Se 2，铜铟镓硒薄膜太阳能电池)是具备很大潜力的一种薄膜太阳能电池，目前产业上制备CIGS的主流方法为共蒸发法和磁控溅射法，基于前两种方法的高真空性，无论从设备还是工艺角度，成本都比较高，因此，类似印刷等非真空低成本制备CIGS的技术被业界不断推动。
当前非真空印刷CIGS采用的涂布浆料或胶体的制备主要有两种方法，第一，采用化学合成方法制备CIGS纳米材料并进一步调制成浆料，但是化学合成的CIGS的纯度低，制备的CIGS薄膜少子寿命低，因此目前采用该种吸收层的电池效率比较低；第二，采用四种单质粉末或几种二三元化合物粉末调配涂布原材料，这种浆料在成膜过程中进一步形成四元化合物时的反应难于控制，不充分的反应会造成组分失配，同时，较高的反应温度也可能造成硒组分的大量流失，从而导致制备的CIGS薄膜质量差。
另外，制备渐变带隙的CIGS薄膜有利于提高薄膜光吸收层的转化效率，而当前印刷制备CIGS薄膜局限于CIGS材料的制备方法，多为单一固定组分的CIGS薄膜，不利于高效电池的制备。
发明概述
以下是对本文详细描述的主题的概述。本概述并非是为了限制权利要求的保护范围。
针对上述问题，本申请提供了一种能够精准控制多元合金成分的制备装置。
本申请提供了一种制备多元合金化合物的装置，所述装置包括反应器、低温蒸发区、高温合成区、封口装置和加热装置，其中：
所述高温合成区和所述低温蒸发区分别设置在所述反应器的两端；
所述加热装置间隔设置在所述反应器的周围，配置为对所述反应器加热，并形成温度梯度；
所述反应器具有开口，所述封口装置配置为能够对所述开口进行密封。
在示例性实施例中，所述低温蒸发区可以为石英舟、坩埚或形成在所述反应器中的凹坑。
在示例性实施例中，所述高温合成区可以为石英舟、坩埚或形成在所述反应器中的凹坑。
在示例性实施例中，所述高温合成区和低温蒸发区可以均为形成在所述反应器中的凹坑。
在示例性实施例中，所述反应器可以为L型反应管。
在示例性实施例中，所述高温合成区可以位于所述L型反应管的长边的一端，所述低温蒸发区可以位于所述L型反应管的短边的一端。
在示例性实施例中，所述L型反应管的长边的长度可以为1100mm至1600mm，短边的长度可以为400mm至700mm，所述L型反应管的直径可以为60mm至80mm。
在示例性实施例中，所述反应器可以为石英管或陶瓷管。
在示例性实施例中，加热装置可以为电加热线圈，其环绕在所述反应器的外表面。
在示例性实施例中，所述L型反应管可以一端封闭，另一端开放并设置有开口。
在示例性实施例中，所述开口可以位于所述L型反应管的长边的一端。
在示例性实施例中，所述开口可以为缩口。
在示例性实施例中，所述封口装置可以为封泡。
在示例性实施例中，所述封泡的长度可以为150mm至250mm，直径为40mm至60mm。在示例性实施例中，所述石英舟可以为直径为50mm至70mm，长为200mm至400mm的半管。
在示例性实施例中，所述多元合金化合物可以为铜铟镓硒化合物。
在本申请中，术语“多元合金化合物”定义为由多种单质制成、并且其中一种单质的升华温度低于由其他单质组成的混合物的熔融温度的化合物。
本申请的制备多元化合物的装置通过使反应器从低温蒸发区的温度梯度增加至高温合成区的温度，避免了单质(例如，硒)升华为气态后得到的蒸气沉降在反应器的管壁上，从而避免了单质升华为气态后的损失，保证了该单质和其他单质(例如，铜、铟、镓)的充分化合反应。由于采用本申请的制备多元化合物的装置可以控制多元合金化合物中各元素的含量，因此可以制备出不同元素含量的多元合金化合物，例如，不同铟镓比的铜铟镓硒化合物，使制备出的合金化合物中各元素的分布更加均匀，质量更加可控。
附图概述
附图用来提供对本申请技术方案的进一步理解，并且构成说明书的一部分，与本申请的实施例一起用于解释本申请的技术方案，并不构成对本申请技术方案的限制。
图1是本申请实施例制备铜铟镓硒化合物的装置示意图。
详述
下面结合说明书附图对本申请做进一步的描述。
以下，仅为本申请的较佳实施例，但本申请的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本申请揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本申请的保护范围之内。因此，本申请的保护范围应该以权利要求所界定的保护范围为准。
实施例1
本实施例提供一种制备多元合金化合物的装置，所述装置包括反应器1、低温蒸发区2、高温合成区3、封口装置4和加热装置5，其中：所述高温合成区3和所述低温蒸发区2分别设置在所述反应器1的两端；所述加热装置5间隔设置在所述反应器1的周围，配置为对所述反应器1加热，并形成温 度梯度；所述反应器1具有开口，所述封口装置4配置为能够对所述开口进行密封。
所述高温合成区3可以为石英舟、坩埚或形成在所述反应器1中的凹坑。
所述低温蒸发区2可以为石英舟、坩埚或形成在所述反应器1中的凹坑。
所述反应器1可以为L型反应管；所述反应器1可以为石英管、陶瓷管或采用其他耐高温材质制备的具有一定刚性的管子。
所述高温合成区3可以位于所述L型反应管的长边的一端，所述低温蒸发区2可以位于所述L型反应管的短边的一端。
高温合成区3和低温蒸发区2分别设置在所述反应器1的两端，使高温合成区3和低温蒸发区2间隔设定的距离，从而可以加热到不同的温度。在满足距离要求的情况下，高温合成区3和低温蒸发区2的位置可以根据需要进行调整。
所述L型反应管的长边的长度可以为1100mm至1600mm，短边的长度可以为400mm至700mm，所述L型反应管的直径可以为60mm至80mm。
所述加热装置5可以配置为能够对所述反应器1进行分区加热，使每个区的温度能够被单独控制并形成温度梯度。
所述加热装置5可以为电加热线圈，其可以环绕在L型石英管外表面，也可以如图所示设置在靠近L型石英管外表面的位置。
对应所述低温蒸发区2和所述高温合成区3的电加热线圈的长度可以为300mm，位于对应所述低温蒸发区2和所述高温合成区3的电加热线圈之间的电加热线圈的长度可以为200mm，并且可以相距100mm间隔设置。所述L型反应管可以设置为一端封闭，另一端开放并具有开口，也可以设置为两端都具有开口。
所述开口可以位于所述L型反应管的长边的一端。
所述开口可以为缩口，所述封口装置4可以为封泡，所述封泡可以与所述缩口的形状相匹配从而能够对所述缩口进行密封。
所述封泡的长度可以为150mm至250mm，直径可以为40mm至60mm，例如，长度可以为200mm，直径可以为50mm。
所述石英舟可以为直径为50mm至70mm、长度为200mm至400mm的半管，例如为直径为66mm、长度为300mm的半管。
本实施例还提供一种制备多元合金化合物的方法，以制备铜铟镓硒化合物为例，所述方法可以包括如下步骤：
S1：提供一真空容器，真空容器包括间隔设置的高温合成区3和低温蒸发区2；
S2：将铜、铟、镓单质放置在高温合成区3，将硒单质放置在低温蒸发区2；
S3：将高温合成区3的铜、铟、镓加热至熔融状态，将低温蒸发区2的硒加热至气态；低温蒸发区2的硒开始转变为气态的时间不早于铜铟镓熔融的时间；
S4：将高温合成区3和低温蒸发区2保温，以使铜铟镓硒进行反应；
S5：将高温合成区3的温度降至不低于铜铟镓硒合金的熔融温度并进行保温，然后将高温合成区3和低温蒸发区2降温至100℃以下；
在上述步骤中，可以始终保持低温蒸发区2与高温合成区3之间存在正向温度梯度，即真空容器的温度从低温蒸发区2到高温合成区3是梯度增加的。
在步骤S1中，提供一种真空容器，该真空容器可以为石英管、陶瓷管等采用耐高温材质制备的具有一定刚性的容器，例如，采用本实施例的反应器。将真空容器中具有一定间隔的部分分别作为高温合成区3和低温蒸发区2。当物料放入上述的容器中后，将容器内的气压抽至10 -1Pa或者以下就成为真空容器。
在步骤S2中，可以使用纯度大于99.999％的Cu、In、Ga和Se单质为原材料，各单质质量可以按照组分CuIn 0.7Ga 0.3Se 2.05去称配，可以将Se单质置于L型石英管短边一端的石英舟内，将Cu、In、Ga单质置于L型石英管长边一端的石英舟内，将L型石英管抽真空至10 -2Pa以下后密封L型石英管放入电热炉中，盛有Se单质的石英舟对应电热炉中的对应低温蒸发区2的低温区，盛有CuInGa单质的石英舟对应电热炉中的对应高温合成区3的高温 区。除了L型石英管之外，也可以采用本实施例的制备多元合金化合物的装置的反应器形成真空容器，可以将反应器抽真空至10 -1Pa或者以下的其他压力，例如，10 -1Pa、10 -2Pa、10 -3Pa或者10 -4Pa。也可以不采用石英舟盛放物料而采用其他耐高温的容器盛放，例如采用坩埚盛放物料。如果在容器的高温合成区3和低温蒸发区2具有凹坑，可以不采用其他容器盛放物料，直接将物料置于凹坑内。也可以采用其他加热装置对L型石英管进行加热，例如采用本实施例提供的制备多元合金化合物的装置的加热装置5。
上述铜铟镓硒化合物的成分并不对本实施例制备的铜铟镓硒化合物的成分形成限定，例如，还可以制备以下组分的铜铟镓硒化合物：CuIn 0.85Ga 0.15Se 2.05，CuIn 0.9Ga 0.1Se 2，CuIn 0.8Ga 0.2Se 2，CuIn 0.75Ga 0.25Se 2；在上述铜铟镓硒化合物的制备过程中，称量时可以按照使铟和镓的摩尔份数之和与铜的摩尔份数基本相等去计算单质铜、铟和镓的质量，例如，可以使铜、铟和镓的摩尔份数之比基本等于期望制备的化合物中的铜、铟和镓的原子个数之比，而硒的摩尔份数可以按照大于铜的摩尔份数的两倍进行计算，例如，可以使硒与铜的摩尔份数之比可以稍大于期望制备的化合物中的硒与铜的原子个数比；例如硒的摩尔份数可以为铜的2.1倍、2.2倍、2.3倍、2.4倍或者2.5倍。将过量的硒放置在低温蒸发区2，这样，在整个反应过程中，由于硒是过量的，能够始终保持在硒蒸气的氛围中进行反应。
在步骤S3中，可以通过调整高温合成区3和低温蒸发区2之间的温控功率，形成从低温到高温的线性温度梯度区间。高温合成区3可以设定85min至90min升温至1100℃至1150℃。当高温合成区3启动升温55min至60min时，高温合成区3的温度可以升至700℃至750℃，此时可以启动对低温蒸发区2升温，可以设定低温蒸发区2在55min至60min升温至550℃至600℃。
例如，可以通过单独调整高温合成区3和低温蒸发区2之间的各个区域所对应的加热装置的加热功率，从而使从低温蒸发区2到高温合成区3形成从低温到高温的温度梯度区间，例如，可以形成线性温度梯度区间。可以设定加热装置的功率使高温合成区3的温度在85min至90min内升温至1100℃至1150℃。可以设定加热装置的功率使低温蒸发区2的温度在55min至60min内升温至550℃至600℃。在步骤S4中，待低温蒸发区2达到最高温 度后保持6h。保温时间可以根据物料的数量、反应类型等条件进行计算，尽量保证使铜铟镓硒充分进行反应。例如，可以待低温蒸发区2达到最高温度后使高温合成区3和低温蒸发区2都保温6h。
低温蒸发区2的硒开始转变为气态的时间不早于铜铟镓熔融的时间可以为低温蒸发区2的硒开始转变为气态的时间不早于铜铟镓完全熔融的时间。
在步骤S5中，将高温合成区3的温度降至不低于铜铟镓硒合金的熔融温度并进行保温，目的是确保合金元素处于正饱和状态，不影响CIGS的逆反应。可以将高温合成区3设定为在15min内降温至950℃至1000℃，再保温1.5h至2h，之后关闭所有加热装置使高温合成区3和低温蒸发区2冷却至100℃以下，在高温合成区3石英舟内得到CIGS四元化合物，合成的CIGS化合物组分为CuIn 0.7Ga 0.3Se 2。本实施例在步骤S2中按照组分CuIn 0.7Ga 0.3Se 2.05去称配各单质的质量，得到的CIGS化合物的组分为CuIn 0.7Ga 0.3Se 2，也就是说若要得到化合物CuIn 0.7Ga 0.3Se 2，可以按照CuIn 0.7Ga 0.3Se 2.05中各元素的原子比去计算待称量的各单质的摩尔比。
为了保证硒蒸气在输运过程中不会凝结在石英管的内壁上，可以使由低温蒸发区2到高温合成区3之间具有正向的温度梯度，为了保证硒蒸气输运速率的稳定性，可以控制整个石英管的低温蒸发区2到高温合成区3之间具有线性的温度梯度。
本实施例的铜铟镓硒化合物制备方法中，首先将铜铟镓加热至熔融状态，使铜铟镓首先反应，然后将硒加热升华为气态，使真空容器中形成硒氛围，从而对铜铟镓进行硒化。为了使铜铟镓能够被均匀硒化，本申请可以使铜铟镓完全熔融的时间不晚于硒开始升华的时间。另外，为了保证硒蒸气能够以稳定的速率向高温合成区3输送，可以使从低温蒸发区2到高温合成区3始终具有一个正向的温度梯度。
实施例2
一种制备铜铟镓硒化合物的方法，所述方法可以包括如下步骤：
S1：提供一真空容器，真空容器包括间隔设置的高温合成区3和低温蒸发区2；
S2：将铜、铟、镓单质放置在高温合成区3，将硒单质放置在低温蒸发区2；
S3：将高温合成区3的铜、铟、镓加热至熔融状态，将低温蒸发区2的硒加热至气态；低温蒸发区2的硒开始转变为气态的时间不早于铜铟镓熔融的时间；
S4：将高温合成区3和低温蒸发区2保温，以使铜铟镓硒进行反应；
S5：将高温合成区3的温度降至不低于铜铟镓硒合金的熔融温度并进行保温，然后将高温合成区3和低温蒸发区2降温至100℃以下；
在上述步骤中，可以始终保持低温蒸发区2与高温合成区3之间存在正向温度梯度。
在步骤S1中，提供一真空容器，所述真空容器可以为L型石英管，真空容器包括高温合成区3和低温蒸发区2，将真空容器中具有一定间隔的部分分别作为高温合成区3和低温蒸发区2，所述L型石英管的两端分别为高温合成区3和低温蒸发区2，高温合成区3放置盛有铜铟硒单质的石英舟，在低温蒸发区2放置盛有硒单质的石英舟；
在步骤S2中，可以使用纯度大于99.999％的Cu、In、Ga和Se单质为原材料，各单质质量可以按照组分CuIn 0.8Ga 0.2Se 2.05去称配，将Se单质置于L型石英管短边一端的石英舟内，将Cu、In、Ga单质置于L型石英管长边一端的石英舟内，可以将石英管抽真空至10 -3Pa以下后密封L型石英管，放入电热炉中，盛有Se单质的石英舟可以对应电热炉中的对应低温蒸发区2的低温区，盛有CuInGa单质的石英舟可以对应电热炉中的对应高温合成区3的高温区。
在步骤S3中，可以通过调整高温合成区和低温合成区之间的温控功率，形成从低温到高温的线性温度梯度区间。高温合成区3可以设定88min升温至1125℃。当高温合成区3启动升温55min时，高温合成区3的温度可以升至725℃，此时可以启动对低温蒸发区2升温，可以设定低温蒸发区2在56min升温至575℃。
在步骤S4中，待低温蒸发区2达到575℃后，可以使高温合成区的温度 和低温蒸发区的温度保持6h。
在步骤S5中，可以将高温合成区设定为15min降温至960℃，再保温2h，之后关闭所有加热装置使高温合成区和低温蒸发区冷却至100℃以下，在高温合成区的石英舟内得到CIGS四元化合物，合成的CIGS化合物组分为CuIn 0.8Ga 0.2Se 2。本实施例在步骤S2中按照组分CuIn 0.8Ga 0.2Se 2.05去称配各单质的质量，得到的CIGS化合物的组分为CuIn 0.8Ga 0.2Se 2，也就是说若要得到化合物CuIn 0.8Ga 0.2Se 2，可以按照CuIn 0.8Ga 0.2Se 2.05中各元素的原子比去计算待称量的各单质的摩尔比。
为了保证硒蒸气在输运过程中不会凝结在石英管的内壁上，可以使由低温蒸发区2到高温合成区3之间具有正向的温度梯度，为了保证硒蒸气输运速率的稳定性，可以控制整个石英管的低温蒸发区2到高温合成区3之间具有线性的温度梯度。
由于本申请的铜铟镓硒合金制备方法在制备过程中能够精准地控制铜铟镓硒合金的成分，因此，在制备渐进带隙的光吸收层时，能够控制各个吸收层的铜铟镓硒的成分，也就能够控制各个吸收层的带隙宽度，从而，使印刷的方法制备渐进带隙的光吸收层能够实现。
本公开内容是本申请实施例的原则的示例，并非对本申请作出任何形式上或实质上的限定，或将本申请限定到具体的实施方案。对本领域的技术人员而言，很显然本申请实施例的技术方案的要素、方法和系统等，可以进行变动、改变、改动、演变，而不背离如上所述的本申请的实施例、技术方案的，如权利要求中所定义的原理、精神和范围。这些变动、改变、改动、演变的实施方案均包括在本申请的等同实施例内，这些等同实施例均包括在本申请的由权利要求界定的范围内。虽然可以许多不同形式来使本申请实施例具体化，但此处详细描述的是本申请的一些实施方案。此外，本申请的实施例包括此处所述的各种实施方案的一些或全部的任意可能的组合，也包括在本申请的由权利要求界定的范围内。在本申请中或在任一个引用的专利、引用的专利申请或其它引用的资料中任何地方所提及的所有专利、专利申请和其它引用资料据此通过引用以其整体并入。
以上公开内容规定为说明性的而不是穷尽性的。对于本领域技术人员来 说，本说明书会暗示许多变化和可选择方案。所有这些可选择方案和变化旨在被包括在本权利要求的范围内，其中术语“包括”意思是“包括，但不限于”。在此完成了对本申请可选择的实施方案的描述。本领域技术人员可认识到此处所述的实施方案的其它等效变换，这些等效变换也为由附于本文的权利要求所包括。

Claims (15)

  1. 一种制备多元合金化合物的装置，所述装置包括反应器(1)、低温蒸发区(2)、高温合成区(3)、封口装置(4)和加热装置(5)，其中：
    所述高温合成区(3)和所述低温蒸发区(2)分别设置在所述反应器(1)的两端；
    所述加热装置(5)间隔设置在所述反应器(1)的周围，配置为对所述反应器(1)加热，并形成温度梯度；
    所述反应器(1)具有开口，所述封口装置(4)配置为能够对所述开口进行密封。
  2. 如权利要求1所述的制备多元合金化合物的装置，其中，所述低温蒸发区(2)为石英舟、坩埚或形成在所述反应器(1)中的凹坑。
  3. 如权利要求1所述的制备多元合金化合物的装置，其中，所述高温合成区(3)为石英舟、坩埚或形成在所述反应器(1)中的凹坑。
  4. 如权利要求1所述的制备多元合金化合物的装置，其中，所述反应器(1)为L型反应管。
  5. 如权利要求4所述的制备多元合金化合物的装置，其中，所述高温合成区(3)位于所述L型反应管的长边的一端，所述低温蒸发区(2)位于所述L型反应管的短边的一端。
  6. 如权利要求5所述的制备多元合金化合物的装置，其中，所述L型反应管的长边的长度为1100mm至1600mm，短边的长度为400mm至700mm，所述L型反应管的直径为60mm至80mm。
  7. 如权利要求1至6中任一项所述的制备多元合金化合物的装置，其中，所述反应器(1)为石英管或陶瓷管。
  8. 如权利要求1至6中任一项所述的制备多元合金化合物的装置，其中，所述加热装置(5)为电加热线圈，其环绕在所述反应器(1)的外表面，并且间隔设置。
  9. 如权利要求4所述的制备多元合金化合物的装置，其中，所述L型反 应管一端封闭，另一端开放并设置有开口。
  10. 如权利要求9所述的制备多元合金化合物的装置，其中，所述开口位于所述L型反应管的长边的一端。
  11. 如权利要求1至6、9和10中任一项所述的制备多元合金化合物的装置，其中，所述开口为缩口。
  12. 如权利要求1至6、9和10中任一项所述的制备多元合金化合物的装置，其中，所述封口装置(4)为封泡。
  13. 如权利要求12所述的制备多元合金化合物的装置，其中，所述封泡的长度为150mm至250mm，直径为40mm至60mm。
  14. 如权利要求2或3所述的制备多元合金化合物的装置，其中，所述石英舟为直径为50mm至70mm、长度为200mm至400mm的半管。
  15. 如权利要求1至6、9和10中任一项所述的制备多元合金化合物的装置，其中，所述多元合金化合物为铜铟镓硒化合物。
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CN207398068U (zh) * 2017-11-06 2018-05-22 北京汉能薄膜发电技术有限公司 一种制备铜铟镓硒化合物的装置
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