CN114195518B - Zinc telluride target, preparation method and thin-film solar cell thereof - Google Patents
Zinc telluride target, preparation method and thin-film solar cell thereof Download PDFInfo
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- CN114195518B CN114195518B CN202111335493.0A CN202111335493A CN114195518B CN 114195518 B CN114195518 B CN 114195518B CN 202111335493 A CN202111335493 A CN 202111335493A CN 114195518 B CN114195518 B CN 114195518B
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- SKJCKYVIQGBWTN-UHFFFAOYSA-N (4-hydroxyphenyl) methanesulfonate Chemical compound CS(=O)(=O)OC1=CC=C(O)C=C1 SKJCKYVIQGBWTN-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000010409 thin film Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
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- 238000000034 method Methods 0.000 claims abstract description 22
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- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 41
- 239000004065 semiconductor Substances 0.000 description 10
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- 230000000052 comparative effect Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
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- 229910052714 tellurium Inorganic materials 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
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- -1 ZnTe compound Chemical class 0.000 description 2
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- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
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- 239000005642 Oleic acid Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- MZEWONGNQNXVKA-UHFFFAOYSA-N [Cu].[Cu].[Te] Chemical compound [Cu].[Cu].[Te] MZEWONGNQNXVKA-UHFFFAOYSA-N 0.000 description 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
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- 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
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Abstract
The invention discloses a zinc telluride target, a preparation method and a thin film solar cell thereof, wherein the preparation method comprises the following steps: crushing a simple substance of zinc telluride, sieving the crushed simple substance by a sieve with 600-10000 meshes and different apertures, selecting four sections of powder with different particle size ranges, and mixing the four sections of powder according to the volume ratio of (4.5-3.5): (2.5-3.5): (2.5-1.5): 1.5-0.5; mixing for 2-5h, and drying the mixed granules at 100-130 deg.C for 1-3h; cold pressing the dried powder under 200-300 MPa to prepare a blank, and keeping the pressure for 10-30 minutes to obtain a cold-pressed blank body; placing the cold-pressed blank in a sealed tank body, filling a layer of superfine zinc telluride powder on the surface and the periphery of the blank, and sealing; sintering in four stages, and cooling to obtain a zinc telluride target; the back contact layer in the thin-film solar cell is prepared from a zinc telluride target. The method overcomes the limitation of the shape of the target material, does not need to consume inert gas, saves time cost, is simple and convenient to operate, and has high purity and high density of the target material, good conductivity, higher mobility and stable overall performance of the thin-film solar cell.
Description
Technical Field
The invention belongs to the technical field of new energy, relates to a semiconductor material, and particularly relates to a zinc telluride target, a preparation method and a thin film solar cell thereof.
Background
The zinc telluride (ZnTe) film is an important semiconductor photoelectric material and has important application in the fields of photoluminescence and electroluminescent devices, solar cells, infrared detectors, thermal imaging technology and the like. Zinc telluride (ZnTe) is a compound of Zn and Te, is a wide bandgap semiconductor material having a bandgap of about 2.26eV, and plays an important role in various semiconductor devices. In general, znTe is used for photoelectric materials for detecting radiation, solar cell materials, high-brightness and high-power led light emitting materials, laser diodes, microwave generators, and the like. ZnTe crystal with high purity and large volume can be prepared by adopting a proper method. The existing preparation methods comprise the following steps: the first is to prepare ZnTe single crystal material by using a bottom seed crystal growth technology. The second method is to add a group IIIA dopant and a group VA dopant to a ZnTe compound semiconductor single crystal grown on a substrate to produce a low-resistance n-type ZnTe compound semiconductor single crystal having a high carrier concentration, and to improve the crystallinity of the crystal while achieving a desired carrier concentration with a doping amount smaller than that in the past. The third is that the ZnTe nano material can be controllably synthesized in one step in the same system by changing a Te source under mild conditions by utilizing a simple solvothermal method. And the fourth method is to realize the oriented growth of the nanocrystalline ZnTe crystal through the annealing temperature control and the substrate control after sputtering. And fifthly, mixing the single tellurium and the single zinc, placing the mixture in a vacuum environment, and preparing the zinc telluride by adopting a step heating method. And sixthly, preparing the round Ag nano sol, and controlling the optimal using amount of oleic acid and tellurium precursors to obtain the ZnTe sol with the corresponding morphology. From the prior art, the preparation and production process of the zinc telluride simple substance is relatively mature.
The zinc telluride is a direct forbidden band semiconductor material with a sphalerite structure, has a forbidden band width of 2.2-2.3eV at room temperature, and can be widely applied to optoelectronic devices, such as: green light LED, electro-optical detector, and solar cell. Along with the rapid development of thin film solar cells, the role of zinc telluride in the solar energy field is more and more emphasized, and at present, zinc telluride films are mostly formed by magnetron sputtering, wherein the conductivity of a zinc telluride target directly influences the sputtering efficiency and the uniformity of the film.
In recent years, with global warming and environmental pollution aggravation, economic development is seriously hindered by problems of shortage of energy supply, price rise and the like, and a serious challenge is brought to the search for clean renewable energy sources. As new energyOne of the best choices of sources is solar energy, which is abundant in reserves, inexhaustible in energy; the transportation is not limited, and the device is also very convenient to use in rural areas, islands, remote areas and desert areas; in the using process, no waste and public nuisance are generated, which is beneficial to protecting the ecological environment. Polycrystalline ZnTe thin films are typically p-type, with low electron affinity (3.53 eV) and high absorption coefficient (10 eV) 4 cm -1 ) Is one of important substrate materials of CdTe thin film solar cells. ZnTe can be used as a transition layer material between a CdTe thin film and an electrode by methods such as electron beam vapor deposition, magnetron sputtering and the like, and ohmic contact is increased, so that the performance of the whole solar cell is improved. Therefore, the demand of the zinc telluride target with high purity and high density in the preparation process of the zinc telluride film is great, and the market prospect is full.
The problems existing in the prior art are as follows:
the existing technology for preparing the high-performance ZnTe target material is relatively weak and is difficult to adapt to the market development requirement of the future solar cell. In the prior art, a hot-pressing sintering technology is used for sintering and forming to obtain the target material of zinc telluride doped with cuprous telluride. However, the hot press forming technique is relatively expensive, and the target product is greatly restricted by the shape and is mostly a planar target. The production cost is high, and the diversity of samples cannot be met.
Disclosure of Invention
The invention aims to solve the technical problem of providing a zinc telluride target and a preparation method thereof aiming at the defects of the prior art, the method can overcome the limitation of the target shape, does not need to consume any inert gas, saves the time cost consumption generated for reaching high vacuum degree, is simple and convenient to operate, and prepares the target with high purity and high density.
The invention further aims to provide a thin film solar cell with good conductivity, higher mobility and stable overall performance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a zinc telluride target comprises the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sieving the powder by using a plurality of screens with different apertures with the aperture of 600-10000 meshes under the condition that the particle size of the powder is less than 25 mu m to obtain a plurality of groups of powder with different particle size ranges, then selecting four sections of powder with different particle size ranges from high to low, and mixing the four sections of powder according to the volume ratio of (4.5-3.5) to (2.5-1.5) to (1.5-0.5) to obtain a mixed granule material;
s2, drying: mixing the mixed granules for 2-5h, and drying the mixed granules at 100-130 ℃ for 1-3h;
s3, cold pressing: directly carrying out cold pressing on the dried powder to prepare a blank, controlling the pressure to be more than 200-300 MPa, and keeping the pressure for 10-30 minutes to obtain a cold-pressed blank body;
s4, packaging the tank body: selecting a sealed tank body with an inner cavity of the same shape and size or basically the same size as the target material, placing the cold-pressed green body in the tank body, filling a layer of superfine zinc telluride powder on the surface and the periphery of the cold-pressed green body, and sealing the tank body;
s5, sintering: directly placing the sealed tank body into a heating furnace, and sintering for four sections; in the initial stage, the temperature is raised to 350-450 ℃ at the heating rate of 10-20 ℃/min, and the temperature is kept for 1-4 hours; the second stage sintering adopts heating speed of 10-20 ℃/min, heating to 550-650 ℃, and preserving heat for 2-6 hours; the third sintering adopts the heating speed of 5 ℃/min, the temperature is heated to 850-1050 ℃, and the temperature is kept for 4-10 hours; cooling the fourth section at the speed of 20-30 ℃/min to 500-600 ℃, and preserving the heat for 2-6 hours; and taking the tank body out of the heating furnace, air-cooling to room temperature, opening the sealing bottom cover, and taking out the sample.
Further, in the preparation method of the zinc telluride target, preferably, in the step S1, the zinc telluride simple substance powder sequentially passes through a 600 mesh, 800 mesh, 1000 mesh, 1340 mesh, 2000 mesh, 5000 mesh, 8000 mesh and 10000 mesh screen to obtain a plurality of groups of powders with different particle size ranges of 25 to 23 μm, 23 to 18 μm, 18 to 13 μm, 13 to 10 μm, 10 to 6.5 μm, 6.5 to 2.6 μm, 2.6 μm to 1.6 μm and less than 1.6 μm.
Further, in the preparation method of the zinc telluride target, preferably, in the step S1, four segments of powder of 23-18 μm, 10-6.5 μm, 2.6-1.6 μm and less than 1.6 μm are selected from the plurality of groups of powder with different particle sizes.
Further, in the preparation method of the zinc telluride target, preferably, in the step S4, the particle size of the ultrafine zinc telluride powder is less than 1.6 μm.
Further, in the preparation method of the zinc telluride target, preferably, in the step S4, the volume of the superfine zinc telluride powder is 0.1-0.5% of the volume of the cold-pressed green body.
Further, in the preparation method of the zinc telluride target, preferably, in the step S4, the height of the inner cavity after the tank body is packaged is 101-110% of the height of the target size.
Further, in the preparation method of the zinc telluride target, preferably, in the step S4, the sealing requirement is as follows: and the sealing is complete, and no gas leaks.
A zinc telluride target is prepared by the preparation method.
A back contact layer in the thin-film solar cell is prepared from the zinc telluride target.
According to the invention, zinc telluride powder with different particle size ranges is selected to be fully mixed, the powder with large particle size forms a target material framework in different particle sizes, and other medium particle sizes and small particle sizes are respectively filled in gaps among the large particle sizes, so that the target material density and uniformity are very good, and the specific shape of the tank body is not limited; the size of the inner cavity of the tank body is controlled to limit the air volume of the inner cavity of the tank body, so that the oxidation of a blank body and the increase of the impurity content of other gases in the high-temperature process are avoided; the superfine zinc telluride powder layer mainly provides protection for the cold-pressed blank, and because the particle size is small and the structure is sparse, the superfine zinc telluride powder layer can react with residual air in the tank body in preference to the high-temperature sintering process, so that the quality of the cold-pressed blank after sintering is improved.
In the step sintering, heat preservation treatment is carried out at 350-450 ℃ in order to remove grease-like organic matters; carrying out homogenization diffusion treatment at 550-650 ℃ to realize the filling of the gaps after the grease organic matter is removed by atomic molecules; sintering at 850-1050 deg.C, and lowering temperature to make large particles become nucleation particles, small particles easily melt in the temperature raising process, and aggregate at large particles, and keeping the temperature to stabilize the final crystal particles; the gaps of the particles after melting and gathering can be diffused and supplemented by cooling to 500-600 ℃ and preserving the temperature, the stability and toughness of the grain structure after sintering can be ensured, and the target material can not crack due to rapid cooling.
The back contact layer of the thin-film solar cell made of the zinc telluride target material enables the cell to have the characteristic of weak light power generation and then can be combined with curtain wall glass. The cadmium telluride thin film photovoltaic solar technology has industry-leading product performance and can also provide a persistent low-cost thin film cell structure.
Drawings
The invention will be further described with reference to the following drawings and examples, in which:
fig. 1 is an electron micrograph of the zinc telluride target prepared in example 1 of the present invention.
FIG. 2 is an electron micrograph of a zinc telluride target prepared in comparative example 1 of the present invention.
Fig. 3 is an electron micrograph of the zinc telluride target prepared in comparative example 2 of the present invention.
Detailed Description
For a more clear understanding of the technical features, objects, and effects of the present invention, embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
A preparation method of a zinc telluride target comprises the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sequentially passing through screens of 600 meshes, 800 meshes, 1000 meshes, 1340 meshes, 2000 meshes, 5000 meshes, 8000 meshes and 10000 meshes to obtain a plurality of groups of powders with the particle sizes of 25-23 mu m, 23-18 mu m, 18-13 mu m, 13-10 mu m, 10-6.5 mu m, 6.5-2.6 mu m, 2.6 mu m-1.6 mu m and less than 1.6 mu m respectively under the condition that the particle size of the powders is less than 25 mu m, and then selecting four sections of powders with different particle sizes from high to low to mix according to the volume ratio of (4.5-3.5) to (2.5-1.5) to (1.5-0.5) to obtain a mixed granule; in the step S1, four powder segments of 23-18 μm, 10-6.5 μm, 2.6-1.6 μm and less than 1.6 μm are preferably selected from the powder with different particle sizes to be mixed.
S2, drying: mixing the mixed granules for 2-5h, and drying the mixed granules at 100-130 ℃ for 1-3h;
s3, cold pressing: directly carrying out cold pressing on the dried powder to prepare a blank, controlling the pressure to be more than 200-300 MPa, and keeping the pressure for 10-30 minutes to obtain a cold-pressed blank body;
s4, packaging the tank body: selecting a sealed tank body with an inner cavity of the same shape and size as or basically the same size as the target material, placing the cold-pressed blank body in the tank body, filling a layer of superfine zinc telluride powder on the surface and the periphery of the cold-pressed blank body, and sealing the tank body; the size of the inner cavity of the sealed and packaged tank body is kept within 101-110% of the size of the target material, wherein the positive deviation means that the size of the inner cavity of the tank body is larger than the size of the target material, and the size means the longitudinal height, the transverse width and the transverse length. The sealing requirements are as follows: and the sealing is complete, and no gas leaks. The volume of the superfine zinc telluride powder is 0.1-0.5% of the volume of the cold-pressed blank. The grain size of the superfine zinc telluride powder is less than 1.6 mu m.
S5, sintering: directly placing the sealed tank body into a heating furnace, and sintering for four sections; in the initial stage, the temperature is raised to 350-450 ℃ at the heating rate of 10-20 ℃/min, and the temperature is kept for 1-4 hours; the second stage sintering adopts heating speed of 10-20 ℃/min, heating to 550-650 ℃, and preserving heat for 2-6 hours; the third sintering adopts the heating speed of 5 ℃/min, the temperature is heated to 850-1050 ℃, and the temperature is kept for 4-10 hours; cooling at 20-30 deg.c/min to 500-600 deg.c in the fourth stage and maintaining for 2-6 hr; and taking the tank body out of the heating furnace, air-cooling to room temperature, opening the closed bottom cover, and taking out the sample.
The following is detailed by specific examples:
embodiment 1, a method for preparing a zinc telluride target includes the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sieving the crushed zinc telluride simple substance by using a plurality of screens (specifically 600 meshes, 800 meshes, 1000 meshes, 1340 meshes, 2000 meshes, 5000 meshes, 8000 meshes and 10000 meshes) with different apertures between 600 meshes and 10000 meshes under the condition that the particle size of the powder is less than 25 mu m to obtain a plurality of groups of powder with different particle size ranges, and mixing the powders with four particle size ranges of 23-18 mu m, 10-6.5 mu m, 2.6-1.6 mu m and less than 1.6 mu m according to a volume ratio of 4.
S2, drying: mixing the mixed granules for 3 hours again in a three-dimensional moving mixer, and then carrying out heat preservation and drying on the mixed granules for 3 hours at 130 ℃;
s3, cold pressing: and directly carrying out cold pressing on the dried powder to prepare a blank, and keeping the pressure for 10 minutes under the pressure of 250MPa to obtain a cold-pressed blank body.
S4, packaging the tank body: and (3) packaging the cold-pressed blank by using a tank, paving zinc telluride powder with the grain size of less than 1.6 mu m on the surface of the blank, wherein the volume of the cold-pressed blank is 0.2 percent of the volume of the cold-pressed blank, the height of an inner cavity after the tank is packaged is 105 percent of the height of the target size, namely the height of a tank cavity is 105 percent of the height of the blank, and welding and sealing the tank.
S5, sintering: directly placing the sealed tank body into a heating furnace, heating to 400 ℃ at a heating rate of 15 ℃/min, and preserving heat for 2 hours; heating to 600 ℃ at a heating speed of 15 ℃/min, and preserving heat for 4 hours; heating to 960 deg.C/min at 5 deg.C/min, and maintaining for 6 hr; cooling to 550 ℃ at the speed of 20 ℃/min, and preserving heat for 3 hours; and taking the tank body out of the heating furnace, air-cooling to room temperature, opening the sealed bottom cover, and taking out the sample, wherein the density of the sample is measured to be 92%. As shown in fig. 1, it can be seen visually that: the size of crystal grains on the surface of the target material is uniform, and no obvious holes or gaps exist, which shows that the process can obtain good sintering effect.
Densification, also called packing ratio or space maximum utilization, refers to the volume percentage of atoms in a unit cell, i.e., the ratio of the volume of atoms contained in a unit cell to the volume of the unit cell. The hardness of the density reaction material is high, and the density of the zinc telluride target material prepared by the method is high and reaches 92%; the material has high hardness and high bending strength.
Embodiment 2, a method for preparing a zinc telluride target includes the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sieving the powder by using a plurality of screens (same as the embodiment 1) with different apertures with the apertures of 600-10000 meshes under the condition that the particle size of the powder is less than 25 microns to obtain a plurality of groups of powder with different particle size ranges, and selecting four types of particles with the sizes of 25-23 microns, 13-10 microns, 2.6 microns-1.6 microns and less than 1.6 microns according to a volume ratio of 4.5.
S2, drying: mixing the mixed granules in a three-dimensional moving mixer for 2 hours again, and then carrying out heat preservation and drying on the mixed granules at 100 ℃ for 1 hour;
s3, cold pressing: and directly carrying out cold pressing on the dried powder to prepare a blank, and maintaining the pressure for 30 minutes under the pressure of 300MPa to obtain a cold-pressed blank body.
S4, packaging the tank body: and (3) packaging the cold-pressed blank by using a tank body, paving zinc telluride powder which accounts for less than 1.6 mu m and accounts for 0.1 percent of the volume of the cold-pressed blank on the surface of the blank, welding and sealing the tank body, wherein the height of a cavity of the tank body is 108 percent of the height of the blank.
S5, sintering: directly placing the sealed tank body into a heating furnace, heating to 350 ℃ at a heating rate of 20 ℃/min, and preserving heat for 4 hours; heating to 650 ℃ at the heating speed of 10 ℃/min, and preserving heat for 2 hours; heating to 850 ℃/min at the temperature of 5 ℃/min, and preserving heat for 8 hours; cooling to 600 ℃ at the speed of 30 ℃/min, and preserving heat for 4 hours; and then taking the tank body out of the heating furnace, air-cooling to room temperature, opening the sealing bottom cover, and taking out the sample to obtain the zinc telluride target. The density of the measured sample was 91%.
Embodiment 3, a method for preparing a zinc telluride target includes the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sieving the powder by using a plurality of screens (same as the embodiment 1) with different apertures with the apertures of 600-10000 meshes under the condition that the particle size of the powder is less than 25 mu m to obtain a plurality of groups of powder with different particle size ranges, and selecting four types of particles with the sizes of 18-13 mu m, 6.5-2.6 mu m, 2.6 mu m-1.6 mu m and less than 1.6 mu m according to a volume ratio of 3.5.
S2, drying: mixing the mixed granules in a three-dimensional moving mixer for 5 hours again, and then drying the mixed granules at 120 ℃ for 1.5 hours;
s3, cold pressing: and directly carrying out cold pressing on the dried powder to prepare a blank, and maintaining the pressure for 15 minutes under the pressure of 200MPa to obtain a cold-pressed blank body.
S4, packaging the tank body: a tank body is used for packaging the cold-pressed blank, zinc telluride powder which accounts for less than 1.6 mu m and accounts for 0.3 percent of the volume of the cold-pressed blank is paved on the surface of the blank, the height of the cavity is 103 percent of the height of the blank, and the tank body is welded and sealed.
S5, sintering: directly placing the sealed tank body into a heating furnace, heating to 450 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1 hour; heating to 550 ℃ at a heating speed of 20 ℃/min, and preserving heat for 6 hours; heating to 1050 ℃/min at the temperature of 5 ℃/min, and preserving the heat for 4 hours; cooling to 500 deg.C at 30 deg.C/min, and maintaining for 6 hr; and then taking the tank body out of the heating furnace, air-cooling to room temperature, opening the sealing bottom cover, and taking out the sample to obtain the zinc telluride target. The density of the measured sample was 90.5%.
Embodiment 4, a method for preparing a zinc telluride target, comprising the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sieving the powder by using a plurality of screens (same as the embodiment 1) with different apertures with the apertures of 600-10000 meshes under the condition that the particle size of the powder is less than 25 microns to obtain a plurality of groups of powder with different particle size ranges, and selecting four types of particles with the sizes of 25-23 microns, 13-6.5 microns, 6.5-2.6 microns and less than 1.6 microns according to a volume ratio of 4.
S2, drying: the mixed granules are mixed for 5 hours again in a three-dimensional moving mixer, and then the mixed granules are subjected to heat preservation and drying for 2 hours at the temperature of 110 ℃;
s3, cold pressing: and directly carrying out cold pressing on the dried powder to prepare a blank, and keeping the pressure for 25 minutes under the pressure of 270MPa to obtain a cold-pressed blank.
S4, packaging the tank body: and (3) packaging the cold-pressed blank by using a tank body, paving zinc telluride powder which accounts for less than 1.6 mu m and accounts for 0.5 percent of the volume of the cold-pressed blank on the surface of the blank, welding and sealing the tank body, wherein the size height of a cavity is 110 percent of the height of the blank.
S5, sintering: directly placing the sealed tank body into a heating furnace, heating to 420 ℃ at a heating rate of 17 ℃/min, and preserving heat for 1 hour; heating to 620 ℃ at the heating speed of 17 ℃/min, and preserving heat for 3 hours; heating to 920 ℃/min at the temperature of 5 ℃/min, and preserving the heat for 6 hours; cooling to 530 ℃ at a speed of 25 ℃/min, and preserving heat for 3 hours; and then taking the tank body out of the heating furnace, air-cooling to room temperature, opening the sealing bottom cover, and taking out the sample to obtain the zinc telluride target. The density of the measured sample was 90.5%.
In comparative example 1, elemental zinc telluride powder is selected, 25 to 23 μm granules are selected and mixed again for 3 hours in a three-dimensional moving mixer, and then the granules are subjected to heat preservation and drying for 3 hours at 130 ℃, and the pressure is maintained for 10 minutes under the pressure of 250MPa, so as to obtain a cold-pressed green body. A cold-pressed blank is packaged by a tank body, zinc telluride powder which accounts for less than 1.6 mu m and accounts for 0.2 percent of the volume of the cold-pressed blank is paved on the surface of the blank, and the height of a cavity is 120 percent of the height of the blank. Directly placing the sealed tank body into a heating furnace, heating to 400 ℃ at a heating rate of 15 ℃/min, and preserving heat for 2 hours; heating to 600 ℃ at a heating speed of 15 ℃/min, and preserving heat for 4 hours; heating to 960 deg.C/min at 5 deg.C/min, and maintaining for 6 hr; cooling to 550 ℃ at the speed of 20 ℃/min, and preserving heat for 3 hours; and taking the tank body out of the heating furnace, air-cooling to room temperature, opening the closed bottom cover, and taking out the sample, wherein the density of the sample is measured to be 78%. As shown in FIG. 2, after sintering with a single size, there are abnormal growth of grains in local areas, very uneven structure, and a large number of gaps in the growth process of the grains.
In comparative example 2, a zinc telluride simple substance is selected, four kinds of particles with sizes of 23-18 μm, 10-6.5 μm, 2.6 μm-1.6 μm and less than 1.6 μm are selected, and mixed powder with gradient sizes is obtained according to a volume ratio of 4. And mixing for 3 hours again in a three-dimensional moving mixer, then carrying out heat preservation and drying on the granular materials for 3 hours at the temperature of 130 ℃, and maintaining the pressure for 10 minutes under the pressure of 250MPa to obtain a cold-pressed green body. And (3) packaging the cold-pressed green body by using a can body, wherein the height of the cavity is 120% of the height of the green body. Directly placing the sealed tank body into a heating furnace, heating to 400 ℃ at a heating rate of 15 ℃/min, and preserving heat for 2 hours; heating to 600 ℃ at a heating speed of 15 ℃/min, and preserving heat for 4 hours; heating to 960 deg.C/min at 5 deg.C/min, and maintaining for 6 hr; cooling to 550 ℃ at the speed of 20 ℃/min, and preserving heat for 3 hours; and taking the tank body out of the heating furnace, air-cooling to room temperature, opening the closed bottom cover, and taking out the sample, wherein the density of the sample is measured to be 76%. As shown in fig. 3, many white stains appeared on the surface, and there were large gaps between the grains in the bonding.
In the two comparative examples, the zinc telluride powder with a single size is adopted in comparative example 1 compared with example 1, and the superfine zinc telluride powder is not adopted to be paved on the outer surface of the cold-pressed green body during sintering in comparative example 2 compared with example 1. Through the above comparative experiments, it can be seen that: only zinc telluride powder with a single size and superfine zinc telluride powder which is not adopted during sintering are paved on the outer surface of the cold-pressed green body, so that the density of the obtained target is below 80 percent, while the density of the target obtained by the embodiment of the invention is above 90 percent. The tests prove that the preparation method can effectively improve the density, and the steps complement each other, have synergistic interaction and achieve good effects.
Example 5, a thin film solar cell, one of the thin films in the thin film solar cell was prepared from the zinc telluride target of examples 1-4.
The thin film battery is a solar battery prepared by a layer of thin film, the silicon consumption is very low, the cost is easier to reduce, and meanwhile, the thin film battery is a high-efficiency energy product, is a novel building material and is easier to perfectly combine with a building. With the background of the continuous tension of silicon raw materials in the international market, thin film solar cells have become a new trend and a new hot spot for the development of the international photovoltaic market. There are mainly 3 types of thin film batteries that have been industrially mass-produced: silicon-based thin film solar cells, copper indium gallium selenide thin film solar Cells (CIGS), cadmium telluride thin film solar cells (CdTe).
The solar thin film cell includes: the solar cell comprises a substrate, a TCO layer, a CdS window layer, a CdTe absorption layer, a back contact layer and a back electrode.
The zinc telluride (ZnTe) is arranged between the cadmium telluride (CdTe) and the back electrode to form a back contact layer, the cadmium telluride (CdTe) directly contacts the metal electrode due to the characteristics of the cadmium telluride (CdTe), the contact resistance is large, the zinc telluride (ZnTe) is used as the transition layer, on one hand, the zinc telluride (CdTe) can be well compatible with the CdTe layer, on the other hand, the zinc telluride (CdTe) can form better ohmic contact with the metal electrode, the CdTe layer is equivalent to the transition layer or the buffer layer, the CdTe has a self-compensation effect, a shallow homojunction with heavy doping and high conductivity is difficult to realize, and stable ohmic contact is difficult to obtain, so a window layer is required to be used for transition, and meanwhile, the ZnTe has a similar structure with the CdTe, the difference of lattice constants is small, and can be well contacted with metal electrolysis, and the zinc telluride is a good window layer material.
The cadmium telluride thin film solar cell is a photovoltaic device formed by sequentially depositing a plurality of thin film structures on a glass substrate or other flexible substrates.
The general standard cadmium telluride thin film solar cell mainly comprises a five-layer structure, which is as follows:
glass substrate: the solar cell bracket mainly plays a role in supporting the cell, preventing pollution and emitting sunlight.
TCO layer: i.e. a transparent conductive oxide layer. The main functions are light transmission and electric conduction.
CdS window layer: the n-type semiconductor and the p-type CdTe form a p-n junction.
A CdTe absorption layer: it is the main light absorbing layer of the cell, and the p-n junction formed with the n-type CdS window layer is the most core part of the whole cell.
Back contact layer and back electrode: in order to reduce the contact potential barrier of the CdTe and the metal electrode, the current is led out, so that the metal electrode and the CdTe form ohmic contact, wherein the zinc telluride target is mainly applied to the back contact layer.
Cadmium telluride thin film solar cells are one of the more rapidly developing photovoltaic devices in thin film solar cells. The cadmium telluride solar cell has the characteristic of weak light power generation and can be combined with curtain wall glass. Cadmium telluride thin film solar modules have been completely classified as high performance products. The cadmium telluride thin film photovoltaic solar technology has the leading product performance in the industry and can also provide a continuous low-cost thin film cell structure.
Example 6, a thin film solar cell, specifically a cadmium telluride thin film solar cell, in which one of the thin films was prepared from the zinc telluride target of examples 1-4.
CdTe is a II-VI compound semiconductor, a direct bandgap semiconductor. Absorption coefficient up to 104cm -1 The thickness of the battery can be 2-3 microns, and the expensive material cost is reduced. The band gap width is 1.5eV, the spectral response of CdTe is very matched with the solar spectrum, and the theoretical photoelectric conversion efficiency of the cadmium telluride thin film solar cell is about 28 percent. The bonding energy of the Cd-Te chemical bond is 5.7eV, and the design service life of a common cadmium telluride thin-film solar cell is 20 years. The elemental Cd and Te can only exist solid CdTe when meeting, and the cadmium telluride thin-film solar cell product has high uniformity and yield and is very suitable for large-scale production. In addition, the cadmium telluride thin film solar cell has good low light characteristics and shows excellent performance in regions which are not illuminated well.
The preparation method comprises the following steps: transparent oxide layer (TCO), cdS and CdTe film are grown on the glass substrate in sequence, and sunlight is irradiated from the upper part of the glass substrate, firstly penetrates through the TCO layer and then enters the CdS/CdTe junction. In a cadmium telluride solar cell, the zinc telluride target is applied to a back contact layer and a back electrode: in order to reduce the contact potential barrier of the CdTe and the metal electrode, the current is led out, and the metal electrode and the CdTe form ohmic contact, wherein the zinc telluride target material is preferably mainly applied to the back contact layer.
Claims (6)
1. The preparation method of the zinc telluride target is characterized by comprising the following steps:
s1, preparing a zinc telluride simple substance mixed particle material: selecting a zinc telluride simple substance, crushing the zinc telluride simple substance, sieving the powder by using a plurality of screens with different apertures with the apertures of 600-10000 meshes under the condition that the particle size of the powder is less than 25 mu m to obtain a plurality of groups of powder with different particle size ranges, and then selecting four sections of powder with different particle size ranges from high to low to mix according to the volume ratio of (4.5-3.5) to (2.5-3.5) to (1.5-1.5) to obtain a mixed granule;
s2, drying: mixing the mixed granules for 2-5h, and drying the mixed granules at 100-130 ℃ for 1-3h;
s3, cold pressing: directly carrying out cold pressing on the dried powder to prepare a blank, controlling the pressure to be 200-300MPa, and keeping the pressure for 10-30 minutes to obtain a cold-pressed blank;
s4, packaging the tank body: selecting a sealed tank body with an inner cavity basically the same as the target in shape and size, placing the cold-pressed blank in the tank body, filling a layer of superfine zinc telluride powder on the surface and the periphery of the cold-pressed blank, and sealing the tank body, wherein the grain size of the superfine zinc telluride powder is less than 1.6 mu m, the volume of the superfine zinc telluride powder is 0.1-0.5% of the volume of the cold-pressed blank, and the height of the inner cavity after the tank body is packaged is 101-110% of the height of the target size;
s5, sintering: directly placing the sealed tank body into a heating furnace, and sintering for four sections; in the initial stage, heating to 350-450 deg.C at a heating rate of 10-20 deg.C/min, and maintaining for 1-4 hr; the second stage sintering adopts heating speed of 10-20 ℃/min, heating to 550-650 ℃, and preserving heat for 2-6 hours; the third sintering is carried out at the heating speed of 5 ℃/min, the temperature is heated to 850-1050 ℃, and the heat preservation is carried out for 4-10 hours; cooling the fourth section at the speed of 20-30 ℃/min to 500-600 ℃, and preserving heat for 2-6 hours; and taking the tank body out of the heating furnace, air-cooling to room temperature, opening the closed bottom cover, and taking out the sample.
2. The method for preparing the zinc telluride target as claimed in claim 1, wherein in step S1, the zinc telluride simple substance powder sequentially passes through a screen mesh of 600 mesh, 800 mesh, 1000 mesh, 1340 mesh, 2000 mesh, 5000 mesh, 8000 mesh and 10000 mesh to obtain a plurality of groups of powders with different particle size ranges of 25 to 23 μm, 23 to 18 μm, 18 to 13 μm, 13 to 10 μm, 10 to 6.5 μm, 6.5 to 2.6 μm, 2.6 to 1.6 μm and less than 1.6 μm.
3. The method for preparing the zinc telluride target as in claim 2, wherein in the step S1, four powder segments of 23-18 μm, 10-6.5 μm, 2.6-1.6 μm and less than 1.6 μm are selected from the plurality of groups of powder with different particle sizes.
4. The method for preparing the zinc telluride target as set forth in claim 1, wherein in the step S4, the sealing requirement is as follows: and the sealing is complete, and no gas leaks.
5. A zinc telluride target material prepared by the preparation method of any one of claims 1 to 4.
6. A thin-film solar cell, characterized in that the back contact layer in the thin-film solar cell is prepared from the zinc telluride target material as defined in claim 5.
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| JP2003082454A (en) * | 2001-09-12 | 2003-03-19 | Nikko Materials Co Ltd | Method for manufacturing sputtering target |
| CN102634756B (en) * | 2012-04-19 | 2013-08-28 | 成都中光电阿波罗太阳能有限公司 | Preparation method of cadmium telluride target |
| CN107805788B (en) * | 2017-11-08 | 2019-10-29 | 先导薄膜材料（广东）有限公司 | The preparation method of zinc telluridse target |
| CN109704766A (en) * | 2019-01-21 | 2019-05-03 | 江西科泰新材料有限公司 | Zinc telluridse mixes the production technology of cuprous telluride target |
| CN112479707A (en) * | 2020-11-13 | 2021-03-12 | 北京航大微纳科技有限公司 | Cold isostatic pressing preparation method of tungsten oxide-based ceramic target material |
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