CN114620996A - High-efficiency rotary ceramic target for solar cell - Google Patents

High-efficiency rotary ceramic target for solar cell Download PDF

Info

Publication number
CN114620996A
CN114620996A CN202210165564.5A CN202210165564A CN114620996A CN 114620996 A CN114620996 A CN 114620996A CN 202210165564 A CN202210165564 A CN 202210165564A CN 114620996 A CN114620996 A CN 114620996A
Authority
CN
China
Prior art keywords
temperature
oxide
target material
ceramic target
sintering
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210165564.5A
Other languages
Chinese (zh)
Inventor
马超宁
许积文
黄誓成
孟红波
姚远
侯远欣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Luoyang Jinglian Photoelectric Material Co ltd
Guilin University of Electronic Technology
Original Assignee
Luoyang Jinglian Photoelectric Material Co ltd
Guilin University of Electronic Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Luoyang Jinglian Photoelectric Material Co ltd, Guilin University of Electronic Technology filed Critical Luoyang Jinglian Photoelectric Material Co ltd
Priority to CN202210165564.5A priority Critical patent/CN114620996A/en
Publication of CN114620996A publication Critical patent/CN114620996A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/245—Oxides by deposition from the vapour phase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • 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
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3258—Tungsten oxides, tungstates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6565—Cooling rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
    • C04B2235/6585—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage above that of air
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Composite Materials (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a rotary ceramic target for a high-efficiency solar cell, which comprises the components of 97-98wt% of indium oxide, 0.5-2wt% of tin oxide and 1-2.5wt% of doped oxide; the doped oxide is 3-5 of titanium oxide, tungsten oxide, molybdenum oxide, zirconium oxide, cerium oxide and silicon oxide. The invention adopts multi-element doping and a specific sintering temperature system, can effectively realize higher target material density and solve the problem of generating tumor on the surface of the target material in the continuous sputtering process. The invention can effectively improve the light transmittance of the film in the infrared band, thereby improving the photoelectric conversion capability of the solar cell in the infrared band.

Description

High-efficiency rotary ceramic target for solar cell
Technical Field
The invention belongs to the technical field of vacuum coating targets, and particularly relates to a rotary ceramic target for a high-efficiency solar cell.
Background
In the field of photovoltaic of solar cells, in order to improve the photoelectric conversion efficiency of the solar cells, solar energy in an infrared band needs to be utilized, and a Transparent Conductive Oxide (TCO) film with high light transmittance in the infrared band is needed. Increasing the transmittance of the TCO film in the infrared band requires decreasing the electron concentration of the film, but in order to ensure excellent conductivity, the resistivity (sheet resistance) needs to be decreased by increasing the electron mobility of the film.
The traditional ITO target material is SnO2High content, high carrier concentration, resulting in low electron mobility. Reduction of SnO2In the case of the content, when the content is in the range of 1% to 5%, the carrier concentration is slightly lowered and the electron mobility is slightly improved. However, the mobility is still not sufficiently high, resulting in a slight decrease in the conductivity of the thin film. More importantly, the target material with ultrahigh density is difficult to be fired, so that the target material is easy to generate surface nodules in the continuous use process, and the quality and the continuous production of the film are further influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-efficiency rotary ceramic target material for a solar cell, which is prepared by using a unique target material composition and a sintering process, so that the ceramic target material with high electron mobility, high infrared light transmittance and ultrahigh density is obtained, the conversion efficiency of the solar cell can be improved, and the rotary ceramic target material is suitable for mass production.
The ceramic target material provided by the invention mainly contains In2O3The minor component is SnO2And contains 3-5 kinds of doped oxides of titanium oxide, tungsten oxide, molybdenum oxide, zirconium oxide, cerium oxide and silicon oxide. In2O397-98wt% of SnO2The content is 0.5-2.0wt%, and the content of doped oxide is 1.0-2.5 wt%.
The preparation method of the ceramic target material provided by the invention comprises the following steps:
(1) and weighing indium oxide powder, tin oxide powder and doped oxide powder according to the proportion.
(2) Adding deionized water and a dispersing agent, and performing coarse grinding and fine grinding to obtain slurry with uniform mixing and good dispersibility.
(3) The slurry after grinding was added with a polyvinyl alcohol binder and spray-granulated using a spray dryer.
(4) And (4) putting the granulated powder into a rubber sleeve die, and pressing by using a cold isostatic press to obtain the target biscuit.
(5) Sintering the biscuit by adopting a specific heating process to obtain the high-density rotary ceramic target material.
The temperature schedule of the sintering process is characterized in that no heat preservation process is carried out from room temperature to the stage of heating to the maximum temperature of 1550 ℃, 7 heating stages are arranged, and the temperature interval and the heating speed are respectively as follows: room temperature is between 120 ℃ and 120 ℃ (1 ℃/min), between 120 ℃ and 400 ℃ (0.8 ℃/min), between 400 ℃ and 750 ℃ (0.5 ℃/min), between 750 ℃ and 1000 ℃ (1 ℃/min), between 1000 ℃ and 1150 ℃ (0.5 ℃/min), between 1150 ℃ and 1300 (2 ℃/min), between 1300 ℃ and 1550 ℃ (0.2 ℃/min). And after the temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at the speed of 10 ℃/min and preserving heat for 5-10h, and then cooling to 1490 ℃ at the same speed and preserving heat for 15-25h so as to adjust the microstructure in the target. Then, the temperature is reduced, the temperature reduction speed is 0.6 ℃/min within the range of 1490-1000 ℃, and then the heat source is closed for natural temperature reduction.
The ceramic target material is usually sintered under pure oxygen atmosphere, and the sintering process of the invention has another characteristic that the sintering process does not require complete pure oxygen atmosphere: and during sintering, heating to 300 ℃, introducing purified air, continuously heating to 1000 ℃, switching to pure oxygen, and stopping introducing oxygen until the temperature is reduced to 1300 ℃.
The invention has the technical characteristics and beneficial effects that:
1. the invention can effectively improve the light transmittance of the film in the infrared band, further improve the photoelectric conversion capability of the solar cell in the infrared band, is beneficial to reducing the electron concentration and improving the mobility, and keeps better conductivity while improving the infrared light transmittance.
2. The invention can effectively improve the problems of mass production of the target material which is difficult to give consideration to the doping design of a single element, such as density, component uniformity, resistivity and the like.
3. The invention adopts multi-element doping and a specific sintering temperature system, can effectively realize higher target material density and solve the problem of generating tumor on the surface of the target material in the continuous sputtering process.
Drawings
FIG. 1 is a schematic diagram of a rubber sleeve mold used for pressing a target biscuit according to an embodiment of the invention;
FIG. 2 is a photograph of the target obtained in example 1 of the present invention.
Detailed Description
Specific examples are given below to illustrate the technical solutions and advantages of the present invention in detail.
Example 1:
(1) respectively weighing 9.7kg of indium oxide powder, 0.2kg of tin oxide powder, 0.03kg of tungsten oxide powder, 0.05kg of cerium oxide powder and 0.02kg of zirconium oxide powder, uniformly mixing with ultrapure water according to the solid content of 55%, and adding 0.3% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated.
(2) And adding the polyvinyl alcohol mixed solution into the third mixed slurry, wherein the addition amount is 2.5 percent calculated by pure polyvinyl alcohol substances, the defoaming agent is 0.06 percent calculated by the mass of the solution, and then sieving the slurry by a 200-mesh sieve for defoaming and impurity removal treatment.
(3) Granulating with spray dryer, setting inlet and outlet temperature parameters of 200 deg.C and 100 deg.C, rotating speed of 11000rpm, feeding frequency of 15, sieving with 80 mesh sieve to remove coarse particles, and its apparent density is 1.57g/cm3。
(4) When the planar target material is formed, the granulated powder is placed in a steel die with the size of 300mm and is subjected to 50MPa dry pressing preforming, and a preformed biscuit is subjected to waterproof packaging by vacuumizing through a rubber bag; when the target material is rotated to be molded, the granulation powder is placed in a mold with a stainless steel mold core and a rubber outer sleeve, and two ends of the granulation powder are sealed by rubber plugs and mechanically fixed; and simultaneously carrying out cold isostatic pressing at 240MPa and maintaining the pressure for 12min to obtain a high-density biscuit.
(5) The plane and the rotary biscuit are put into a sintering furnace for sintering, and the temperature interval and the temperature rise speed are as follows: room temperature is between 120 ℃ and 120 ℃ (1 ℃/min), between 120 ℃ and 400 ℃ (0.8 ℃/min), between 400 ℃ and 750 ℃ (0.5 ℃/min), between 750 ℃ and 1000 ℃ (1 ℃/min), between 1000 ℃ and 1150 ℃ (0.5 ℃/min), between 1150 ℃ and 1300 (2 ℃/min), between 1300 ℃ and 1550 ℃ (0.2 ℃/min). And after the temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at a cooling rate of 10 ℃/min and preserving heat for 5 hours, and then cooling to 1490 ℃ and preserving heat for 15 hours so as to adjust the microstructure in the target. Then, the temperature is continuously reduced, the temperature reduction rate is 0.6 ℃/min within the range of 1490-.
Sintering atmosphere: air is introduced when the temperature is raised to 300 ℃, pure oxygen is introduced when the temperature is raised to 1000 ℃, and the introduction of oxygen is stopped when the temperature is lowered to 1300 ℃ after sintering is finished.
The target material was subjected to density test, and the film prepared by magnetron sputtering was subjected to electron mobility test, and the test results are shown in table 1. The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 98.9 percent by the Archimedes drainage method.
Machining and binding the obtained planar target material to prepare a sputtering target material with the diameter of 6 inches in a straight lineCoating in a magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (no water vapor or hydrogen is introduced), and the electron mobility of the film prepared under the optimized process conditions is 40.56cm2/V·s。
Example 2:
(1) respectively weighing 9.7kg of indium oxide powder, 0.05kg of tin oxide powder, 0.05kg of tungsten oxide powder, 0.05kg of cerium oxide powder and 0.15kg of zirconium oxide powder, uniformly mixing with ultrapure water according to the solid content of 65%, and adding 0.8% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated.
(2) And adding the polyvinyl alcohol mixed solution into the third mixed slurry, wherein the addition amount is 0.5 percent calculated by pure polyvinyl alcohol substances, the defoaming agent is 0.03 percent calculated by the mass of the solution, and then sieving the slurry by a 200-mesh sieve for defoaming and impurity removal treatment.
(3) Granulating with spray dryer, setting inlet and outlet temperature parameters of 200 deg.C and 100 deg.C, rotating speed of 11000rpm, feeding frequency of 15, sieving with 80 mesh sieve to remove coarse particles, and its apparent density is 1.61g/cm3。
(4) When the planar target material is formed, the granulated powder is placed in a steel die with the size of 300mm and is subjected to 50MPa dry pressing preforming, and a preformed biscuit is subjected to waterproof packaging by vacuumizing through a rubber bag; when the target material is rotated to be molded, the granulation powder is placed in a mold with a stainless steel mold core and a rubber outer sleeve, and two ends of the granulation powder are sealed by rubber plugs and mechanically fixed; and simultaneously carrying out cold isostatic pressing at 300MPa and maintaining the pressure for 12min to obtain a high-density biscuit.
(5) The plane and the rotary biscuit are put into a sintering furnace for sintering, and the temperature interval and the temperature rise speed are as follows: room temperature to 120 deg.C (1 deg.C/min), 120 deg.C to 400 deg.C (0.8 deg.C/min), 400 deg.C to 750 deg.C (0.5 deg.C/min), 750 deg.C to 1000 deg.C (1 deg.C/min), 1000 deg.C to 1150 deg.C (0.5 deg.C/min), 1150 deg.C to 1300 deg.C (2 deg.C/min), 1300 deg.C to 1550 deg.C (0.2 deg.C/min). And after the temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at a cooling rate of 10 ℃/min and preserving heat for 5h, and then cooling to 1490 ℃ and preserving heat for 15h so as to adjust the microstructure in the target. Then, the temperature is continuously reduced, the temperature reduction rate in the range of 1490-1000 ℃ is 0.6 ℃/min, and then the power is cut off for natural temperature reduction.
Sintering atmosphere: air is introduced when the temperature is raised to 300 ℃, pure oxygen is introduced when the temperature is raised to 1000 ℃, and the introduction of oxygen is stopped when the temperature is lowered to 1300 ℃ after sintering is finished.
The target material was subjected to density test, and the film prepared by magnetron sputtering was subjected to electron mobility test, and the test results are shown in table 1. The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 98.6 percent by the Archimedes drainage method.
Machining and binding the obtained planar target to prepare a sputtering target with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 50.23cm2/V·s。
Example 3:
(1) respectively weighing 9.7kg of indium oxide powder, 0.1kg of tin oxide powder, 0.05kg of molybdenum oxide powder, 0.05kg of titanium oxide powder and 0.1kg of zirconium oxide powder, uniformly mixing with ultrapure water according to the solid content of 60%, and adding 0.6% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated.
(2) And adding the polyvinyl alcohol mixed solution into the third mixed slurry, wherein the adding amount is 1.2 percent calculated by pure polyvinyl alcohol substances, the defoaming agent is 0.05 percent calculated by the mass of the solution, and then sieving the slurry by a 200-mesh sieve for defoaming and impurity removal treatment.
(3) Granulating with spray dryer, setting inlet and outlet temperature parameters of 200 deg.C and 100 deg.C, rotating speed of 11000rpm, feeding frequency of 15, and sieving with 80 mesh sieve to remove coarse powderGranules having a bulk density of 1.56g/cm3。
(4) When the planar target material is formed, the granulated powder is placed in a steel die with the size of 300mm and is subjected to 50MPa dry pressing preforming, and a preformed biscuit is subjected to waterproof packaging by vacuumizing through a rubber bag; when the target material is rotated to be molded, the granulation powder is placed in a mold with a stainless steel mold core and a rubber outer sleeve, and two ends of the granulation powder are sealed by rubber plugs and mechanically fixed; and simultaneously carrying out cold isostatic pressing at 300MPa and maintaining the pressure for 12min to obtain a high-density biscuit.
(5) The plane and the rotary biscuit are put into a sintering furnace for sintering, and the temperature interval and the temperature rise speed are as follows: room temperature is between 120 ℃ and 120 ℃ (1 ℃/min), between 120 ℃ and 400 ℃ (0.8 ℃/min), between 400 ℃ and 750 ℃ (0.5 ℃/min), between 750 ℃ and 1000 ℃ (1 ℃/min), between 1000 ℃ and 1150 ℃ (0.5 ℃/min), between 1150 ℃ and 1300 (2 ℃/min), between 1300 ℃ and 1550 ℃ (0.2 ℃/min). And after the temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at a cooling rate of 10 ℃/min and preserving heat for 5h, and then cooling to 1490 ℃ and preserving heat for 15h so as to adjust the microstructure in the target. Then, the temperature is continuously reduced, the temperature reduction rate in the range of 1490-1000 ℃ is 0.6 ℃/min, and then the power is cut off for natural temperature reduction.
Sintering atmosphere: and after the temperature is raised to 300 ℃, air is introduced, pure oxygen is introduced when the temperature is raised to 1000 ℃, and the introduction of oxygen is stopped when the temperature is lowered to 1300 ℃ after sintering is finished.
The target material was subjected to density test, and the film prepared by magnetron sputtering was subjected to electron mobility test, and the test results are shown in table 1. The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 99.2 percent by the Archimedes drainage method.
Machining and binding the obtained planar target to prepare a sputtering target with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 60.12cm2/V·s。
Example 4:
(1) respectively weighing 9.75kg of indium oxide powder, 0.15kg of tin oxide powder, 0.03kg of molybdenum oxide powder, 0.05kg of titanium oxide powder and 0.02kg of zirconium oxide powder, uniformly mixing with ultrapure water according to the solid content of 65%, and adding 0.8% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated.
(2) And adding the polyvinyl alcohol mixed solution into the third mixed slurry, wherein the addition amount is 0.5 percent calculated by pure polyvinyl alcohol substances, the defoaming agent is 0.03 percent calculated by the mass of the solution, and then sieving the slurry by a 200-mesh sieve for defoaming and impurity removal treatment.
(3) Granulating with spray dryer at inlet and outlet temperature of 200 deg.C and 100 deg.C, rotation speed of 11000rpm, and feeding frequency of 15, sieving with 80 mesh sieve to remove coarse particles, and making the granulated powder have bulk density of 1.61g/cm3。
(4) When the planar target material is formed, the granulated powder is placed in a steel die with the size of 300mm and is subjected to 50MPa dry pressing preforming, and a preformed biscuit is subjected to waterproof packaging by vacuumizing through a rubber bag; when the target material is rotated to be molded, the granulation powder is placed in a mold with a stainless steel mold core and a rubber outer sleeve, and two ends of the granulation powder are sealed by rubber plugs and mechanically fixed; and simultaneously carrying out cold isostatic pressing at 300MPa and maintaining the pressure for 12min to obtain a high-density biscuit.
(5) The plane and the rotary biscuit are put into a sintering furnace for sintering, and the temperature interval and the temperature rise speed are as follows: room temperature is between 120 ℃ and 120 ℃ (1 ℃/min), between 120 ℃ and 400 ℃ (0.8 ℃/min), between 400 ℃ and 750 ℃ (0.5 ℃/min), between 750 ℃ and 1000 ℃ (1 ℃/min), between 1000 ℃ and 1150 ℃ (0.5 ℃/min), between 1150 ℃ and 1300 (2 ℃/min), between 1300 ℃ and 1550 ℃ (0.2 ℃/min). And after the temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at a cooling rate of 10 ℃/min and preserving heat for 5h, and then cooling to 1490 ℃ and preserving heat for 15h so as to adjust the microstructure in the target. Then, the temperature is continuously reduced, the temperature reduction rate is 0.6 ℃/min within the range of 1490-1000 ℃, and then the power is cut off for natural temperature reduction.
Sintering atmosphere: and after the temperature is raised to 300 ℃, air is introduced, pure oxygen is introduced when the temperature is raised to 1000 ℃, and the introduction of oxygen is stopped when the temperature is lowered to 1300 ℃ after sintering is finished.
The target material was subjected to density test, and the film prepared by magnetron sputtering was subjected to electron mobility test, and the test results are shown in table 1. The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 99.1 percent by testing through an Archimedes drainage method.
Machining and binding the obtained planar target to prepare a sputtering target with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 51.24cm2/V·s。
Example 5:
(1) respectively weighing 9.75kg of indium oxide powder, 0.1kg of tin oxide powder, 0.1kg of molybdenum oxide powder, 0.025kg of titanium oxide powder, 0.02kg of cerium oxide powder and 0.005kg of silicon oxide powder, uniformly mixing with ultrapure water according to 60 percent of solid content, and adding 0.6 percent of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated.
(2) And adding the polyvinyl alcohol mixed solution into the third mixed slurry, wherein the adding amount is 1.0 percent calculated by pure polyvinyl alcohol substances, the defoaming agent is 0.04 percent calculated by the mass of the solution, and then sieving the slurry by a 200-mesh sieve for defoaming and impurity removal treatment.
(3) Granulating with spray dryer, setting inlet and outlet temperature parameters of 200 deg.C and 100 deg.C, rotating speed of 11000rpm, feeding frequency of 15, sieving with 80 mesh sieve to remove coarse particles, and its apparent density is 1.57g/cm3。
(4) When the planar target material is formed, the granulated powder is placed in a steel die with the size of 300mm and is subjected to 50MPa dry pressing preforming, and a preformed biscuit is subjected to waterproof packaging by vacuumizing through a rubber bag; when the target material is rotated to be molded, the granulation powder is placed in a mold with a stainless steel mold core and a rubber outer sleeve, and two ends of the granulation powder are sealed by rubber plugs and mechanically fixed; and simultaneously carrying out cold isostatic pressing at 300MPa and keeping the pressure for 12min to obtain a high-density biscuit.
(5) The plane and the rotary biscuit are put into a sintering furnace for sintering, and the temperature interval and the temperature rise speed are as follows: room temperature is between 120 ℃ and 120 ℃ (1 ℃/min), between 120 ℃ and 400 ℃ (0.8 ℃/min), between 400 ℃ and 750 ℃ (0.5 ℃/min), between 750 ℃ and 1000 ℃ (1 ℃/min), between 1000 ℃ and 1150 ℃ (0.5 ℃/min), between 1150 ℃ and 1300 (2 ℃/min), between 1300 ℃ and 1550 ℃ (0.2 ℃/min). And after the temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at a cooling rate of 10 ℃/min and preserving heat for 5 hours, and then cooling to 1490 ℃ and preserving heat for 15 hours so as to adjust the microstructure in the target. Then, the temperature is continuously reduced, the temperature reduction rate is 0.6 ℃/min within the range of 1490-1000 ℃, and then the power is cut off for natural temperature reduction.
Sintering atmosphere: air is introduced when the temperature is raised to 300 ℃, pure oxygen is introduced when the temperature is raised to 1000 ℃, and the introduction of oxygen is stopped when the temperature is lowered to 1300 ℃ after sintering is finished.
The target material was subjected to density test, and the film prepared by magnetron sputtering was subjected to electron mobility test, and the test results are shown in table 1. The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 99.3 percent by testing through an Archimedes drainage method.
Machining and binding the obtained planar target material to prepare a sputtering target material with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 48.69cm2/V·s。
Example 6:
(1) respectively weighing 9.75kg of indium oxide powder, 0.1kg of tin oxide powder, 0.03kg of tungsten oxide powder, 0.03kg of molybdenum oxide powder, 0.04kg of cerium oxide powder and 0.05kg of zirconium oxide powder, uniformly mixing with ultrapure water according to 60% of solid content, and adding 0.6% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated. The other processing procedures of the target material were the same as in example 5.
The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 98.7 percent by the Archimedes drainage method.
Machining and binding the obtained planar target to prepare a sputtering target with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 53.34cm2/V·s。
Example 7:
(1) respectively weighing 9.8kg of indium oxide powder, 0.1kg of tin oxide powder, 0.03kg of tungsten oxide powder, 0.03kg of cerium oxide powder, 0.03kg of zirconium oxide powder, 0.005kg of silicon oxide powder and 0.005kg of titanium oxide, uniformly mixing with ultrapure water according to 60% of solid content, and adding 0.6% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated. The other processing procedures of the target material were the same as in example 5.
The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 99 percent by testing through an Archimedes drainage method.
Machining and binding the obtained planar target to prepare a sputtering target with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 49.23cm2/V·s。
Example 8:
(1) respectively weighing 9.8kg of indium oxide powder, 0.1kg of tin oxide powder, 0.02kg of molybdenum oxide powder, 0.02kg of cerium oxide powder, 0.05kg of zirconium oxide powder, 0.002kg of silicon oxide powder and 0.008kg of titanium oxide, uniformly mixing with ultrapure water according to the solid content of 60%, and adding 0.6% of dispersing agent. Firstly, 1-2mm zirconium balls are used for rough grinding in a sand mill for 2h, then 0.3-0.5mm zirconium balls are used for fine grinding in the sand mill for 6h, and a grinding cavity is made of polyurethane. The above pulping process is repeated for 3 times, and then mixed together and added with adhesive and spray granulated. The other processing procedures of the target material were the same as in example 5.
The rotary target material with the length of 300mm is obtained by grinding the inner circle and the outer circle and cutting the end head, and the relative density of the rotary target material is 99 percent by testing through an Archimedes drainage method.
Machining and binding the obtained planar target to prepare a sputtering target with the diameter of 6 inches, coating in a direct-current magnetron sputtering system, wherein the substrate is Corning glass with the thickness of 0.7mm, the sputtering gas is argon, the working gas is oxygen (water vapor or hydrogen is not introduced), and the electron mobility of the film prepared under the optimized process condition is 50.57cm2/V·s。
Comparative example 1:
the ITO target having a commercial composition ratio of 90/10 had a relative density of 99.6% and a diameter of 6 inches. Coating in a DC magnetron sputtering system with a substrate of Corning glass with a thickness of 0.7mm, a sputtering gas of argon, a working gas of oxygen (without introducing water vapor or hydrogen), and an electron mobility of the film prepared under optimized process conditions of 14.78cm2/V·s。
Comparative example 2:
the ITO target having a compositional ratio of 97/3 was purchased, and had a relative density of 98.4% and a diameter of 6 inches. Coating in a DC magnetron sputtering system with a substrate of Corning glass with a thickness of 0.7mm, a sputtering gas of argon, a working gas of oxygen (without introducing water vapor or hydrogen), and an electron mobility of the film prepared under optimized process conditions of 25.66cm2/V·s。
The following table is the experimental data for all examples and comparative examples.
Figure DEST_PATH_IMAGE001
Compared with the comparative example, the electron mobility and the relative density of the target are obviously improved, the conversion efficiency of the magnetron sputtering thin-film solar cell can be improved, and the surface nodule poisoning phenomenon in the sputtering process is reduced.

Claims (3)

1. A rotary ceramic target material for a high-efficiency solar cell is characterized in that the components of the ceramic target material are 97-98wt% of indium oxide, 0.5-2wt% of tin oxide and 1-2.5wt% of doped oxide; the doped oxide is 3-5 of titanium oxide, tungsten oxide, molybdenum oxide, zirconium oxide, cerium oxide and silicon oxide.
2. The ceramic target according to claim 1, wherein the method of preparing the ceramic target comprises:
and (3) sintering the formed ceramic target biscuit in a sintering furnace at the following sintering temperature:
(1) the first temperature interval: the room temperature is 120 ℃ below zero, and the heating speed is 1 ℃/min;
(2) the second temperature interval: at the temperature of 120 ℃ and 400 ℃, the heating speed is 0.8 ℃/min;
(3) the third temperature interval: 400 ℃ and 750 ℃, and the temperature rising speed is 0.5 ℃/min;
(4) a fourth temperature interval: 750-;
(5) a fifth temperature interval: 1000 and 1150 ℃, and the heating rate is 0.5 ℃/min;
(6) sixth temperature interval: 1150-1300 ℃ and the heating speed is 2 ℃/min;
(7) a seventh temperature interval: 1300 ℃ and 1550 ℃, and the heating speed is 0.2 ℃/min;
(8) eighth temperature interval: after the highest temperature reaches 1550 ℃, firstly cooling to 1520 ℃ at a cooling speed of 10 ℃/min and preserving heat for 5-10h, then cooling to 1490 ℃ at the same speed and preserving heat for 15-25 h;
(9) ninth temperature interval: 1490-;
(10) tenth temperature interval: and (5) closing a heat source to naturally cool at the temperature of 1000-room temperature.
3. The ceramic target material according to claim 2, wherein in the preparation method, the formed ceramic target material biscuit is placed in a sintering furnace for sintering, purified air is started to be introduced after the temperature is raised to 300 ℃, pure oxygen is switched when the temperature reaches 1000 ℃, and the introduction of the pure oxygen is stopped until the temperature is reduced to 1300 ℃.
CN202210165564.5A 2022-02-23 2022-02-23 High-efficiency rotary ceramic target for solar cell Pending CN114620996A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210165564.5A CN114620996A (en) 2022-02-23 2022-02-23 High-efficiency rotary ceramic target for solar cell

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210165564.5A CN114620996A (en) 2022-02-23 2022-02-23 High-efficiency rotary ceramic target for solar cell

Publications (1)

Publication Number Publication Date
CN114620996A true CN114620996A (en) 2022-06-14

Family

ID=81899928

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210165564.5A Pending CN114620996A (en) 2022-02-23 2022-02-23 High-efficiency rotary ceramic target for solar cell

Country Status (1)

Country Link
CN (1) CN114620996A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115893988A (en) * 2022-12-07 2023-04-04 洛阳晶联光电材料有限责任公司 Evaporation target material for solar cell and preparation method thereof
CN116199497A (en) * 2022-12-16 2023-06-02 华南理工大学 Oxide target and preparation method thereof
CN116425514A (en) * 2023-03-15 2023-07-14 中山智隆新材料科技有限公司 Multi-element oxide doped indium oxide-based target material and preparation method and application thereof
CN116730710A (en) * 2023-02-07 2023-09-12 中山智隆新材料科技有限公司 High-valence element doped indium tin oxide material and preparation method and application thereof
CN116813314A (en) * 2023-06-01 2023-09-29 先导薄膜材料（广东）有限公司 Alumina doped titanium praseodymium oxide target material and preparation method thereof

Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1119850A (en) * 1993-02-11 1996-04-03 维苏威乌斯坩埚公司 Method of manufacturing an ito sintered body, and article produced thereby
JP2002275624A (en) * 2001-03-19 2002-09-25 Sumitomo Metal Mining Co Ltd Sintered compact target for depositing transparent electrically conductive thin film, production method therefor and transparent electrically conductive thin film obtained therefrom
JP2003105532A (en) * 2001-06-26 2003-04-09 Mitsui Mining & Smelting Co Ltd Sputtering target for highly resistant transparent conductive film, and manufacturing method of highly resistant transparent conductive film
US20030218153A1 (en) * 2002-03-27 2003-11-27 Sumitomo Metal Mining Co., Ltd. Transparent conductive thin film, process for producing the same, sintered target for producing the same, and transparent, electroconductive substrate for display panel, and organic electroluminescence device
JP2004315951A (en) * 2003-04-21 2004-11-11 Nikko Materials Co Ltd Ito sputtering target, manufacturing method therefor, and transparent electroconductive ito film
JP2005126766A (en) * 2003-10-23 2005-05-19 Sumitomo Metal Mining Co Ltd Indium-oxide-based target and manufacturing method therefor
JP2006022373A (en) * 2004-07-07 2006-01-26 Sumitomo Metal Mining Co Ltd Method for manufacturing sputtering target for preparing transparent conductive thin film
JP2008308385A (en) * 2007-06-18 2008-12-25 Sumitomo Metal Mining Co Ltd Method of manufacturing indium oxide-based sputtering target
US20120043509A1 (en) * 2009-10-06 2012-02-23 Jx Nippon Mining & Metals Corporation Indium Oxide Sintered Compact, Indium Oxide Transparent Conductive Film, and Manufacturing Method of Indium Oxide Transparent Conductive Film
CN102731067A (en) * 2012-07-04 2012-10-17 韶关西格玛技术有限公司 Preparation method of high-density ITO (indium tin oxide) evaporation target
JP2014073959A (en) * 2013-11-25 2014-04-24 Jx Nippon Mining & Metals Corp Oxide sintered body, and method for producing the same
CN105294072A (en) * 2015-11-06 2016-02-03 广西晶联光电材料有限责任公司 Pressureless sintering method for TFT-grade ITO target
CN108863343A (en) * 2018-06-22 2018-11-23 广东凯盛光伏技术研究院有限公司 A kind of method of the sintering integrated formula production ITO target of degreasing-
CN110741106A (en) * 2017-08-08 2020-01-31 三井金属矿业株式会社 Oxide sintered body and sputtering target
CN113149613A (en) * 2021-05-24 2021-07-23 先导薄膜材料（广东）有限公司 ITWO target material and preparation method thereof

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1119850A (en) * 1993-02-11 1996-04-03 维苏威乌斯坩埚公司 Method of manufacturing an ito sintered body, and article produced thereby
JP2002275624A (en) * 2001-03-19 2002-09-25 Sumitomo Metal Mining Co Ltd Sintered compact target for depositing transparent electrically conductive thin film, production method therefor and transparent electrically conductive thin film obtained therefrom
JP2003105532A (en) * 2001-06-26 2003-04-09 Mitsui Mining & Smelting Co Ltd Sputtering target for highly resistant transparent conductive film, and manufacturing method of highly resistant transparent conductive film
US20030218153A1 (en) * 2002-03-27 2003-11-27 Sumitomo Metal Mining Co., Ltd. Transparent conductive thin film, process for producing the same, sintered target for producing the same, and transparent, electroconductive substrate for display panel, and organic electroluminescence device
JP2004315951A (en) * 2003-04-21 2004-11-11 Nikko Materials Co Ltd Ito sputtering target, manufacturing method therefor, and transparent electroconductive ito film
JP2005126766A (en) * 2003-10-23 2005-05-19 Sumitomo Metal Mining Co Ltd Indium-oxide-based target and manufacturing method therefor
JP2006022373A (en) * 2004-07-07 2006-01-26 Sumitomo Metal Mining Co Ltd Method for manufacturing sputtering target for preparing transparent conductive thin film
JP2008308385A (en) * 2007-06-18 2008-12-25 Sumitomo Metal Mining Co Ltd Method of manufacturing indium oxide-based sputtering target
US20120043509A1 (en) * 2009-10-06 2012-02-23 Jx Nippon Mining & Metals Corporation Indium Oxide Sintered Compact, Indium Oxide Transparent Conductive Film, and Manufacturing Method of Indium Oxide Transparent Conductive Film
CN102731067A (en) * 2012-07-04 2012-10-17 韶关西格玛技术有限公司 Preparation method of high-density ITO (indium tin oxide) evaporation target
JP2014073959A (en) * 2013-11-25 2014-04-24 Jx Nippon Mining & Metals Corp Oxide sintered body, and method for producing the same
CN105294072A (en) * 2015-11-06 2016-02-03 广西晶联光电材料有限责任公司 Pressureless sintering method for TFT-grade ITO target
CN110741106A (en) * 2017-08-08 2020-01-31 三井金属矿业株式会社 Oxide sintered body and sputtering target
CN108863343A (en) * 2018-06-22 2018-11-23 广东凯盛光伏技术研究院有限公司 A kind of method of the sintering integrated formula production ITO target of degreasing-
CN113149613A (en) * 2021-05-24 2021-07-23 先导薄膜材料（广东）有限公司 ITWO target material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李金桂主编: "《现代表面工程设计手册》", 30 September 2000, 国防工业出版社 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115893988A (en) * 2022-12-07 2023-04-04 洛阳晶联光电材料有限责任公司 Evaporation target material for solar cell and preparation method thereof
CN115893988B (en) * 2022-12-07 2023-09-08 洛阳晶联光电材料有限责任公司 Evaporation target material for solar cell and preparation method thereof
CN116199497A (en) * 2022-12-16 2023-06-02 华南理工大学 Oxide target and preparation method thereof
CN116730710A (en) * 2023-02-07 2023-09-12 中山智隆新材料科技有限公司 High-valence element doped indium tin oxide material and preparation method and application thereof
CN116425514A (en) * 2023-03-15 2023-07-14 中山智隆新材料科技有限公司 Multi-element oxide doped indium oxide-based target material and preparation method and application thereof
CN116425514B (en) * 2023-03-15 2023-12-22 中山智隆新材料科技有限公司 Multi-element oxide doped indium oxide-based target material and preparation method and application thereof
CN116813314A (en) * 2023-06-01 2023-09-29 先导薄膜材料（广东）有限公司 Alumina doped titanium praseodymium oxide target material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN114620996A (en) High-efficiency rotary ceramic target for solar cell
CN101468915A (en) Polycrystal alumina transparent ceramic with preferred orientation and preparation thereof
CN114031376B (en) Preparation method of high-hardness fine-grain ZTA system complex phase ceramic material
CN108218419B (en) Preparation method of indium tin oxide ceramic target material
JPH11322332A (en) Zno-based sintered product and its production
CN114524664A (en) Ceramic target material for solar cell and preparation method thereof
JPH10158827A (en) Ito (indium tin oxide) sintered body and ito sputtering target
CN112813397B (en) Preparation method of molybdenum-sodium alloy plate-shaped target
CN112723863A (en) Manufacturing method of advanced-generation TFT-grade fine-grain ITO target
CN112723875A (en) Gallium oxide doped tin oxide ceramic target material and preparation method thereof
CN108002428B (en) Preparation method of ITO (indium tin oxide) particles for evaporation and ITO particles prepared by method
CN114736013B (en) Zinc-magnesium oxide target material and preparation method thereof
CN113149652A (en) High-light-transmittance transparent ceramic prepared based on cold sintering technology and preparation method thereof
CN112624739A (en) Nickel oxide-based ceramic target material, thin film and thin film preparation process
CN108623287A (en) A kind of short flow process of indium gallium zinc sintered body
CN106587940B (en) High-purity compact magnesium oxide target material and preparation method thereof
CN102443765B (en) Preparation method of MgZnO semiconductor film
CN109354497B (en) Ho-doped transparent scandium oxide ceramic and preparation method thereof
CN112374554A (en) High-purity high-activity nickel oxide-based powder, preparation method and application
JP2023155427A (en) IGZO sputtering target
JPH07243036A (en) Ito sputtering target
CN102453865A (en) Preparation method of MgZnO film and application thereof
CN116396076A (en) Preparation method of conductive lithium niobate target material
CN114592173B (en) CdIn alloy target and preparation method thereof
CN113233888A (en) Method for preparing IGZO target material by recycling IGZO waste biscuit

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20220614