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WO2018190461A1 - Procédé de préparation, à partir de déchets d'ito, de poudre pour une cible en ito de haute pureté présentant une densité relative élevée à l'aide d'acide nitrique et poudre ainsi préparée - Google Patents

Procédé de préparation, à partir de déchets d'ito, de poudre pour une cible en ito de haute pureté présentant une densité relative élevée à l'aide d'acide nitrique et poudre ainsi préparée Download PDF

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WO2018190461A1
WO2018190461A1 PCT/KR2017/005537 KR2017005537W WO2018190461A1 WO 2018190461 A1 WO2018190461 A1 WO 2018190461A1 KR 2017005537 W KR2017005537 W KR 2017005537W WO 2018190461 A1 WO2018190461 A1 WO 2018190461A1
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powder
ito
waste
nitric acid
relative density
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Korean (ko)
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이재용
송싱현
윤상혁
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Hanchung RF Co
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Hanchung RF Co
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    • 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
    • C04B35/457—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 based on tin oxides or stannates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
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    • 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
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    • 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
    • C04B35/64—Burning or sintering processes
    • 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
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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    • 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
    • C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density

Definitions

  • the present invention relates to a method for producing a high purity ITO target powder having high relative density from waste ITO scrap using nitric acid, and more particularly, to dissolving waste ITO scrap powder using a nitric acid (HNO3) solution.
  • HNO3 nitric acid
  • ITO (indium-tin composite oxide) film is widely used as a transparent electrode film of a display device centered on a liquid crystal display.
  • a method of forming this ITO film a method generally called a physical vapor deposition method such as a vacuum deposition method or a sputtering method is usually used.
  • the magnetron sputtering method is often used for operability and film stability.
  • the formation of the film by the sputtering method physically collides cations such as argon (Ar) ions with the target provided on the cathode, and releases the material constituting the target by the collision energy, thereby causing the surface of the target to face the substrate on the anode side. This is done by laminating films of approximately the same composition as the material.
  • the coating method by the sputtering method has a feature that it can form from the thin film of the Angstrom unit to the dozens of thick film at a stable film forming speed by adjusting the processing time and the power supply.
  • Indium (In) one of the materials of the transparent electrode, has an atomic number of 49 and is one of rare metals. It is a bright-gloss silver-white metal with good ductility and malleability and softness, so it has good workability and has a low melting point of 156.6.
  • tin another material, is mainly used for plating, compound preparation, etc., and is a metal having an atomic number of tin of 50, which is not easily oxidized in air, and is resistant to corrosion and does not react with water. It is mainly used for anti-corrosion plating and alloy of other metals, and is a metal used as the main constituent raw material of ITO together with indium.
  • indium oxide and tin oxide are used to make transparent electrodes of various flat panel devices including light emitting diodes (LEDs) and liquid crystal displays (LCD panels).
  • Indium tin oxide in which indium oxide and tin oxide are mixed is manufactured into a sintered body obtained by molding and sintering a raw material powder and used for a transparent conductive film.
  • one of the problems in forming a transparent conductive film using an ITO target is that the use efficiency of the ITO target is low, and the remaining ITO target after about 20-30% in general sputtering is scrapped. Recycling this scrap is very important in terms of utilizing scarce resources.
  • ITO powder from ITO scrap There are several ways to produce ITO powder from ITO scrap, one of which is to recover indium and tin as an oxidized powder, and then mix them at a predetermined ratio. This method has to recover the indium oxide powder and tin oxide powder separately, and the installation cost of the equipment is very large, there is a disadvantage that a lot of time for uniform mixing. Usually expensive indium is mainly recovered, and a method for selectively recovering indium from waste ITO scrap has already been proposed in the prior art.
  • Patent Document 1 Registered Patent No. 10-0850009
  • Patent Document 2 Prior Document 2: Registration No. 10-1002088
  • the present invention has been made to solve the above problems, and after dissolving the waste ITO scrap with nitric acid for the production method of high purity and high density ITO target powder obtained from the waste ITO scrap, the dissolved waste ITO solution is metatin acid, ITO
  • the residue is separated by an indium nitrate solution.
  • the indium nitrate solution is purified by removing impurities using a solvent extraction method to increase the purity.
  • the separated indium nitrate and ITO residue is neutralized with an indium nitrate liquid having high purity, and an alkaline liquid containing a dispersant, and the powder obtained by neutralization is washed and dried, and then the dried powder is calcined.
  • the present invention can solve the inconvenience, cost and process problems of recovering and mixing indium oxide powder and tin oxide powder, respectively, and further provide a method for producing a high density sintered ITO target.
  • the present invention dissolves waste ITO scrap with nitric acid, improves purity, neutralizes them with an alkaline liquid containing a dispersant, and uses high-density and high-density ITO having a high relative density of 99% or more using a powder obtained through neutralization. To provide a target.
  • the particle size of the waste ITO scrap of step (a) is characterized in that the powder form of 1 ⁇ 20.
  • reaction scheme in the dissolution step of preparing the mixed solution of step (a) is characterized in that the reaction of the following formula (1) and (2).
  • organic solvent used in the solvent extraction method in the step (c) is characterized in that selected from the group consisting of carboxylic acid, organic phosphoric acid and combinations thereof.
  • the organic solvent may be selected from the group consisting of tributyl phosphate, 2-ethylhexyl phosphoric acid, di- (2-ethylhexyl) phosphoric acid, and combinations thereof.
  • the alkaline solution is characterized in that any one or more of NaOH, KOH, NH 4 OH, NH 4 HCO 3 , CH 3 COONH 4 .
  • step (d) when the alkaline solution is NH 4 OH, it characterized in that following the reaction of the formula (3) and 4.
  • the pH is characterized in that the range of 9 to 11.
  • the heat treatment temperature of the step (f) is characterized in that the 300 ⁇ 900 range.
  • the content of the binder of the step (g) is characterized in that 1 to 5 parts by weight based on 100 parts by weight of the heat-treated powder.
  • the molded ITO target of step (i) is characterized in that the sintering in a high temperature oxygen atmosphere of 1500 ⁇ 1600.
  • ITO target powder is characterized in that it is obtained by a method for producing a high purity ITO target powder having a high relative density from waste ITO scrap using nitric acid as described above.
  • FIG. 1 is a schematic diagram of a method for producing a powder for high purity and high density ITO targets obtained from the waste ITO scrap of the present invention.
  • Figure 2 (a) is a scanning electron microscope image of the lung ITO scrap used according to the embodiment, (b) is an enlarged image.
  • 3 (a) and 3 (c) are scanning electron microscope images of meta-tartrate and ITO residues prepared according to the embodiment, and (b) and (d) are enlarged images.
  • 4 (a) and 4 (c) are scanning electron microscope images of the ITO oxide powder prepared according to the embodiment, and (b) and (d) are enlarged images.
  • a method for producing a high purity and high density ITO target powder obtained from waste ITO scrap is a) dissolving waste ITO scrap in nitric acid to produce indium nitrate solution and metatartrate, and producing a mixed liquid in which insoluble ITO residue remains.
  • step (a) the waste ITO scrap in the form of powder having a particle size of about 1 to 20 is added with 3-7 times the nitric acid to the scrap weight, so that In in the waste ITO scrap is indium nitrate (In (No 3 )). 3 ), allow meta-tartrate to be produced and insoluble ITO residues remain.
  • the reaction scheme for the dissolution process is as follows.
  • the mixed solution is filtered and separated into indium nitrate solution, meta-tartrate acid and ITO residue, respectively.
  • the indium nitrate solution obtained in the step (b) is purified by removing metal ion impurities that inhibit purity by using solvent extraction.
  • the organic solvent used in the solvent extraction method used to increase the purity in the step (c) is preferably selected from the group consisting of carboxylic acid, organic phosphoric acid, and combinations thereof, and specific examples are tributyl phosphate. , TBP), 2-ethylhexyl 2-ethylhexyl phosphonic acid (PC88A), di- (2-ethylhexyl) phosphonic acid (di- (2-ethyl hexyl) phosphonic acid, D2EHPA) and combinations thereof You can choose from the group consisting of.
  • an alkali containing OH ⁇ group is dissolved and diluted in ultrapure water, and the neutralized process is performed by adding a small amount of the separated indium nitrate solution, metatartrate acid and ITO residue.
  • a small amount of dispersant was added to the alkaline liquid in order to ensure uniform dispersibility and high sinterability of the powder during neutralization.
  • the pH is preferably in the range of about 9 to 11, and examples of the alkali that can be used include NaOH, KOH, NH 4 OH, NH 4 HCO 3 , CH 3 COONH 4 , and the like.
  • NH 4 OH can be used.
  • reaction scheme for the neutralization process is as follows.
  • the reason why the pH range is set to 9 to 11 is that when the pH is 9 or less, precipitation of the hydroxide powder produced after neutralization may be delayed, which may cause a problem in the washing step, and when the pH is 11 or more, the size of the hydroxide powder particles may be unevenly formed. It may be undesirable.
  • step (e) ultrapure water (DI water) is added to the product produced through the neutralization step of step (d), and decantation is used to remove ammonium nitrate and other salts in the product.
  • DI water ultrapure water
  • the product is hydroxide.
  • NH 4 OH to use the by-product produced in the neutralization reaction medium NH 4 NO 3 is the advantage of being soluble in water and from 0 118.3g / 100g, the solubility is very high, readily cleaned when removed from the 30 241.8g / 100g have.
  • step (e) the washed product is dried to remove moisture, and then crushed using a pulverization apparatus to powder it. This is because the pulverized and powdered form can perform a uniform heat treatment than the lumped product than the lumped product.
  • step (f) the powdered product is oxidized, and a calcined powder in angular form is formed.
  • the heat treatment temperature ranges from 300 to 900. If the heat treatment temperature is less than 300, the In (OH) 3 -Sn (OH) 4 precipitate is difficult to be converted to In 2 O 3 -SnO 2 , and if the heat treatment temperature is 900 or more, It is undesirable because the particle size can grow.
  • heat processing atmosphere can be performed in oxygen, argon, nitrogen, and air atmosphere.
  • the reaction scheme for the process is as follows.
  • step (g) by adding an appropriate amount of the binder to the heat-treated powder to increase the moldability of the heat-treated powder.
  • the content of the binder may be added 1 to 5 parts by weight based on 100 parts by weight of the heat-treated powder.
  • the content of the binder is 1 part by weight or less, the moldability of the oxidized powder may be lowered.
  • the content of the binder is 5 parts by weight or more, the moldability is increased, but the relative density is significantly lowered.
  • the powder having improved moldability obtained through the step (g) is put into a circular mold and press-molded to produce a cylindrical ITO target, and the cylindrical ITO target is sintered under oxygen pressure conditions at a high temperature of 1500 to 1600.
  • an ITO target having a relative density of at least 7.1 g / cm 3 is produced.
  • the powder for ITO target manufactured by the manufacturing method of the powder for high purity and high density ITO target obtained from waste ITO scrap can be obtained.
  • high purity and high density ITO targets can be produced using the powder for ITO targets.
  • the pulmonary ITO scrap was observed by the scanning electron microscope to determine the shape and size of the particles, as shown in Figure 1 to identify the powder having an angular form of about 1 micron.
  • 500 g of waste ITO scrap powder was added to 2 L of 60% nitric acid, dissolved at 110 to 20 hours, and filtered to separate indium nitrate, metatartrate and ITO residue.
  • the separated precipitate powder was observed with a scanning electron microscope, and it was confirmed that meta-tartrate and ITO residues coexist as shown in Example 1 of FIGS. 3 (a) and 3 (b).
  • Solvent extraction was carried out using PC88A, an organic solvent, to remove impurities contained in the filtered indium nitrate solution.
  • the washed hydroxide was dried for about 12 hours in an 80 oven to evaporate water, and then coarsely pulverized with a blender to obtain a hydroxide powder, and heat treated at 900 for 2.5 hours to obtain an oxidized powder. Observing the powder particles with a scanning electron microscope, it was confirmed that the particles of the angular form as shown in Example 1 of Figure 4 (a) and (b).
  • the binder was treated to 2% by weight of the powder to increase the moldability of the powder, and the binder-treated oxide powder was molded to prepare an ITO target, followed by sintering. After sintering, the relative density was measured and found to be 7.12 g / cm 3 , which was 99.46% of ITO.
  • Indium nitrate, meta-tartrate and ITO residues were added in small amounts to an alkaline solution containing a dispersant to reverse neutralization, and the neutralized hydroxide was washed six times with pure water.
  • the washed hydroxide was dried for about 16 hours in an 70 oven to evaporate moisture, and then coarsely pulverized with a blender to obtain a hydroxide powder, and heat treated at 900 for 2.5 hours to obtain an oxidized powder. Observing the powder particles with a scanning electron microscope, it was confirmed that the particles of the angular form as shown in Example 2 of Figure 4 (c) and (d).
  • the binder was treated with 2.5% by weight of the powder to increase the moldability of the powder, and the binder-treated oxide powder was molded to prepare an ITO target, followed by sintering. After sintering, the relative density measurement showed a value of 7.13 g / cm 3 , which was 99.58% compared to ITO.

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Abstract

La présente invention concerne un procédé de préparation, à partir de déchets d'ITO, d'une poudre pour une cible en ITO de haute pureté présentant une densité relative élevée à l'aide d'acide nitrique et la poudre ainsi préparée et, plus particulièrement : un procédé de préparation, à partir de déchets d'ITO, d'une poudre pour une cible en ITO de haute pureté présentant une densité relative élevée à l'aide d'acide nitrique, le procédé permettant de recycler des ressources rares lors de l'utilisation d'une poudre pour cible en ITO de haute pureté, qui est préparée à l'aide d'une solution d'acide nitrique (HNO3) de manière à faire fondre la poudre de déchets d'ITO, ce qui permet de la purifier et de la neutraliser afin d'obtenir une poudre pour cible d'ITO de haute pureté, puis de réaliser une étape de cuisson ; et la poudre ainsi préparée. A cet effet, la présente invention comprend : a) une étape de fusion consistant à faire fondre des déchets d'ITO dans de l'acide nitrique de façon à préparer une solution de mélange dans laquelle une solution de nitrate d'indium et de l'acide métastannique sont générés et un résidu d'ITO insoluble reste ; b) une étape de filtration consistant à séparer, à partir de la solution de mélange, la solution de nitrate d'indium, l'acide métastannique et l'ITO insoluble ; c) une étape de purification consistant à éliminer, par un procédé d'extraction par un solvant, des impuretés métalliques de la solution de nitrate d'indium séparée à l'étape b) ; d) une étape de neutralisation consistant à injecter, dans une solution alcaline contenant un dispersant, une petite quantité de la solution purifiée obtenue à l'étape c) et de l'acide métastannique et de l'ITO insoluble, qui sont obtenus à l'étape b), ce qui les neutralise ; e) une étape de lavage et de séchage du produit généré à l'étape d), puis de sa transformation en poudre par broyage ; f) une étape de cuisson consistant à traiter thermiquement la poudre obtenue à l'étape e) ; g) une étape d'auto-assemblage consistant à augmenter l'aptitude au façonnage de la poudre par addition d'un liant à la poudre traitée thermiquement obtenue à l'étape f) ; h) une étape de préparation d'une cible en ITO moulée par injection, dans un moule, de la poudre présentant une aptitude au façonnage améliorée, obtenue à l'étape g) ; et i) une étape de frittage de la cible en ITO moulée.
PCT/KR2017/005537 2017-04-13 2017-05-26 Procédé de préparation, à partir de déchets d'ito, de poudre pour une cible en ito de haute pureté présentant une densité relative élevée à l'aide d'acide nitrique et poudre ainsi préparée Ceased WO2018190461A1 (fr)

Applications Claiming Priority (2)

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