WO2015114886A1 - 水酸化インジウム粉の製造方法及び陰極 - Google Patents

水酸化インジウム粉の製造方法及び陰極 Download PDF

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WO2015114886A1
WO2015114886A1 PCT/JP2014/077193 JP2014077193W WO2015114886A1 WO 2015114886 A1 WO2015114886 A1 WO 2015114886A1 JP 2014077193 W JP2014077193 W JP 2014077193W WO 2015114886 A1 WO2015114886 A1 WO 2015114886A1
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cathode
hydroxide powder
indium hydroxide
electrodes
particle size
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PCT/JP2014/077193
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English (en)
French (fr)
Japanese (ja)
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剛 岩佐
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住友金属鉱山株式会社
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Priority to KR1020167007052A priority Critical patent/KR102300880B1/ko
Priority to CN201480058844.XA priority patent/CN105683416B/zh
Publication of WO2015114886A1 publication Critical patent/WO2015114886A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00—Compounds of gallium, indium or thallium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00—Compounds of gallium, indium or thallium
    • C01G15/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/14—Alkali metal compounds
    • C25B1/16—Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Definitions

  • the present invention relates to a method for producing indium hydroxide powder by an electrolytic method and a cathode used in the method for producing indium hydroxide powder.
  • transparent conductive film forming materials such as sputtering targets
  • indium oxide-based sintered materials are mainly used, and indium oxide powder is used as the main raw material.
  • Patent Document 1 as a method for producing indium oxide powder, there is a method of producing indium oxide powder by precipitating indium hydroxide powder by electrolytic treatment of metal indium and so-called electrolytic method. are listed.
  • the distance between the electrodes is defined as 25 mm to 50 mm in the embodiment.
  • the distance between the electrodes and the electrolytic voltage are closely related, and it is desirable that the distance between the electrodes is as close as possible from the viewpoint of the liquid temperature between the electrodes and the pH control due to the voltage increase.
  • the present invention has been proposed in view of the above-described conventional situation, suppresses the increase in the liquid temperature and pH between the electrodes, the indium hydroxide powder has excellent uniformity in particle size, and the particle size distribution width.
  • the present invention provides a method for producing indium hydroxide powder capable of obtaining a narrow indium hydroxide powder, and a cathode used in the method for producing indium hydroxide powder.
  • indium hydroxide powder is produced by electrolysis in an electrolytic solution using a plurality of anodes and cathodes made of metal indium.
  • the main surface portion of the cathode used for electrolysis is formed in a net shape.
  • the liquid temperature between the anode and the cathode is controlled within a range of ⁇ 2 ° C. with respect to the set temperature of the electrolyzer, and the pH of the electrolyte between the anode and the cathode is controlled. It is preferable to control within the range of 3.2 to 4.0.
  • the cathode according to the present invention is a cathode used in the method for producing indium hydroxide powder, and is a cathode formed by forming the main surface portion of the cathode in a net shape.
  • FIG. 1 is a diagram showing an example of the shape of a net-like cathode to which the present invention is applied.
  • FIG. 1A is a diagram illustrating an example of a net-like cathode when lath processing is performed
  • FIG. 1B is a diagram illustrating an example of a net-like cathode when punching is performed. is there.
  • FIG. 2 is a diagram showing the transition of the liquid temperature between the anode and the cathode during electrolysis in Examples and Comparative Examples.
  • FIG. 3 is a diagram showing the transition of the pH of the electrolyte solution between the anode and the cathode during electrolysis in Examples and Comparative Examples.
  • FIG. 4 is a diagram showing the particle size of the indium hydroxide powder obtained by Examples and Comparative Examples.
  • indium hydroxide powder is obtained by utilizing an electrolytic reaction using an electrolytic solution with adjusted concentration, pH, solubility and the like.
  • metal indium as a raw material is used as an anode
  • a conductive metal is used for a cathode (cathode) as a counter electrode, and both are immersed in an electrolytic solution to generate a potential difference between both electrodes to generate a current.
  • dissolution of the metal proceeds at the anode.
  • the indium hydroxide slurry crystallizes and precipitates by adjusting the pH so that the solubility of the generated indium hydroxide powder is low in the electrolytic solution. .
  • the metal indium used for the anode is not particularly limited, but it is desirable to have a high purity in order to suppress contamination of impurities in the indium oxide powder obtained by calcining indium hydroxide powder.
  • metal indium a purity of 99.9999% (commonly called 6N product) can be mentioned as a suitable product.
  • the cathode may be made of a material that does not corrode by the electrolytic solution, and a conductive metal or the like is used.
  • a conductive metal or the like is used as the cathode.
  • an insoluble titanium plate or the like can be used, and an insoluble electrode obtained by coating a titanium plate with platinum, a stainless steel (SUS) plate, an In plate, or the like can be used.
  • the cathode has a main surface formed in a net shape.
  • the interelectrode distance between the anode and the cathode is not particularly specified, but is preferably 10 to 25 mm. If it exceeds 25 mm, the voltage increases due to the liquid resistance, so the liquid temperature and pH between the electrodes increase, the particle size of the indium hydroxide powder becomes non-uniform, and the width of the particle size distribution becomes wider. In the case of less than 10 mm, contact between electrodes and short circuit are likely to occur.
  • an aqueous solution of a general electrolyte salt such as a water-soluble nitrate, sulfate, or chloride salt can be used.
  • aqueous ammonium nitrate solution using ammonium nitrate in which nitrate ions and ammonium ions are removed as nitrogen compounds after precipitation of indium hydroxide powder and calcination is left as impurities is preferable.
  • the electrolyte preferably has a solubility of the produced indium hydroxide powder in the range of 10 ⁇ 6 to 10 ⁇ 3 mol / L.
  • solubility of the indium hydroxide powder is lower than 10 ⁇ 6 mol / L, indium ions dissolved from the anode are easily nucleated, so that the primary particle diameter becomes too fine.
  • the primary particle diameter is too fine, it is not preferable because it becomes difficult to separate and recover the indium hydroxide powder in the subsequent step of recovering the indium hydroxide powder.
  • the solubility of the indium hydroxide powder is higher than 10 ⁇ 3 mol / L, the grain growth is promoted, so that the primary particle diameter becomes large. For this reason, the larger the particle is grown, the larger the difference in particle size between the growing particle and the non-growing particle. Since the difference in particle diameter affects the degree of aggregation, as a result, the width of the particle size distribution of the indium hydroxide powder becomes wide. If the width of the particle size distribution of the indium hydroxide powder becomes wider, the width of the particle size distribution of the indium oxide powder obtained by calcining the indium hydroxide powder also becomes wider, and the density of the sputtering target obtained by sintering this becomes higher. This is not preferable because it is difficult to achieve density.
  • the solubility of the indium hydroxide powder in the electrolytic solution may be in the range of 10 ⁇ 6 to 10 ⁇ 3 mol / L, and the solubility can be controlled by the ammonium nitrate concentration, pH, liquid temperature, and the like.
  • the concentration of the electrolytic solution is not particularly limited, but is preferably 0.1 to 2.0 mol / L. If it is thinner than 0.1 mol / L, the voltage rise during electrolysis will increase, and the amount of heat generated will increase at places where the contact resistance is high, such as the contact portion of the electrode. As a result, problems such as an increase in the temperature of the electrolytic solution and an increase in power cost due to heat generation of the electrodes are not preferable.
  • the concentration is higher than 2.0 mol / L, the indium hydroxide particles are coarsened by electrolysis and the variation in the particle size becomes large, which is not preferable.
  • the pH of the electrolyte solution between the anode and the cathode is not particularly limited, but is preferably 3.2 to 4.0.
  • the pH of the electrolyte is less than 3.2, hydroxide precipitation is difficult to occur, and when it is greater than 4.0, the precipitation rate of the hydroxide is too high and the concentration is not uniform. Is not preferable because the particle size is non-uniform and the particle size distribution width is widened.
  • the pH of the entire electrolyte is preferably 3.2 to 4.0.
  • the electrolyte solution can be easily circulated through the cathode network holes, and the increase in pH between the electrodes can be suppressed by uniformly mixing the electrolyte solution as a whole. .
  • the concentration of ammonium nitrate is adjusted to 0.1 to 2.0 mol / L
  • the pH is adjusted to 3.2 to 4.0
  • the solution temperature between the electrodes is adjusted to a range of 20 to 60 ° C.
  • the solubility of the indium hydroxide powder can be controlled in the range of 10 ⁇ 6 to 10 ⁇ 3 mol / L.
  • the pH can be adjusted by the amount of ammonium nitrate added.
  • the temperature of the electrolyte solution between the anode and the cathode is lower than 20 ° C., the deposition rate is too slow, and when it is higher than 60 ° C., the deposition rate is too high and precipitates are formed with non-uniform concentration. Therefore, the particle size becomes non-uniform and the particle size distribution width of the indium hydroxide powder is widened, which is not preferable.
  • the temperature of the electrolyte between the electrodes within a range of ⁇ 2 ° C with respect to the set temperature of the electrolyzer, it is possible to obtain indium hydroxide powder having excellent particle size uniformity and a narrow particle size distribution range. it can.
  • the main surface of the cathode is formed in a net-like shape, which makes it easier for the electrolyte to circulate through the cathode-like holes in the cathode, and prevents the increase in the liquid temperature between the electrodes by mixing the electrolyte uniformly. it can.
  • an oxygen-containing chelate compound such as citric acid, tartaric acid or glycolic acid or a nitrogen-containing chelate such as EDTA may be added to the electrolytic solution as necessary in order to improve the dissolution stability of the indium hydroxide powder.
  • the electrolysis conditions are not particularly limited, but the current density is preferably 3 A / dm 2 to 24 A / dm 2 .
  • the current density is lower than 3 A / dm 2 , the production efficiency of indium hydroxide powder is lowered.
  • the current density is higher than 24 A / dm 2 , the electrolysis voltage increases, so that the liquid temperature and pH between the electrodes increase, the particle size of the indium hydroxide powder becomes uneven, and the width of the particle size distribution is wide. Become.
  • the main surface portion of the cathode used for electrolysis is formed in a net shape, so that the electrolytic solution is easily circulated through the net holes of the cathode.
  • the electrolytic solution is uniformly mixed as a whole, the rise in the temperature and pH between the electrodes is suppressed, the particle size is excellent in uniformity, and the particle size distribution width is narrow. Indium powder can be obtained. Furthermore, by controlling the temperature of the liquid between the electrodes within a range of ⁇ 2 ° C.
  • the cathode has a main surface formed in a net shape.
  • the cathode is mainly an insoluble electrode.
  • a cathode 1A as shown in FIG. Cathode 1A has a contact portion 2A that is electrically connected to a power supply portion of a power source, and a main surface portion 3A that is mainly in contact with an electrolytic solution and undergoes an electrolytic reaction.
  • the cathode 1A has a net-like shape by forming holes 4A by lath processing on the main surface portion 3A of the cathode.
  • the cathode 1A is formed by forming a large number of slits alternately on a 1.0 mm-thick Ti plate and applying a lath process to extend the plate material in a direction perpendicular to the slits to form a net. By processing the cathode 1A into a net shape, the electrolyte existing between the electrodes is circulated between the electrodes without stagnation.
  • the net shape is not particularly limited, but when a Ti plate having a thickness of 1.0 mm is used, a net shape with rhombic holes having a vertical dimension of 3 mm to 4 mm and a horizontal dimension of 6 mm to 7 mm is preferable.
  • a cathode 1B as shown in FIG. 1B may be used as the cathode.
  • Cathode 1B has a contact portion 2B that is electrically connected to a power supply portion of the power source, and a main surface portion 3B that is mainly in contact with the electrolyte and undergoes an electrolytic reaction.
  • the cathode 1B has a net-like shape by forming holes 4B by punching in the main surface portion 3B of the cathode.
  • the cathode can be circulated without stagnation of the electrolyte solution between the electrodes, so punching board or hole processing by etching is also effective.
  • cathodes 1A and 1B shown in FIG. 1 are examples, and the shape, size, number, interval, and the like of the holes are not limited to these.
  • a plurality of reticulated cathodes as described above are electrolyzed together with an anode made of indium metal in an electrolytic solution.
  • the shape of the cathode is made reticulated so that the electrolyte circulates through the reticulated cathode without staying between the anode and the cathode.
  • the electrolytic solution is uniformly mixed as a whole, the rise in the temperature and pH between the electrodes can be suppressed, and indium hydroxide powder having excellent particle size uniformity and a narrow particle size distribution width can be obtained. it can.
  • a 1 mol / L ammonium nitrate aqueous solution was used as the electrolyte.
  • the liquid temperature between the electrodes was set to 40 ° C.
  • the pH was set to 3.5
  • 14 sheets of metal indium were electrolyzed as an anode by an electrolysis method with a current density of 12 A / dm 2
  • An indium hydroxide slurry was prepared.
  • the temperature between the electrodes is measured by immersing a thermometer in the electrolyte between the electrodes.
  • the pH between the electrodes is obtained by collecting the electrolyte between the electrodes and immediately adjusting the pH of the electrolyte to a pH meter. Measured with
  • Example 1 In Example 1, as a cathode with respect to the anode, a 1 mm thick Ti plate was subjected to lath processing with a mesh pitch of 1 mm to form rhombic holes having a longitudinal dimension of 3.2 mm and a lateral dimension of 6 mm, and a mesh shape of 30 cm ⁇ 30 cm ⁇ 1 mm thickness The cathode plate was used. Electrolysis was performed with the distance between the anode and the cathode being 17 mm, and the transition of the liquid temperature and pH between the electrodes during electrolysis and the particle size distribution of the obtained indium hydroxide powder were confirmed.
  • the liquid temperature between the electrodes was approximately constant at about 40 ° C.
  • the pH of the electrolytic solution was almost constant at about 3.5.
  • Example 2 As a cathode with respect to the anode, a 1 mm thick Ti plate was subjected to lath processing with a mesh pitch of 1 mm to form rhomboid holes having a longitudinal dimension of 3.2 mm and a lateral dimension of 6 mm, and a mesh shape of 30 cm ⁇ 30 cm ⁇ 1 mm thickness The cathode plate was used. Electrolysis was performed with the distance between the anode and the cathode being 25 mm, and the transition of the liquid temperature and pH between the electrodes during electrolysis and the particle size distribution of the obtained indium hydroxide powder were confirmed.
  • the liquid temperature between the electrodes was approximately constant at about 40 ° C.
  • the pH of the electrolytic solution was almost constant at about 3.5.
  • Comparative Example 1 In Comparative Example 1, a flat plate having a thickness of 30 cm ⁇ 30 cm ⁇ 1 mm was used as a cathode for the anode, not a net-like cathode. Electrolysis was performed with the distance between the anode and the cathode being 17 mm, and the transition of the liquid temperature and pH between the electrodes during electrolysis and the particle size distribution of the obtained indium hydroxide powder were confirmed.
  • the liquid temperature between the electrodes increased with time.
  • the pH of the electrolyte also increased with the passage of time.
  • Comparative Example 2 In Comparative Example 2, a flat plate having a thickness of 30 cm ⁇ 30 cm ⁇ 1 mm was used as a cathode for the anode, not a net-like cathode. Electrolysis was performed with the distance between the anode and the cathode being 25 mm, and the transition of the liquid temperature and pH between the electrodes during electrolysis and the particle size distribution of the obtained indium hydroxide powder were confirmed.
  • the liquid temperature between the electrodes increased with time.
  • the pH of the electrolyte also increased with the passage of time.
  • FIG. 2 shows the transition of the liquid temperature between the electrodes
  • FIG. 3 shows the transition of the pH in the electrolyte solution between the electrodes
  • FIG. 4 shows the particle size of the obtained indium hydroxide powder.
  • the pH of the electrolyte solution is substantially constant at about 3.5 in Examples 1 and 2, whereas in Comparative Examples 1 and 2, the pH value increases with time. I'm stuck. Therefore, it can be seen that an increase in pH between the electrodes can be suppressed by using a net-like cathode.
  • the 10% particle size is not so different from Examples 1 and 2 and Comparative Examples 1 and 2, whereas the 90% particle size is Comparative Example 1 and 2 in Example 1. Compared to 2, it is about twice as large. That is, indium hydroxide powder having excellent particle size uniformity and a narrow particle size distribution width is obtained when Example 1 or 2 is applied, compared with the case where Comparative Example 1 or 2 is applied. I understand.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
PCT/JP2014/077193 2014-01-29 2014-10-10 水酸化インジウム粉の製造方法及び陰極 WO2015114886A1 (ja)

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CN201480058844.XA CN105683416B (zh) 2014-01-29 2014-10-10 氢氧化铟粉的制造方法及阴极

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CN110644013B (zh) * 2019-10-30 2022-05-03 广东先导稀材股份有限公司 一种氧化铟及其前驱体的制备方法
CN112323084A (zh) * 2020-09-15 2021-02-05 先导薄膜材料（广东）有限公司 一种纳米氧化铟的制备方法

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JPH1095615A (ja) * 1996-06-20 1998-04-14 Mitsubishi Materials Corp 高密度焼結体用酸化インジウム粉末
JP2003096585A (ja) * 2001-09-21 2003-04-03 Furukawa Co Ltd 硫酸コバルト溶液の製造方法
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JP2013036074A (ja) * 2011-08-05 2013-02-21 Jx Nippon Mining & Metals Corp 水酸化インジウム及び水酸化インジウムを含む化合物の製造方法
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JPH1095615A (ja) * 1996-06-20 1998-04-14 Mitsubishi Materials Corp 高密度焼結体用酸化インジウム粉末
JP2004501281A (ja) * 2000-06-19 2004-01-15 エイチ・シー・スタルク・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング 金属の水酸化物または金属の塩基性炭酸塩の製造法
JP2003096585A (ja) * 2001-09-21 2003-04-03 Furukawa Co Ltd 硫酸コバルト溶液の製造方法
JP2013036074A (ja) * 2011-08-05 2013-02-21 Jx Nippon Mining & Metals Corp 水酸化インジウム及び水酸化インジウムを含む化合物の製造方法
WO2013179553A1 (ja) * 2012-05-31 2013-12-05 株式会社アルバック 金属水酸化物の製造方法及びｉｔｏスパッタリングターゲットの製造方法

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CN105683416B (zh) 2017-12-15
KR102300880B1 (ko) 2021-09-13
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CN105683416A (zh) 2016-06-15
TW201529479A (zh) 2015-08-01
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