JP2013006710A - Method for recovering indium tin oxide and method for manufacturing indium tin oxide target - Google Patents
Method for recovering indium tin oxide and method for manufacturing indium tin oxide target Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 37
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 31
- 239000012670 alkaline solution Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- KVXKIRARVMGHKF-UHFFFAOYSA-G indium(3+);tin(4+);heptahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[In+3].[Sn+4] KVXKIRARVMGHKF-UHFFFAOYSA-G 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 24
- 238000000151 deposition Methods 0.000 abstract description 6
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 18
- 229910052738 indium Inorganic materials 0.000 description 12
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 11
- 229910052718 tin Inorganic materials 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 10
- 238000011084 recovery Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 5
- 239000003513 alkali Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000010979 pH adjustment Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000005478 sputtering type Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Processing Of Solid Wastes (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
本発明は、酸化インジウムスズの回収方法及び酸化インジウムスズターゲットの製造方法に関する。 The present invention relates to a method for recovering indium tin oxide and a method for manufacturing an indium tin oxide target.
液晶ディスプレイやプラズマディスプレイ等のフラットパネルディスプレイにおいては、電極として酸化インジウムスズ（以下、「ＩＴＯ」という）膜たる透明導電膜が用いられている。ＩＴＯ膜の成膜には、量産性等を考慮してスパッタリング装置が広く利用され、この種のスパッタリング装置としては、インジウムスズからなるターゲットを用い、酸素ガスを導入した反応性スパッタリングによりＩＴＯ膜を成膜するものやＩＴＯ製のターゲットを用い、当該ターゲットに高周波電力を投入してＩＴＯ膜を成膜するものがある。 In flat panel displays such as liquid crystal displays and plasma displays, a transparent conductive film as an indium tin oxide (hereinafter referred to as “ITO”) film is used as an electrode. In order to form an ITO film, a sputtering apparatus is widely used in consideration of mass productivity and the like. As this type of sputtering apparatus, an ITO film is formed by reactive sputtering using a target made of indium tin and introducing oxygen gas. There are those that form a film and those that use a target made of ITO and deposit an ITO film by applying high-frequency power to the target.
ここで、スパッタリング装置による成膜方法は収率が低いことが一般に知られている。他方、上記ターゲットに含まれるインジウムは、資源的に乏しい希少金属である。このため、インジウムを有効利用して製造コストの低下を図る等のためには、ターゲットライフまで使用した使用済みのターゲットを回収して再利用するだけでなく、成膜時、真空チャンバに設置したシールドやアノード部材等のスパッタリング装置の構成部品に付着、堆積したものまで回収して再利用する必要があるが、使用済みのターゲットや構成部品から回収したもの（以下、これらを「ＩＴＯスクラップ」という）には、アルミニウムや鉄といった不純物が含まれている。ＩＴＯ製のターゲットに不純物が含まれていると、成膜したＩＴＯ膜の抵抗値が高くなり、フラットパネルディスプレイの電極として利用できない場合が生じる。 Here, it is generally known that a film forming method using a sputtering apparatus has a low yield. On the other hand, indium contained in the target is a rare metal with scarce resources. For this reason, in order to effectively reduce the manufacturing cost by effectively using indium, the used target used up to the target life is not only collected and reused but also placed in a vacuum chamber during film formation. It is necessary to collect and reuse even the deposits and deposits on the components of the sputtering equipment such as the shield and anode member, but those collected from the used targets and components (hereinafter referred to as “ITO scrap”) ) Contains impurities such as aluminum and iron. When impurities are contained in the ITO target, the resistance value of the deposited ITO film becomes high, and there are cases where it cannot be used as an electrode of a flat panel display.
従来、ＩＴＯスクラップから高純度でインジウムを回収する方法は例えば特許文献１で知られている。このものでは、先ず、ＩＴＯスクラップを塩酸に溶解させ、溶解した溶解液のｐＨが０．５〜４になるようにアルカリ溶液を添加して中和する。これにより、スズのみが水酸化スズとして沈殿する。次に、水酸化スズを除去した後、硫化水素ガスを吹き込んで銅や亜鉛を硫化銅や硫化亜鉛として析出させる。最後に、硫化銅及び硫化亜鉛を除去し、電気分解することでインジウムが回収される。然し、上記従来例のものでは、インジウムとスズとを分離回収するため、ＩＴＯスクラップから高純度のＩＴＯターゲットを再生する上で効率のよいものではなかった。つまり、一旦分離回収したインジウムとスズとを夫々酸化させて酸化インジウム及び酸化スズとし、これら酸化インジウム及び酸化スズを混錬し、混錬により得られた混錬物を成形し、成形したものを焼成するといった多くの工程が必要となり、ターゲット再生の生産性も悪い。 Conventionally, a method for recovering indium with high purity from ITO scrap is known, for example, in Patent Document 1. In this method, first, ITO scrap is dissolved in hydrochloric acid, and neutralized by adding an alkaline solution so that the pH of the dissolved solution becomes 0.5-4. Thereby, only tin precipitates as tin hydroxide. Next, after removing the tin hydroxide, hydrogen sulfide gas is blown to precipitate copper or zinc as copper sulfide or zinc sulfide. Finally, copper sulfide and zinc sulfide are removed and electrolysis is performed to recover indium. However, in the above conventional example, indium and tin are separated and recovered, it is not efficient in reproducing a high-purity ITO target from ITO scrap. In other words, indium and tin once separated and recovered are oxidized into indium oxide and tin oxide, these indium oxide and tin oxide are kneaded, a kneaded product obtained by kneading is molded, and a molded product is obtained. Many processes such as firing are required, and the productivity of target regeneration is also poor.
本発明は、以上の点に鑑み、ＩＴＯスクラップから高純度のＩＴＯとして回収することができる酸化インジウムスズの回収方法及びターゲット再生の生産性のよい酸化インジウムスズターゲットの製造方法を提供することをその課題とする。 In view of the above points, the present invention provides a method for recovering indium tin oxide that can be recovered from ITO scrap as high-purity ITO and a method for manufacturing an indium tin oxide target with good target regeneration productivity. Let it be an issue.
上記課題を解決するために、本発明のＩＴＯの回収方法は、酸化インジウムスズ含有のスクラップを酸に溶解させて所定の溶解液を得る第１工程と、この溶解液にアルカリ溶液を添加して中和し、インジウムスズの水酸化物を含むスラリー液を得る第２工程と、スラリー液を水熱反応させて酸化インジウムスズを含む水和物を析出させる第３工程と、前記水和物を所定温度で乾燥する第４工程と、を含むことを特徴とする。 In order to solve the above problems, the ITO recovery method of the present invention includes a first step of dissolving a scrap containing indium tin oxide in an acid to obtain a predetermined solution, and adding an alkaline solution to the solution. A second step of neutralizing and obtaining a slurry liquid containing a hydroxide of indium tin, a third step of hydrothermally reacting the slurry liquid to precipitate a hydrate containing indium tin oxide, and the hydrate. And a fourth step of drying at a predetermined temperature.
本発明によれば、第１工程にてＩＴＯスクラップを溶解し、第２工程にて溶解した溶解液にアルカリ溶液を添加して中和させた後、第３工程にてインジウムスズの水酸化物を含むスラリー液を水熱反応させる。これにより、スラリー液中にインジウムやスズ以外の不純物が溶解した状態となり、ＩＴＯの水和物が析出する。このため、析出したＩＴＯの水和物は高純度となる。そして、第４工程にて水和物を所定温度で乾燥すれば、高純度のＩＴＯが回収される。 According to the present invention, ITO scrap is dissolved in the first step, neutralized by adding an alkaline solution to the solution dissolved in the second step, and then indium tin hydroxide in the third step. The slurry liquid containing is hydrothermally reacted. Thereby, impurities other than indium and tin are dissolved in the slurry liquid, and ITO hydrate is precipitated. For this reason, the deposited ITO hydrate has high purity. And if a hydrate is dried at predetermined temperature in a 4th process, highly purified ITO will be collect | recovered.
このように本発明は、ＩＴＯスクラップから高純度でＩＴＯを直接回収でき、しかも、この回収したＩＴＯからＩＴＯターゲットを再生する場合、インジウムとスズとを分離回収してＩＴＯターゲットを再生する上記従来例と比較して、少ない工程数でＩＴＯターゲットを再生できるため、ターゲット再生の生産性がよく、製造コストの低下を図ることができる。 As described above, the present invention can recover ITO directly from ITO scrap with high purity, and when reproducing the ITO target from the collected ITO, the above-described conventional example in which indium and tin are separated and recovered to regenerate the ITO target. Since the ITO target can be regenerated with a small number of steps, the productivity of target regeneration is good, and the manufacturing cost can be reduced.
本発明において、ＩＴＯを高い回収率で回収するために、スラリー液をｐＨ５〜６の範囲内に調整することが望ましい。ｐＨ５未満では、析出反応が不十分となるためＩＴＯの回収率が低くなり（５０％未満）、他方、ｐＨ６を超えると、水熱反応中にスラリー液に不純物が溶解し難くなり、回収したＩＴＯ中の不純物濃度が高くなる。 In this invention, in order to collect | recover ITO with a high collection | recovery rate, it is desirable to adjust a slurry liquid in the range of pH 5-6. If the pH is less than 5, the precipitation reaction becomes insufficient, so that the ITO recovery rate is low (less than 50%). On the other hand, if the pH exceeds 6, impurities are hardly dissolved in the slurry during the hydrothermal reaction, and the recovered ITO is recovered. Impurity concentration inside increases.
本発明において、水熱反応の反応温度を５０℃〜２４０℃の範囲内に設定することが望ましい。これにより、スラリー液中にインジウムやスズ以外の不純物が溶解した状態でＩＴＯの水和物が確実に析出させることができる。反応温度が５０℃未満では、析出速度が過剰に遅くなるという不具合があり、２４０℃を超えると、容器が溶け出し（腐食し）コンタミの原因となるという不具合がある。 In the present invention, it is desirable to set the reaction temperature of the hydrothermal reaction within the range of 50 ° C to 240 ° C. Thereby, ITO hydrate can be reliably deposited in a state where impurities other than indium and tin are dissolved in the slurry liquid. When the reaction temperature is less than 50 ° C., there is a problem that the deposition rate is excessively slow, and when it exceeds 240 ° C., there is a problem that the container is melted (corroded) and causes contamination.
ところで、ＩＴＯスクラップが、例えば一般のスパッタリング装置で用いられるアルミナ製の防着板から回収したものである場合、このＩＴＯスクラップには、アルミやアルミの酸化物が不純物として多く含まれていることが多い。このような場合には、第１工程に先立ち、当該ＩＴＯスクラップをアルカリ溶液に溶解させる工程を更に含むことが望ましい。ＩＴＯスクラップに含まれるアルミニウムを事前に除去しておくことで、水熱反応における不純物除去効果を高く維持することができ、回収されるＩＴＯの純度を一層高めることができる。 By the way, when the ITO scrap is recovered from, for example, an alumina deposition plate used in a general sputtering apparatus, the ITO scrap may contain a large amount of aluminum or aluminum oxide as impurities. Many. In such a case, it is desirable to further include a step of dissolving the ITO scrap in an alkaline solution prior to the first step. By removing the aluminum contained in the ITO scrap in advance, the effect of removing impurities in the hydrothermal reaction can be maintained high, and the purity of the recovered ITO can be further increased.
また、本発明のＩＴＯターゲットの製造方法は、請求項１乃至４の何れか１項記載のＩＴＯの回収方法により得られたＩＴＯの水和物を乾燥し焼成してＩＴＯターゲットを製造することを特徴とする。これによれば、ＩＴＯの水和物を乾燥及び焼成するという簡単な工程により、ＩＴＯターゲットを製造できる。 Moreover, the manufacturing method of the ITO target of this invention is manufacturing the ITO target by drying and baking the ITO hydrate obtained by the ITO collection | recovery method of any one of Claims 1 thru | or 4. Features. According to this, an ITO target can be manufactured by a simple process of drying and baking ITO hydrate.
以下、図面を参照して、使用済みのＩＴＯターゲットを粉砕してＩＴＯスクラップを作製し、このＩＴＯスクラップからＩＴＯを回収する場合を例に、本発明の実施形態のＩＴＯの回収方法及び酸化インジウムスズターゲットの製造方法を説明する。ＩＴＯターゲットの粉砕方法としては、ロールミルやクラッシャー等が挙げられる。このとき、ＩＴＯスクラップは粉砕されていればよく、粉砕後の平均粒径は特に限定されない。 Hereinafter, with reference to the drawings, an ITO recovery method and indium tin oxide according to an embodiment of the present invention will be described by taking as an example a case where ITO scrap is produced by pulverizing a used ITO target and ITO is recovered from this ITO scrap. A method for manufacturing the target will be described. Examples of the method for pulverizing the ITO target include a roll mill and a crusher. At this time, the ITO scrap should just be grind | pulverized and the average particle diameter after a grinding | pulverization is not specifically limited.
第１工程では、上記ＩＴＯスクラップが酸に溶解される。酸としては、ＩＴＯスクラップを溶解し得るものであれば特に限定はなく、例えば、塩酸、硫酸及び硝酸を用いることができ、特に、ＩＴＯに対する溶解能の高い塩酸を用いることが好ましい。 In the first step, the ITO scrap is dissolved in acid. The acid is not particularly limited as long as it can dissolve the ITO scrap. For example, hydrochloric acid, sulfuric acid and nitric acid can be used, and hydrochloric acid having a high dissolving ability for ITO is particularly preferable.
第２工程では、上記溶解液にアルカリ溶液を添加して中和し、インジウムスズの水酸化物（水酸化インジウム及び水酸化スズ）を含むスラリー液を得る。アルカリ溶液としては、例えば２５％水酸化ナトリウム溶液を用いることができる。この場合、スラリー液の濃度は、１０〜５００ｇ／ｌの範囲内であることが望ましい。１０ｇ／ｌ未満では、回収されるＩＴＯの量が少なく生産効率が悪く、他方、５００ｇ／ｌを超えると、粘度が高くなり過ぎて流動性がなくなるため、作業性が悪くなるという不具合がある。 In the second step, an alkaline solution is added to the solution and neutralized to obtain a slurry containing indium tin hydroxide (indium hydroxide and tin hydroxide). As the alkaline solution, for example, a 25% sodium hydroxide solution can be used. In this case, the concentration of the slurry liquid is desirably in the range of 10 to 500 g / l. If it is less than 10 g / l, the amount of recovered ITO is small and the production efficiency is poor. On the other hand, if it exceeds 500 g / l, the viscosity becomes too high and the fluidity is lost.
次に、ｐＨ調整工程として、上記スラリー液にアルカリ溶液が更に添加され、ｐＨが５〜６の範囲内に調整される。添加するアルカリ溶液としては、例えば２５％水酸化ナトリウム溶液を用いることができる。ｐＨ５未満では、析出反応が不十分となり、ＩＴＯの回収率が５０未満になってしまう。ｐＨ６を超えると、後述する水熱反応時にスラリー液中に不純物が溶解し難くなり、回収されるＩＴＯに含まれる不純物の濃度が高くなる。 Next, as a pH adjustment step, an alkaline solution is further added to the slurry solution, and the pH is adjusted within the range of 5-6. As the alkaline solution to be added, for example, a 25% sodium hydroxide solution can be used. If the pH is less than 5, the precipitation reaction becomes insufficient and the ITO recovery rate becomes less than 50. When the pH exceeds 6, impurities hardly dissolve in the slurry during a hydrothermal reaction described later, and the concentration of impurities contained in the recovered ITO increases.
第３工程では、上記各工程を経たスラリー液が水熱反応される。水熱反応には次の水熱反応装置が用いられる。即ち、水熱反応装置としては、スラリー液を注入する内筒とステンレス製の外筒とからなる公知のオートクレーブ（「密閉式溶解るつぼ」ともいう）と、このオートクレーブを収容して加熱する恒温槽とで構成されるものが用いられる。 In a 3rd process, the slurry liquid which passed through each said process is hydrothermally reacted. The following hydrothermal reactor is used for the hydrothermal reaction. That is, as a hydrothermal reactor, a known autoclave (also referred to as “sealing type melting crucible”) composed of an inner cylinder for injecting slurry and an outer cylinder made of stainless steel, and a thermostatic chamber for containing and heating the autoclave What is comprised is used.
上記水熱反応装置にて水熱反応させる場合、先ず、るつぼ内に上記スラリー液を注入し、るつぼを恒温槽の所定位置に設置する。そして、恒温槽によりるつぼを所定温度に加熱する。これにより、スラリー液中に不純物が溶解した状態で、ＩＴＯの水和物が析出する。このため、析出したＩＴＯの水和物は高純度となる。水熱反応の反応温度は、５０℃〜２４０℃に調整することが望ましい。このとき、るつぼ内の圧力は、１２３．３９ｈＰａ〜３６０７８．９８ｈＰａとなる。５０℃未満では、ＩＴＯの水和物が析出しないか、析出しても水和物の量が少ない。他方、２４０℃を超えると、ＡｌやＦｅの析出が始まり、不純物の除去性能が低下する。水熱反応の反応時間は、反応温度に応じて、例えば２ｍｉｎ〜４ｈの範囲内で設定できる。 When hydrothermal reaction is performed in the hydrothermal reactor, first, the slurry liquid is poured into a crucible, and the crucible is installed at a predetermined position in a thermostatic bath. And a crucible is heated to predetermined temperature with a thermostat. Thereby, ITO hydrate precipitates in a state where impurities are dissolved in the slurry liquid. For this reason, the deposited ITO hydrate has high purity. The reaction temperature of the hydrothermal reaction is desirably adjusted to 50 ° C to 240 ° C. At this time, the pressure in the crucible is 123.39 hPa to 36078.98 hPa. Below 50 ° C., ITO hydrate does not precipitate or even if it precipitates, the amount of hydrate is small. On the other hand, when it exceeds 240 ° C., precipitation of Al and Fe starts, and the performance of removing impurities deteriorates. The reaction time of the hydrothermal reaction can be set within a range of 2 min to 4 h, for example, depending on the reaction temperature.
水熱反応後の液を濾別した後、第４工程では、ＩＴＯの水和物を洗浄し、乾燥することで、粒径が０．１〜２μｍ（ＳＥＭ観察結果による）の一次粒子が凝集した二次粒子の状態で平均粒径が１〜５μｍの範囲内のＩＴＯの粉末が回収される。水和物の洗浄液としては、主に水が用いられる。また、乾燥温度は、例えば９０℃に設定できる。 After the liquid after the hydrothermal reaction is filtered off, in the fourth step, the ITO hydrate is washed and dried, thereby agglomerating primary particles of 0.1 to 2 μm (according to SEM observation results). ITO powder having an average particle size in the range of 1 to 5 μm is recovered in the state of the secondary particles. As the hydrate cleaning liquid, water is mainly used. The drying temperature can be set at 90 ° C., for example.
上記にて回収されたＩＴＯからＩＴＯターゲットを再生する場合、公知の構造の成形機を用いて所定形状に成形した後、成形されたものを所定の条件下で焼成することで、ＩＴＯターゲットが製造（再生）される。焼成条件としては、例えば、大気中で、焼成温度を５００℃、焼成時間を１ｈに設定すればよい。 When regenerating an ITO target from the ITO collected as described above, an ITO target is manufactured by forming the product into a predetermined shape using a molding machine having a known structure and then firing the molded product under predetermined conditions. (Replayed). As firing conditions, for example, the firing temperature may be set to 500 ° C. and the firing time may be set to 1 h in the air.
以上によれば、ＩＴＯスクラップを塩酸に溶解し、溶解した溶解液に水酸化ナトリウム溶液を添加して中和させた後、中和により得られたインジウムスズの水酸化物を含むスラリー液を水熱反応させる。このとき、スラリー液中にインジウムやスズ以外の不純物が溶解した状態で、ＩＴＯの水和物が析出する。このため、析出したＩＴＯの水和物は高純度のものとなる。そして、このＩＴＯの水和物を所定温度で乾燥すれば、高純度のＩＴＯの粉末が回収される。従って、ＩＴＯスクラップから高純度でＩＴＯを直接回収できる。しかも、水熱反応前に先立ち、スラリー液をｐＨ５〜６の範囲内に調整することでＩＴＯの回収率を５０％以上にすることができる。 According to the above, after dissolving ITO scrap in hydrochloric acid and adding the sodium hydroxide solution to the dissolved solution to neutralize it, the slurry solution containing indium tin hydroxide obtained by neutralization is washed with water. Heat reaction. At this time, ITO hydrate precipitates in a state where impurities other than indium and tin are dissolved in the slurry. For this reason, the deposited ITO hydrate has a high purity. And if this ITO hydrate is dried at a predetermined temperature, highly pure ITO powder is recovered. Therefore, ITO can be directly recovered from ITO scrap with high purity. In addition, prior to the hydrothermal reaction, the recovery rate of ITO can be increased to 50% or more by adjusting the slurry liquid within the range of pH 5-6.
これにより、回収したＩＴＯからＩＴＯターゲットを再生すれば、インジウムとスズとを分離回収してＩＴＯターゲットを製造する従来方法に比べて、少ない工程数でＩＴＯターゲットを再生できるため、ターゲット再生の生産性がよく、製造コストの低下を図ることができる。 As a result, if the ITO target is regenerated from the recovered ITO, the ITO target can be regenerated with a smaller number of steps than the conventional method of producing an ITO target by separating and recovering indium and tin. The manufacturing cost can be reduced.
以上、本発明の実施形態について説明したが、本発明は上記実施形態に限定されるものではない。上記実施形態では、アルカリ溶液として水酸化ナトリウム溶液を用いる場合について説明したが、水酸化ナトリウム溶液以外のアルカリ溶液を用いる場合でもＩＴＯスクラップから高純度のＩＴＯを回収できることを確認した。 As mentioned above, although embodiment of this invention was described, this invention is not limited to the said embodiment. Although the case where a sodium hydroxide solution is used as the alkaline solution has been described in the above embodiment, it has been confirmed that high-purity ITO can be recovered from the ITO scrap even when an alkaline solution other than the sodium hydroxide solution is used.
また、上記実施形態では、ＩＴＯスクラップをＩＴＯターゲットを粉砕したものとしたが、スパッタリング装置の構成部品たる防着板から剥離回収したものとできる。図２を参照して、本発明の他の実施形態について、防着板から剥離回収したＩＴＯスクラップからＩＴＯを回収する場合を例に説明する。 Moreover, in the said embodiment, although the ITO scrap was what grind | pulverized the ITO target, it can be made to peel and collect from the adhesion prevention board which is a component of a sputtering device. With reference to FIG. 2, another embodiment of the present invention will be described by taking as an example the case of recovering ITO from the ITO scrap peeled and recovered from the deposition preventing plate.
防着板から剥離したＩＴＯスクラップは一般にアルミニウムを含む。そこで、本実施形態では、上記第１工程に先立ち、アルカリ溶解工程を行う。アルカリ溶解工程では、ＩＴＯスクラップをアルカリ溶液に溶解させ、ＩＴＯスクラップに含まれるアルミニウムを溶解除去する。アルカリ溶液としては、例えば２５％水酸化ナトリウム溶液を用いることができる。なお、アルカリ溶解工程以外の工程については、上記実施形態と同じであるため、その説明を省略する。 The ITO scrap peeled off from the deposition plate generally contains aluminum. Therefore, in the present embodiment, an alkali dissolution step is performed prior to the first step. In the alkali melting step, the ITO scrap is dissolved in an alkaline solution, and aluminum contained in the ITO scrap is dissolved and removed. As the alkaline solution, for example, a 25% sodium hydroxide solution can be used. In addition, about processes other than an alkali dissolution process, since it is the same as the said embodiment, the description is abbreviate | omitted.
本実施形態によれば、ＩＴＯスクラップに含まれるアルミニウムを事前に除去しておくことで、水熱反応中にスラリー液に溶解するアルミニウムの量が減少するため、水熱反応における不純物除去効果を高く維持することができ、回収されるＩＴＯの純度を一層高めることができる。 According to this embodiment, by removing aluminum contained in the ITO scrap in advance, the amount of aluminum dissolved in the slurry liquid during the hydrothermal reaction is reduced, so the effect of removing impurities in the hydrothermal reaction is increased. The purity of the collected ITO can be further increased.
実施例１では、Ｉｎ及びＳｎ並びに不純物であるＡｌ及びＦｅを塩酸に溶解し、この溶解したものにその他の不純物を含む原子吸光分析用標準溶液を混合し、混合により得られたものを標準試料とした。この標準試料たる溶解液のＩＣＰ発光分析を行なったところ、上記標準試料に含まれるIn-Snの濃度は94.15%（In:82.67%、Sn:11.48%）であり、In-Sn以外の不純物濃度は、Al:4.51%、Ca:0.1703%、Cu:0.0815%、Fe:0.7693%、Ni:0.0700%、Pb:0.0628%、Si:0.0846%、Zr:0.0961%であった。この溶解液に２５％の水酸化ナトリウム溶液を添加して中和し、水酸化インジウム及び水酸化スズを含むスラリー液を得て、得られたスラリー液に２５％水酸化ナトリウム溶液を更に添加してｐＨを５．０２に調整した。なお、スラリー液の濃度は、１００ｇ／ｌであった。そして、ｐＨ調整後のスラリー液をオーエムラボテック社製の密閉式溶解るつぼに収容し、このるつぼを恒温槽に入れてスラリー液を水熱反応させ、ＩＴＯの水和物を析出させた。ここで、水熱反応の温度を５０℃、２２０℃、２３０℃、２４０℃に設定し、反応時間を２分、５分、３時間、４時間、２４時間に設定した。析出した水和物を濾別し、水洗し、９０℃の温度で乾燥させて粉末（試料＃１〜＃１６）を得た。この粉末を５００℃の温度で焼成し、この焼成したもののＸ線回折分析を行ったところ、ＩＴＯであることが確認された。得られた粉末状のＩＴＯを塩酸に溶解させ、その溶解液のＩＣＰ発光分析を行った結果を図３に示す。これによれば、In-Sn濃度が高い高純度のＩＴＯ（試料＃１〜＃１６）が回収されたことが確認された。特に、水熱反応の温度を５０℃〜２２０℃に設定し、反応時間を５分〜３時間に設定した場合に、In-Sn濃度を９７％以上に高めることができることが確認された（試料＃２、３、７、８）。また、反応温度を２３０℃〜２４０℃に設定し、反応時間を５分〜１時間に設定した場合も、In-Sn濃度を９７％以上に高めることができることが確認された（試料＃１０、１１、１４、１５）。 In Example 1, In and Sn and impurities, Al and Fe, are dissolved in hydrochloric acid, and a standard solution for atomic absorption analysis containing other impurities is mixed with the dissolved one, and a sample obtained by mixing is used as a standard sample. It was. When ICP emission analysis was performed on the lysate as the standard sample, the concentration of In-Sn contained in the standard sample was 94.15% (In: 82.67%, Sn: 11.48%). Concentration of impurities other than In-Sn Al: 4.51%, Ca: 0.1703%, Cu: 0.0815%, Fe: 0.7693%, Ni: 0.0700%, Pb: 0.0628%, Si: 0.0846%, Zr: 0.0961%. A 25% sodium hydroxide solution is added to the solution to neutralize it to obtain a slurry solution containing indium hydroxide and tin hydroxide, and a 25% sodium hydroxide solution is further added to the resulting slurry solution. The pH was adjusted to 5.02. The concentration of the slurry liquid was 100 g / l. Then, the slurry liquid after pH adjustment was accommodated in a closed melting crucible manufactured by OM Lab Tech Co., Ltd., and the crucible was placed in a thermostatic bath to cause hydrothermal reaction of the slurry liquid, thereby precipitating ITO hydrate. Here, the temperature of the hydrothermal reaction was set to 50 ° C., 220 ° C., 230 ° C., and 240 ° C., and the reaction time was set to 2 minutes, 5 minutes, 3 hours, 4 hours, and 24 hours. The precipitated hydrate was separated by filtration, washed with water, and dried at a temperature of 90 ° C. to obtain powders (samples # 1 to # 16). This powder was baked at a temperature of 500 ° C., and X-ray diffraction analysis of the baked product was confirmed to be ITO. The obtained powdered ITO was dissolved in hydrochloric acid, and the result of ICP emission analysis of the solution is shown in FIG. According to this, it was confirmed that high-purity ITO (samples # 1 to # 16) having a high In-Sn concentration was recovered. In particular, it was confirmed that the In-Sn concentration can be increased to 97% or more when the temperature of the hydrothermal reaction is set to 50 ° C. to 220 ° C. and the reaction time is set to 5 minutes to 3 hours (sample). # 2, 3, 7, 8). It was also confirmed that the In-Sn concentration could be increased to 97% or higher when the reaction temperature was set to 230 ° C to 240 ° C and the reaction time was set to 5 minutes to 1 hour (sample # 10, 11, 14, 15).
実施例２では、スラリー液のｐＨを５．８９に調整した以外は、実施例１と同様の方法とした。本実施例にて析出させたＩＴＯの水和物を濾別し、水洗し、９０℃で乾燥させてＩＴＯの粉末（試料＃２１〜＃３６）を回収した。回収したＩＴＯを塩酸に溶解させ、その溶解液のＩＣＰ発光分析を行った結果を図４に示す。これによれば、上記実施例１の結果と同様に、In-Sn濃度が高い高純度のＩＴＯ（試料＃２１〜＃３６）が回収されたことが確認された。上記実施例１と同様に、水熱反応の温度を５０℃〜２２０℃に設定し、反応時間を５分〜３時間に設定した場合に、In-Sn濃度を９７％以上に高めることができることが確認された（試料＃２２、２３、２７、２８）。また、反応温度を２３０℃〜２４０℃に設定し、反応時間を５分〜１時間に設定した場合も、In-Sn濃度を９７％以上に高めることができることが確認された（試料＃３０、３１、３４、３５）。 In Example 2, the method was the same as Example 1 except that the pH of the slurry was adjusted to 5.89. The ITO hydrate precipitated in this example was filtered off, washed with water, and dried at 90 ° C. to recover ITO powder (samples # 21 to # 36). The collected ITO was dissolved in hydrochloric acid, and the result of ICP emission analysis of the dissolved solution is shown in FIG. According to this, it was confirmed that high-purity ITO (samples # 21 to # 36) having a high In-Sn concentration was recovered, similar to the result of Example 1 above. As in Example 1 above, the In-Sn concentration can be increased to 97% or more when the temperature of the hydrothermal reaction is set to 50 ° C. to 220 ° C. and the reaction time is set to 5 minutes to 3 hours. Was confirmed (Samples # 22, 23, 27, and 28). Further, it was confirmed that the In-Sn concentration could be increased to 97% or more when the reaction temperature was set to 230 ° C. to 240 ° C. and the reaction time was set to 5 minutes to 1 hour (sample # 30, 31, 34, 35).
実施例３では、スラリー液のｐＨを６．５０又は４．５に調整した以外は、実施例１と同様の方法とした。本実施例にて析出させたＩＴＯの水和物を濾別し、水洗し、９０℃で乾燥させてＩＴＯの粉末（試料＃４１〜＃４４）を回収した。回収したＩＴＯを塩酸に溶解させ、その溶解液のＩＣＰ発光分析を行った結果を図５に示す。これによれば、スラリー液のｐＨを６．５０に調整した場合には、In-Sn濃度が低くなり、高純度のＩＴＯを回収できないことが確認された（試料＃４１、４２）。また、ｐＨを４．５に調整した場合には、ＩＴＯの回収率が４０％以下と低くなることが確認された（試料＃４３、４４）。 In Example 3, the method was the same as Example 1 except that the pH of the slurry was adjusted to 6.50 or 4.5. The ITO hydrate precipitated in this example was filtered off, washed with water, and dried at 90 ° C. to recover ITO powder (samples # 41 to # 44). The collected ITO was dissolved in hydrochloric acid, and the result of ICP emission analysis of the dissolved solution is shown in FIG. According to this, when the pH of the slurry was adjusted to 6.50, it was confirmed that the In-Sn concentration was low and high-purity ITO could not be recovered (samples # 41 and 42). Further, when the pH was adjusted to 4.5, it was confirmed that the ITO recovery rate was as low as 40% or less (samples # 43 and 44).
実施例４では、スラリー液の濃度を１０ｇ／ｌ又は５００ｇ／ｌに調整した以外は、実施例１と同様の方法とした。本実施例にて析出させたＩＴＯの水和物を濾別し、水洗し、９０℃で乾燥させてＩＴＯの粉末（試料＃５１〜＃５８）を回収した。回収したＩＴＯを塩酸に溶解させ、その溶解液のＩＣＰ発光分析を行った結果を図６に示す。これによれば、スラリー液の濃度を１０ｇ／ｌ〜５００ｇ／ｌの範囲内に調整すれば、In-Sn濃度を９７％以上に高めることができることが確認された（試料＃５１〜＃５８）。 In Example 4, the method was the same as Example 1 except that the concentration of the slurry liquid was adjusted to 10 g / l or 500 g / l. The ITO hydrate precipitated in this example was filtered off, washed with water, and dried at 90 ° C. to recover ITO powder (samples # 51 to # 58). The collected ITO was dissolved in hydrochloric acid, and the result of ICP emission analysis of the dissolved solution is shown in FIG. According to this, it was confirmed that the In-Sn concentration can be increased to 97% or more by adjusting the concentration of the slurry liquid within the range of 10 g / l to 500 g / l (Samples # 51 to # 58). .
実施例５では、防着板から剥離回収したＩＴＯスクラップを用意した。このＩＴＯスクラップに含まれるIn-Snの濃度は72.71%（In:65.7%、Sn:7.01%）であり、In-Sn以外の不純物濃度は、Al:4.82%、Ca:0.001%、Cu:0.002%、Fe:0.023%、Ni:0.002%、Pb:0.005%、Si:0.05%、Zr:0.02%であった。このＩＴＯスクラップを２５％水酸化ナトリウム溶液に１時間溶解させ、ＩＴＯスクラップに含まれるアルミニウムを溶解除去した。その結果、図７に示すように、Ａｌ濃度が0.028%に低減されたことが確認された。次いで、ＩＴＯスクラップを塩酸に溶解し、溶解により得られた溶解液に２５％水酸化ナトリウム溶液を添加して中和し、水酸化インジウム及び水酸化スズを含むスラリー液を得て、得られたスラリー液に２５％水酸化ナトリウム溶液を更に添加してｐＨを５．３９に調整した。そして、ｐＨ調整後のスラリー液を水熱反応させ、ＩＴＯの水和物を析出させた。水熱反応の温度は２２０℃、反応時間は１ｈに設定した。析出させたＩＴＯの水和物を濾別し、水洗し、９０℃の温度で乾燥させてＩＴＯ粉末を回収した。回収したＩＴＯ粉末を塩酸に溶解させ、その溶解液のＩＣＰ発光分析を行った結果を図７に示す。これによれば、In-Sn濃度が９９．９０％と高い高純度のＩＴＯが回収されたことが確認された。 In Example 5, ITO scraps peeled and collected from the deposition preventive plate were prepared. The concentration of In-Sn contained in this ITO scrap is 72.71% (In: 65.7%, Sn: 7.01%). The impurity concentration other than In-Sn is Al: 4.82%, Ca: 0.001%, Cu: 0.002. %, Fe: 0.023%, Ni: 0.002%, Pb: 0.005%, Si: 0.05%, Zr: 0.02%. This ITO scrap was dissolved in a 25% sodium hydroxide solution for 1 hour to dissolve and remove aluminum contained in the ITO scrap. As a result, as shown in FIG. 7, it was confirmed that the Al concentration was reduced to 0.028%. Next, the ITO scrap was dissolved in hydrochloric acid, and a 25% sodium hydroxide solution was added to the solution obtained by dissolution to neutralize the slurry, thereby obtaining a slurry solution containing indium hydroxide and tin hydroxide. A 25% sodium hydroxide solution was further added to the slurry to adjust the pH to 5.39. And the slurry liquid after pH adjustment was made to react hydrothermally, and the hydrate of ITO was deposited. The temperature of the hydrothermal reaction was set to 220 ° C., and the reaction time was set to 1 h. The deposited ITO hydrate was separated by filtration, washed with water, and dried at a temperature of 90 ° C. to recover ITO powder. The collected ITO powder was dissolved in hydrochloric acid, and the result of ICP emission analysis of the dissolved solution is shown in FIG. According to this, it was confirmed that high purity ITO with a high In-Sn concentration of 99.90% was recovered.
Claims (5)
前記溶解液にアルカリ溶液を添加して中和し、インジウムスズの水酸化物を含むスラリー液を得る第２工程と、
前記スラリー液を水熱反応させて酸化インジウムスズを含む水和物を析出させる第３工程と、
前記水和物を所定温度で乾燥する第４工程と、を含むことを特徴とする酸化インジウムスズの回収方法。 A first step of dissolving a scrap containing indium tin oxide in an acid to obtain a predetermined solution;
A second step of neutralizing the solution by adding an alkaline solution to obtain a slurry containing indium tin hydroxide;
A third step of hydrothermally reacting the slurry liquid to precipitate a hydrate containing indium tin oxide;
And a fourth step of drying the hydrate at a predetermined temperature. A method for recovering indium tin oxide, comprising:
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| CN111620367A (en) * | 2020-06-08 | 2020-09-04 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
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| CN113292345A (en) * | 2021-05-28 | 2021-08-24 | 芜湖映日科技股份有限公司 | Preparation process for recycling residual target after ITO target sputtering |
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