JPS63270428A - Treatment for gallium-containing material - Google Patents
Treatment for gallium-containing materialInfo
- Publication number
- JPS63270428A JPS63270428A JP62102749A JP10274987A JPS63270428A JP S63270428 A JPS63270428 A JP S63270428A JP 62102749 A JP62102749 A JP 62102749A JP 10274987 A JP10274987 A JP 10274987A JP S63270428 A JPS63270428 A JP S63270428A
- Authority
- JP
- Japan
- Prior art keywords
- gallium
- hydrochloric acid
- treatment
- metallic impurities
- dissolution
- 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
Links
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 229910052738 indium Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 12
- 238000007158 vacuum pyrolysis Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 150000002259 gallium compounds Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910005540 GaP Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- OEYOHULQRFXULB-UHFFFAOYSA-N arsenic trichloride Chemical compound Cl[As](Cl)Cl OEYOHULQRFXULB-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- HZXMRANICFIONG-UHFFFAOYSA-N gallium phosphide Chemical compound [Ga]#P HZXMRANICFIONG-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔技術分野〕
本発明は、金属ガリウム回収のために真空熱分解処理に
供給される金属不純物を含むガリウム含有物から、それ
に含まれる金属不純物を除去するための処理方法に関す
るものである。[Detailed Description of the Invention] [Technical Field] The present invention relates to a processing method for removing metal impurities contained in a gallium-containing material that is supplied to a vacuum pyrolysis treatment for recovering metal gallium. It is related to.
金属ガリウムは半導体製造原料として用いられる有用な
ものであるが、その資源不足を補うために、ガリウムを
含むスクラップ、不良品、廃棄物等のガリウム含有物を
真空熱分解処理して金属ガリウムを回収することは知ら
れている。Metallic gallium is a useful material used as a raw material for semiconductor manufacturing, but in order to compensate for resource shortages, metallic gallium is recovered by vacuum pyrolysis of gallium-containing materials such as scrap, defective products, and waste. It is known to do.
ところで、このような真空熱分解処理においては、被処
理原料であるガリウム含有物中に含まれる金属不純物は
、生成される金属ガリウム中に含まれるようになり、回
収金属ガリウムの純度を低下させる原因となる。従来、
このようなガリウム含有物中の金属不純物を除去する方
法としては、酸化剤を含む濃塩酸で処理する方法が知ら
れている(特開昭57−101625号公報)、シかし
、この酸化剤を含む塩酸水溶処理の場合、酸化剤の作用
により、砒素やリン等の有害元素を含む廃水が生じる他
に、砒素塩化物やリン塩化物等の有毒ガスが発生するの
で、好ましい方法とはいうことができない。By the way, in such a vacuum pyrolysis treatment, metal impurities contained in the gallium-containing material, which is the raw material to be treated, become contained in the generated metal gallium, which causes a decrease in the purity of the recovered metal gallium. becomes. Conventionally,
As a method for removing such metal impurities in gallium-containing materials, a method of treatment with concentrated hydrochloric acid containing an oxidizing agent is known (Japanese Patent Application Laid-Open No. 101625/1983). In the case of aqueous hydrochloric acid treatment, the action of the oxidizing agent not only generates wastewater containing harmful elements such as arsenic and phosphorus, but also generates toxic gases such as arsenic chloride and phosphorus chloride, so this is not the preferred method. I can't.
本発明は、従来技術に見られる前記欠点の克服されたガ
リウム含有物からの金属不純物の除去方法を提供するこ
とを目的とする。It is an object of the present invention to provide a method for removing metal impurities from a gallium-containing material, which overcomes the above-mentioned drawbacks found in the prior art.
本発明によれば、真空熱分解処理に供給される金属不純
物を含むガリウム含有物を、0.1〜10規定の塩酸又
は硝酸で処理することを特徴とするガリウム含有物の処
理方法が提供される。According to the present invention, there is provided a method for treating a gallium-containing material, which comprises treating a gallium-containing material containing metal impurities to be supplied to vacuum pyrolysis treatment with 0.1 to 10N hydrochloric acid or nitric acid. Ru.
本発明で用いる被処理原料としては、砒化ガリウムやリ
ン化ガリウム等のガリウム化合物を含有する種々のスク
ラップ、不良品、廃棄物、ガリウム化合物を熱分解して
得られた分解残渣物から液体金属ガリウムを分離した後
の残漬物等が挙げられる。この場合、金属不純物として
は、インジウム、アルカリ金属、アルカリ土類金属、ア
ルミニウム、鉄、ニッケル、クロム等が挙げられる。The raw materials to be processed used in the present invention include various scraps, defective products, and waste containing gallium compounds such as gallium arsenide and gallium phosphide, as well as liquid metal gallium from decomposition residue obtained by thermally decomposing gallium compounds. Examples include pickled vegetables left after separating. In this case, examples of metal impurities include indium, alkali metals, alkaline earth metals, aluminum, iron, nickel, and chromium.
本発明においては、被処理原料であるガリウム含有物を
、0.1〜10規定(N)、好ましくは0.5N〜5N
の塩酸又は硝酸あるいはそれらの混合物で処理する。In the present invention, the gallium-containing material, which is the raw material to be treated, is 0.1 to 10 normal (N), preferably 0.5 to 5 N.
of hydrochloric acid or nitric acid or a mixture thereof.
この場合、被処理原料が塊状物や板状物の場合には微粉
末にしてから本発明の処理に付され、また泥状物の場合
には、水性のものではそのまま、油性のものでは公知の
方法によって油分を除去し、必要であれば粉砕した後、
本発明の処理に付される。処理温度は一10〜150℃
、好ましくは0〜100℃である。本発明で用いる塩酸
又は硝酸としては、新しく作られたものの他、金属処理
に用いた廃酸等も用いることができる。In this case, if the raw material to be treated is a lump or plate-like material, it is pulverized and then subjected to the treatment of the present invention, and in the case of a muddy material, an aqueous material is used as it is, while an oil-based material is subjected to the treatment of the present invention. After removing the oil and grinding if necessary,
Subjected to the treatment of the present invention. Processing temperature is -10~150℃
, preferably 0 to 100°C. As the hydrochloric acid or nitric acid used in the present invention, in addition to newly produced ones, waste acids used in metal processing can also be used.
本発明による処理生成物は、濾過、遠心分離。The processed products according to the invention are subjected to filtration, centrifugation.
沈降分離等の固液分離法により、処理されたガリウム含
有物を処理液から分離回収する。このようにして処理さ
れたガリウム含有物は、無機系又は有機系バインダーと
混合し、必要に応じて成形した後、50〜300℃で乾
燥し、300〜1000℃で焼結して真空熱分解処理に
付される。The treated gallium-containing material is separated and recovered from the treated liquid by a solid-liquid separation method such as sedimentation separation. The gallium-containing material treated in this way is mixed with an inorganic or organic binder, shaped as necessary, dried at 50 to 300°C, sintered at 300 to 1000°C, and vacuum pyrolyzed. Submitted for processing.
本発明によれば、ガリウム含有物に含まれる金属不純物
、例えば、鉄、アルミニウム、カルシウム、マグネシウ
ム、インジウム等を溶解除去することができる0本発明
の場合は、酸化剤を用いないことから、砒素やリンの有
害化合物を含む廃液が生じない上、砒素やリンの塩化物
等のガス状有害物も生成しない。According to the present invention, metal impurities contained in gallium-containing materials, such as iron, aluminum, calcium, magnesium, and indium, can be dissolved and removed. In addition to not producing waste liquid containing harmful compounds such as phosphorus and phosphorus, it also does not produce gaseous harmful substances such as arsenic or chloride of phosphorus.
本発明において、0.IN〜1ON、好ましくは0.5
N〜5Nの塩酸を用いる時には、ガリウムと化学的性質
が類似し、ガリウムから分離困難なインジウムを、ガリ
ウムの溶解を抑制して、選択的に溶解除去することがで
きる。In the present invention, 0. IN~1ON, preferably 0.5
When N to 5N hydrochloric acid is used, indium, which has similar chemical properties to gallium and is difficult to separate from gallium, can be selectively dissolved and removed by suppressing the dissolution of gallium.
次に本発明を実施例によりさらに詳細に説明する。 Next, the present invention will be explained in more detail with reference to Examples.
実施例1
砒化ガリウム単結晶のウェハーへの切削工程において生
じたドロスを本法により塩酸洗浄してインジウムおよび
その他の不純物を選択的に除去した。Example 1 Dross generated in the process of cutting a gallium arsenide single crystal into a wafer was washed with hydrochloric acid according to the present method to selectively remove indium and other impurities.
即ち、先ず、ドロスをアセトンを用いて洗浄したのち、
100℃にて乾燥した。このものの不純物金属は以下の
とおりであった。単位はρpm。That is, first, after washing the dross with acetone,
It was dried at 100°C. The impurity metals in this product were as follows. The unit is ρpm.
A Q /75、Ca/32、Cr/ 1 、8、Cu
/4.5. Fe/379、K/9.5、In/630
0、Mg/11 Na/8.0、Si/127. Ni
/1.lS。AQ/75, Ca/32, Cr/1,8, Cu
/4.5. Fe/379, K/9.5, In/630
0, Mg/11 Na/8.0, Si/127. Ni
/1. lS.
次に、上記洗浄乾燥物を0.5規定塩酸水溶液を加え温
度20℃にて120分撹拌後濾紙で濾過し、塩酸による
不純物抽出を行った。濾過残留物はアセトン洗浄後10
0℃にて乾燥した。この乾燥残留物の不純物金属はAQ
、Ca、 K、 Mg、 Na、Niは0.5ppm以
下、Cr 0.8ppm、Fa 144ppm、 Cu
4.ippm、 In 6200ppm、 Si 1
20ppmとなった。この塩酸抽出では原料乾燥物中の
ガリウムの0.2%が溶解抽出されていた。Next, a 0.5N aqueous hydrochloric acid solution was added to the washed and dried product, stirred at a temperature of 20° C. for 120 minutes, and filtered through a filter paper to extract impurities with hydrochloric acid. The filtration residue was washed with acetone.
It was dried at 0°C. The impurity metal in this dry residue is AQ
, Ca, K, Mg, Na, Ni 0.5 ppm or less, Cr 0.8 ppm, Fa 144 ppm, Cu
4. ippm, In 6200ppm, Si 1
It became 20 ppm. In this hydrochloric acid extraction, 0.2% of the gallium in the dry raw material was dissolved and extracted.
また、塩酸抽出液についてのガリウム、インジウムの分
析から各々の抽出率の比、インジウム/ガリウムは0.
62であった。この実験と同一にして塩酸濃度のみを変
えてガリウム、インジウムの抽出率の比およびガリウム
抽出率を求めたところ下記の値が得られた。Furthermore, from the analysis of gallium and indium in the hydrochloric acid extract, the ratio of their respective extraction rates, indium/gallium, was 0.
It was 62. The ratio of the extraction rates of gallium and indium and the extraction rate of gallium were determined by changing only the hydrochloric acid concentration in the same manner as in this experiment, and the following values were obtained.
2.0 0,3 2.3 7.7(倍
)4.0 0.5 69 138(倍
)なお同様の実験を2規定の硝酸水溶液を用いて行った
ところ、ガリウム抽出率が24%、インジウム抽出選択
率0.42が得られた。また、酸の種類、濃度によって
、インジウム以外の不純物金属の溶解度はほとんど変ら
なかった。2.0 0.3 2.3 7.7 (times) 4.0 0.5 69 138 (times) When a similar experiment was conducted using a 2N nitric acid aqueous solution, the gallium extraction rate was 24%, An indium extraction selectivity of 0.42 was obtained. Furthermore, the solubility of impurity metals other than indium hardly changed depending on the type and concentration of acid.
本実施例から明らかなように、0.5規定〜5規定の塩
酸水溶液による抽出によりインジウムの選択抽出が可能
である。As is clear from this example, indium can be selectively extracted by extraction with a 0.5N to 5N hydrochloric acid aqueous solution.
実施例2
上記の4規定塩酸水溶液により抽出処理したドロス粉末
にでんぷんを3%(重量)加え、水を加えて固めたもの
を800℃にて焼結し、1150℃にて真空熱分解して
ガリウムを回収した。Example 2 3% (by weight) of starch was added to the dross powder extracted with the above 4N hydrochloric acid aqueous solution, solidified by adding water, sintered at 800°C, and vacuum pyrolyzed at 1150°C. Collected gallium.
この実験で得られた熱分解残渣物を100メツシユ濾布
にて濾過した残渣を本性により酸処理した。The thermal decomposition residue obtained in this experiment was filtered through a 100-mesh filter cloth, and the residue was acid-treated depending on its nature.
濾過残漬物中の主要不純物金属は以下のとおりであった
。単位p p II *
Cu/ 2、Fe/1600、In/1100%Si/
1100゜この濾過残渣物を20メツシュ以上に微粉砕
したものを実施例1と同様にして4規定塩酸水溶液をも
ちいて抽出したところ、ガリウム抽出率が2.1%、イ
ンジウム抽出率が81%であった。また、抽出残留物中
の不純物金属は次の通りであった。単位ppm。The main impurity metals in the filtered residue were as follows. Unit p p II * Cu/ 2, Fe/1600, In/1100%Si/
1100゜This filtration residue was finely pulverized to 20 meshes or more and extracted using a 4N hydrochloric acid aqueous solution in the same manner as in Example 1. The gallium extraction rate was 2.1% and the indium extraction rate was 81%. there were. Further, the impurity metals in the extracted residue were as follows. Unit: ppm.
Cu/1.4、Fe/190゜Cu/1.4, Fe/190°
Claims (3)
リウム含有物を0.1〜10規定の塩酸又は硝酸で処理
することを特徴とするガリウム含有物の処理方法。(1) A method for treating a gallium-containing material, which comprises treating a gallium-containing material containing metal impurities supplied to vacuum pyrolysis treatment with 0.1 to 10N hydrochloric acid or nitric acid.
渣物から金属ガリウムを分離除去した後の残渣物である
特許請求の範囲第1項の方法。(2) The method according to claim 1, wherein the gallium-containing material is a residue obtained by separating and removing metallic gallium from the thermal decomposition residue of the gallium-containing material.
規定の塩酸で処理する特許請求の範囲第1項の方法。(3) 0.1 to 10 gallium-containing substances including indium
A method according to claim 1, comprising treatment with defined hydrochloric acid.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62102749A JPS63270428A (en) | 1987-04-24 | 1987-04-24 | Treatment for gallium-containing material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62102749A JPS63270428A (en) | 1987-04-24 | 1987-04-24 | Treatment for gallium-containing material |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS63270428A true JPS63270428A (en) | 1988-11-08 |
Family
ID=14335870
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP62102749A Pending JPS63270428A (en) | 1987-04-24 | 1987-04-24 | Treatment for gallium-containing material |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63270428A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009144220A (en) * | 2007-12-17 | 2009-07-02 | Mitsubishi Materials Corp | Method for recovering metal from used solid oxide type fuel cell |
JP2009144219A (en) * | 2007-12-17 | 2009-07-02 | Mitsubishi Materials Corp | Method for recovering metal from used solid oxide type fuel cell |
-
1987
- 1987-04-24 JP JP62102749A patent/JPS63270428A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009144220A (en) * | 2007-12-17 | 2009-07-02 | Mitsubishi Materials Corp | Method for recovering metal from used solid oxide type fuel cell |
JP2009144219A (en) * | 2007-12-17 | 2009-07-02 | Mitsubishi Materials Corp | Method for recovering metal from used solid oxide type fuel cell |
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