JP2014019590A - Method for manufacturing aqueous gallium nitrate solution - Google Patents
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本発明は、硝酸ガリウム水溶液の製造方法に関し、特に、酸化ガリウムの製造などに使用する硝酸ガリウム水溶液の製造方法に関する。 The present invention relates to a method for producing an aqueous gallium nitrate solution, and more particularly to a method for producing an aqueous gallium nitrate solution used for producing gallium oxide.
硝酸ガリウム水溶液は、半導体や発光素子などの製造原料として使用される酸化ガリウムの製造などに使用されている。このような硝酸ガリウム水溶液は、高純度の金属ガリウムを濃硝酸に投入して撹拌しながら溶解させて、加熱することによって得ることができる（例えば、特許文献１参照）。 Gallium nitrate aqueous solution is used for the production of gallium oxide used as a production raw material for semiconductors and light emitting devices. Such an aqueous gallium nitrate solution can be obtained by putting high-purity metallic gallium into concentrated nitric acid, dissolving it with stirring, and heating (for example, see Patent Document 1).
しかし、酸化ガリウム製造用の硝酸ガリウム水溶液を製造するために、高純度（５〜６Ｎ）のガリウムを硝酸で溶解しようとしても、非常に溶け難く、溶解時間が非常に長いという問題がある。 However, in order to produce a gallium nitrate aqueous solution for producing gallium oxide, there is a problem that even if high purity (5-6N) gallium is dissolved in nitric acid, it is very difficult to dissolve and the dissolution time is very long.
したがって、本発明は、このような従来の問題点に鑑み、ガリウムを短時間で硝酸水溶液に溶解させて硝酸ガリウム水溶液を製造することができる、硝酸ガリウム水溶液の製造方法を提供することを目的とする。 Accordingly, the present invention has been made in view of the above-described conventional problems, and an object of the present invention is to provide a method for producing an aqueous gallium nitrate solution that can produce an aqueous gallium nitrate solution by dissolving gallium in an aqueous nitric acid solution in a short time. To do.
本発明者らは、上記課題を解決するために鋭意研究した結果、液体ガリウムを微粒化して硝酸水溶液に溶解させることにより、ガリウムを短時間で硝酸水溶液に溶解させて硝酸ガリウム水溶液を製造することができることを見出し、本発明を完成するに至った。 As a result of diligent research to solve the above problems, the inventors of the present invention have made liquid gallium atomized and dissolved in an aqueous nitric acid solution, thereby dissolving gallium in an aqueous nitric acid solution in a short time to produce an aqueous gallium nitrate solution. As a result, the present invention has been completed.
すなわち、本発明による硝酸ガリウム水溶液の製造方法は、液体ガリウムを微粒化して硝酸水溶液に溶解させて硝酸ガリウム水溶液を製造することを特徴とする。この硝酸ガリウム水溶液の製造方法において、硝酸水溶液を撹拌しながら細管を通して液体ガリウムを硝酸水溶液に添加することにより、あるいは、水を撹拌しながら細管を通して液体ガリウムを水に添加した後に硝酸を添加することにより、液体ガリウムを微粒化して硝酸水溶液に溶解させるのが好ましい。この場合、撹拌が２４０〜１０００ｒｐｍの強撹拌であるのが好ましく、あるいは、撹拌が硝酸水溶液の容積当りの動力を１Ｗ／Ｌ以上として行われるのが好ましく、また、細管が内径０．１〜５ｍｍの１本以上のチューブであるのが好ましい。また、液体ガリウムを硝酸水溶液または水に添加する際に硝酸水溶液または水の温度を６０℃以上に維持するのが好ましい。さらに、液体ガリウムを硝酸水溶液に溶解させる際に硝酸水溶液に過酸化水素を添加するのが好ましい。 That is, the method for producing an aqueous gallium nitrate solution according to the present invention is characterized in that liquid gallium is atomized and dissolved in an aqueous nitric acid solution to produce an aqueous gallium nitrate solution. In this method for producing an aqueous gallium nitrate solution, the liquid gallium is added to the aqueous nitric acid solution through a thin tube while stirring the aqueous nitric acid solution, or the nitric acid is added after adding the liquid gallium to the water through the thin tube while stirring water. Thus, it is preferable to atomize liquid gallium and dissolve it in an aqueous nitric acid solution. In this case, stirring is preferably strong stirring at 240 to 1000 rpm, or stirring is preferably performed with a power per volume of nitric acid aqueous solution of 1 W / L or more, and the narrow tube has an inner diameter of 0.1 to 5 mm. One or more tubes are preferred. In addition, when adding liquid gallium to an aqueous nitric acid solution or water, the temperature of the aqueous nitric acid solution or water is preferably maintained at 60 ° C. or higher. Further, it is preferable to add hydrogen peroxide to the aqueous nitric acid solution when the liquid gallium is dissolved in the aqueous nitric acid solution.
本発明によれば、液体ガリウムを微粒化して硝酸水溶液に溶解させることにより、ガリウムを短時間で硝酸水溶液に溶解させて硝酸ガリウム水溶液を製造することができる。 According to the present invention, liquid gallium is atomized and dissolved in an aqueous nitric acid solution, whereby gallium can be dissolved in an aqueous nitric acid solution in a short time to produce an aqueous gallium nitrate solution.
本発明による硝酸ガリウム水溶液の製造方法の実施の形態では、液体ガリウム（例えば、高純度（５〜６Ｎ）の液体ガリウム）を微粒化して硝酸水溶液に溶解させて硝酸ガリウム水溶液を製造する。 In the embodiment of the method for producing a gallium nitrate aqueous solution according to the present invention, liquid gallium (for example, high purity (5-6N) liquid gallium) is atomized and dissolved in the nitric acid aqueous solution to produce the gallium nitrate aqueous solution.
この硝酸ガリウム水溶液の製造方法の実施の形態では、硝酸水溶液を撹拌しながら細管を通して液体ガリウムを硝酸水溶液に添加することにより、あるいは、水を撹拌しながら細管を通して液体ガリウムを水に添加した後に硝酸を添加することにより、液体ガリウムを微粒化して硝酸水溶液に溶解させるのが好ましい。従来のように、ガリウムの塊をそのまま硝酸水溶液に添加したり、温水に添加した後に硝酸を添加するのではなく、（予め溶解させた）液体ガリウムを（微粒滴状態に）微粒化して硝酸水溶液に溶解させることにより、ガリウム粒子の表面積を増大して硝酸水溶液への溶解速度を向上させる。 In the embodiment of the method for producing an aqueous gallium nitrate solution, the liquid gallium is added to the aqueous nitric acid solution through the capillary while stirring the aqueous nitric acid solution, or after adding the liquid gallium to the water through the capillary tube while stirring the water. It is preferable that liquid gallium is atomized and dissolved in an aqueous nitric acid solution. Instead of adding the gallium lump directly to the aqueous nitric acid solution or adding the nitric acid after adding it to the warm water as in the past, the liquid gallium (preliminarily dissolved) is atomized (in the form of fine droplets) and the aqueous nitric acid solution To increase the surface area of the gallium particles and improve the dissolution rate in the aqueous nitric acid solution.
液体ガリウムを微粒化するためには、硝酸水溶液を強く撹拌しながら細管を通して液体ガリウムを硝酸水溶液に添加することにより、あるいは、水を強く撹拌しながら細管を通して液体ガリウムを水に添加した後に硝酸を添加することにより、液体ガリウムが硝酸水溶液中または水中で分散して浮遊可能な微粒滴（粒径０．１〜１００μｍ、好ましくは０．１〜１０μｍ、さらに好ましくは０．１〜７μｍ）に微粒化して硝酸水溶液または水に分散させるのが好ましい。 In order to atomize liquid gallium, the liquid gallium is added to the aqueous nitric acid solution through a thin tube while stirring the aqueous nitric acid solution vigorously, or after adding the liquid gallium to the water through the thin tube while stirring water strongly. Addition of fine particles into fine droplets (particle size 0.1 to 100 μm, preferably 0.1 to 10 μm, more preferably 0.1 to 7 μm) in which liquid gallium can be dispersed and floated in an aqueous nitric acid solution or in water It is preferable to disperse it in a nitric acid aqueous solution or water.
この撹拌は、撹拌羽根などにより２４０〜１０００ｒｐｍ（または容積当りの動力が１／Ｗ以上）の高い撹拌速度で行うのが好ましい。液体ガリウムは比重が大きいため、硝酸水溶液または水を撹拌しないと、液体ガリウムが硝酸水溶液中または水中で沈降して、硝酸水溶液への溶解速度が低くなるが、硝酸水溶液または水を撹拌しながら細管を通して液体ガリウムを硝酸水溶液または水に添加することにより、液体ガリウムを微粒化して硝酸水溶液または水に分散させれば、硝酸水溶液への溶解速度を高くすることができる。なお、撹拌速度が２４０ｒｐｍより低いと、液体ガリウムが硝酸水溶液中または水中で沈降し易くなるので、撹拌速度を２４０〜１０００ｒｐｍにするのが好ましく、４００〜８００ｒｐｍにするのがさらに好ましい。例えば、撹拌速度を１００ｒｐｍとして低速で撹拌した場合に、投入した液体ガリウムの６０％を硝酸水溶液に溶解するのに要した時間が３２時間以上であっても、撹拌速度を６００ｒｐｍとして高速で撹拌すると、その溶解時間を５時間程度にすることができる。 This stirring is preferably performed at a high stirring speed of 240 to 1000 rpm (or a power per volume of 1 / W or more) with a stirring blade or the like. Since liquid gallium has a large specific gravity, if the nitric acid aqueous solution or water is not stirred, the liquid gallium will settle in the nitric acid aqueous solution or water, and the dissolution rate in the nitric acid aqueous solution will be low. If liquid gallium is atomized and dispersed in aqueous nitric acid or water by adding liquid gallium to aqueous nitric acid or water, the dissolution rate in aqueous nitric acid can be increased. If the stirring speed is lower than 240 rpm, liquid gallium tends to settle in an aqueous nitric acid solution or in water. Therefore, the stirring speed is preferably 240 to 1000 rpm, and more preferably 400 to 800 rpm. For example, when stirring is performed at a low speed with a stirring speed of 100 rpm, even if the time required to dissolve 60% of the charged liquid gallium in the aqueous nitric acid solution is 32 hours or more, stirring at a high speed with a stirring speed of 600 rpm. The dissolution time can be about 5 hours.
なお、液体ガリウムを硝酸水溶液に添加するより、液体ガリウムを最初に水に添加した後に硝酸を添加した方が、表面酸化により微粒滴同士が凝集し難くなって、浮遊状態を維持し易くなるので、液体ガリウムを水に添加した後に硝酸を添加するのが好ましい。 Rather than adding liquid gallium to an aqueous nitric acid solution, adding liquid nitric acid to water first and then adding nitric acid makes it more difficult for the droplets to aggregate due to surface oxidation, making it easier to maintain a floating state. It is preferable to add nitric acid after adding liquid gallium to water.
この撹拌では、液体ガリウムが硝酸水溶液中または水中で分散して浮遊可能な微粒滴になればよく、せん断力の強い撹拌機の他、スタティックミキサ、ラインミキサ、ホモジナイザ、超音波分散機、サンドグラインダなどを使用することができる。 In this stirring, liquid gallium may be dispersed in nitric acid aqueous solution or in water to form fine droplets that can float. In addition to a stirrer with strong shearing force, static mixer, line mixer, homogenizer, ultrasonic disperser, sand grinder Etc. can be used.
また、液体ガリウムの添加は、内径０．１〜５ｍｍ（好ましくは１〜３ｍｍ）の１本以上のチューブからなる細管を通して行うのが好ましい。液体ガリウムを通過させるチューブが細くなるほど、ガリウム粒子が小さくなって、ガリウム粒子１個当たりの表面積が増大して、硝酸水溶液への溶解速度が高くなるが、単位時間当りに供給できる液体ガリウムの量が少なくなって（液体ガリウムの添加速度が低くなって）、経済性に劣るので、チューブの内径は、０．１〜５ｍｍであるのが好ましく、１〜３ｍｍであるのがさらに好ましい。なお、チューブを細くするとともにチューブの数を増やせば、１本のチューブによる液体ガリウムの添加速度が低くても、全チューブによる液体ガリウムの添加速度を高めることができるので、硝酸水溶液への溶解速度と高めるとともに液体ガリウムの単位時間当たりの供給量を増大することができる。 The addition of liquid gallium is preferably carried out through a thin tube composed of one or more tubes having an inner diameter of 0.1 to 5 mm (preferably 1 to 3 mm). The thinner the tube through which liquid gallium passes, the smaller the gallium particles, the greater the surface area per gallium particle and the higher the dissolution rate in aqueous nitric acid solution, but the amount of liquid gallium that can be supplied per unit time Therefore, the inner diameter of the tube is preferably from 0.1 to 5 mm, and more preferably from 1 to 3 mm. If the number of tubes is reduced and the number of tubes is increased, the liquid gallium addition rate of all tubes can be increased even if the liquid gallium addition rate of one tube is low. And the supply amount of liquid gallium per unit time can be increased.
また、液体ガリウムの添加は、液体ガリウムを噴霧して行ってもよい。例えば、細管の先端にベンチュリ管を接続して圧縮空気により液体ガリウムを噴霧して添加しても、液体ガリウムを微粒化して硝酸水溶液に溶解させることができる。 The addition of liquid gallium may be performed by spraying liquid gallium. For example, even when a Venturi tube is connected to the tip of a thin tube and liquid gallium is sprayed and added with compressed air, the liquid gallium can be atomized and dissolved in an aqueous nitric acid solution.
また、液体ガリウムの硝酸水溶液への溶解速度を高めるために、液体ガリウムを硝酸水溶液に溶解させる際に硝酸水溶液の温度を６０℃以上に維持するのが好ましい。しかし、液体ガリウムを硝酸水溶液に溶解させる際に硝酸水溶液の温度を６０℃以上に維持すると、硝酸の分解によりＮＯｘが生成する。このようなＮＯｘの生成を最小限に抑えるとともに、硝酸の分解により生成されたＮＯｘを硝酸に戻して、硝酸の酸化力を回復させ、液体ガリウムの硝酸水溶液への溶解率を高めて、所望のガリウム濃度（例えば、５〜１５質量％）の硝酸ガリウム水溶液を得るために、液体ガリウムを硝酸水溶液に溶解させる際に（途中で）硝酸水溶液に過酸化水素を添加するのが好ましい。例えば、液体ガリウムを硝酸水溶液に添加してから１日経過後に過酸化水素を添加するのが好ましい。このように過酸化水素を添加することにより、液体ガリウムの硝酸水溶液の溶解率を１００％にすることができる。 In order to increase the dissolution rate of liquid gallium in an aqueous nitric acid solution, the temperature of the aqueous nitric acid solution is preferably maintained at 60 ° C. or higher when the liquid gallium is dissolved in the aqueous nitric acid solution. However, if the temperature of the aqueous nitric acid solution is maintained at 60 ° C. or higher when liquid gallium is dissolved in the aqueous nitric acid solution, NOx is generated due to decomposition of nitric acid. In addition to minimizing the production of such NOx, the NOx produced by the decomposition of nitric acid is returned to nitric acid to recover the oxidizing power of nitric acid, and increase the dissolution rate of liquid gallium in aqueous nitric acid solution to achieve a desired level. In order to obtain a gallium nitrate aqueous solution having a gallium concentration (for example, 5 to 15% by mass), it is preferable to add hydrogen peroxide to the nitric acid aqueous solution when liquid gallium is dissolved in the nitric acid aqueous solution. For example, it is preferable to add hydrogen peroxide one day after adding liquid gallium to the aqueous nitric acid solution. Thus, by adding hydrogen peroxide, the dissolution rate of the aqueous solution of nitric acid in liquid gallium can be made 100%.
以下、本発明による硝酸ガリウム水溶液の製造方法の実施例について詳細に説明する。 Hereinafter, the Example of the manufacturing method of the gallium nitrate aqueous solution by this invention is described in detail.
［実施例１］
２枚のタービン羽根と４枚の邪魔板を備えた撹拌機を１０Ｌのビーカーに設置し、純水５，０００ｇと６０％の硝酸２．７１１ｇ（２６モル、３３．８質量％、１００％の硝酸に換算すると２０．３質量％）をビーカーに入れた後、硝酸水溶液を６０℃に維持して、攪拌速度６００ｒｐｍで攪拌しながら、内径３ｍｍの１本のチューブ（テフロン（登録商標）チューブ）を通して、（予め溶解させた）液体ガリウム３００ｇ（４．３モル、３．７質量％）を硝酸水溶液に添加した（ＨＮＯ３（モル）／（Ｇａ（モル）／３）当量は１．５７）。
[Example 1]
A stirrer equipped with two turbine blades and four baffle plates was placed in a 10 L beaker, and 5,000 g of pure water and 2.711 g of 60% nitric acid (26 mol, 33.8% by mass, 100% (20.3% by mass in terms of nitric acid) was placed in a beaker, and the nitric acid aqueous solution was maintained at 60 ° C. and stirred at a stirring speed of 600 rpm, and a single tube having an inner diameter of 3 mm (Teflon (registered trademark) tube) Through, 300 g (4.3 mol, 3.7 mass%) of liquid gallium (predissolved) was added to the aqueous nitric acid solution (HNO 3 (mol) / (Ga (mol) / 3) equivalent was 1.57) .
液体ガリウムを添加してから２時間後、４時間後、７時間後、８時間後の水溶液を５０ｍＬずつサンプリングして、水溶液中のガリウム濃度をＩＣＰで測定し、ガリウムの溶解進捗率を算出したところ、水溶液中のガリウム濃度は、それぞれ１．３５質量％、２．３５質量％、２．８８質量％、３．０９質量％であり、ガリウムの溶解進捗率は、それぞれ３６．０５％、６２．７５％、７６．９１％、８２．５１％であった。 After 2 hours, 4 hours, 7 hours, and 8 hours after the addition of liquid gallium, 50 mL of the aqueous solution was sampled, the gallium concentration in the aqueous solution was measured by ICP, and the dissolution progress rate of gallium was calculated. However, the gallium concentration in the aqueous solution is 1.35% by mass, 2.35% by mass, 2.88% by mass, and 3.09% by mass, respectively, and the dissolution progress rates of gallium are 36.05% and 62%, respectively. .75%, 76.91%, 82.51%.
［比較例１］
チューブを通さずに液体ガリウムをそのまま硝酸水溶液に添加し、撹拌速度を１００ｒｐｍとした以外は、実施例１と同様の方法により、液体ガリウムを硝酸水溶液に添加したところ、液体ガリウムが大きな塊になってビーカーの底に溜まっていた。
[Comparative Example 1]
Liquid gallium was added to the nitric acid aqueous solution by the same method as in Example 1 except that liquid gallium was added as it was to the nitric acid aqueous solution without passing through the tube, and the stirring speed was 100 rpm. At the bottom of the beaker.
また、液体ガリウムを硝酸水溶液に添加してから４時間後、７時間後、２６時間後、２９時間後、３２時間後の水溶液を５０ｍＬずつサンプリングして、水溶液中のガリウム濃度をＩＣＰで測定し、ガリウムの溶解進捗率を算出したところ、水溶液中のガリウム濃度は、それぞれ０．０７質量％、０．１３質量％、１．７６質量％、２．０３質量％、２．２０質量％であり、ガリウムの溶解進捗率は、それぞれ１．８７％、３．４７％、４７．００％、５４．２１％、５８．７５％であった。 In addition, 4 hours, 7 hours, 26 hours, 29 hours, and 32 hours after the addition of liquid gallium to the nitric acid aqueous solution, 50 mL each of the aqueous solution was sampled, and the gallium concentration in the aqueous solution was measured by ICP. When the progress rate of dissolution of gallium was calculated, the gallium concentration in the aqueous solution was 0.07% by mass, 0.13% by mass, 1.76% by mass, 2.03% by mass, and 2.20% by mass, respectively. The progress rates of dissolution of gallium were 1.87%, 3.47%, 47.00%, 54.21%, and 58.75%, respectively.
［比較例２〜３］
撹拌速度をそれぞれ１００ｒｐｍ（比較例２）および２００ｒｐｍ（比較例３）とした以外は、実施例１と同様の方法により、液体ガリウムを硝酸水溶液に添加したところ、比較例１と同様に、液体ガリウムが大きな塊になってビーカーの底に溜まっていた。
[Comparative Examples 2-3]
Liquid gallium was added to the aqueous nitric acid solution by the same method as in Example 1 except that the stirring speed was 100 rpm (Comparative Example 2) and 200 rpm (Comparative Example 3), respectively. Became a big lump and collected at the bottom of the beaker.
［比較例４］
チューブを通さずに液体ガリウムをそのまま硝酸水溶液に添加した以外は、実施例１と同様の方法により、液体ガリウムを硝酸水溶液に添加したところ、比較例１と同様に、液体ガリウムが大きな塊になってビーカーの底に溜まっており、６００ｒｐｍで強く撹拌しても、液体ガリウムの塊をほとんど微粒滴に分離することができなかった。
[Comparative Example 4]
When liquid gallium was added to the nitric acid aqueous solution by the same method as in Example 1 except that liquid gallium was added as it was to the nitric acid aqueous solution without passing through the tube, the liquid gallium became a large lump as in Comparative Example 1. The liquid gallium lump could hardly be separated into fine droplets even when vigorously stirred at 600 rpm.
実施例１および比較例１の結果を図１および図２に示す。これらの図から、実施例１では、比較例１と比べて、非常に短い時間で液体ガリウムを溶解させることができるのがわかる。 The results of Example 1 and Comparative Example 1 are shown in FIGS. From these figures, it can be seen that in Example 1, liquid gallium can be dissolved in a very short time compared to Comparative Example 1.
［実施例２］
実際の製造プラントとして、６０℃の温水２００ｋｇを（インバーター周波数４０Ｈｚで容積４００Ｌ当りの動力を１Ｗ／Ｌ（＝電流１．５Ａ×電圧２００Ｖ×√３×０．８（力率）／４００Ｌ）にして）撹拌機により２４０ｒｐｍの高速で撹拌しながら、（予め６０℃で溶融させた）液体ガリウム５０ｋｇを添加速度１５０ｇ／分で内径３ｍｍの１本のチューブを通して、温水に添加した後、６０％の硝酸２９０ｋｇを添加して、液体ガリウムを溶解させたところ、３日で９５％のガリウムを溶解することができた。なお、液体ガリウムの温水への添加が終了した直後で硝酸を添加する前の溶液のレーザー顕微鏡写真を図３に示す。この写真から、温水に添加された液体ガリウムが粒径２〜７μｍの微粒滴状態に微粒化されて温水中に分散しているのがわかる。
[Example 2]
As an actual manufacturing plant, 200 kg of 60 ° C hot water (inverter frequency 40 Hz and power per 400 L volume is 1 W / L (= 1.5 A current × 200 V × √3 × 0.8 (power factor) / 400 L) While stirring with a stirrer at a high speed of 240 rpm, 50 kg of liquid gallium (previously melted at 60 ° C.) was added to warm water through a single tube with an inner diameter of 3 mm at an addition rate of 150 g / min, and then 60% When 290 kg of nitric acid was added to dissolve liquid gallium, 95% gallium could be dissolved in 3 days. FIG. 3 shows a laser micrograph of the solution immediately after the addition of liquid gallium to the warm water and before the addition of nitric acid. From this photograph, it can be seen that the liquid gallium added to the warm water is atomized into fine droplets having a particle diameter of 2 to 7 μm and dispersed in the warm water.
［比較例５］
温水を撹拌しなかった以外は、実施例２と同様の方法により、液体ガリウムを溶解させたところ、９５％のガリウムを溶解するのに７日以上かかった。
[Comparative Example 5]
When liquid gallium was dissolved by the same method as in Example 2 except that hot water was not stirred, it took 7 days or more to dissolve 95% gallium.
［比較例６］
温水を（インバーター周波数１０Ｈｚで容積４００Ｌ当りの動力を０．１Ｗ／Ｌにして）６０ｒｐｍの低速で撹拌した以外は、実施例２と同様の方法により、液体ガリウムを溶解させたところ、９５％のガリウムを溶解するのに７日以上かかった。
[Comparative Example 6]
The liquid gallium was dissolved by the same method as in Example 2 except that the hot water was stirred at a low speed of 60 rpm (with an inverter frequency of 10 Hz and a power per 400 L of volume of 0.1 W / L). It took more than 7 days to dissolve gallium.
［実施例３］
チューブの先端にベンチュリ管を接続して圧縮空気により液体ガリウムを硝酸水溶液に噴霧して添加した以外は、実施例１と同様の方法により、液体ガリウムを微粒化して硝酸水溶液に溶解させたところ、実施例１と同様に、非常に短い時間で液体ガリウムを溶解させることができた。
[Example 3]
A liquid gallium was atomized and dissolved in an aqueous nitric acid solution by the same method as in Example 1 except that a venturi tube was connected to the tip of the tube and liquid gallium was sprayed and added to the aqueous nitric acid solution with compressed air. As in Example 1, liquid gallium could be dissolved in a very short time.
Claims (8)
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| CN108046311A (en) * | 2017-12-25 | 2018-05-18 | 清远先导材料有限公司 | The preparation method of high-purity gallium oxide |
| WO2021079571A1 (en) * | 2019-10-24 | 2021-04-29 | 信越化学工業株式会社 | Method for producing gallium precursor, and method for producing layered product using same |
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