JP4100696B2 - Te separation method from Rh solution - Google Patents
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Description
本発明は、銅電解殿物より高純度Rhを回収するためRh溶液を精製する工程において、不純物である少量のTeを除去する方法に関する。 The present invention relates to a method for removing a small amount of Te, which is an impurity, in a step of purifying an Rh solution in order to recover high purity Rh from a copper electrolytic product.
特開2004-332041号（特許文献１）においては、Teおよび白金族金属を含む原料は、塩素雰囲気中で塩化揮発処理を行い、Teを揮発性の塩化物で除去し、白金族金属を可溶性の塩にして、Teを除去した白金族溶液を得る。次いで白金族溶液を蒸留、溶媒抽出、中和工程によってRh以外の成分を除去したRh溶液から、Rhを塩化アンモニウムによりヘキサクロロロジウム酸アンモニウム（(NH4)3RhCl6）として晶析し、これを焼成してRhのスポンジメタルを得る。 In Japanese Patent Application Laid-Open No. 2004-332041 (Patent Document 1), a raw material containing Te and a platinum group metal is subjected to a chlorinated volatilization treatment in a chlorine atmosphere, Te is removed with a volatile chloride, and the platinum group metal is soluble. To obtain a platinum group solution from which Te has been removed. Next, Rh was crystallized as ammonium hexachlororhodate ((NH 4 ) 3 RhCl 6 ) with ammonium chloride from the Rh solution from which components other than Rh were removed by distillation, solvent extraction and neutralization steps. Bake to obtain Rh sponge metal.
Teを多く（約10 mass %以上）含む原料は塩化揮発工程でTeを分離して水溶液にするが、少量のTe（Rhに対して約100〜5,000mass ppm）が水溶液に混入する。Teは蒸留、溶媒抽出、中和、晶析、還元などの工程でRhと同じような挙動を示すため、Rhとほとんど分離されない。このため、Rhのスポンジメタル中に約100〜5,000mass
ppmのTeが混入する。
A raw material containing a large amount of Te (about 10 mass% or more) separates Te into an aqueous solution by the chlorination volatilization process, but a small amount of Te (about 100 to 5,000 mass ppm relative to Rh) is mixed in the aqueous solution. Te exhibits the same behavior as Rh in processes such as distillation, solvent extraction, neutralization, crystallization, and reduction, so it is hardly separated from Rh. Because of this, about 100-5,000mass in Rh sponge metal
Contains ppm Te.
本発明では上記の欠点を解決するためになされたもので、高純度Rhを回収するためRh溶液を精製する工程において、不純物である少量のTeを除去する方法を提供することを目的とする。 The present invention has been made to solve the above-described drawbacks, and an object thereof is to provide a method for removing a small amount of Te, which is an impurity, in a process of purifying an Rh solution in order to recover high-purity Rh.
Rhを塩化アンモニウムにより晶析する工程で、アルコールを加えて加熱して析出する(NH4)3RhCl6およびTeをろ別し、これを純水でリパルプすると(NH4)3RhCl6だけが溶解するので、未溶解のTeをろ過分離する。その結果、Teを含まないRh溶液を得ることができる。 In the process of crystallizing Rh with ammonium chloride, (NH 4 ) 3 RhCl 6 and Te precipitated by adding alcohol and heating are filtered off and repulped with pure water to give only (NH 4 ) 3 RhCl 6 Since it dissolves, undissolved Te is separated by filtration. As a result, an Rh solution containing no Te can be obtained.
：
即ち本発明は、
（１）Rhおよび少なくとも少量のTeを含む塩酸溶液からRhを塩化アンモニウムで(NH4)3RhCl6として晶析する工程において、晶析前液にアルコールを加えて(NH4)3RhCl6とTeの混合物を沈殿させ、ろ過して得たこれらの混合物を、純水に分散させ（以下、前記行為をリパルプと称す。）、純水に可溶な(NH4)3RhCl6を溶解回収し、純水に溶解しないTeをろ過分離除去するRhおよび少量のTeを含む塩酸溶液からTeを除去する方法。
（２）上記（１）記載の方法において、晶析前液にアルコールを加えて (NH4)3RhCl6とTeの混合物の沈殿を生成する時の条件が温度50℃以上で1時間以上保持することを特徴とするRhおよび少量のTeを含む塩酸溶液からTeを分離する方法。
（３）上記（１）記載の方法において、アルコールが、エチルアルコール、メチルアルコール、イソプロピルアルコールおよびこれらから2種類以上が選ばれた混合物であることを特徴とするRhおよび少量のTeを含む塩酸溶液からTeを分離する方法。
を提供する。
:
That is, the present invention
(1) In a step of crystallizing Rh with ammonium chloride as (NH 4 ) 3 RhCl 6 from a hydrochloric acid solution containing Rh and at least a small amount of Te, alcohol is added to the pre-crystallization solution and (NH 4 ) 3 RhCl 6 These mixtures obtained by precipitating and filtering the Te mixture are dispersed in pure water (hereinafter, the above action is referred to as “repulp”) , and (NH 4 ) 3 RhCl 6 soluble in pure water is dissolved and recovered. A method of removing Te from a hydrochloric acid solution containing Rh and a small amount of Te, which separates and removes Te that does not dissolve in pure water.
(2) In the method described in (1) above, the condition when a mixture of (NH 4 ) 3 RhCl 6 and Te is formed by adding alcohol to the pre-crystallization solution is maintained at a temperature of 50 ° C. or more for 1 hour or more. A method for separating Te from a hydrochloric acid solution containing Rh and a small amount of Te.
(3) A hydrochloric acid solution containing Rh and a small amount of Te, wherein the alcohol is ethyl alcohol, methyl alcohol, isopropyl alcohol or a mixture selected from two or more thereof in the method described in (1) above How to separate Te from
I will provide a.
本発明の方法を用いて、Rhの晶析工程でアルコールを加え、晶析物から純水に溶解しないTeをろ過分離することで、Rhのスポンジメタル中のTe品位を20mass ppm以下に低減できる。
高純度のRhを製造することが可能になる。
Using the method of the present invention, by adding alcohol in the Rh crystallization process, and separating and filtering Te that does not dissolve in pure water from the crystallized product, the Te quality in the Rh sponge metal can be reduced to 20 mass ppm or less. .
It becomes possible to produce high-purity Rh.
本発明の詳細について述べる。
電解殿物のようなTeおよび白金族金属を含む原料は、塩素雰囲気中で塩化揮発処理を行い、Teを揮発性の塩化物で除去し、白金族金属を可溶性の塩にして、Teを除去した白金族溶液を得る。次いで白金族溶液を蒸留、溶媒抽出、中和等の精製工程によってRh以外の成分を除去したRh溶液から、Rhを塩化アンモニウムにより(NH4)3RhCl6として晶析、還元、焼成等の工程を経てRhのスポンジメタルを得る。
ここで原料中のTe品位が数mass %以下と低い場合は、塩化揮発処理で十分にTeを除去することができる。このようにTe濃度が十分に低いRh溶液から、Rhを塩化アンモニウムにより晶析、焼成して得たRhのスポンジメタルはTeをほとんど含まない。
一方、原料中のTe品位が10mass%以上と高い場合、塩化揮発処理で十分にTeを除去することができず、溶液中に少量のTeが含まれる。Teは蒸留、溶媒抽出、中和、晶析、還元などの精製工程でRhと同じような挙動を示すため、Rhとほとんど分離されない。このため、Rhのスポンジメタル中に約100〜5,000
mass ppmのTeが残留するため、高純度のRhを得ることができない。そこで、少量のTeを含むRh溶液からTeを分離する方法を見出した。
Details of the present invention will be described.
Raw materials containing Te and platinum group metals, such as electrolytic deposits, are chlorinated and volatilized in a chlorine atmosphere, Te is removed with volatile chlorides, platinum group metals are made soluble salts, and Te is removed. A platinum group solution is obtained. Next, from the Rh solution from which components other than Rh have been removed by purification steps such as distillation, solvent extraction, and neutralization of the platinum group solution, Rh is converted to (NH 4 ) 3 RhCl 6 with ammonium chloride, steps of crystallization, reduction, firing, etc. To get Rh sponge metal.
Here, when the Te quality in the raw material is as low as several mass% or less, Te can be sufficiently removed by chlorination volatilization treatment. The Rh sponge metal obtained by crystallization and baking of Rh from ammonium chloride from an Rh solution having a sufficiently low Te concentration contains almost no Te.
On the other hand, when the Te quality in the raw material is as high as 10 mass% or more, Te cannot be sufficiently removed by the chlorination volatilization treatment, and a small amount of Te is contained in the solution. Te exhibits the same behavior as Rh in purification processes such as distillation, solvent extraction, neutralization, crystallization, and reduction, so it is hardly separated from Rh. For this reason, about 100-5,000 in Rh sponge metal
Since mass ppm Te remains, high-purity Rh cannot be obtained. Therefore, a method for separating Te from an Rh solution containing a small amount of Te was found.
蒸留、溶媒抽出、中和等の精製工程によってRh以外の成分を除去したRh溶液からRhを回収する方法は、塩酸濃度が3〜6mol/Lとなるように調整した溶液に塩化アンモニウムを加えて70〜95℃程度に加熱し、(NH4)3RhCl6として晶析する。この工程で(NH4)3RhCl6が生成するが溶解度が大きいので、溶解度を下げて晶析を促進するためにアルコールを加える。このとき溶液を50℃以上で1時間以上加熱すると、Rhが晶析すると共にTeを還元して析出するので、ろ過して(NH4)3RhCl6と還元Teの混合物を得る。RhとTeの還元電位はそれぞれ0.43V、0.52Vと近いので、還元電位差による分離は困難である。ここでRhはアルコールによる還元反応が遅いので、(NH4)3RhCl6として晶析する。このためアルコールは実用上Teだけを還元することができることを発見した。
塩化アンモニウムとアルコールを同時に加えると、アルコールが塩化アンモニウムの溶解度を下げるため、未反応の塩化アンモニウムが析出してしまうこと、アルコールを加えることで沸点が下がることから、(NH4)3RhCl6を効率的に生成することができなくなる。このため、アルコールは(NH4)3RhCl6が生成した晶析液に加えることが望ましい。
加えるアルコールの種類はエチルアルコール、メチルアルコール、イソプロピルアルコールまたはこれらの混合物が望ましい。炭素数が多いアルコールは還元力が大きくなるが、同時に還元して水に未溶解のRhを生成してしまい、Teと一緒に分離されて回収率が低下する。
加えるアルコールの量は、Teを還元して (NH4)3RhCl6が晶析可能であれば特に規定されないが、目安として水溶液の0.5〜2倍量である。
加熱条件を50℃以上で1時間以上とした理由を述べる。晶析工程でTeは塩化アンモニウムと反応して水溶性のテルル酸アンモニウム（(NH4)2TeO4）となるが、アルコールで還元Teに十分に還元するためである。還元が不十分であると、水溶性のテルル酸アンモニウム（(NH4)2TeO4）が残留するが、アルコール混合液中では溶解度が小さいため、(NH4)3RhCl6と一緒に晶析する。加熱温度が50℃未満あるいは加熱時間が1時間未満ではTeの還元が十分でなく、純水でリパルプすると、(NH4)3RhCl6と共に（(NH4)2TeO4）が溶解し、ろ別することができないためである。
本発明において、純水とは、例えば、イオン交換水、蒸留水等である。
The method of recovering Rh from the Rh solution from which components other than Rh have been removed by purification steps such as distillation, solvent extraction, and neutralization is to add ammonium chloride to the solution adjusted to have a hydrochloric acid concentration of 3 to 6 mol / L. Heat to about 70-95 ° C. and crystallize as (NH 4 ) 3 RhCl 6 . In this step, (NH 4 ) 3 RhCl 6 is produced, but the solubility is high, so alcohol is added to lower the solubility and promote crystallization. At this time, when the solution is heated at 50 ° C. or higher for 1 hour or longer, Rh is crystallized and Te is reduced and precipitated, and is filtered to obtain a mixture of (NH 4 ) 3 RhCl 6 and reduced Te. Since the reduction potentials of Rh and Te are close to 0.43V and 0.52V, respectively, separation by the reduction potential difference is difficult. Here, Rh crystallizes as (NH 4 ) 3 RhCl 6 because of the slow reduction reaction with alcohol. For this reason, it was discovered that alcohol can reduce only Te in practice.
When ammonium chloride and alcohol are added at the same time, the alcohol lowers the solubility of ammonium chloride, so that unreacted ammonium chloride is precipitated and the boiling point is lowered by adding alcohol. (NH 4 ) 3 RhCl 6 It cannot be generated efficiently. For this reason, it is desirable to add alcohol to the crystallization solution in which (NH 4 ) 3 RhCl 6 is formed.
The kind of alcohol to be added is preferably ethyl alcohol, methyl alcohol, isopropyl alcohol or a mixture thereof. Alcohols with a large number of carbons have a higher reducing power, but at the same time, they are reduced to produce undissolved Rh in water, which is separated together with Te to reduce the recovery rate.
The amount of alcohol to be added is not particularly limited as long as (NH 4 ) 3 RhCl 6 can be crystallized by reducing Te, but it is 0.5 to 2 times the amount of the aqueous solution as a guide.
The reason why the heating condition is set to 50 ° C. or more for 1 hour or more is described. This is because Te reacts with ammonium chloride to form water-soluble ammonium tellurate ((NH 4 ) 2 TeO 4 ) in the crystallization process, but is sufficiently reduced to reduced Te with alcohol. If the reduction is insufficient, water-soluble ammonium tellurate ((NH 4 ) 2 TeO 4 ) remains, but the solubility in the alcohol mixture is low, so crystallization occurs with (NH 4 ) 3 RhCl 6 To do. When the heating temperature is less than 50 ° C or the heating time is less than 1 hour, Te is not sufficiently reduced, and when repulped with pure water, (NH 4 ) 3 RhCl 6 and ((NH 4 ) 2 TeO 4 ) dissolve and filter. This is because they cannot be separated.
In the present invention, pure water is, for example, ion exchange water, distilled water or the like.
ろ過して得た(NH4)3RhCl6と還元Teの混合物を純水でリパルプすると、純水に可溶性の(NH4)3RhCl6だけが溶解し、純水に不溶性のTeが未溶解として残る。これをろ過分離することでTeを含まないRh溶液を得る。このろ過で用いるろ材は、未溶解の還元Teは粒子が非常に微細であるので、孔径が１ミクロン以下のメンブランフィルター等を用いることが望ましい。 When the mixture of (NH 4 ) 3 RhCl 6 and reduced Te obtained by filtration is repulped with pure water, only (NH 4 ) 3 RhCl 6 soluble in pure water is dissolved, and Te insoluble in pure water is not dissolved. Remain as. This is separated by filtration to obtain an Rh solution containing no Te. The filter medium used in this filtration is preferably a membrane filter having a pore size of 1 micron or less because the undissolved reduced Te has very fine particles.
Teを分離したRh溶液は還元剤にギ酸等を加えて加熱して、Rhブラックとして回収する。Rhブラックは、粒子が微細で取り扱い性が悪く、酸素を含有するので、通常は水素あるいは不活性ガス雰囲気でRhのスポンジメタルにして回収する。このようにして得たRhのスポンジメタルは、Te品位を20mass
ppm以下に低減できる。
あるいはTeを分離したRh溶液は、塩酸と塩化アンモニウムを加えて(NH4)3RhCl6を再晶析、ろ別して、晶析物を水素あるいは不活性ガス雰囲気で分解・焼成して、Rhのスポンジメタルとしても良い。
The Rh solution from which Te has been separated is recovered by adding formic acid or the like to the reducing agent and heating to recover Rh black. Since Rh black has fine particles and poor handleability and contains oxygen, it is usually collected as Rh sponge metal in hydrogen or an inert gas atmosphere. The Rh sponge metal thus obtained has a Te quality of 20 mass.
Can be reduced to ppm or less.
Alternatively, the Rh solution from which Te has been separated is added with hydrochloric acid and ammonium chloride to recrystallize (NH 4 ) 3 RhCl 6 and filter, and the crystallized product is decomposed and fired in an atmosphere of hydrogen or an inert gas. It is good as sponge metal.
以下に本発明の実施例を説明する。
表1に実施例1で使用したTeおよび白金族金属を含む原料の組成を示す。これを塩素雰囲気中で塩化揮発処理を行い、Teを揮発性の塩化物で除去した後、塩化ナトリウムを加えて塩化焙焼処理して白金族金属を可溶性の塩を得て、水溶液とした。これを蒸留、溶媒抽出、中和の精製工程でRh以外の成分を除去した。
表２にこの方法で得たTe分離前のRh溶液の液組成を示す。原料中のTe品位が高かったため、Rh溶液中に少量のTeが残留した。
この溶液100mLに塩酸濃度が6mol/Lとなるように塩酸を加え、塩化アンモニウムを(NH4)3RhCl6生成に必要な2当量を加えて、90℃で1時間加熱した。これにエチルアルコールを150mL加えて70℃で1時間加熱して、放冷後、ろ紙（JIS No.5C）でろ過し、(NH4)3RhCl6と還元Teの混合物を得た。この混合物を200mLの純水でリパルプし、(NH4)3RhCl6を溶解後、孔径0.1ミクロンのメンブランフィルターでろ過して還元Teを分離した。表２にTe分離後の液組成を示す。Teの濃度は分析限界の1mg/L以下に低下した。
Te分離後のRh液はギ酸をRhの還元に必要な5当量を加えて、90℃で2時間加熱して、Rhブラックを回収した。Rhブラックは5%水素−アルゴン混合ガス中で1,000℃で1時間の焼成を行って、Rhのスポンジメタルにした。このRhをグロー放電質量分析装置（GDMS）で品位を分析した。表３にRhのスポンジメタルの分析結果を示すが、Rh中のTeは1mass
ppmであった。
Examples of the present invention will be described below.
Table 1 shows the composition of the raw materials containing Te and platinum group metals used in Example 1. This was subjected to chlorination and volatilization treatment in a chlorine atmosphere, Te was removed with volatile chlorides, sodium chloride was added and chlorination roasting treatment was performed to obtain a platinum group metal soluble salt, and an aqueous solution was obtained. Components other than Rh were removed in the purification steps of distillation, solvent extraction and neutralization.
Table 2 shows the liquid composition of the Rh solution before Te separation obtained by this method. Since Te quality in the raw material was high, a small amount of Te remained in the Rh solution.
Hydrochloric acid was added to 100 mL of this solution so that the hydrochloric acid concentration was 6 mol / L, and 2 equivalents of ammonium chloride necessary for the production of (NH 4 ) 3 RhCl 6 were added, followed by heating at 90 ° C. for 1 hour. 150 mL of ethyl alcohol was added thereto, heated at 70 ° C. for 1 hour, allowed to cool, and then filtered through filter paper (JIS No. 5C) to obtain a mixture of (NH 4 ) 3 RhCl 6 and reduced Te. This mixture was repulped with 200 mL of pure water, dissolved (NH 4 ) 3 RhCl 6 , and then filtered through a membrane filter having a pore size of 0.1 μm to separate reduced Te. Table 2 shows the liquid composition after Te separation. The concentration of Te decreased below the analytical limit of 1 mg / L.
The Rh solution after Te separation was added with 5 equivalents of formic acid required for the reduction of Rh and heated at 90 ° C. for 2 hours to recover Rh black. Rh black was fired in a 5% hydrogen-argon mixed gas at 1,000 ° C. for 1 hour to make Rh sponge metal. The quality of this Rh was analyzed with a glow discharge mass spectrometer (GDMS). Table 3 shows the analysis result of Rh sponge metal. Te in Rh is 1 mass.
ppm.
実施例２は、晶析工程で加えたアルコールにイソプロピルアルコールを使用したこと以外は実施例1と同じ条件で実施した。表４にTe分離前後の液組成を示すが、Teの濃度は分析限界の1mg/L以下に低下していた。
表５にRhのスポンジメタルの分析結果を示すが、Rh中のTeは1mass ppm未満であった。
Example 2 was performed under the same conditions as Example 1 except that isopropyl alcohol was used as the alcohol added in the crystallization step. Table 4 shows the liquid composition before and after the separation of Te. The Te concentration was lowered to 1 mg / L or less, which is the limit of analysis.
Table 5 shows the analysis results of Rh sponge metal, and Te in Rh was less than 1 mass ppm.
以下比較例を説明する。比較例は晶析でエチルアルコールを添加するまでは実施例1と同じ条件で実施した。表６に比較例の晶析前の液組成を示す。比較例は、エチルアルコールを添加して加熱しないで(NH4)3RhCl6を晶析し、ろ紙（JIS No.5C）でろ過した。これを200mLの純水でリパルプし、(NH4)3RhCl6を溶解後、ギ酸をRhの還元に必要な5当量を加えて、90℃で2時間加熱して、Rhブラックを回収した。Rhブラックは5%水素−アルゴン混合ガス中で1,000℃で1時間の焼成を行って、Rhのスポンジメタルにした。表７にRhのスポンジメタルの分析結果を示すが、Rh中のTeは4,100mass
ppmと多く、高純度のRhを得られなかった。
A comparative example will be described below. The comparative example was carried out under the same conditions as in Example 1 until ethyl alcohol was added during crystallization. Table 6 shows the liquid composition of the comparative example before crystallization. In the comparative example, (NH 4 ) 3 RhCl 6 was crystallized without adding ethyl alcohol and heating, and filtered through a filter paper (JIS No. 5C). This was repulped with 200 mL of pure water, dissolved (NH 4 ) 3 RhCl 6 , 5 equivalents of formic acid required for the reduction of Rh were added, and heated at 90 ° C. for 2 hours to recover Rh black. Rh black was fired in a 5% hydrogen-argon mixed gas at 1,000 ° C. for 1 hour to make Rh sponge metal. Table 7 shows the analysis results of Rh sponge metal. Te in Rh is 4,100 mass.
High purity Rh could not be obtained.
Claims (3)
モニウムで(NH4)3RhCl6として晶析する工程において、晶析前液にアル
コールを加えて(NH4)3RhCl6とTeの混合物を沈殿させ、ろ過して得た
これらの混合物を、純水に分散させ（以下、前記行為をリパルプと称す。）、純水に可溶な(NH4)3RhCl6を溶解回収し、純水に溶解しないTeをろ過分離除去することを特徴とするRhおよび少量のTeを含む塩酸溶液からTeを除去する方法。 In the step of crystallizing Rh with ammonium chloride as (NH 4 ) 3 RhCl 6 from a hydrochloric acid solution containing Rh and at least a small amount of Te, a mixture of (NH 4 ) 3 RhCl 6 and Te is added to the pre-crystallization solution by adding alcohol. These mixtures obtained by precipitating and filtering are dispersed in pure water (hereinafter, the above action is referred to as repulping) , and (NH 4 ) 3 RhCl 6 soluble in pure water is dissolved and recovered. A method for removing Te from a hydrochloric acid solution containing Rh and a small amount of Te, characterized by filtering and removing Te that does not dissolve in water.
(NH4)3RhCl6とTeの混合物の沈殿を生成する時の条件が温度50℃以上
で1時間以上保持することを特徴とするRhおよび少量のTeを含む塩
酸溶液からTeを分離する方法。 The method according to claim 1, wherein alcohol is added to the pre-crystallization solution.
A method for separating Te from a hydrochloric acid solution containing Rh and a small amount of Te, characterized in that the conditions for producing a precipitate of a mixture of (NH 4 ) 3 RhCl 6 and Te are maintained at a temperature of 50 ° C. or higher for 1 hour or longer. .
メチルアルコール、イソプロピルアルコールおよびこれらから2種類
以上が選ばれた混合物であることを特徴とするRhおよび少量のTeを
含む塩酸溶液からTeを分離する方法。 The method of claim 1, wherein the alcohol is ethyl alcohol,
A method for separating Te from a hydrochloric acid solution containing Rh and a small amount of Te, characterized in that it is methyl alcohol, isopropyl alcohol, or a mixture of two or more of these.
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| JP2005088185A JP4100696B2 (en) | 2005-03-25 | 2005-03-25 | Te separation method from Rh solution |
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| JP4964814B2 (en) * | 2008-03-28 | 2012-07-04 | Ｊｘ日鉱日石金属株式会社 | Recovery method of rhodium |
| KR101451789B1 (en) * | 2012-10-23 | 2014-10-16 | 한국과학기술연구원 | Separation of tellurium by solvent extraction method |
| CN102897853B (en) * | 2012-11-05 | 2014-08-13 | 中国海洋石油总公司 | Method for preparing water-soluble hexachlororhodate by medium-temperature chlorination of rhodium powder |
| TWI871574B (en) * | 2023-02-03 | 2025-02-01 | 南亞塑膠工業股份有限公司 | Self-healing resin composition and artificial leather manufactured therefrom |
| CN119020594B (en) * | 2024-08-16 | 2025-12-09 | 云南锡业股份有限公司铜业分公司 | Process for recycling multiple metals from complex rare materials by full wet method |
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