KR100968727B1 - Refining method of High purity gold from gold bonding wire scrap - Google Patents
Refining method of High purity gold from gold bonding wire scrap Download PDFInfo
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Abstract
본 발명은 금 본딩 와이어 스크랩으로부터 고순도 금의 정제방법에 관한 것으로, 그 목적은 금 본딩 와이어 제조 과정에서 발생하는 금본딩 와이어 스크랩으로부터 순도가 99.995%이상의 고순도 금을 신속하고 용이하게 정제하여, 금 정제공정의 효율을 향상시킬 수 있는 고순도 금 정제방법을 제공하는데 있다.The present invention relates to a method for purifying high purity gold from gold bonding wire scrap, and an object thereof is to rapidly and easily purify high purity gold having a purity of 99.995% or more from gold bonding wire scrap generated in the process of manufacturing a gold bonding wire. It is to provide a high purity gold purification method that can improve the efficiency of the process.
본 발명의 구성은 금 본딩 와이어를 제조할 때 사용한 도핑제(Dopant)로 사용한 Ga, Ge, Ca이 불순물 함유되어 있는 금본딩 와이어 스크랩의 정제방법에 있어서, Ga, Ge, Ca이 불순물 함유되어 있는 금본딩 와이어 스크랩에 요오드(Iodide)를 첨가하여 혼합한 후 석영관에 장입 후 가열하여 요오드화금(gold Iodie)을 제조한 후, 이를 에틸알콜(Ethyl Alcohol) 또는 에테르(Ether)로 환원·석출 시킨 후 여과하여 순수로 세정하고 건조시켜 고순도 금으로 정제하는 방법을 특징으로 한다.The constitution of the present invention is a method for refining a gold bonding wire scrap containing impurity Ga, Ge, and Ca used as a dopant used to prepare a gold bonding wire, wherein Ga, Ge and Ca are impurity-containing. Iodide was added to the gold bonding wire scrap, mixed, charged in a quartz tube and heated to prepare gold iodie, and then reduced and precipitated with ethyl alcohol or ether. After filtration, washing with pure water, drying, and purified by high purity gold.
금, 정제, 와어스크랩, 고순도, 불순물 Gold, Refined, Washer Scrap, High Purity, Impurities
Description
본 발명은 금의 정제방법에 관한 것으로, 자세하게는 반도체용 금본딩 와이어의 제조 과정에서 발생한 스크랩에 함유되어 있는 불순물을 제거하여 고순도 금으로 정제하는 방법에 관한 것으로, 특히 금본딩 와이어 스크랩에 요오드를 첨가하여 혼합한 후 석영관에 장입 후 가열하여 요오드화금을 제조한 후 이를 에틸알콜, 에테르로 환원·석출 시킨 후 여과하여 순수로 세정하고 건조시켜 순도가 99.995% 이상인 고순도 금으로 정제하는 방법에 관한 것이다.The present invention relates to a method for refining gold, and more particularly, to a method for refining high purity gold by removing impurities contained in a scrap generated during the manufacture of a gold bonding wire for semiconductors. After adding and mixing, charged into a quartz tube and heated to produce gold iodide, reduced and precipitated with ethyl alcohol, ether, filtered, washed with pure water and dried to purify with high purity gold of 99.995% or more. will be.
금은 장식, 장신구 뿐만 아니라 급속도로 성장을 더해가고 있는 반도체 및 전자산업 산업에서 필수적으로 사용되고 있는 소재이다. Gold is an essential material for the semiconductor and electronics industries, which are growing rapidly as well as for decoration and jewelry.
특히 고순도 금은 반도체를 제조할 때 반도체 소자와 기판을 연결해주는 금 본딩 와이어(Gold Bonding Wire) 제조에 사용되며 연신율을 높이기 위하여 금의 순도는 99.995% 이상으로 유지하여야 한다. In particular, high purity gold is used to manufacture a gold bonding wire that connects a semiconductor device and a substrate when manufacturing a semiconductor. In order to increase elongation, the purity of gold should be maintained at 99.995% or more.
또한 고순도 금의 경우 가격이 매우 높기 때문에 금 본딩 와이어 제조 과정에서 다량 발생되고 있는 스크랩을 가능한 간단한 정제공정을 적용하여 금의 정제시간을 단축하므로 정제비용을 낮추고 원자재에 대한 금리의 부담을 줄일 수 있어 제품의 경쟁력을 높이는 것이 금리면에서 매우 중요하다.In addition, high-purity gold has a very high price, which reduces the cost of refining and reduces the burden of interest rates on raw materials by applying a simple refining process to scrap a large amount of scrap generated in the process of manufacturing gold bonding wires. Increasing the competitiveness of a product is very important in terms of interest rates.
종래에 금을 정제하는 방법을 살펴보면, 금 본딩 와이어 스크??을 왕수에 용해한 후 가열하여 질소 산화물을 제거하고 가열하여 증발, 건고한 후 이 건고물을 진한 황산에 용해하고, 다시 가열하여 온도를 200℃로 유지시키면서 아황산 가스를 발생시키면서 용액 중에 함유되어 있는 금이온을 선택적으로 환원석출 시키는 화학정제 방법과 스크랩을 용융하여 양극으로 주조한 후 전기분해하여 정제하는 전해정제 방법이었다.In the conventional method of purifying gold, the gold bonding wire scrubber is dissolved in aqua regia, heated to remove nitrogen oxides, heated to evaporate and dry, and then the dried material is dissolved in concentrated sulfuric acid, and heated again to increase the temperature. Chemical purification was performed to selectively reduce and precipitate the gold ions contained in the solution while maintaining sulfuric acid gas, and electrolytic refining to melt and cast scrap into an anode, followed by electrolysis.
그러나 상기에 의한 정제방법 중 화학정제 방법은 금 본딩 와이어 스크랩을 왕수에 용해하는 과정에서 질소산화물이 다량 발생하며 진한 황산을 가하여 금을 환원, 석출시키는 과정에서 또한 많은 양의 아황산 가스가 배기가스로 방출되어 심각한 대기오염을 야기시킨다는 문제점이 있다.However, in the above purification method, the chemical purification method generates a large amount of nitrogen oxides in the process of dissolving the gold bonding wire scrap in aqua regia, and in the process of reducing and depositing gold by adding concentrated sulfuric acid, a large amount of sulfurous acid gas is used as exhaust gas. There is a problem that they are released and cause serious air pollution.
또한 상기 전해정제 방법은 융융, 주조한 양극표면에 산화 피막이 형성되어 부동태 현상을 초래하기 때문에 분극전압의 상승으로 인한 전해정제 반응이 연속적으로 진행되지 않기 때문에 스크랩을 양극으로 용융, 주조하기 전에 화학정제하여 불순물을 제거하는 과정이 필요하게 되어 이 과정에서 금이 정제공정에 장시간 체류하게 되므로 원재료에 대한 금리의 부담이 높고 설비비가 높다는 단점이 있다.In addition, since the electrolytic refining method forms an oxide film on the surface of the melted and cast anode, which causes a passivation phenomenon, the electrolytic refining reaction does not proceed continuously due to an increase in the polarization voltage. Therefore, the process of removing impurities is required. In this process, gold stays in the refining process for a long time, so the burden of interest rates on raw materials is high and equipment costs are high.
상기와 같은 문제점을 해결하기 위한 본 발명의 목적은 금 본딩 와이어 제조 과정에서 발생하는 금본딩 와이어 스크랩으로부터 순도가 99.995%이상의 고순도 금을 신속하고 용이하게 정제하여, 금 정제공정의 효율을 향상시킬 수 있는 고순도 금 정제방법을 제공하는데 있다.An object of the present invention for solving the above problems is to quickly and easily purify high purity gold having a purity of 99.995% or more from the gold bonding wire scrap generated during the gold bonding wire manufacturing process, to improve the efficiency of the gold refining process To provide a high purity gold purification method.
상기한 바와 같은 목적을 달성하고 종래의 결점을 제거하기 위한 과제를 수행하는 본 발명은 금 본딩 와이어를 제조할 때 사용한 도핑제(Dopant)로 사용한 Ga, Ge, Ca이 불순물 함유되어 있는 금본딩 와이어 스크랩의 정제방법에 있어서,The present invention to achieve the object as described above and to perform the problem to eliminate the conventional defects is a gold bonding wire containing Ga, Ge, Ca as impurities used as a dopant used when manufacturing the gold bonding wire In the purification method of scrap,
Ga, Ge, Ca이 불순물 함유되어 있는 금본딩 와이어 스크랩에 요오드(Iodide)를 첨가하여 혼합한 후 석영관에 장입 후 가열하여 요오드화금(gold Iodie)을 제조한 후, 이를 에틸알콜(Ethyl Alcohol) 또는 에테르(Ether)로 환원·석출 시킨 후 여과하여 순수로 세정하고 건조시켜 고순도 금으로 정제하는 방법을 특징으로 하는 금 본딩 와이어 스크랩으로부터 고순도 금의 정제방법을 제공함으로써 달성된다. Iodide was added to the gold-bonded wire scrap containing Ga, Ge, and Ca, and then mixed, charged in a quartz tube, heated, to prepare gold iodie, and then ethyl alcohol. Or it is achieved by providing a method for purifying high purity gold from gold bonding wire scrap characterized in that the reduction and precipitation with ether, followed by filtration, washing with pure water, drying and purifying with high purity gold.
상기에서 고순도 금은 순도가 99.995% 이상인 것을 특징으로 한다.The high purity gold is characterized in that the purity is more than 99.995%.
상기에서 금본딩 와이어 스크랩 10g 당 요오드 20~30g를 첨가하는 것을 특징으로 한다. In the above it is characterized in that 20 to 30g of iodine is added per 10g of gold bonding wire scrap.
상기 석영관에 혼합 장입 된 금본딩 와이어 스크랩와 요오드는 80∼100℃로 가열하여 180~240분 동안 유지하는 것을 특징으로 한다. The gold-bonded wire scrap and iodine mixed in the quartz tube are heated at 80 to 100 ° C. for 180 to 240 minutes.
상기에서 요오드화 금을 에틸알콜 또는 에테르에 분산시, 요오드화 금 20g당 에틸알콜 또는 에테르 150~200ml에 분산, 용해하여 환원, 석출하는 것을 특징으로 한다. When the gold iodide is dispersed in ethyl alcohol or ether, it is characterized in that it is dispersed, dissolved in 150-200 ml of ethyl alcohol or ether per 20 g of gold iodide, and reduced and precipitated.
상기 환원·석출된 금을 건조시 60~ 70℃로 건조하는 것을 특징으로 한다.The reduced and precipitated gold is characterized in that the drying at 60 ~ 70 ℃.
본 발명은 금 본딩 와이어를 제조할 때 사용한 도핑제(Doppant)로 Ga, Ge, Ca이 불순물 함유되어 있는 금 본딩 와이어 스크랩을 요오드와 혼합한 후 석영관에 장입하고 가열하여 80~100℃를 유지하여 요오드화 금(Gold Iodide)을 제조하는 단계와 요오드화 금을 에틸알콜과 에테르에 분산시켜 금을 환원, 석출시키는 단계로 구성되어 금 정제공정에서 불순물인 Ga, Ge, Ca을 비교적 간단한 과정을 거쳐 제거가 가능하여 이로 인해 고가의 금이 정제공정에 다량으로 체류하게 되는 것을 방지하고, 정제시간을 단축시킴과 동시에, 원재료에 대한 금리의 부담을 절감시키는 효 과를 가진 유용한 발명으로 산업상 그 이용이 크게 기대되는 발명인 것이다.In the present invention, a gold bonding wire scrap containing Ga, Ge, and Ca as an impurity is mixed with iodine and then charged into a quartz tube and heated to maintain 80 to 100 ° C as a dopant used when manufacturing a gold bonding wire. The process consists of preparing gold iodide and dispersing gold iodide in ethyl alcohol and ether to reduce and precipitate gold, thereby removing Ga, Ge and Ca as impurities in the gold refining process. This prevents expensive gold from staying in the refining process, shortens the refining time, and reduces the burden of interest rates on raw materials. It is the invention which is expected greatly.
이하 본 발명의 실시 예인 구성과 그 작용을 첨부도면에 연계시켜 상세히 설명하면 다음과 같다. 또한 본 발명을 설명함에 있어서, 관련된 공지기능 혹은 구성에 대한 구체적인 설명이 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 경우 그 상세한 설명은 생략한다.Hereinafter, the configuration and the operation of the embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.
도 1은 본 발명에 따른 금본딩 와이어 스크랩으로부터 금을 정제하는 한 실시예에 따른 공정도를 도시한 것으로, 본 발명은 금 본딩 와이어를 제조할 때 사용한 도핑제(Dopant)로 사용한 Ga, Ge, Ca이 불순물 함유되어 있는 금본딩 와이어 스크랩에 요오드(Iodide)를 첨가하여 혼합한 후 석영관에 장입 후 80∼100℃로 가열하여 요오드화금(gold Iodie)을 제조한 후 이를 에틸알콜(Ethyl Alcohol) 또는 에테르(Ether)로 환원·석출 시킨 후 여과하여 순수로 세정하고 건조시켜 순도가 99.995% 이상인 고순도 금으로 정제하는 방법이다.1 is a process diagram according to an embodiment of refining gold from a gold bonding wire scrap according to the present invention, the present invention Ga, Ge, Ca used as a dopant (Dopant) used when manufacturing the gold bonding wire Iodide was added to the gold-bonded wire scrap containing impurities, mixed, charged in a quartz tube, heated to 80 to 100 ° C. to prepare gold iodie, and then ethyl alcohol or ethyl alcohol. It is reduced, precipitated with ether, filtered, washed with pure water, dried and purified with high purity gold with a purity of 99.995% or more.
즉, 본 발명은 도핑제인 Ga, Ge, Ca이 불순물로 함유되어 있는 금 본딩 와이어 스크랩에 요오드를 첨가하여 혼합한 후 석영관에 장입하고 가열하여 80∼100℃로 가열 후 유지하여 요오드화 금(Gold Iodide)을 제조하는 과정에서 1차로 주원소인 금과 불순물인 Ga, Ge, Ca를 분리하는 단계를 거친 후, 상기 요오드화 금을 에 틸알콜 또는 에테르에 분산시켜 금을 선택적으로 환원,석출시겨 2차로 불순물을 제거하여 고순도의 금을 정제하는 것이다.That is, the present invention is added to the gold bonding wire scrap containing the dopants Ga, Ge, Ca as impurities, mixed with iodine, charged in a quartz tube, heated to 80 to 100 ℃ and maintained by maintaining gold iodide (Gold) In the process of manufacturing iodide), the gold is first iodide and the impurities Ga, Ge, Ca are separated, and then the gold iodide is dispersed in ethyl alcohol or ether to selectively reduce and precipitate gold. Secondly, impurities are removed to purify gold of high purity.
상기에서 금본딩 와이어 스크랩 10g 당 요오드 20~30g를 첨가한다. 이와같이 한정한 이유는 요오드 첨가량 20g 이하에서는 금본딩 와이어 스크랩이 완전히 요오드화 금으로 변환되지 않으며 30g 이상에서는 완전히 요오드화 금으로 변환되나 요오드의 소모량이 커지므로 스크랩 10g 당 요오드 20~30g를 첨가하면 스크랩을 완전히 요오드화 금으로 변환시킬 수 있다In the above, 20-30 g of iodine is added per 10 g of gold bonding wire scrap. The reason for this limitation is that when the amount of iodine added is less than 20 g, the gold bonding wire scrap is not completely converted to gold iodide. Can be converted to Gold Iodide
또한 석영관에 금본딩 와이어 스크랩에 요오드를 장입하고 온도가 80∼100℃로 180~240분 동안 유지하는데, 그 이유는 스크랩을 완전히 요오드화 금으로 변환시키기 위함으로, 온도 80℃ 이하에서는 요오드화 금으로 변화시키는 온도유지 시간이 너무 길어지고, 100℃이상에서는 요오드화 금으로 변화되기 때문에 온도를 더 이상 높힐 필요가 없가. 따라서, 온도가 80∼100℃가 적절하였다. 이에 따라 80℃에서는 240분간, 100℃에서 180분간 유지하면 완전히 요오드화 금으로 변화되었다.In addition, iodine is charged into a gold-bonded wire scrap into a quartz tube and maintained at a temperature of 80 to 100 ° C. for 180 to 240 minutes, because it completely converts the scrap into gold iodide. The temperature holding time to change is too long, and it changes to gold iodide above 100 ℃, so there is no need to increase the temperature anymore. Therefore, 80-100 degreeC of temperature was appropriate. As a result, the result was completely changed to gold iodide when maintained at 80 ° C for 240 minutes and at 100 ° C for 180 minutes.
또한 요오드화 금을 에틸알콜 또는 에테르에 분산시킨다는 것은 비이커에 에틸알콜 또는 에테르를 넣은 후 요드화 금을 장입하고 교반하면 요오드화 금이 서서히 용해하면서 금으로 환원, 석출하게 된다. 이때 요오드화 금 및 에틸알콜 또는 에테르의 반응양은 요오드화 금 20g 당 에틸알콜 또는 에테르 150∼200ml를 투입한다. 이와 같은 비율일때 요오드화 금이 서서히 용해하면서 금으로 완전히 환원, 석출한다.In addition, dispersing gold iodide in ethyl alcohol or ether, after adding ethyl alcohol or ether to a beaker and charging and stirring gold iodide, gold iodide is gradually dissolved and reduced and precipitated into gold. At this time, the reaction amount of gold iodide and ethyl alcohol or ether is added 150-200 ml of ethyl alcohol or ether per 20 g of gold iodide. At such a ratio, gold iodide slowly dissolves and precipitates completely into gold.
또한 건조시 60~70℃를 유지하는데, 60℃이하에서는 수분이 완전히 건조될 때 걸리는 시간이 오래 걸리며 70℃보다 온도가 높아지면 완전히 건조되는 시간이 단축되나 약간씩 산화피막이 형성되는 문제점이 있다. In addition, when the drying is maintained at 60 ~ 70 ℃, it takes a long time when the moisture is completely dried below 60 ℃, and when the temperature is higher than 70 ℃ is a short time to dry completely, but there is a problem that the oxide film is formed slightly.
이하 본 발명을 실시예를 통하여 상세히 설명하면 다음과 같다. Hereinafter, the present invention will be described in detail with reference to the following Examples.
실시예 1Example 1
도핑제인 Ga 350ppm, Ge 280ppm, Ca 115ppm이 불순물로 함유 금 본딩 와이어 스크랩 10g과 요오드 20∼30g을 혼합하여 석영관에 장입하고 온도를 100℃ 로 240분 동안 유지하여 요오드화 금을 제조하여 이를 에틸알콜 200ml에 분산하여 60분간 금을 환원, 석출하였다. 환원된 금을 여과, 세척하여 70℃로 건조하여 원자흡광 분석법으로 불순물의 함유량을 분석한 결과 환원, 석출된 금 중에는 불순물로 Ga 12ppm, Ge 8ppm, Ca 5ppm이 함유되어 있어 금의 순도는 99.995% 이상이었다.Dopant Ga 350ppm, Ge 280ppm, Ca 115ppm is mixed with impurities 10g of gold bonding wire scrap and 20-30g of iodine, charged in a quartz tube and maintained at 100 ℃ for 240 minutes to prepare gold iodide, which is ethyl alcohol Dispersion was carried out in 200 ml, and gold was reduced and precipitated for 60 minutes. After filtering and washing the reduced gold and drying it at 70 ℃, the content of impurities was analyzed by atomic absorption spectrometry. The reduced and precipitated gold contained Ga 12ppm, Ge 8ppm and Ca 5ppm as impurities, so the purity of gold was 99.995%. It was above.
실시예 2Example 2
도핑제인 Ga 420ppm, Ge 310ppm, Ca 130ppm이 불순물로 함유 금 본딩 와이어 스크랩 10g과 요오드 20∼30g을 혼합하여 석영관에 장입하고 온도를 100℃ 로 240분 동안 유지하여 요오드화 금을 제조하여 이를 에테르 200ml에 분산하여 60분간 금을 환원, 석출하였다. 환원된 금을 여과, 세척하여 70℃로 건조하여 원자흡광 분석법으로 불순물의 함유량을 분석한 결과 환원, 석출된 금 중에는 불순물로 Ga 26ppm, Ge 12ppm, Ca 9ppm이 함유되어 있어 금의 순도는 99.9953% 이상이었다.Ga 420ppm, Ge 310ppm, Ca 130ppm containing dopant 10g of gold bonding wire scrap and 20-30g of iodine were mixed with impurity, charged in quartz tube and maintained at 100 ° C for 240 minutes to prepare gold iodide, which was then 200ml of ether. Dispersed in, and the gold was reduced and precipitated for 60 minutes. After filtering and washing the reduced gold and drying it at 70 ℃, the content of impurities was analyzed by atomic absorption spectrometry. The reduced and precipitated gold contained Ga 26ppm, Ge 12ppm and Ca 9ppm as impurities, so the purity of gold was 99.9953%. It was above.
본 발명은 상술한 특정의 바람직한 실시 예에 한정되지 아니하며, 청구범위에서 청구하는 본 발명의 요지를 벗어남이 없이 당해 발명이 속하는 기술분야에서 통상의 지식을 가진 자라면 누구든지 다양한 변형실시가 가능한 것은 물론이고, 그와 같은 변경은 청구범위 기재의 범위 내에 있게 된다. The present invention is not limited to the above-described specific preferred embodiments, and various modifications can be made by any person having ordinary skill in the art without departing from the gist of the present invention claimed in the claims. Of course, such changes will fall within the scope of the claims.
도 1은 본 발명에 따른 금본딩 와이어 스크랩으로부터 금을 정제하는 공정도이다.1 is a process chart for refining gold from the gold bonding wire scrap according to the present invention.
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| KR890002443A (en) * | 1987-07-14 | 1989-04-10 | 다나까 준-이찌로 | Gold refining method and apparatus |
| JP2005307271A (en) | 2004-04-21 | 2005-11-04 | Dowa Mining Co Ltd | Method for producing high purity gold |
| JP2007016259A (en) | 2005-07-05 | 2007-01-25 | Kyoei Metal Kk | System for collecting gold while recycling iodine ion in gold-removing liquid |
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| KR890002443A (en) * | 1987-07-14 | 1989-04-10 | 다나까 준-이찌로 | Gold refining method and apparatus |
| JP2005307271A (en) | 2004-04-21 | 2005-11-04 | Dowa Mining Co Ltd | Method for producing high purity gold |
| JP2007016259A (en) | 2005-07-05 | 2007-01-25 | Kyoei Metal Kk | System for collecting gold while recycling iodine ion in gold-removing liquid |
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