TW201416459A - Manufacturing method of a high purity Au target through a recycle of Au spent target by sintering process - Google Patents

Manufacturing method of a high purity Au target through a recycle of Au spent target by sintering process Download PDF

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Publication number
TW201416459A
TW201416459A TW102138035A TW102138035A TW201416459A TW 201416459 A TW201416459 A TW 201416459A TW 102138035 A TW102138035 A TW 102138035A TW 102138035 A TW102138035 A TW 102138035A TW 201416459 A TW201416459 A TW 201416459A
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Taiwan
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target
powder
waste
purity
gold
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TW102138035A
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Chinese (zh)
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Dong-Han Kang
Won-Kyu Yoon
Seung-Ho Yang
Gil-Su Hong
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Hee Sung Metal Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F8/00—Manufacture of articles from scrap or waste metal particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2202/00—Treatment under specific physical conditions
    • B22F2202/13—Use of plasma
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Abstract

The present invention is related to a manufacturing method of Au target which is widely used in a semiconductor RDL(Redistributed Layer) or Bump and in particular, it is related to a method for manufacturing including a step for laminating powder on a waste target. A wet method which is a conventional Au target manufacturing method includes a melting process using nitrohydrochloric acid. Thus, it takes much time to perform processes because of recovery due to the melting process. According to the present invention, reduction of a production time and cost is realized since a waste target is used and thus, the present invention is very effective in terms of a cost and a process time. In order to realize these purposes, the present invention is characterized in that a surface treatment of a waste target is performed, high purity powder is produced within a very short time by using plasma which is a kind of a dry process for a power production, and Au target of high purity is produced by injecting produced high purity powder into the waste target.

Description

利用燒結製程通過回收廢棄的黃金標靶製造一種高純度黃金標靶的方法 Method for producing a high-purity gold target by recycling a discarded gold target using a sintering process

本發明是一種使用廢棄的黃金標靶的回收技術，亦即，本發明係關於一種藉由使用高於30%之廢棄的黃金標靶製造黃金標靶的方法，以及填佈高純度粉末及燒結製程的步驟。尤其，本發明係關於廢棄的黃金標靶之表面洗滌的前製程，以及一種製造具有高純度細化晶粒之黃金標靶的方法。 The present invention is a recycling technique using a discarded gold target, that is, the present invention relates to a method for producing a gold target by using a gold target of more than 30% of waste, and filling a high-purity powder and sintering The steps of the process. In particular, the present invention relates to a pre-process for surface cleaning of discarded gold targets, and a method of making a gold target having high purity refinement grains.

黃金標靶已被廣泛地運用於重分佈層(RDI)或凸塊。重分佈層(RDI)製程是一種簡單改變一半導體晶片之輸入及輸出終端的製程。就NAND快閃記憶體而言，焊墊被排列在其中央部位，因此在層壓時封裝變得複雜且線路長度變長。結果，降低了製程速度。為了解決此問題，係運用將焊墊配置於邊緣部位使層壓更加容易的製程。此製程即為重分佈層(RDI)製程。 Gold targets have been widely used in redistribution layers (RDI) or bumps. The redistribution layer (RDI) process is a process that simply changes the input and output terminals of a semiconductor wafer. In the case of NAND flash memory, the pads are arranged at the center thereof, so that the package becomes complicated and the line length becomes long at the time of lamination. As a result, the process speed is reduced. In order to solve this problem, a process in which the bonding pad is disposed on the edge portion to make lamination easier is employed. This process is the redistribution layer (RDI) process.

就半導體封裝製程而言，這是有利的，但在黏 著製程中會產生金屬剝離的現象。若金屬厚度太薄，此現象會產生問題。為了因應此問題，需要經由濺射形成均勻的黃金標靶薄膜。 In terms of semiconductor packaging process, this is advantageous, but in the stick Metal peeling occurs during the manufacturing process. This phenomenon can cause problems if the metal thickness is too thin. In order to cope with this problem, it is necessary to form a uniform gold target film by sputtering.

凸塊製程是一種後處理，其中一晶圓片及一外部電路的電性接觸不是在半導體封裝及組裝製程中透過習見的線路焊接而連接，而是藉由形成金屬凸塊而傳送一電子信號。近來，由於半導體晶片領域需要高品質功能、高整合性及輕薄、短小的形式，習見技術往往不能符合快速改變的需求。凸塊技術浮現作為新的替代方案。 The bump process is a post-processing in which electrical contact between a wafer and an external circuit is not connected through conventional wire bonding in a semiconductor package and assembly process, but an electronic signal is transmitted by forming a metal bump. . Recently, since the field of semiconductor wafers requires high-quality functions, high integration, and a thin, short form, the conventional technology often fails to meet the rapidly changing needs. Bump technology emerges as a new alternative.

隨著半導體製程急遽的發展，黃金標靶的特性迫切地需要改善。在半導體薄膜形成製程中，需要產生具有細化晶粒之黃金標靶以及製造一高純度標靶以控制均勻厚度及在表面的不純物質，另外，隨著使用量逐漸增加，必須認真考量回收使用過的標靶來降低成本。 With the rapid development of semiconductor processes, the characteristics of gold targets are urgently needed to be improved. In the semiconductor thin film formation process, it is necessary to produce a gold target with fine grains and to manufacture a high-purity target to control uniform thickness and impurities on the surface. In addition, as the usage increases, it must be carefully considered for recycling. Targets have been reduced to reduce costs.

為了解決上述問題，本發明的目標是藉由使用廢棄的黃金標靶，製造高純度細化粉末以填入到一廢棄標靶，並進行燒結以清洗表面。為了達成上述目標，本發明提供一種方法，係去除存在於一廢棄標靶表面的不純物質，運用電漿法產生高純度粉末，以及藉由熱壓製程產生一包含高純度細化晶粒的標靶。 In order to solve the above problems, an object of the present invention is to produce a high-purity refined powder by using a discarded gold target to be filled into a waste target and sintered to clean the surface. In order to achieve the above object, the present invention provides a method for removing impure substances present on the surface of a discarded target, producing a high-purity powder by a plasma method, and producing a high-purity refined grain by a hot pressing process. target.

為了達成上述目標，本發明藉由使用廢棄的黃金標靶讓回收能夠實現，藉由申請將氮處理用於一廢棄標靶表面而去除不純物質，以及經由一電漿製程產生將要注入到廢棄標靶的粉末。根據本發明產生的粉末，係在洗滌製程後被注入或經由使用高純度量而產生。 In order to achieve the above object, the present invention enables recycling by using a discarded gold target, which removes impurities by applying nitrogen treatment to a waste target surface, and generates a waste to be injected through a plasma process. The powder of the target. The powder produced according to the present invention is injected after the washing process or produced by using a high purity amount.

藉由使用電漿法去除剩餘不純的物質後，可藉由增加電漿溫度而獲得蒸發粉末。 After removing the remaining impure material by using the plasma method, the evaporated powder can be obtained by increasing the plasma temperature.

茲將說明根據本發明之藉由回收廢棄的黃金標靶製造高純度的黃金標靶的方法。此方法包括一剝離廢棄標靶的步驟、一去除附著於表面之不純物質的步驟、一產生將被額外注入之高純度粉末的步驟、一將高純度粉末填佈到廢棄標靶及進行燒結的步驟、以及一使用燒結物進行洗滌製程的步驟。 A method of producing a high-purity gold target by recycling a discarded gold target according to the present invention will be explained. The method includes a step of stripping the waste target, a step of removing the impure substance attached to the surface, a step of producing a high-purity powder to be additionally injected, a high-purity powder being filled to the waste target, and sintering. And a step of performing a washing process using the sinter.

如上所述，本發明的特點在於藉由回收製程來製造用於一半導體重分佈層(RDI)或凸塊的黃金標靶。 As described above, the present invention is characterized in that a gold target for a semiconductor redistribution layer (RDI) or bump is fabricated by a recycling process.

根據本發明之標靶是由層壓一在廢棄標靶的新供應的粉末所製造而成。因此大大減少製程時間及製造成本。 The target according to the invention is manufactured by laminating a freshly supplied powder in a waste target. Therefore, the process time and manufacturing cost are greatly reduced.

S10‧‧‧剝離 S10‧‧‧ stripping

S20‧‧‧去除銦及不純的物質 S20‧‧‧Removal of indium and impure substances

S30‧‧‧製造粉末 S30‧‧‧Manufacture of powder

S40‧‧‧燒結 S40‧‧‧Sintering

S50‧‧‧黏著製程 S50‧‧‧ adhesive process

第1圖係顯示一根據本發明藉由使用一廢棄標靶產生高純度黃金標靶之工作程序的圖示。 Figure 1 is a graphical representation of a working procedure for producing a high purity gold target by using a waste target in accordance with the present invention.

第2圖係顯示一根據本發明由電漿產生黃金粉末FESEM影像的圖示。 Figure 2 is a graphical representation of a FESEM image of a gold powder produced from a plasma in accordance with the present invention.

第3圖係顯示一根據本發明的熱壓製程產生黃金標靶OM影像的圖示。 Figure 3 is a graphical representation of a gold target OM image produced by a hot stamping process in accordance with the present invention.

以下將參考附圖與實施例詳細說明本發明。 The invention will be described in detail below with reference to the accompanying drawings and embodiments.

第1圖係顯示一根據本發明藉由使用一廢棄標靶產生高純度黃金標靶之工作程序的圖示。第2圖係顯示一根據本發明由電漿產生黃金粉末FESEM影像的圖示。第3圖係顯示一根據本發明的熱壓製程產生黃金標靶OM影像的圖示。 Figure 1 is a graphical representation of a working procedure for producing a high purity gold target by using a waste target in accordance with the present invention. Figure 2 is a graphical representation of a FESEM image of a gold powder produced from a plasma in accordance with the present invention. Figure 3 is a graphical representation of a gold target OM image produced by a hot stamping process in accordance with the present invention.

本發明係關於一種利用燒結製程通過回收廢棄的黃金標靶製造一種高純度黃金標靶的方法，包括回收廢棄標靶以產生標靶時剝離廢棄的標靶的步驟(S10)、去除附著於一表面之不純物質的步驟(S20)、產生將被額外注入之高純度粉末的步驟(S30)、將高純度粉末填佈到廢棄的標靶並進行燒結的步驟(S40)、以及使用一燒結物進行洗滌製程的步驟(S50)。 The invention relates to a method for manufacturing a high-purity gold target by recycling a discarded gold target by using a sintering process, comprising the steps of removing the discarded target to remove the discarded target when the target is generated (S10), and removing the attached one. a step of impure substance on the surface (S20), a step of producing a high-purity powder to be additionally injected (S30), a step of filling a high-purity powder to a waste target and sintering (S40), and using a sintered body The step of performing the washing process (S50).

具體而言，首先，進行廢棄標靶的剝離製程(S10)。 Specifically, first, a peeling process for discarding the target is performed (S10).

在攝氏200-250度(℃)執行一剝離製程，並且將一高溫使用的膠帶附著到廢棄標靶以便防止在此製程前由於銦及不純物質的汙染。在附加後的階段增加攝氏5-10度(℃)使溫度增加到攝氏200-250度(℃)。若一溫度快速增加攝氏10度(℃)以上，可能會產生焊墊板變形，因此，溫度的增加要少於攝氏10度(℃)。若溫度達到攝氏200-250度(℃)，維持這樣的溫度30分鐘並且執行一剝離製程。在剝離製程期間，必須將表面上的銦與一黏著邊完全去除。若銦去除製程的時間持續比預期更長，且銦在剝離製程期間沒有完全被去除，銦將與燒結期間一樣是不純物質。因此，可能會有銦造成標靶特性變差的風險。就廢棄標靶之剝離製程而言，係使用硝酸或硝基鹽酸(S20)來去除銦或表面污染物。 A stripping process is performed at 200-250 degrees Celsius (° C.), and a high temperature used tape is attached to the waste target to prevent contamination by indium and impurities before the process. Increasing the temperature by 5-10 degrees Celsius (°C) in the post-addition phase increases the temperature to 200-250 degrees Celsius (°C). If a temperature increases rapidly by 10 degrees Celsius (°C) or more, the pad may be deformed. Therefore, the temperature increase is less than 10 degrees Celsius (°C). If the temperature reaches 200-250 degrees Celsius (° C.), the temperature is maintained for 30 minutes and a stripping process is performed. During the stripping process, the indium on the surface must be completely removed with an adhesive edge. If the indium removal process lasts longer than expected and indium is not completely removed during the stripping process, the indium will be as pure as during sintering. Therefore, there may be a risk that indium causes the target characteristics to deteriorate. For the stripping process of the waste target, nitric acid or nitrohydrochloric acid (S20) is used to remove indium or surface contaminants.

藉由注入廢棄標靶到硝酸以去除剩餘的銦或表面汙染物。 The remaining indium or surface contaminants are removed by injecting the waste target to nitric acid.

首先，將廢棄標靶注入到硝酸後，維持此狀況1-3小時。在製程維持期間，會確認是否消除黏著到一表面上的不純物質。每小時擷取一片實驗片進行ICP分析。若分析值高於99.995重量百分比(wt%)，該製程進入下一程序。若分析值低於99.995重量百分比(wt%)，再次執行硝酸製程。 First, after the waste target is injected into the nitric acid, the condition is maintained for 1-3 hours. During process maintenance, it is confirmed whether or not the impurities adhering to a surface are eliminated. One piece of experimental piece was taken every hour for ICP analysis. If the analytical value is higher than 99.995 weight percent (wt%), the process proceeds to the next procedure. If the analytical value is less than 99.995 weight percent (wt%), the nitric acid process is performed again.

藉由電漿法產生即將注入的廢棄標靶粉末 (S30)。 Producing waste target powder to be injected by plasma method (S30).

使用電漿設備來產生所述粉末。使用電漿將高於99.995重量百分比(wt%)之廢棄標靶或顆粒進行切割並在一個大氣壓力下注入到一腔體內。此時，將被注入的重量應該不超過500-2000克。若被注入的重量低於500克，電漿將與坩堝一起反應，而可能導致坩堝的破損。如被注入的重量超過2000克，一溶融的金屬將溢出到坩堝外，因此，有可能黏著到腔體上。在使用一旋轉幫浦降低壓力到5.0×10-2陶爾(torr)經由注入氬氣(Ar)形成氬氣環境。電漿係藉由注入成型和高純度的W電極棒而形成，藉此產生黃金粉末。藉由注入原料及提供低的功耗(低於30瓩)並執行簡單的熔融而形成電漿。接著，不純物質即被去除。此時，具低溶融溫度的不純物質經由調整電漿功率到低位準而蒸發，然後藉由真空裝置將其去除到外面。特別是，這可以有效的去除標靶生產過程中使用的銦。 A plasma device is used to produce the powder. The spent target or granules above 99.995 weight percent (wt%) are cut using a plasma and injected into a chamber at an atmospheric pressure. At this time, the weight to be injected should not exceed 500-2000 grams. If the injected weight is less than 500 grams, the plasma will react with the ruthenium and may cause damage to the ruthenium. If the injected weight exceeds 2000 grams, a molten metal will spill out of the crucible and, therefore, may stick to the cavity. The argon atmosphere was formed by injecting argon (Ar) by using a rotary pump to reduce the pressure to 5.0 x 10 -2 torr. The plasma is formed by injection molding and a high-purity W electrode rod, thereby producing a gold powder. The plasma is formed by injecting the raw material and providing low power consumption (less than 30 Å) and performing simple melting. Then, the impurities are removed. At this time, the impurity having a low melting temperature evaporates by adjusting the plasma power to a low level, and then is removed to the outside by a vacuum device. In particular, this can effectively remove the indium used in the target production process.

在不純物質去除後，經由功率增加而產生高純度粉末。此時，藉由將功率增加到15-25瓩(Kw)而產生粉末。再者，藉由使用氬氣或一包含氬氣及氮氣的混合氣體作為電漿氣體而產生粉末。粉末的生產時間持續30-60分鐘並在大氣壓力(760陶爾(torr))下被回收。接著進行分配以確保生產粉末的均勻性。以150目數(mesh)的分配網格進行分配並使用低於150目數之粉末燒結。再次使用高於150目 數的粉末以生產新的粉末。 After the removal of the impurities, a high purity powder is produced via an increase in power. At this time, the powder was produced by increasing the power to 15-25 瓩 (Kw). Further, a powder is produced by using argon gas or a mixed gas containing argon gas and nitrogen gas as a plasma gas. The powder is produced for 30-60 minutes and is recovered at atmospheric pressure (760 torr). The dispensing is then carried out to ensure uniformity of the produced powder. The distribution was carried out with a mesh mesh of 150 mesh and sintered using a powder of less than 150 mesh. Use again above 150 mesh A number of powders are used to produce new powders.

藉由注入已去除不純物質之廢棄標靶並使用熱壓製法進行燒結(S40)。 The sintering is performed by injecting a waste target from which the impurity has been removed and using a hot pressing method (S40).

首先，將一廢棄標靶注入到一碳模具後填佈新的粉末。所注入粉末為最終標靶重量的110-120%。若一廢棄標靶及粉末的重量低於110%，可能無法在最後製程達到想要的標靶厚度。如注入的重量高於120%，則製程時間將會持續很長一段時間。此外，由於製程過程中邊角料的增加，使得回收時間及成本增加。在填充一廢棄標靶並粉末填入一碳模具之後，將其引入熱壓腔體，藉由一真空泵執行減壓。此時，真空環境乃被排出直到5.0×10-4陶爾(torr)的狀態且執行燒結。此燒結的溫度為攝氏650-750度(℃)，時間持續5-15小時。施加10至20MPa的壓力。燒結完成後，若腔體溫度低於攝式100度(℃)，即擷取一燒結物。如該擷取之燒結物其相對密度高於99.0%，終極程序完成。如該擷取之燒結物其相對密度低於99.0%，在一薄膜形成過程中可能產生顆粒或結節。該燒結物於粉末製程中將被再次使用。 First, a waste target is injected into a carbon mold and a new powder is filled. The injected powder is 110-120% of the final target weight. If the weight of a discarded target and powder is less than 110%, it may not be possible to achieve the desired target thickness in the final process. If the injected weight is higher than 120%, the process time will last for a long time. In addition, due to the increase in scrap during the process, the recovery time and cost increase. After filling a waste target and filling the powder into a carbon mold, it is introduced into a hot press chamber, and decompression is performed by a vacuum pump. At this time, the vacuum environment was discharged to a state of 5.0 × 10 -4 torr and sintering was performed. The sintering temperature is 650-750 degrees Celsius (° C.) for a period of 5-15 hours. A pressure of 10 to 20 MPa is applied. After the sintering is completed, if the temperature of the cavity is lower than 100 degrees (° C.), a sintered product is taken. If the drawn sinter has a relative density higher than 99.0%, the ultimate procedure is completed. If the drawn sinter has a relative density of less than 99.0%, particles or nodules may be formed during film formation. The sinter will be reused in the powder process.

使用燒結物進行黏著製程(S50)。 The sinter is used for the adhesion process (S50).

附著於燒結物表面的碳藉由一車床移除後，進行黏著製程。黏著程序係藉由於在攝氏200-250度(℃)使用銦進行黏著。黏著後藉由超音波測量黏著率。測得的黏著率必須在99.0%以上。若黏著率低於99.0%，於剝離製程後 要再次執行黏著製程。黏著後經由使用一車床而獲得最終的厚度。在經過處理標靶的背板上進行焊珠製程。該處理標靶在半導體洗滌後被封裝。 The carbon attached to the surface of the sinter is removed by a lathe and then adhered. The adhesion procedure is by adhesion using indium at 200-250 degrees Celsius (°C). Adhesion is measured by ultrasonic waves after adhesion. The measured adhesion rate must be above 99.0%. If the adhesion rate is lower than 99.0%, after the stripping process To perform the adhesive process again. The final thickness is obtained by using a lathe after adhesion. The bead process is performed on the back sheet of the treated target. The treatment target is encapsulated after semiconductor cleaning.

[具體實施例] [Specific embodiment]

針對4英吋用過的廢棄標靶500克進行一剝離流程。使用前標靶的大小、厚度及重量分別為4英吋、5毫米及780克。在將廢棄標靶的溫度維持在攝氏230度約30分鐘後執行一剝離流程。於解離後，殘留於標靶表面上的銦在剝離流程後被去除。銦去除後之廢棄標靶被注入到一含有氮氣的燒杯以至於剩餘的銦及不純物質可被去除。去除銦及不純物質所需時間持續2小時。使用ICP對不純物質進行分析，結果顯示可確保99.998重量百分比(wt%)的純度。新注射的粉末藉由電漿設備而產生。700克的黃金廢棄標靶被注入到一坩鍋作為一晶錠。藉由一旋轉幫浦降低壓力到5.0×10-2陶爾(torr)後，藉由注入氬氣(Ar)形成氬氣環境。藉由在一注入的模具及一高純度的W電極棒形成電漿而產生黃金粉末。在最初階段，藉由5瓩(kw)功率去除廢棄標靶所殘留不純物質並藉由將使用功率增加為15瓩(kw)而產生細化的高純度粉末。該黃金粉末製造流程調整使用電漿之電力如表1所示。藉由使用電漿產生500克粉末，並藉由配置所產生的粉末而能確保有440克之150目數的粉末。為了進行比較，將使用功率增加至25瓩(kw)來產生粉末。該生產流程如表2 所示。 A stripping process was performed for 500 grams of the discarded target of 4 inches. The size, thickness and weight of the target before use were 4 inches, 5 mm and 780 grams, respectively. A stripping process was performed after maintaining the temperature of the discarded target at 230 degrees Celsius for about 30 minutes. After dissociation, the indium remaining on the target surface is removed after the stripping process. The waste target after indium removal is injected into a beaker containing nitrogen so that the remaining indium and impurities can be removed. The time required to remove indium and impurities is 2 hours. Analysis of the impurities using ICP showed that 99.998 weight percent (wt%) purity was ensured. The newly injected powder is produced by a plasma device. A 700 gram gold waste target was injected into a crucible as an ingot. After the pressure was reduced to 5.0 × 10 -2 torr by a rotary pump, an argon atmosphere was formed by injecting argon (Ar). The gold powder is produced by forming a plasma in an injection mold and a high-purity W electrode rod. In the initial stage, the impurity remaining in the waste target is removed by 5 瓩 (kw) power and a refined high-purity powder is produced by increasing the power used to 15 瓩 (kw). The gold powder manufacturing process adjusts the electricity used by the plasma as shown in Table 1. By using a plasma to produce 500 grams of powder, and by arranging the resulting powder, it is possible to ensure 440 grams of 150 mesh powder. For comparison, the power used was increased to 25 瓩 (kw) to produce a powder. The production process is shown in Table 2.

所製得粉末之功率純度、平均粉末大小及碳含量如表3所示。 The power purity, average powder size and carbon content of the obtained powder are shown in Table 3.

由表3的結果可以清楚看出，在由電漿法所產生的黃金粉末條件下，確保可得6-10微米(μm)之球狀粉末。另外，純度可確保99.995-99.998重量百分比(wt%)。當功率增加時，碳含量會快速增加。當功率增加時，存在於坩堝表面之碳即用以重製粉末，因此增加碳含量。當用以重製粉末之碳含量增加時，可能影響到使用最終標靶之薄膜形成過程中顆粒的形成。 As is clear from the results of Table 3, it was confirmed that a spherical powder of 6 to 10 μm was obtained under the conditions of the gold powder produced by the plasma method. In addition, the purity can ensure 99.995-99.998 weight percent (wt%). As the power increases, the carbon content increases rapidly. When the power is increased, the carbon present on the surface of the crucible is used to reconstitute the powder, thus increasing the carbon content. When the carbon content used to reconstitute the powder increases, it may affect the formation of particles during film formation using the final target.

第2圖係顯示由電漿產生之黃金粉末的FESEM結果。依第2圖所示結果極為明顯，如黃金粉末係由電漿產生，即可認定其為10微米(μm)之球狀粉末。 Figure 2 shows the FESEM results for the gold powder produced by the plasma. The results shown in Figure 2 are extremely obvious. For example, if the gold powder is produced by plasma, it can be considered as a spherical powder of 10 micrometers (μm).

440克新產生的粉末注入500克之廢棄標靶以執行燒結製程。燒結製程執行時燒結溫度為攝氏650度(℃)、攝氏700度(℃)、及攝氏750度(℃)，持續時數達10小時且壓力為15Mpa。燒結之結果顯示於表4。 440 grams of the newly produced powder was injected into a 500 gram waste target to perform a sintering process. The sintering process was performed at a temperature of 650 ° C (°C), 700 ° C (°C), and 750 ° C (°C) for 10 hours and a pressure of 15 MPa. The results of sintering are shown in Table 4.

從表4的結果可以清楚地看出，在溫度為攝氏750度(℃)、維持時數達10小時以及壓力為15MPa的條件下，可確保一高密度的燒結物，其相對密度高於99.5%以上。第3圖顯示一經由實施例3產生的細微的燒結物結構。 It can be clearly seen from the results in Table 4 that a high-density sintered product having a relative density higher than 99.5 can be ensured at a temperature of 750 ° C (° C.), a maintenance time of 10 hours, and a pressure of 15 MPa. %the above. Figure 3 shows a fine sintered structure produced via Example 3.

S10‧‧‧剝離 S10‧‧‧ stripping

S20‧‧‧去除銦及不純的物質 S20‧‧‧Removal of indium and impure substances

S30‧‧‧製造粉末 S30‧‧‧Manufacture of powder

S40‧‧‧燒結 S40‧‧‧Sintering

S50‧‧‧黏著製程 S50‧‧‧ adhesive process

Claims (6)

一種利用燒結製程通過回收廢棄黃金標靶製成高純度黃金標靶之製造方法，包含：(a)藉由回收廢棄標靶而重製標靶時剝離廢棄標靶的步驟；(b)去除附著表面之不純物質的步驟；(c)生產用以額外注入之高純度粉末的步驟；(d)填佈高純度粉末至廢棄標靶內且執行燒結的步驟；以及(e)執行完成並使用燒結物進行洗滌的步驟。 A manufacturing method for producing a high-purity gold target by recycling a waste gold target by using a sintering process, comprising: (a) a step of peeling off the waste target when the target is reworked by recycling the waste target; (b) removing the adhesion a step of impure a substance on the surface; (c) a step of producing a high-purity powder for additional injection; (d) a step of filling a high-purity powder into the waste target and performing sintering; and (e) performing and using sintering The step of washing. 如申請專利範圍第1項所述利用燒結製程通過回收廢棄黃金標靶製成高純度黃金標靶之製造方法，其中該附著於廢棄標靶之不純物質係使用硝酸或硝酸氯化氫酸去除。 The method for manufacturing a high-purity gold target by recycling a waste gold target by using a sintering process as described in the first aspect of the patent application, wherein the impurity substance attached to the waste target is removed by using nitric acid or nitric acid hydrogen chloride. 如申請專利範圍第1項所述利用燒結製程通過回收廢棄黃金標靶製成高純度黃金標靶之製造方法，其中被製造並額外注入之粉末為10微米(μm)結晶粒子之球狀粉末。 A method for producing a high-purity gold target by recycling a waste gold target by a sintering process as described in the first aspect of the patent application, wherein the powder produced and additionally injected is a spherical powder of 10 micrometer (μm) crystal particles. 如申請專利範圍第1項所述利用燒結製程通過回收廢棄黃金標靶製成高純度黃金標靶之製造方法，其中被產生並額外注入之高純度粉末的純度為99.995重量百分比(wt%)。 A method for producing a high-purity gold target by recycling a waste gold target by a sintering process as described in the first aspect of the patent application, wherein the purity of the high-purity powder produced and additionally injected is 99.995 weight% (wt%). 如申請專利範圍第1項所述利用燒結製程通過回收廢棄黃金標靶製成高純度黃金標靶之製造方法，其中藉由額外注入已製成之高純度粉末執行燒結處理，該粉末額外注入至廢棄標靶之溫度為攝氏650-750度(℃)。 A method for producing a high-purity gold target by recycling a waste gold target by using a sintering process as described in claim 1, wherein the sintering process is performed by additionally injecting the prepared high-purity powder, and the powder is additionally injected into The temperature of the discarded target is 650-750 degrees Celsius (°C). 如申請專利範圍第1項所述利用燒結製程通過回收廢棄黃金標靶製成高純度黃金標靶之製造方法，其中產生的燒結物其相對密度為99.5%。 The manufacturing method for producing a high-purity gold target by recycling a waste gold target by using a sintering process as described in the first aspect of the patent application, wherein the sintered body has a relative density of 99.5%.
TW102138035A 2012-10-26 2013-10-22 Manufacturing method of a high purity Au target through a recycle of Au spent target by sintering process TW201416459A (en)

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