WO2014065452A1 - Method for preparing high-purity au target by recycling waste au target through sintering - Google Patents

Method for preparing high-purity au target by recycling waste au target through sintering Download PDF

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WO2014065452A1
WO2014065452A1 PCT/KR2012/008954 KR2012008954W WO2014065452A1 WO 2014065452 A1 WO2014065452 A1 WO 2014065452A1 KR 2012008954 W KR2012008954 W KR 2012008954W WO 2014065452 A1 WO2014065452 A1 WO 2014065452A1
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target
powder
waste
purity
recycling
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PCT/KR2012/008954
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French (fr)
Korean (ko)
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강동한
윤원규
양승호
홍길수
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희성금속 주식회사
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Publication of WO2014065452A1 publication Critical patent/WO2014065452A1/en

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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

Definitions

  • the present invention relates to a recycling method using Au waste targets, and to a method of manufacturing an Au target through a sintering process by filling powders of high purity using Au waste targets used more than 30%, and the surface through the Au waste target pretreatment process.
  • the present invention relates to a method for preparing an Au target having fine grains of cleansing and high purity.
  • Au targets are widely used for RDL (Redistributed Layer) or Bump.
  • the process for RDL is a process of changing a semiconductor chip input / output terminal to a package easily.
  • NAND flash has a problem in that the pad position is located in the center, so that when the lamination is complicated, the package becomes complicated and the wire length becomes longer, thereby decreasing the speed.
  • RLD process is used to facilitate stacking by placing pads at edges.
  • the semiconductor packaging process is advantageous, but the metal breaks during bonding. There is a problem that occurs mainly when the metal thickness is thin. To compensate for this, the Au target through sputtering must be uniformly formed.
  • Bumping is a post-semiconductor process that delivers electrical signals by forming bump-shaped metals without connecting the electrical contacts of the wafer house and external circuits with conventional bonding wires during semiconductor packaging and assembly. Recently, as semiconductor chips have been improved in high performance, high integration, and shorter and lighter, bumping technology has emerged as an alternative to the conventional wire method.
  • the Au target used is also required to improve performance.
  • the crystal grains of the Au target are fine and a high purity target is required.
  • a method of recycling the used target is required to reduce costs.
  • an object of the present invention is to clean the surface by using the Au waste target, characterized in that the fine and high-purity powder after the filling in the waste target after sintering.
  • to remove impurities contaminated on the surface of the waste target to provide a method of manufacturing a target having a high purity fine grains through the hot press process after manufacturing a high purity powder using a plasma.
  • the present invention it is possible to recycle using the Au waste target, the surface of the waste target to remove impurities through nitric acid treatment, the powder to be injected into the waste target was prepared through a plasma process .
  • Powder prepared in the present invention is injected after cleaning the waste target, or proceed to manufacture using a high purity bulk. After removing impurities remaining using the plasma, the plasma temperature is increased to obtain a vaporized powder.
  • the high purity target manufacturing process using the Au waste target of the present invention is as follows. Debonding the waste target, removing impurities attached to the surface, preparing a high purity powder to be added, sintering by filling the high purity powder into the waste target, and processing and cleaning using a sintered body. It is characterized in that the configuration.
  • the present invention is characterized in that the Au target used for RDL (Redistributed Layer) or Bump is manufactured using a recycling process.
  • a method of manufacturing a target by stacking a new powder on a waste target the process time and manufacturing cost is significantly reduced.
  • 1 is a work flow chart for producing a high purity Au target using the waste target of the present invention.
  • the present invention in the manufacture of the target by recycling the waste target, debonding the waste target, removing impurities attached to the surface, preparing a high-purity powder to be added, by filling a high-purity powder in the waste target It provides a high-purity Au target manufacturing method by recycling the waste target Au through the sintering process, characterized in that the step of sintering, processing and cleaning using a sintered body.
  • FIG. 1 is a flow chart of the production of high purity Au target using the waste target of the present invention
  • Figure 2 is a FESEM image of the Au powder produced by the plasma of the present invention
  • Figure 3 is prepared by the Hot Press process of the present invention OM image of the target Au target.
  • Filling the high purity powder in the waste target (S40), processing and cleaning using a sintered body (S50) is a high purity Au target manufacturing method by recycling the Au waste target through the sintering process, characterized in that consisting of to be.
  • Debonding is carried out at a temperature of 200 ⁇ 250 °C and attached to the waste target area using high temperature tape to prevent contamination of indium and impurities before proceeding. After attaching, it heats up to 200-250 degreeC by 5-10 degreeC temperature. If the temperature is rapidly increased to 10 °C or higher, the deformation of the backing plate may occur. Therefore, the temperature is raised to 10 °C or lower. When the temperature reaches 200 ⁇ 250 °C, it is held for 30 minutes and then debonded. When debonding, the indium on the surface and the bonding surface must be completely removed. Indium removal process is prolonged on the surface, and if not completely removed during the process, there is a risk of presenting as impurities during sintering to deteriorate target properties.
  • the debonded waste target is removed with indium and surface contaminants using nitric acid or aqua regia (S20).
  • the waste target is added to nitric acid to remove residual indium and surface contaminants.
  • Powder to be put into the waste target is prepared by the plasma method (S30).
  • Powder production proceeds using a plasma apparatus.
  • the granules or waste targets of 99.995 wt% or more are cut into the chamber where the vacuum is evacuated.
  • the input weight should not exceed 500 ⁇ 2000gr. If the input weight is less than 500gr, there is a high risk that the plasma reacts with the crucible and is damaged. If the input weight is more than 2000gr, there is a possibility that the molten metal overflows the outside of the crucible and adheres to the chamber.
  • the injected raw material forms a plasma with low power (30 Kw or less), and is simply melted to remove impurities. At this time, by controlling the plasma power low, the impurities of low melting point is vaporized and removed to the outside by the vacuum apparatus. It is particularly effective for removing indium used in target manufacturing processes.
  • the power is increased to prepare a powder of high purity.
  • the power used to increase the power to 15 ⁇ 25kw to produce a powder.
  • the plasma gas is used to prepare a powder using argon or a mixture of argon and nitrogen.
  • Classification is carried out to ensure uniformity of the powders produced. Classification is carried out using a 150mesh classifier, which is used for sintering powders of 150mesh or less, and powders of 150mesh or more are reused to produce new powders.
  • the powder is put into the waste target from which impurities are removed and sintering is performed by using a hot press (S40).
  • the waste target is put into the carbon mold and new powder is filled.
  • the injected powder is added at 110-120% of the final target weight. If the waste target and powder weight is 110% or less, the final thickness may not reach the target thickness. If the input weight is more than 120%, the processing time is long, and the recovery time and cost increase due to the increase of processing scrap.
  • After filling the carbon mold with the waste target and powder it is charged into a hot press chamber and decompressed using a vacuum pump. At this time, the vacuum atmosphere is exhausted to 5.0x10 -4 torr or less and then sintered. Sintering temperature is carried out at 650 ⁇ 750 °C, time is maintained for 5 to 15 hours, the pressure is carried out to 10 ⁇ 20MPa.
  • the sintered compact is taken out when the chamber temperature becomes 100 ° C or lower. If the relative density of the extracted sintered body is 99.0% or more, the process proceeds to the final processing step. If the relative density is less than 99.0%, the likelihood of particle or nodule is increased during film formation.
  • Bonding is performed after the carbon adhering to the sintered body is removed using a shelf. Bonding is carried out using indium and the temperature is carried out at 200 ⁇ 250 °C. After bonding, the bonding rate is measured using ultrasonic flaw detection. The measured bonding rate should be 99.0% or more. If the bonding rate is 99.0% or less, perform bonding after debonding again. After bonding, the lathe is processed to the final thickness. Beading is applied to the backing plate surface of the machined target. The processed target is packaged after semiconductor cleaning.
  • the waste target was debonded after maintaining at 200 ° C. for 30 minutes. After debonding, the indium remaining on the target surface is removed. A waste target from which indium is removed is put into a beaker containing nitric acid to remove residual indium and impurities. The removal time was carried out for 2 hours, the purity of 99.998wt% was obtained as a result of impurity analysis using ICP.
  • the new powder to be prepared was prepared using a plasma equipment. Charge the Au waste target 700gr into the crucible.
  • Au powder was prepared by forming a plasma on the injected molded body and a high purity W electrode. Initially, impurities remaining in the waste target were removed at 5 kw, and power consumption was increased by 15 kw to prepare fine powder of high purity.
  • Table 1 shows Au powder manufacturing process conditions using plasma. 500gr of the powder was prepared by using plasma, and 150mesh powder 440gr was obtained by classifying the prepared powder. The powder was prepared by raising the power to 25 kw for comparison. The manufacturing process is shown in Table 2.
  • Table 1 Process item Process condition-Example Tier 1 (Low Power) Stage 2 (high power) Applied plasma output 5Kw 15Kw Gas for plasma Furtherance Ar Ar Gas flow rate 20L / min 20L / min Atmospheric gas composition (flow rate) Ar + N2 (150 L / min) Ar + N2 (150 L / min)
  • the FESEM results of the Au powder prepared using the plasma are shown in FIG. 2. It can be seen from FIG. 2 that the Au powder prepared using plasma is spherical powder of 10 ⁇ m.
  • Sintering is carried out by adding 440 gr of the newly produced powder to the waste target 500 gr.
  • Sintering temperature was 650 degreeC, 700 degreeC, 750 degreeC, holding time 10 hours, and the pressure was sintered by 15 Mpa. The results are shown in Table 4.
  • Example 2 Sintering Temperature (°C) 650 700 750 Retention time (hr) 10 10 10 Sintering Pressure (MPa) 15 15 15 Relative Density (%) 95 99.2 99.6 Grain size ( ⁇ m) 15 21 35
  • the present invention is characterized by manufacturing an Au target used for RDL (Redistributed Layer) or Bump using a recycling process, a method of manufacturing a target by laminating new powder on a waste target, process time and manufacturing cost Decreases significantly.

Abstract

The present invention relates to a method for preparing an Au target, which is used for a semiconductor redistributed layer (RDL) or a bump, and relates to a method for preparing the same by layering a powder on a waste target. A wet method, which is a conventional method for preparing an Au target, requires a long processing time since recovery is carried out through dissolution using aqua regia. By recycling a waste target, the present invention is effective in preparation time and cost reduction. To this end, a high-purity Au target is prepared by: surface-treating a waste target; preparing a high-purity powder within a short time using plasma, which is a dry process for a powder preparation; and injecting the prepared high-purity powder into the waste target.

Description

소결 공정을 통한 Ａｕ 폐타겟 재활용에 의한 고순도 Ａｕ 타겟 제조방법Manufacturing method of high purity Aug target by recycling Auger target by sintering process
본 발명은 Au 폐타겟을 이용한 재활용 방안으로, 30% 이상 사용한 Au 폐타겟을 이용하여 고순도의 분말을 충진하여 소결 공정을 통한 Au 타겟을 제조하는 방법에 관한 것이며, Au 폐타겟 전처리 공정을 통한 표면 청정화 및 고순도의 미세한 결정립을 가지는 Au 타겟 제조방법에 관한 것이다.The present invention relates to a recycling method using Au waste targets, and to a method of manufacturing an Au target through a sintering process by filling powders of high purity using Au waste targets used more than 30%, and the surface through the Au waste target pretreatment process. The present invention relates to a method for preparing an Au target having fine grains of cleansing and high purity.
Au 타겟은 RDL(Redistributed Layer)용 또는 Bump 용으로 널리 사용되고 있다. RDL용 프로세스는 반도체 칩 입출력 단자를 패키지에 용이하도록 변경시키는 공정이다. 낸드플래시는 패드의 위치가 중앙에 위치하고 있어 적층 할 때 패키지가 복잡해지고 와이어 길이가 길어져 속도가 저하되는 문제가 있다. 이를 해결하기 위해 패드 위치를 edge에 위치시켜 적층을 용의 하게 하는 공정이 RLD Process이다.Au targets are widely used for RDL (Redistributed Layer) or Bump. The process for RDL is a process of changing a semiconductor chip input / output terminal to a package easily. NAND flash has a problem in that the pad position is located in the center, so that when the lamination is complicated, the package becomes complicated and the wire length becomes longer, thereby decreasing the speed. In order to solve this problem, RLD process is used to facilitate stacking by placing pads at edges.
반도체 패키징 공정 측면에서는 유리하나 본딩 중에 Metal이 뜯기는 현상이 발생한다. 주로 Metal 두께가 얇을 경우 발생하는 문제점이 있다. 이를 보완하기 위해서는 스퍼터링을 통한 Au 타겟을 균일하게 성막을 해야한다.The semiconductor packaging process is advantageous, but the metal breaks during bonding. There is a problem that occurs mainly when the metal thickness is thin. To compensate for this, the Au target through sputtering must be uniformly formed.
범핑은 반도체 패키징과 어셈블리 과정에서 웨이퍼 집과 외부 회로의 전기 접점을 기존 본딩 와이어로 연결하지 않고 돌기 모양(Bump)의 금속을 형성해 전기적 신호를 전달해 주는 반도체 후공정이다. 최근 반도체 칩이 고성능화, 고집적화, 경박 단소화 되어 감에 따라 기존 와이어 방식으로는 기술적 한계가 나타나면서 그 대안으로 범핑 기술이 부각되고 있다.Bumping is a post-semiconductor process that delivers electrical signals by forming bump-shaped metals without connecting the electrical contacts of the wafer house and external circuits with conventional bonding wires during semiconductor packaging and assembly. Recently, as semiconductor chips have been improved in high performance, high integration, and shorter and lighter, bumping technology has emerged as an alternative to the conventional wire method.
반도체 공정이 급속도로 발전함에 따라 사용되는 Au 타겟 또한 성능 향상이 요구되고 있다. 반도체 성막공정에서 균일한 두께 및 표면 불순물을 제어하기 위해서는 Au 타겟의 결정립이 미세하며 고순도의 타겟 제조가 필요하다. 또한 사용량이 증가함에 따라 비용 절감을 위해서는 사용된 타겟의 재활용 방안이 요구되고 있다.As the semiconductor process develops rapidly, the Au target used is also required to improve performance. In order to control uniform thickness and surface impurities in the semiconductor film forming process, the crystal grains of the Au target are fine and a high purity target is required. In addition, as the usage increases, a method of recycling the used target is required to reduce costs.
상기 문제점을 해결하기 위해, 본 발명의 목적은 Au 폐타겟을 이용하여 표면 청정화를 하고, 미세하며 고순도의 분말 제조 후 폐타겟에 충진 후 소결하는 것을 특징으로 한다. 이를 위해 폐타겟 표면에 오염된 불순물을 제거하며, 플라즈마를 이용하여 고순도화 분말을 제조 후 Hot Press 공정을 통하여 고순도의 미세한 결정립을 가지는 타겟을 제조하는 방법을 제공하는 것이다.In order to solve the above problems, an object of the present invention is to clean the surface by using the Au waste target, characterized in that the fine and high-purity powder after the filling in the waste target after sintering. To this end, to remove impurities contaminated on the surface of the waste target, to provide a method of manufacturing a target having a high purity fine grains through the hot press process after manufacturing a high purity powder using a plasma.
상기 목적을 달성하기 위해, 본 발명은, Au 폐타겟을 이용하여 재활용을 가능하게 하였으며, 폐타겟 표면을 질산처리를 통하여 불순물을 제거하였으며, 폐타겟에 투입되는 분말은 플라즈마 공정을 통하여 제조를 하였다. 본 발명에서 제조되는 분말은 폐타겟을 청정화 후 투입하거나, 고순도 Bulk를 이용하여 제조를 진행한다. 플라즈마를 이용하여 잔존하는 불순물을 제거한 후, 플라즈마 온도를 상승시켜 기화된 분말을 얻는 것을 특징으로 한다.In order to achieve the above object, the present invention, it is possible to recycle using the Au waste target, the surface of the waste target to remove impurities through nitric acid treatment, the powder to be injected into the waste target was prepared through a plasma process . Powder prepared in the present invention is injected after cleaning the waste target, or proceed to manufacture using a high purity bulk. After removing impurities remaining using the plasma, the plasma temperature is increased to obtain a vaporized powder.
본 발명의 Au 폐타겟을 이용한 고순도 타겟 제조 공정은 다음과 같다. 폐타겟을 디본딩하는 단계, 표면에 부착된 불순물을 제거하는 단계, 추가 투입될 고순도 분말을 제조하는 단계, 폐타겟에 고순도 분말을 충진하여 소결하는 단계, 소결체를 이용하여 가공 및 세정하는 단계로 구성되는 것을 특징으로 한다.The high purity target manufacturing process using the Au waste target of the present invention is as follows. Debonding the waste target, removing impurities attached to the surface, preparing a high purity powder to be added, sintering by filling the high purity powder into the waste target, and processing and cleaning using a sintered body. It is characterized in that the configuration.
상기 설명한 바와 같이, 본 발명은 RDL(Redistributed Layer)용 또는 Bump 용으로 사용되는 Au 타겟을 재활용 공정을 이용하여 제조하는 것을 특징으로 한다.As described above, the present invention is characterized in that the Au target used for RDL (Redistributed Layer) or Bump is manufactured using a recycling process.
본 발명의 경우 폐타겟에 신규분말을 적층하여 타겟을 제조하는 방법으로, 공정시간 및 제조 원가가 대폭적으로 감소한다.In the present invention, a method of manufacturing a target by stacking a new powder on a waste target, the process time and manufacturing cost is significantly reduced.
도 1은 본 발명의 폐타겟을 이용한 고순도 Au타겟 제조를 하는 작업 순서도이다.1 is a work flow chart for producing a high purity Au target using the waste target of the present invention.
도 2는 본 발명의 플라즈마에 의해 제조된 Au 분말의 FESEM 이미지이다.2 is an FESEM image of Au powder prepared by the plasma of the present invention.
도 3은 본 발명의 Hot Press 공정에 의해 제조된 Au 타겟의 OM 이미지이다.3 is an OM image of the Au target produced by the Hot Press process of the present invention.
본 발명은 폐타겟을 재활용하여 타겟을 제조하는데 있어서, 폐타겟을 디본딩하는 단계, 표면에 부착된 불순물을 제거하는 단계, 추가 투입될 고순도 분말을 제조하는 단계, 폐타겟에 고순도 분말을 충진하여 소결하는 단계, 소결체를 이용하여 가공 및 세정하는 단계로 구성되는 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법을 제공한다.In the present invention, in the manufacture of the target by recycling the waste target, debonding the waste target, removing impurities attached to the surface, preparing a high-purity powder to be added, by filling a high-purity powder in the waste target It provides a high-purity Au target manufacturing method by recycling the waste target Au through the sintering process, characterized in that the step of sintering, processing and cleaning using a sintered body.
이하 첨부된 도면 및 실시예를 참조하여 본 발명에 대해 상세하게 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings and embodiments.
도 1은 본 발명의 폐타겟을 이용한 고순도 Au타겟 제조를 하는 작업 순서도이며, 도 2는 본 발명의 플라즈마에 의해 제조된 Au 분말의 FESEM 이미지이며, 도 3은 본 발명의 Hot Press 공정에 의해 제조된 Au 타겟의 OM 이미지이다.1 is a flow chart of the production of high purity Au target using the waste target of the present invention, Figure 2 is a FESEM image of the Au powder produced by the plasma of the present invention, Figure 3 is prepared by the Hot Press process of the present invention OM image of the target Au target.
본 발명은 폐타겟을 재활용하여 타겟을 제조하는데 있어서, 폐타겟을 디본딩하는 단계(S10), 표면에 부착된 불순물을 제거하는 단계(S20), 추가 투입될 고순도 분말을 제조하는 단계(S30), 폐타겟에 고순도 분말을 충진하여 소결하는 단계(S40), 소결체를 이용하여 가공 및 세정하는 단계(S50)로 구성되는 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법이다.In the present invention, in the manufacture of the target by recycling the waste target, the step of debonding the waste target (S10), removing the impurities attached to the surface (S20), preparing a high-purity powder to be added (S30) Filling the high purity powder in the waste target (S40), processing and cleaning using a sintered body (S50) is a high purity Au target manufacturing method by recycling the Au waste target through the sintering process, characterized in that consisting of to be.
더욱 상세하게는, 먼저, 폐타겟을 디본딩을 진행한다(S10).More specifically, first, de-bonding the waste target (S10).
디본딩은 200~250℃ 온도에서 진행하며 진행 전 폐타겟 부분에 인듐 및 불순물 오염을 방지하기 위해 고온용 테이프를 이용하여 부착한다. 부착 후 5~10℃ 온도로 200~250℃까지 승온을 실시한다. 10℃ 이상의 온도로 급격히 승온을 실시하면 Backing Plate 변형이 발생할 가능성이 있으므로 10℃ 이하의 온도로 승온한다. 200~250℃ 온도에 도달하면 30분간 유지 후 디본딩을 실시하도록 한다. 디본딩시 표면 및 본딩면의 인듐을 완벽히 제거해야한다. 표면에 인듐 제거 공정이 길어지며, 공정시 완벽히 제거가 되지 못하면 소결 시 불순물로 존재하여 타겟 특성을 저하시킬 우려가 있다.Debonding is carried out at a temperature of 200 ~ 250 ℃ and attached to the waste target area using high temperature tape to prevent contamination of indium and impurities before proceeding. After attaching, it heats up to 200-250 degreeC by 5-10 degreeC temperature. If the temperature is rapidly increased to 10 ℃ or higher, the deformation of the backing plate may occur. Therefore, the temperature is raised to 10 ℃ or lower. When the temperature reaches 200 ~ 250 ℃, it is held for 30 minutes and then debonded. When debonding, the indium on the surface and the bonding surface must be completely removed. Indium removal process is prolonged on the surface, and if not completely removed during the process, there is a risk of presenting as impurities during sintering to deteriorate target properties.
디본딩된 폐타겟을 질산 또는 왕수를 이용하여 인듐 및 표면 오염물을 제거 한다(S20).The debonded waste target is removed with indium and surface contaminants using nitric acid or aqua regia (S20).
폐타겟을 질산에 투입하여 잔존하는 인듐 및 표면 오염물 제거를 실시한다.The waste target is added to nitric acid to remove residual indium and surface contaminants.
먼저 폐타겟을 질산에 투입 후 1~3시간 유지한다. 유지 공정 중 표면에 부착된 불순물이 제거되는지 확인한다. 시간별로 시편을 채취하여 ICP분석을 실시한다.분석치가 99.995wt% 이상이면 다음 공정으로 진행하여, 미만의 경우 질산 처리를 재진행을 한다.First, put waste target into nitric acid and keep it for 1 ~ 3 hours. Ensure that impurities attached to the surface are removed during the maintenance process. Specimens should be taken over time and subjected to ICP analysis. If the analytical value is greater than 99.995 wt%, proceed to the next step and, if less, redox again.
폐타겟에 투입할 분말을 플라즈마 공법에 의해 제조한다(S30). Powder to be put into the waste target is prepared by the plasma method (S30).
분말 제조는 플라즈마 장치를 이용하여 진행을 한다. 진공이 배기된 챔버 내부에 99.995wt% 이상의 과립(granule) 또는 폐타겟을 절단하여 투입한다. 이때 투입되는 중량은 500~2000gr 이상이 넘지 않도록 한다. 투입 중량이 500gr 이하의 경우 플라즈마가 도가니와 반응하여 파손될 위험이 크며, 투입 중량이 2000gr 이상의 경우 용탕이 도가니 외부로 넘쳐 챔버와 부착될 가능성이 존재한다. 주입된 원료는 저 전력(30Kw이하)에 의한 플라즈마를 형성시켜 단순 용융시킨 후 불순물을 제거한다. 이때 플라즈마 전력을 낮게 조절하여 저 융점의 불순물을 기화시켜 진공장치에 의해 외부로 제거한다. 특히 타겟 제조 공정에서 사용되는 인듐 제거에 효과적이다.Powder production proceeds using a plasma apparatus. The granules or waste targets of 99.995 wt% or more are cut into the chamber where the vacuum is evacuated. At this time, the input weight should not exceed 500 ~ 2000gr. If the input weight is less than 500gr, there is a high risk that the plasma reacts with the crucible and is damaged. If the input weight is more than 2000gr, there is a possibility that the molten metal overflows the outside of the crucible and adheres to the chamber. The injected raw material forms a plasma with low power (30 Kw or less), and is simply melted to remove impurities. At this time, by controlling the plasma power low, the impurities of low melting point is vaporized and removed to the outside by the vacuum apparatus. It is particularly effective for removing indium used in target manufacturing processes.
불순물이 제거된 후 전력을 상승시켜 고순도의 분말의 제조 한다. 이때 사용되는 전력은 15~25kw로 전력을 상승시켜 분말을 제조한다. 이때 사용되는 플라즈마 가스는 아르곤 또는 아르곤과 질소를 혼합가스를 이용하여 분말을 제조한다. 제조된 분말의 균일성을 확보하기 위해 분급을 실시한다. 분급은 150mesh 분급체를 이용하여 실시하며, 150mesh 이하의 분말을 소결시 사용하며 150mesh 이상의 분말은 새로운 분말제조를 위해 재사용된다.After the impurities are removed, the power is increased to prepare a powder of high purity. At this time, the power used to increase the power to 15 ~ 25kw to produce a powder. At this time, the plasma gas is used to prepare a powder using argon or a mixture of argon and nitrogen. Classification is carried out to ensure uniformity of the powders produced. Classification is carried out using a 150mesh classifier, which is used for sintering powders of 150mesh or less, and powders of 150mesh or more are reused to produce new powders.
불순물이 제거된 폐타겟에 분말을 투입하여 Hot Press를 이용하여 소결을 진행한다(S40). The powder is put into the waste target from which impurities are removed and sintering is performed by using a hot press (S40).
먼저 카본 몰드에 폐타겟을 투입 후 신규분말을 충진한다. 투입되는 분말은 최종 타겟 중량의 110~120% 투입한다. 폐타겟과 분말 중량이 110% 이하일 경우 최종 가공 시 목적 두께에 미달할 수 있다. 투입 중량이 120% 이상일 경우 가공 시간이 장시간 소요되며, 가공 Scrap 증가로 인하여 회수 시간 및 비용이 증가된다. 카본몰드에 폐타겟 및 분말충진 후 Hot Press 챔버에 장입 후 진공펌프를 이용하여 감압을 실시한다. 이때 진공 분위기는 5.0x10-4 torr 이하까지 배기를 실시 후 소결을 진행한다. 소결 온도는 650~750℃에서 실시하며, 시간은 5~15시간 유지하며, 압력은 10~20MPa로 가압을 실시한다. 소결 완료 후 챔버온도가 100℃ 이하가 되면 소결체를 취출한다. 취출된 소결체의 상대밀도가 99.0% 이상일 경우 최종 가공단계로 넘어간다. 상대밀도가 99.0% 이하일 경우 성막시 Particle 이나 Nodule이 발생할 가능성이 높아지므로 소결체를 분말 제조 공정에 재사용한다.First, the waste target is put into the carbon mold and new powder is filled. The injected powder is added at 110-120% of the final target weight. If the waste target and powder weight is 110% or less, the final thickness may not reach the target thickness. If the input weight is more than 120%, the processing time is long, and the recovery time and cost increase due to the increase of processing scrap. After filling the carbon mold with the waste target and powder, it is charged into a hot press chamber and decompressed using a vacuum pump. At this time, the vacuum atmosphere is exhausted to 5.0x10 -4 torr or less and then sintered. Sintering temperature is carried out at 650 ~ 750 ℃, time is maintained for 5 to 15 hours, the pressure is carried out to 10 ~ 20MPa. After the completion of sintering, the sintered compact is taken out when the chamber temperature becomes 100 ° C or lower. If the relative density of the extracted sintered body is 99.0% or more, the process proceeds to the final processing step. If the relative density is less than 99.0%, the likelihood of particle or nodule is increased during film formation.
소결체를 이용하여 가공 및 본딩을 실시한다(S50).Processing and bonding are performed using a sintered compact (S50).
소결체 표면에 부착된 카본을 선반을 이용하여 제거 후 본딩을 실시한다. 본딩은 인듐을 이용하여 실시하며, 온도는 200~250℃에서 실시한다. 본딩 후 초음파 탐상을 이용하여 본딩율을 측정한다. 측정된 본딩율은 99.0% 이상이 되어야 한다.본딩율이 99.0% 이하일 경우 디본딩 후 본딩을 재실시한다. 본딩 후 선반을 이용하여 최종목적 두께까지 가공을 실시한다. 가공된 타겟의 Backing Plate 면에 비드 처리를 실시한다. 가공된 타겟은 반도체 세정 후 포장을 실시한다.Bonding is performed after the carbon adhering to the sintered body is removed using a shelf. Bonding is carried out using indium and the temperature is carried out at 200 ~ 250 ℃. After bonding, the bonding rate is measured using ultrasonic flaw detection. The measured bonding rate should be 99.0% or more. If the bonding rate is 99.0% or less, perform bonding after debonding again. After bonding, the lathe is processed to the final thickness. Beading is applied to the backing plate surface of the machined target. The processed target is packaged after semiconductor cleaning.
[실시예]EXAMPLE
사용된 4inch 폐타겟을 500gr을 디본딩을 실시한다. 소모전 타겟 Size, 두께 및 중량은 4inch, 5mm(t), 780gr이다. 폐타겟을 200℃에서 30min 유지 후 디본딩을 실시하였다. 디본딩 후 타겟 표면에 잔존한 인듐을 제거한다. 인듐이 제거된 폐타겟을 질산이 담긴 비커에 투입하여 잔존하는 인듐 및 불순물을 제거한다. 제거 시간은 2시간을 실시하였으며, ICP를 이용한 불순물 분석 결과 순도 99.998wt%를 확보하였다. 신규 투입할 분말을 플라즈마 장비를 이용하여 제조하였다. 도가니에 잉곳으로 Au 폐타겟 700gr을 장입한다. 로타리 펌프를 이용하여 5.0x10-2torr까지 감압 후 아르곤(Ar)투입에 의해 Ar분위기를 조성한다. 투입된 성형체와 고순도의 W 전극봉에 플라즈마를 형성시켜 Au 분말을 제조하였다. 초기에는 5kw로 폐타겟에 잔류하는 불순물을 제거하였으며, 사용 전력을 15kw 상승하여 고순도의 미세한 분말을 제조하였다. 플라즈마를 이용한 Au 분말 제조공정조건을 표 1에 나타내었다. 플라즈마를 이용하여 분말을 500gr 제조하였으며 제조된 분말을 분급을 통하여 150mesh 분말 440gr을 확보하였다. 비교를 위해 전력 25kw로 상승시켜 분말을 제조하였다. 제조 공정을 표 2에 나타내었다.Debond 500 gr of the used 4 inch closed target. Target size, thickness and weight before consumption are 4inch, 5mm (t), 780gr. The waste target was debonded after maintaining at 200 ° C. for 30 minutes. After debonding, the indium remaining on the target surface is removed. A waste target from which indium is removed is put into a beaker containing nitric acid to remove residual indium and impurities. The removal time was carried out for 2 hours, the purity of 99.998wt% was obtained as a result of impurity analysis using ICP. The new powder to be prepared was prepared using a plasma equipment. Charge the Au waste target 700gr into the crucible. After reducing the pressure to 5.0x10 -2 torr using a rotary pump, Ar is formed by argon (Ar) injection. Au powder was prepared by forming a plasma on the injected molded body and a high purity W electrode. Initially, impurities remaining in the waste target were removed at 5 kw, and power consumption was increased by 15 kw to prepare fine powder of high purity. Table 1 shows Au powder manufacturing process conditions using plasma. 500gr of the powder was prepared by using plasma, and 150mesh powder 440gr was obtained by classifying the prepared powder. The powder was prepared by raising the power to 25 kw for comparison. The manufacturing process is shown in Table 2.
제조된 분말의 순도, 평균 분말 크기 및 카본 함량을 표 3에 나타내었다.The purity, average powder size and carbon content of the prepared powders are shown in Table 3.
표 1
공정항목 공정조건-실시예
1단계(저전력) 2단계(고전력)
인가된 플라즈마 출력 5Kw 15Kw
플라즈마용 가스 조성 Ar Ar
가스유량 20L/min 20L/min
분위기 가스조성(유량) Ar+N2(150L/min) Ar+N2(150L/min)
Table 1
Process item Process condition-Example
Tier 1 (Low Power) Stage 2 (high power)
Applied plasma output 5Kw 15Kw
Gas for plasma Furtherance Ar Ar
Gas flow rate 20L / min 20L / min
Atmospheric gas composition (flow rate) Ar + N2 (150 L / min) Ar + N2 (150 L / min)
표 2
공정항목 공정조건-비교예
인가된 플라즈마 출력(kw) 25
플라즈마용 가스 조성 Ar
가스유량(L/min) 20
분위기 가스조성(L/min) Ar+N2(150)
TABLE 2
Process item Process Condition-Comparative Example
Applied Plasma Output (kw) 25
Gas for plasma Furtherance Ar
Gas flow rate (L / min) 20
Atmosphere gas composition (L / min) Ar + N2 (150)
표 3
분말 특성 실시예 비교예
순도(wt%) 99.998 99.995
평균분말 크기(㎛) 10 6
카본 함량(ppm) 40 200
TABLE 3
Powder properties Example Comparative example
Purity (wt%) 99.998 99.995
Average powder size (㎛) 10 6
Carbon content (ppm) 40 200
표 3의 결과로부터, 플라즈마에 의해 제조된 Au 분말의 경우 6~10㎛ 수준의 구상화된 분말을 확보하였다. 또한 순도 99.995~99.998wt%의 결과를 확보하였다. 카본 함량은 전력이 증가함에 따라 급격히 상승하는 경향을 보이고 있다. 전력이 증가하면 도가니 표면의 카본이 제조된 분말과 반응하여 카본 함량이 증가되는 경향을 보인다. 제조된 분말의 카본이 높아지면 최종 타겟을 이용한 성막시 Nodule형성 등의 영향을 줄 수 있다.From the results in Table 3, in the case of Au powder prepared by plasma, a spherical powder of 6-10 μm level was obtained. In addition, a purity of 99.995 ~ 99.998wt% was obtained. The carbon content tends to increase rapidly with increasing power. When the power is increased, the carbon content of the crucible surface reacts with the prepared powder. When the carbon of the prepared powder becomes high, it may have an influence such as nodule formation during film formation using the final target.
플라즈마를 이용하여 제조한 Au 분말에 대한 FESEM결과를 도 2에 나타내었다. 도 2로부터 플라즈마를 이용하여 제조된 Au 분말의 경우 10㎛의 구상화된 분말임을 알 수 있다.The FESEM results of the Au powder prepared using the plasma are shown in FIG. 2. It can be seen from FIG. 2 that the Au powder prepared using plasma is spherical powder of 10 μm.
폐타겟 500gr에 신규 제조 분말 440gr을 투입하여 소결을 진행한다. 소결온도는 650℃, 700℃, 750℃, 유지 시간 10시간, 압력은 15MPa로 소결을 실시하였다. 진행된 결과를 표4에 나타내었다. Sintering is carried out by adding 440 gr of the newly produced powder to the waste target 500 gr. Sintering temperature was 650 degreeC, 700 degreeC, 750 degreeC, holding time 10 hours, and the pressure was sintered by 15 Mpa. The results are shown in Table 4.
표 4
특성 실시예1 실시예2 실시예3
소결 온도(℃) 650 700 750
유지 시간(hr) 10 10 10
소결 압력(MPa) 15 15 15
상대밀도(%) 95 99.2 99.6
결정입경(㎛) 15 21 35
Table 4
characteristic Example 1 Example 2 Example 3
Sintering Temperature (℃) 650 700 750
Retention time (hr) 10 10 10
Sintering Pressure (MPa) 15 15 15
Relative Density (%) 95 99.2 99.6
Grain size (㎛) 15 21 35
표 4 결과로부터 750℃, 10시간, 15MPa 조건에서 상대밀도가 99.5% 이상의 고밀도 소결체를 확보하였다. 도 3에는 실시예3을 통해 제조된 소결체의 미세조직을 나타내었다.From the results of Table 4, a high-density sintered body having a relative density of 99.5% or more under 750 ° C, 10 hours, and 15 MPa conditions was secured. Figure 3 shows the microstructure of the sintered body produced through Example 3.
본 발명은 RDL(Redistributed Layer)용 또는 Bump 용으로 사용되는 Au 타겟을 재활용 공정을 이용하여 제조하는 것을 특징으로 하며, 폐타겟에 신규분말을 적층하여 타겟을 제조하는 방법으로, 공정시간 및 제조 원가가 대폭적으로 감소한다.The present invention is characterized by manufacturing an Au target used for RDL (Redistributed Layer) or Bump using a recycling process, a method of manufacturing a target by laminating new powder on a waste target, process time and manufacturing cost Decreases significantly.

Claims (6)

  1. 폐타겟을 재활용하여 타겟을 제조하는데 있어서, 폐타겟을 디본딩하는 단계, 표면에 부착된 불순물을 제거하는 단계, 추가 투입될 고순도 분말을 제조하는 단계, 폐타겟에 고순도 분말을 충진하여 소결하는 단계, 소결체를 이용하여 가공 및 세정하는 단계로 구성되는 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법.In manufacturing the target by recycling the waste target, debonding the waste target, removing impurities attached to the surface, preparing a high-purity powder to be added, sintering by filling the high-purity powder into the waste target Method for producing a high purity Au target by recycling the waste target Au through the sintering process, characterized in that the step of processing and cleaning using a sintered body.
  2. 제 1항에 있어서, The method of claim 1,
    폐타겟에 부탁된 불순물은 질산 또는 왕수를 이용하여 제거하는 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법.A method of manufacturing a high purity Au target by recycling Au waste targets through a sintering process, characterized in that impurities deposited on a waste target are removed using nitric acid or aqua regia.
  3. 제 1항에 있어서,The method of claim 1,
    상기 추가 투입될 분말의 결정립은 10㎛의 구상분말인 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법.The grain of the powder to be added is a high purity Au target manufacturing method by recycling Au waste targets through the sintering process, characterized in that the spherical powder of 10㎛.
  4. 제 1항에 있어서,The method of claim 1,
    제조된 추가 투입될 고순도 분말의 순도는 99.995wt%인 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법.Purity of the high-purity powder to be added added is 99.995wt%, the high purity Au target production method by recycling the waste Au target by the sintering process.
  5. 제 1항에 있어서,The method of claim 1,
    폐타겟에 제조된 추가 투입될 고순도 분말을 투입하여 소결하는 온도는 650~750℃인 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법.The method of manufacturing a high-purity Au target by recycling the Au waste target recycling through the sintering process, characterized in that the sintering temperature by adding the high-purity powder to be added to the waste target is 650 ~ 750 ℃.
  6. 제 1항에 있어서,The method of claim 1,
    제조된 소결체의 상대밀도는 99.5%인 것을 특징으로 하는 소결 공정을 통한 Au 폐타겟 재활용에 의한 고순도 Au 타겟 제조방법.Relative density of the prepared sintered body is a high purity Au target manufacturing method by recycling the waste target Au through the sintering process, characterized in that 99.5%.
PCT/KR2012/008954 2012-10-26 2012-10-29 Method for preparing high-purity au target by recycling waste au target through sintering WO2014065452A1 (en)

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Publication number Priority date Publication date Assignee Title
KR0142933B1 (en) * 1995-10-05 1998-07-15 이정성 Recovering indium method from in-sn target
JP2000144395A (en) * 1998-11-10 2000-05-26 Hitachi Metals Ltd Ruthenium target and its manufacture
KR100637868B1 (en) * 2005-08-09 2006-10-23 희성금속 주식회사 A manufacturing method of ito powder collected from a waste ito sputtering target for producing high density target and a manufacturing method of sputtering target
KR100676983B1 (en) * 2002-05-10 2007-01-31 베.체. 헤레우스 게엠베하 운트 코. 카게 Method for the production of a metal oxide powder or a semiconductor oxide powder, oxide powder, solid body, and the use thereof
JP2010159482A (en) * 2009-01-07 2010-07-22 Solar Applied Materials Technology Corp Refurbished sputtering target and method for making the same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR0142933B1 (en) * 1995-10-05 1998-07-15 이정성 Recovering indium method from in-sn target
JP2000144395A (en) * 1998-11-10 2000-05-26 Hitachi Metals Ltd Ruthenium target and its manufacture
KR100676983B1 (en) * 2002-05-10 2007-01-31 베.체. 헤레우스 게엠베하 운트 코. 카게 Method for the production of a metal oxide powder or a semiconductor oxide powder, oxide powder, solid body, and the use thereof
KR100637868B1 (en) * 2005-08-09 2006-10-23 희성금속 주식회사 A manufacturing method of ito powder collected from a waste ito sputtering target for producing high density target and a manufacturing method of sputtering target
JP2010159482A (en) * 2009-01-07 2010-07-22 Solar Applied Materials Technology Corp Refurbished sputtering target and method for making the same

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