KR20110082894A - The method and device for the recycling of waste silicon wafer sludge - Google Patents

The method and device for the recycling of waste silicon wafer sludge Download PDF

Info

Publication number
KR20110082894A
KR20110082894A KR1020100002827A KR20100002827A KR20110082894A KR 20110082894 A KR20110082894 A KR 20110082894A KR 1020100002827 A KR1020100002827 A KR 1020100002827A KR 20100002827 A KR20100002827 A KR 20100002827A KR 20110082894 A KR20110082894 A KR 20110082894A
Authority
KR
South Korea
Prior art keywords
cutting oil
sludge
silicon wafer
sic powder
waste silicon
Prior art date
Application number
KR1020100002827A
Other languages
Korean (ko)
Other versions
KR101179521B1 (en
Inventor
오세천
김종생
Original Assignee
주식회사 이앤알이
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 주식회사 이앤알이 filed Critical 주식회사 이앤알이
Priority to KR1020100002827A priority Critical patent/KR101179521B1/en
Publication of KR20110082894A publication Critical patent/KR20110082894A/en
Application granted granted Critical
Publication of KR101179521B1 publication Critical patent/KR101179521B1/en

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/08Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs
    • B01D3/085Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs using a rotary evaporator
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/08Separating or sorting of material, associated with crushing or disintegrating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/12Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/121Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
    • C02F11/127Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering by centrifugation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02002Preparing wafers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C2201/00Codes relating to disintegrating devices adapted for specific materials
    • B02C2201/06Codes relating to disintegrating devices adapted for specific materials for garbage, waste or sewage
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/20Waste processing or separation
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/82Recycling of waste of electrical or electronic equipment [WEEE]

Abstract

PURPOSE: A method and an apparatus for recycling wasted silicon wafer sludge are provided to separate and collect the sludge of the wasted silicon wafer in a pure form and collect other components of the wasted silicon wafer in a mixture form. CONSTITUTION: The mixed silicon, silicon carbide, and cutting oil of wasted silicon wafer sludge are prepared. The cutting oil is separated and collected through a distillation process and an evaporating process. The silicon and the silicon carbide of the wasted silicon wafer sludge without the cutting oil are pulverized. The pulverized silicon and silicon carbide are mixed with caustic soda and water. Silicon powder is mixed and reacted with the caustic soda. The pure silicon carbide powder is separated and collected by a centrifugal separating process. The mixture silicon powder and caustic soda mixed solution is collected.

Description

폐 실리콘웨이퍼 슬러지의 재활용 방법 및 장치{The method and device for the recycling of waste silicon wafer sludge}The method and device for the recycling of waste silicon wafer sludge}

본 발명은 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 그리고 절삭유 성분을 각각 재 활용 가능하게 분리, 회수하되, 순수한 성분으로 분리, 회수 가능한 것은 순수한 성분으로 분리, 회수하고, 순수한 성분으로 분리, 회수가 불가능한 것은 또 다른 산업소재의 원료로 활용 가능한 혼합물 형태로 분리, 회수하여 전량 재 활용하도록 하는 폐 실리콘웨이퍼 슬러지의 재활용 방법 및 장치에 관한 것이다.
The present invention is to separate and recover the Si and SiC and the cutting oil components of the waste silicon wafer sludge generated during the semiconductor manufacturing process, respectively. The impossibility of separating and recovering is related to a method and apparatus for recycling waste silicon wafer sludge which is separated and recovered in the form of a mixture that can be used as a raw material of another industrial material to reuse the whole amount.

현대 산업은 소형, 경량화 기술이 발전되면서 반도체 산업이 점차 더 크게 부상하고 있다.In the modern industry, the semiconductor industry is gradually increasing due to the development of compact and lightweight technologies.

상기한 반도체 제조 과정중 잉곳 절단 후 실리콘웨이퍼 제조시에 폐 슬러지가 다량 발생된다.After the ingot cutting during the semiconductor manufacturing process, a large amount of waste sludge is generated during silicon wafer manufacturing.

이러한 폐 실리콘웨이퍼 슬러지는 다량의 Si, SiC 분말과 절삭유가 포함되어 있다.This waste silicon wafer sludge contains a large amount of Si, SiC powder and cutting oil.

종래 상기 폐 실리콘웨이퍼 슬러지는 SiC 및 절삭유를 어느 일정 함량까지 회수한 후 나머지를 전량 폐기 처리하였다.Conventionally, the waste silicon wafer sludge recovers the SiC and the cutting oil to a certain content, and then discards the rest of the silicon wafer sludge.

즉, 상기 폐기 처리되는 폐 실리콘웨이퍼 슬러지에는 다량의 Si 및 SiC분말과 절삭유 또한 적지 않은 양이 함유되어 있기 때문에 각 성분별 분리 회수가 가능하면 다양한 산업 소재로 재 활용될 수 있음에도 불구하고 아직 뚜렷한 재활용 기술이 개발되어 있지 못해 그 활용에 많은 제약이 따르고 있었다.That is, since the waste silicon wafer sludge to be disposed of contains a large amount of Si and SiC powder and cutting oil, it is still remarkably recycled even though it can be recycled to various industrial materials if separation and recovery for each component is possible. Since technology was not developed, there were many restrictions on its use.

특히, 종래 폐 실리콘웨이퍼 슬러지의 재활용 기술은 대부분 SiC분말의 회수목적에 치중되어 있고, 나머지 절삭유나 Si성분의 경우에 뚜렷한 재활용 방법이 제시되어 있지 못하여 폐 실리콘웨이퍼 슬러지를 전량 재활용하는데 있어 그 한계를 가지고 있었다.
In particular, the recycling technology of conventional waste silicon wafer sludge is mainly focused on the recovery purpose of SiC powder, and in the case of the remaining cutting oil or Si component, there is no clear recycling method, so the limit of recycling waste silicon wafer sludge is limited. I had.

본 발명은 상기한 종래 기술이 갖는 제반 문제점을 해결하고자 발명된 것으로서, 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 그리고 절삭유 성분을 각각 재 활용 가능하게 분리, 회수하되, 순수한 성분으로 분리, 회수 가능한 것은 순수한 성분으로 분리, 회수하고, 순수한 성분으로 분리, 회수가 불가능한 것은 또 다른 산업소재의 원료로 활용 가능한 혼합물 형태로 분리, 회수하여 전량 재 활용하도록 하는데 그 목적이 있다.
The present invention has been invented to solve the above problems of the prior art, the Si and SiC and the cutting oil components of the waste silicon wafer sludge generated during the semiconductor manufacturing process, respectively, to be recycled and recovered, but separated into pure components. The purpose of this is to separate and recover the pure components into pure components, and to separate and recover the pure components into separate mixtures that can be used as raw materials for other industrial materials.

이러한 본 발명은,This invention,

반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하는 절삭유 분리 회수단계와; 상기 절삭유가 분리 회수된 폐 실리콘웨이퍼 슬러지의 Si, SiC 분말 성분을 분쇄하는 분쇄단계와; 상기 Si, SiC 분말 성분에 가성소다와 물을 혼합시켜, 상기 Si 분말 성분이 가성소다와 혼합 반응하도록 하는 혼합반응 단계와; 상기 SiC 분말 성분과 Si 분말 성분이 가성소다와 혼합 반응된 용액의 혼합물을 원심분리에 의해 순수 SiC 분말 성분을 분리 회수하고, 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리, 회수하는 분리, 회수단계에 의한 폐 실리콘웨이퍼 슬러지의 재활용 방법과;A cutting oil separation and recovery step of separating and recovering cutting oil by distillation and evaporation in a state in which Si, SiC powder components and cutting oil of waste silicon wafer sludge generated in a semiconductor manufacturing process are mixed; A grinding step of grinding the Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered; A mixing reaction step of mixing caustic soda and water with the Si and SiC powder components to mix and react the Si powder component with caustic soda; Centrifugally separating and recovering the mixture of the SiC powder component and the Si powder component with caustic soda by centrifugation to separate pure SiC powder component and separating the mixed reaction solution of Si and caustic soda that can be used as a raw material of the remaining liquid refractory material. Recycling the waste silicon wafer sludge by the separating and recovering step;

반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하는 절삭유 분리 회수단계와; 상기 절삭유가 분리 회수된 폐 실리콘웨이퍼 슬러지의 Si, SiC 분말 성분을 분쇄하는 분쇄단계와; 상기 Si, SiC 분말 성분을 열처리하는 단계와; 상기 Si, SiC 분말 성분에 내화재 원료로 사용하기 적합하도록 추가 Si, SiC 분말을 혼합하면서 함량 조절하여 내화재 원료로 사용하는 Si, SiC 혼합분말 회수단계에 의한 폐 실리콘웨이퍼 슬러지의 재활용 방법을 제공함에 그 특징이 있다.A cutting oil separation and recovery step of separating and recovering cutting oil by distillation and evaporation in a state in which Si, SiC powder components and cutting oil of waste silicon wafer sludge generated in a semiconductor manufacturing process are mixed; A grinding step of grinding the Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered; Heat-treating the Si and SiC powder components; Providing a method for recycling the waste silicon wafer sludge by the Si, SiC mixed powder recovery step used as a refractory material by adjusting the content while mixing additional Si, SiC powder to be suitable as a refractory raw material to the Si, SiC powder components. There is a characteristic.

본 발명은 고농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 투입하여 고순도 절삭유를 증류하여 분리 회수하는 증류기와; 상기 고순도 절삭유를 분리 회수한 슬러지와 저농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 투입하여 회전 이송하면서 저순도 절삭유를 분리 회수하는 회전형 증발기와; 상기 절삭유를 분리 회수한 나머지 Si, SiC 분말 성분을 분쇄하는 분쇄기와; 상기 분쇄기에 의해 분쇄된 Si, SiC 분말 성분에 가성소다와 물을 투입하여 혼합 반응시키는 혼합반응기 및; 상기 혼합 반응된 혼합물을 원심 분리하여 순수한 SiC 분말 성분과 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리 회수하는 원심분리기로 구성된 폐 실리콘웨이퍼 슬러지의 재활용 장치를 제공함에 그 특징이 있다.
The present invention comprises a distillation unit for distilling and recovering high-purity cutting oil by inputting waste silicon wafer sludge containing high concentration cutting oil; A rotary evaporator for separating and recovering the low-purity cutting oil while rotating and transporting the sludge from which the high-purity cutting oil is separated and recovered and the waste silicon wafer sludge containing the low-concentration cutting oil; A grinder for separating and recovering the cutting oil to grind the remaining Si and SiC powder components; A mixing reactor for mixing and mixing caustic soda and water into Si and SiC powder components ground by the mill; It provides a recycling apparatus for waste silicon wafer sludge composed of a centrifuge for centrifuging the mixed reaction mixture to recover the mixed reaction solution of Si and caustic soda that can be used as a raw material of pure SiC powder and the remaining liquid refractory material. There is this.

이러한 본 발명은, 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 그리고 절삭유 성분을 각각 재 활용 가능하게 분리, 회수하되, 절삭유, SiC 분말과 같이 순수한 성분으로 분리, 회수 가능한 것은 순수한 성분으로 분리, 회수하고, Si 분말과 같이 순수한 성분으로 분리, 회수가 불가능한 것은 또 다른 산업소재(내화재)의 원료로 활용 가능한 Si 혼합물 형태로 분리, 회수하여 전량 재 활용하도록 하므로 경제성을 극대화하는 효과를 갖는 것이다.
In the present invention, the Si and SiC and the cutting oil components of the waste silicon wafer sludge generated during the semiconductor manufacturing process can be separated and recovered to be reused, respectively, and the pure and soluble components can be separated and recovered as pure components such as cutting oil and SiC powder. It is not possible to separate and recover, and to be able to separate and recover with pure ingredients such as Si powder, to separate and recover in the form of Si mixture that can be used as a raw material of another industrial material (refractory material), so that the entire amount can be reused. will be.

도 1은 본 발명 방법의 일 실시 예를 보여주는 공정도.
도 2는 본 발명 방법의 다른 실시 예를 보여주는 공정도.
도 3은 본 발명 장치의 전체 구성도.
도 4는 본 발명 장치의 다른 실시 예를 보여주는 전체 구성도.
1 is a process diagram showing one embodiment of the method of the present invention.
2 is a process diagram showing another embodiment of the method of the present invention.
3 is an overall configuration diagram of the apparatus of the present invention.
Figure 4 is an overall configuration showing another embodiment of the device of the present invention.

먼저, 본 발명의 폐 실리콘웨이퍼 슬러지의 재활용 방법에 대해 도 1을 참조하여 살펴보기로 한다.First, a method for recycling waste silicon wafer sludge of the present invention will be described with reference to FIG. 1.

본 발명은 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하는 절삭유 분리 회수단계와;The present invention provides a cutting oil separation and recovery step of separating and recovering cutting oil by distillation and evaporation in a mixed state of Si and SiC powder components and cutting oil of waste silicon wafer sludge generated during a semiconductor manufacturing process;

상기 절삭유가 분리 회수된 폐 실리콘웨이퍼 슬러지의 Si, SiC 분말 성분을 분쇄하는 분쇄단계와;A grinding step of grinding the Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered;

상기 Si, SiC 분말 성분에 가성소다와 물을 혼합시켜, 상기 Si 분말 성분이 가성소다와 혼합 반응하도록 하는 혼합반응 단계와;A mixing reaction step of mixing caustic soda and water with the Si and SiC powder components to mix and react the Si powder component with caustic soda;

상기 SiC 분말 성분과 Si 분말 성분이 가성소다와 혼합 반응된 용액의 혼합물을 원심분리에 의해 순수 SiC 분말 성분을 분리 회수하고, 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리, 회수하는 분리, 회수단계에 의한 방법을 제공한다.Centrifugally separating and recovering the mixture of the SiC powder component and the Si powder component with caustic soda by centrifugation to separate pure SiC powder component and separating the mixed reaction solution of Si and caustic soda that can be used as a raw material of the remaining liquid refractory material. It provides a method by the separation, recovery step of recovering.

그리고, 상기 절삭유 분리 회수단계는 고농도 절삭유 함유 슬러지와 저농도 절삭유 함유 슬러지에서 고농도, 저농도 절삭유를 분리 회수하고자 하는 경우, 고농도 절삭유 함유 슬러지를 증류 공정에 의해 고순도 절삭유를 분리 회수하는 1단계후, 상기 1단계에서 고순도 절삭유를 분리 회수한 슬러지에 저농도 절삭유 함유 슬러지와 함께 회전형 증발기를 통과시켜 저순도 절삭유를 분리 회수하는 2단계에 의해 고순도 절삭유와 저순도 절삭유를 각각 분리 회수하는 방법을 제공한다.The cutting oil separation and recovering step may be performed after separating and recovering the high-purity cutting oil containing sludge from the high concentration and the low concentration cutting oil by the distillation process. Provided is a method for separating and recovering high-purity cutting oil and low-purity cutting oil by two steps of separating and recovering low-purity cutting oil by passing a rotary evaporator together with a low concentration of cutting oil-containing sludge to the sludge from which the high-purity cutting oil is recovered and recovered in the step.

이때, 상기 회전형 증발기는 내부 압력이 70mmHg, 온도 200℃ 이하로 형성함이 바람직한데, 에너지 절감을 위한 감압 기술 및 절삭유 재활용을 위한 성분 변화 방지를 위해 환원성 분위기의 기술을 모두 적용하게 된다.At this time, the rotary evaporator is preferably formed at an internal pressure of 70mmHg, the temperature of 200 ℃ or less, it is to apply all of the technology of the reducing atmosphere to reduce the pressure reduction technology for energy saving and component change for cutting oil recycling.

또한, 상기 혼합반응 단계에서 가성소다는 총 혼합물 대비 2~15 중량부, 물은 총 혼합물 대비 60~80 중량부로 혼합함이 바람직하다.In addition, caustic soda in the mixing reaction step is preferably 2 to 15 parts by weight based on the total mixture, water is mixed at 60 to 80 parts by weight relative to the total mixture.

이러한 본 발명은 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하되, 고농도 절삭유 함유 슬러지와 저농도 절삭유 함유 슬러지가 모두 발생하는 경우, 먼저 고농도 절삭유 함유 슬러지를 증류 공정에 의해 고순도 절삭유를 분리 회수하고, 고순도 절삭유를 분리 회수한 슬러지에 저농도 절삭유 함유 슬러지와 함께 회전형 증발기를 통과시켜 저순도 절삭유를 분리 회수하는 것이다.The present invention is to recover and separate the cutting oil by distillation and evaporation in the mixed state of the Si and SiC powder components of the waste silicon wafer sludge produced during the semiconductor manufacturing process and the cutting oil, the high concentration of cutting oil containing sludge and low concentration of cutting oil containing sludge In this case, first, high-purity cutting oil-containing sludge is separated and recovered by a distillation process, and the low-purity cutting oil is separated and recovered by passing the sludge from which the high-purity cutting oil is separated and recovered by passing a rotary evaporator together with the low-concentration cutting oil-containing sludge.

그리고 상기 절삭유를 분리 회수한 폐 실리콘웨이퍼 슬러지의 나머지 Si, SiC 분말 성분을 분쇄 및 가성소다와 물을 혼합시켜, 상기 Si 분말 성분이 가성소다와 혼합 반응하도록 한 후, 원심 분리에 의해 순수 SiC 분말 성분을 분리 회수하고, 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리, 회수하여 폐 실리콘웨이퍼 슬러지를 전량 재활용 가능하게 되는 것이다.Then, the remaining Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered are pulverized and mixed with caustic soda and water to allow the Si powder components to react with caustic soda, followed by centrifugal separation of pure SiC powder. The components are separated and recovered, and the mixed reaction solution of Si and caustic soda, which can be used as the remaining liquid refractory material, is separated and recovered, so that the entire amount of waste silicon wafer sludge can be recycled.

또한, 본 발명은 폐 실리콘웨이퍼 슬러지에 SiC 분말 성분이 소량 함유되어 SiC 분말 성분을 별도 분리 회수할 필요성이 없는 경우에는 도 2에 도시된 바와 같이, 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하는 절삭유 분리 회수단계와;In addition, in the present invention, when a small amount of SiC powder component is contained in the waste silicon wafer sludge so that it is not necessary to separately collect and recover the SiC powder component, as shown in FIG. 2, the Si of the waste silicon wafer sludge generated in the semiconductor manufacturing process is generated. Cutting oil separation and recovery step of separating and recovering the cutting oil by distillation and evaporation in a state where the SiC powder component and the cutting oil are mixed;

상기 절삭유가 분리 회수된 폐 실리콘웨이퍼 슬러지의 Si, SiC 분말 성분을 분쇄하는 분쇄단계와;A grinding step of grinding the Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered;

상기 Si, SiC 분말 성분을 열처리하는 단계와;Heat-treating the Si and SiC powder components;

상기 Si, SiC 분말 성분에 내화재 원료로 사용하기 적합하도록 추가 Si, SiC 분말을 혼합하면서 함량 조절하여 내화재 원료로 사용하는 Si, SiC 혼합분말 회수단계에 의한 방법을 제공한다.It provides a method by the Si, SiC mixed powder recovery step to be used as a refractory material by adjusting the content while mixing the additional Si, SiC powder to be suitable for use as a refractory raw material to the Si, SiC powder component.

즉, 이러한 본 발명은 전술한 방법과 비교하여 볼때, 반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수한 후, SiC 분말 성분이 소량 함유되어 있기 때문에 별도 분리 회수하지 않고 Si, SiC 분말 성분을 분쇄 및 열처리하여 내화재 원료로 사용하기 적합하도록 추가 Si, SiC 분말을 혼합하면서 함량 조절하여 Si, SiC 혼합분말을 회수하므로 폐 실리콘웨이퍼 슬러지를 전량 재활용 가능하게 되는 것이다.
That is, compared with the above-described method, the present invention separates and recovers the cutting oil by distillation and evaporation in the mixed state of the Si and SiC powder components of the waste silicon wafer sludge generated during the semiconductor manufacturing process and the cutting oil, followed by SiC powder. Because it contains a small amount of components, Si and SiC powders are pulverized and heat treated without separate separation and recovery, and the content is adjusted while mixing additional Si and SiC powders to be suitable for use as refractory materials. The entire amount of wafer sludge can be recycled.

다음은 상기한 본 발명의 방법을 달성하기 위한 장치를 첨부도면을 참조하여 설명하기로 한다.The following describes an apparatus for achieving the above-described method of the present invention with reference to the accompanying drawings.

즉, 본 발명의 장치는 도 3에 도시된 바와 같이, 고농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 투입하여 고순도 절삭유를 증류하여 분리 회수하는 증류기(10)와;That is, the apparatus of the present invention, as shown in Figure 3, a high-temperature cutting oil containing waste silicon wafer sludge by distilling the high-purity cutting oil by distillation and recovery;

상기 고순도 절삭유를 분리 회수한 슬러지와 저농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 투입하여 회전 이송하면서 저순도 절삭유를 분리 회수하는 회전형 증발기(20)와;A rotary evaporator 20 for separating and recovering the low-purity cutting oil while rotating conveying the sludge from which the high-purity cutting oil is separated and recovered and the waste silicon wafer sludge containing the low-concentration cutting oil;

상기 절삭유를 분리 회수한 나머지 Si, SiC 분말 성분을 분쇄하는 분쇄기(30)와;A crusher 30 for crushing the remaining Si and SiC powder components after separating and recovering the cutting oil;

상기 분쇄기에 의해 분쇄된 Si, SiC 분말 성분에 가성소다와 물을 투입하여 혼합 반응시키는 혼합반응기(40) 및; 상기 혼합 반응된 혼합물을 원심 분리하여 순수한 SiC 분말 성분과 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리 회수하는 원심분리기(50)로 구성되어 이루어진다.A mixing reactor (40) for mixing and mixing caustic soda and water to Si and SiC powder components ground by the mill; Centrifugal separation of the mixed reaction mixture consists of a centrifuge (50) for separating and recovering the mixed reaction solution of Si and caustic soda that can be used as the raw material of the pure SiC powder and the remaining liquid refractory material.

이때 상기 회전형 증발기(10)는 내부 압력 70mmHg, 온도 200℃ 이하로 형성함이 바람직한데, 에너지 절감을 위한 감압 기술 및 절삭유의 재활용을 위한 성분 변화 방지를 위해 환원성 분위기의 기술을 적용하게 된다.At this time, the rotary evaporator 10 is preferably formed at an internal pressure of 70 mmHg and a temperature of 200 ° C. or less, and applies a reducing atmosphere technology for reducing energy and reducing components for recycling of cutting oil.

이러한 본 발명 장치의 작동 및 작용에 대해 살펴보기로 한다.This operation and operation of the device of the present invention will be described.

반도체 제조과정에서 발생되는 고농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 증류기(10)에 투입하여 고순도 절삭유를 1차적으로 증류하여 분리 회수한다.Waste silicon wafer sludge containing high concentration cutting oil generated during the semiconductor manufacturing process is introduced into the distiller 10 to separate and recover the high purity cutting oil primarily.

그리고 상기 고순도 절삭유를 분리 회수한 슬러지와 저농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 회전형 증발기(20)에 투입하여 스크류에 의해 회전 이송하면서 저순도 절삭유를 분리 회수한다.Then, the sludge from which the high purity cutting oil is separated and collected and the waste silicon wafer sludge containing the low concentration of cutting oil are introduced into the rotary evaporator 20, and the low purity cutting oil is separated and recovered while being rotated by a screw.

이와 같이 고순도 절삭유와 저순도 절삭유를 분리 회수한 폐 슬러지의 Si, SiC 분말 성분은 분쇄기(30)에 의해 분쇄한 후, 혼합반응기(40)에 일정 양의 가성소다와 물을 함께 투입하여 혼합 반응시키도록 한다.The Si and SiC powder components of the waste sludge from which the high-purity cutting oil and the low-purity cutting oil are separated and recovered are pulverized by the pulverizer 30, and then a predetermined amount of caustic soda and water are added to the mixed reactor 40 to mix and react. Let's do it.

이때 상기 가성소다는 Si 분말 성분과 혼합 반응되어 용액 상태로 존재하게 되는 것이다.At this time, the caustic soda is mixed with the Si powder component to exist in the solution state.

이와 같이 혼합반응된 혼합물을 원심분리기(50)에서 원심 분리로 순수 SiC 분말 성분을 분리 회수하게 되는 것이다.In this way, the mixed reaction is centrifuged in the centrifuge 50 to separate and recover the pure SiC powder component.

이와 같이 분리된 순수 SiC 분말 성분은 세척, 건조 과정을 거친 후 순수 SiC 분말로 재활용하게 되는 것이다.The pure SiC powder component thus separated is recycled into pure SiC powder after washing and drying.

그리고 상기 순수 SiC 분말 성분의 세척과정에 사용된 물은 회수하여 혼합반응기(40)에서 재활용한다.The water used in the washing process of the pure SiC powder component is recovered and recycled in the mixed reactor 40.

또한, 상기 순수 SiC 분말 성분을 분리 회수한 나머지 Si와 가성소다의 혼합 반응 용액은 액상 내화물 원료로 즉시 재활용하게 되는 것이다.In addition, the mixed reaction solution of the Si and the caustic soda after the separated and recovered the pure SiC powder component is immediately recycled as a liquid refractory raw material.

결국, 반도체 제조과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 절삭유, SiC 분말과 같이 순수한 성분으로 분리, 회수 가능한 것은 순수한 성분으로 분리, 회수하고, Si 분말과 같이 순수한 성분으로 분리, 회수가 불가능한 것은 또 다른 산업소재(내화재)의 원료로 활용 가능한 Si 혼합물 형태로 분리, 회수하여 전량 재 활용하게 되는 것이다.After all, it is possible to separate and recover the pure components such as cutting oil of waste silicon wafer sludge produced during the semiconductor manufacturing process and the pure components such as SiC powder, and to recover the pure components such as Si powder. It will be recycled and recycled in the form of Si mixture that can be used as a raw material for industrial materials (fireproof materials).

한편, 본 발명의 장치는 도 4에 도시된 바와 같이, 반도체 제조과정에서 발생되는 페 실리콘웨이퍼 슬러지의 고농도 또는 저농도 절삭유를 구분하지 않고 처리하기 위해 증류기- 회전형 증발기의 2단계 절삭유 분리 회수 구성을 회전형 증발기(20) 만을 구성하여 절삭유를 분리 회수하도록 한 것이다.On the other hand, the apparatus of the present invention, as shown in Figure 4, to separate the high- or low-concentration coolant of the silicon wafer sludge generated in the semiconductor manufacturing process to separate the two-stage cutting oil separation recovery configuration of the distiller-rotary evaporator Only the rotary evaporator 20 is configured to separate and recover the cutting oil.

그 밖에 모든 과정은 도 3의 실시 예와 동일하므로 자세한 설명을 생략하기로 한다.
All other processes are the same as in the embodiment of FIG. 3, so a detailed description thereof will be omitted.

10: 증류기
20: 회전형 증발기
30: 분쇄기
40: 혼합반응기
50: 원심분리기
10: still
20: rotary evaporator
30: grinder
40: mixed reactor
50: centrifuge

Claims (5)

반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하는 절삭유 분리 회수단계와;
상기 절삭유가 분리 회수된 폐 실리콘웨이퍼 슬러지의 Si, SiC 분말 성분을 분쇄하는 분쇄단계와;
상기 Si, SiC 분말 성분에 가성소다와 물을 혼합시켜, 상기 Si 분말 성분이 가성소다와 혼합 반응하도록 하는 혼합반응 단계와;
상기 SiC 분말 성분과 Si 분말 성분이 가성소다와 혼합 반응된 용액의 혼합물을 원심분리에 의해 순수 SiC 분말 성분을 분리 회수하고, 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리, 회수하는 분리, 회수단계에 의한 것을 특징으로 하는 폐 실리콘웨이퍼 슬러지의 재활용 방법.
A cutting oil separation and recovery step of separating and recovering cutting oil by distillation and evaporation in a state in which Si, SiC powder components and cutting oil of waste silicon wafer sludge generated in a semiconductor manufacturing process are mixed;
A grinding step of grinding the Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered;
A mixing reaction step of mixing caustic soda and water with the Si and SiC powder components to mix and react the Si powder component with caustic soda;
Centrifugally separating and recovering the mixture of the SiC powder component and the Si powder component with caustic soda by centrifugation to separate pure SiC powder component and separating the mixed reaction solution of Si and caustic soda that can be used as a raw material of the remaining liquid refractory material. Method for recycling the waste silicon wafer sludge, characterized in that by the separation, recovery step to recover.
제1항에 있어서,
상기 절삭유 분리 회수단계는 고농도 절삭유 함유 슬러지와 저농도 절삭유 함유 슬러지에서 고농도, 저농도 절삭유를 분리 회수하고자 하는 경우, 고농도 절삭유 함유 슬러지를 증류 공정에 의해 고순도 절삭유를 분리 회수하는 1단계후, 상기 1단계에서 고순도 절삭유를 분리 회수한 슬러지에 저농도 절삭유 함유 슬러지와 함께 회전형 증발기를 통과시켜 저순도 절삭유를 분리 회수하는 2단계에 의해 고순도 절삭유와 저순도 절삭유를 각각 분리 회수하는 것을 특징으로 하는 폐 실리콘웨이퍼 슬러지의 재활용 방법.
The method of claim 1,
The cutting oil separation and recovering step may be performed after the step of separating and recovering the high-purity cutting oil-containing sludge by a distillation process to recover the high-density and low-concentration cutting oil from the high concentration cutting oil-containing sludge and the low concentration cutting oil-containing sludge. Waste silicon wafer sludge characterized in that the high-purity cutting oil and the low-purity cutting oil are separated and recovered by two stages of separating and recovering the low-purity cutting oil by passing through the rotary evaporator together with the low-concentration cutting oil-containing sludge to the sludge from which the high-purity cutting oil is recovered and recovered. Method of recycling.
반도체 제조 과정에서 발생되는 폐 실리콘웨이퍼 슬러지의 Si와 SiC 분말 성분 그리고 절삭유의 혼합 상태에서 절삭유를 증류, 증발에 의해 분리 회수하는 절삭유 분리 회수단계와;
상기 절삭유가 분리 회수된 폐 실리콘웨이퍼 슬러지의 Si, SiC 분말 성분을 분쇄하는 분쇄단계와;
상기 Si, SiC 분말 성분을 열처리하는 단계와;
상기 Si, SiC 분말 성분에 내화재 원료로 사용하기 적합하도록 추가 Si, SiC 분말을 혼합하면서 함량 조절하여 내화재 원료로 사용하는 Si, SiC 혼합분말 회수단계에 의한 것을 특징으로 하는 폐 실리콘웨이퍼 슬러지의 재활용 방법.
A cutting oil separation and recovery step of separating and recovering cutting oil by distillation and evaporation in a state in which Si, SiC powder components and cutting oil of waste silicon wafer sludge generated in a semiconductor manufacturing process are mixed;
A grinding step of grinding the Si and SiC powder components of the waste silicon wafer sludge from which the cutting oil is separated and recovered;
Heat-treating the Si and SiC powder components;
Recycling waste silicon wafer sludge, characterized in that by the Si, SiC mixed powder recovery step used as a refractory material by adjusting the content while mixing additional Si, SiC powder to be suitable as a refractory raw material to the Si, SiC powder component .
반도체 제조과정에서 발생되는 고농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 투입하여 고순도 절삭유를 증류하여 분리 회수하는 증류기(10)와;
상기 고순도 절삭유를 분리 회수한 슬러지와 저농도 절삭유 함유 폐 실리콘웨이퍼 슬러지를 투입하여 회전 이송하면서 저순도 절삭유를 분리 회수하는 회전형 증발기(20)와;
상기 절삭유를 분리 회수한 나머지 Si, SiC 분말 성분을 분쇄하는 분쇄기(30)와;
상기 분쇄기에 의해 분쇄된 Si, SiC 분말 성분에 가성소다와 물을 투입하여 혼합 반응시키는 혼합반응기(40) 및; 상기 혼합 반응된 혼합물을 원심 분리하여 순수한 SiC 분말 성분과 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리 회수하는 원심분리기(50)로 구성되어 이루어진 것을 특징으로 하는 폐 실리콘웨이퍼 슬러지의 재활용 장치.
A distillation unit 10 for distilling and recovering high-purity cutting oil by inputting waste silicon wafer sludge containing high concentration cutting oil generated during semiconductor manufacturing;
A rotary evaporator 20 for separating and recovering the low-purity cutting oil while rotating conveying the sludge from which the high-purity cutting oil is separated and recovered and the waste silicon wafer sludge containing the low-concentration cutting oil;
A crusher 30 for crushing the remaining Si and SiC powder components after separating and recovering the cutting oil;
A mixing reactor (40) for mixing and mixing caustic soda and water to Si and SiC powder components ground by the mill; Waste silicon wafer, characterized in that consisting of a centrifugal separator 50 for centrifuging the mixed reaction mixture to recover the mixed reaction solution of Si and caustic soda that can be used as a raw material of the pure SiC powder and the remaining liquid refractory material Sludge recycling unit.
반도체 제조과정에서 발생되는 폐 실리콘웨이퍼 슬러지를 투입하여 회전 이송하면서 절삭유를 분리 회수하는 회전형 증발기(20)와;
상기 절삭유를 분리 회수한 나머지 Si, SiC 분말 성분을 분쇄하는 분쇄기(30)와;
상기 분쇄기에 의해 분쇄된 Si, SiC 분말 성분에 가성소다와 물을 투입하여 혼합 반응시키는 혼합반응기(40) 및; 상기 혼합 반응된 혼합물을 원심 분리하여 순수한 SiC 분말 성분과 나머지 액상의 내화재 원료로 사용가능한 Si와 가성소다의 혼합 반응 용액을 분리 회수하는 원심분리기(50)로 구성되어 이루어진 것을 특징으로 하는 폐 실리콘웨이퍼 슬러지의 재활용 장치.
A rotary evaporator 20 for separating and recovering cutting oil while rotating and transferring waste silicon wafer sludge generated in a semiconductor manufacturing process;
A crusher 30 for crushing the remaining Si and SiC powder components after separating and recovering the cutting oil;
A mixing reactor (40) for mixing and mixing caustic soda and water to Si and SiC powder components ground by the mill; Waste silicon wafer, characterized in that consisting of a centrifugal separator 50 for centrifuging the mixed reaction mixture to recover the mixed reaction solution of Si and caustic soda that can be used as a raw material of the pure SiC powder and the remaining liquid refractory material Sludge recycling unit.
KR1020100002827A 2010-01-12 2010-01-12 The method and device for the recycling of waste silicon wafer sludge KR101179521B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020100002827A KR101179521B1 (en) 2010-01-12 2010-01-12 The method and device for the recycling of waste silicon wafer sludge

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020100002827A KR101179521B1 (en) 2010-01-12 2010-01-12 The method and device for the recycling of waste silicon wafer sludge

Publications (2)

Publication Number Publication Date
KR20110082894A true KR20110082894A (en) 2011-07-20
KR101179521B1 KR101179521B1 (en) 2012-09-07

Family

ID=44920730

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020100002827A KR101179521B1 (en) 2010-01-12 2010-01-12 The method and device for the recycling of waste silicon wafer sludge

Country Status (1)

Country Link
KR (1) KR101179521B1 (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101349137B1 (en) * 2013-02-21 2014-01-16 조선내화 주식회사 A method for fabrication of refractory material by recycling of silicone sludge and refractory material produced therefrom
KR101352372B1 (en) * 2012-04-12 2014-01-22 한국지질자원연구원 Method for producing silicon chloride from silicon sludge
KR101355816B1 (en) * 2012-04-11 2014-01-28 한국지질자원연구원 Method for separation and recovery of silicon from silicon sludge
WO2016060387A1 (en) * 2014-10-13 2016-04-21 주식회사 포스코 Method for manufacturing briquette and briquette manufactured by using same
KR20160112617A (en) * 2015-03-20 2016-09-28 주식회사 씨에스이엔지 Manufacturing method of heat increasing and component controlling element for steel making
WO2018147508A1 (en) * 2017-02-09 2018-08-16 한국지질자원연구원 Method for preparing silicon-carbon-graphene composite, composite prepared according thereto, and secondary battery to which same is applied
KR102569360B1 (en) * 2022-12-30 2023-08-22 주식회사 에스피이엔지 Sludge removal device generated in the semiconductor cleaning process

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102501829B1 (en) * 2020-07-21 2023-02-21 주식회사 무한에너지 Non-combustible coating agent for insulation materials and its manufacturing methods

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100542208B1 (en) 2004-03-30 2006-01-11 고등기술연구원연구조합 System for recycling waste sludge of semiconductor wafer
KR100776966B1 (en) 2006-07-25 2007-11-21 장영철 Apparatus for recycling the disposed slurry produced in the manufacturing process of the silicon wafer

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101355816B1 (en) * 2012-04-11 2014-01-28 한국지질자원연구원 Method for separation and recovery of silicon from silicon sludge
US9296617B2 (en) 2012-04-11 2016-03-29 Korea Institute Of Geoscience And Mineral Resources Method for separating and recovering silicon from silicon sludge
KR101352372B1 (en) * 2012-04-12 2014-01-22 한국지질자원연구원 Method for producing silicon chloride from silicon sludge
KR101349137B1 (en) * 2013-02-21 2014-01-16 조선내화 주식회사 A method for fabrication of refractory material by recycling of silicone sludge and refractory material produced therefrom
WO2016060387A1 (en) * 2014-10-13 2016-04-21 주식회사 포스코 Method for manufacturing briquette and briquette manufactured by using same
CN107075593A (en) * 2014-10-13 2017-08-18 株式会社Posco For the block for manufacturing the method for block and being manufactured using this method
KR20160112617A (en) * 2015-03-20 2016-09-28 주식회사 씨에스이엔지 Manufacturing method of heat increasing and component controlling element for steel making
WO2018147508A1 (en) * 2017-02-09 2018-08-16 한국지질자원연구원 Method for preparing silicon-carbon-graphene composite, composite prepared according thereto, and secondary battery to which same is applied
US11362326B2 (en) 2017-02-09 2022-06-14 Korea Institute Of Geoscience And Mineral Resources Method for preparing silicon-carbon-graphene composite, composite prepared according thereto, and secondary battery to which same is applied
KR102569360B1 (en) * 2022-12-30 2023-08-22 주식회사 에스피이엔지 Sludge removal device generated in the semiconductor cleaning process

Also Published As

Publication number Publication date
KR101179521B1 (en) 2012-09-07

Similar Documents

Publication Publication Date Title
KR101179521B1 (en) The method and device for the recycling of waste silicon wafer sludge
CN101528597B (en) Silicon reclamation apparatus and method of reclaiming silicon
Sergiienko et al. Silicon and silicon carbide powders recycling technology from wire-saw cutting waste in slicing process of silicon ingots
US20110059002A1 (en) Methods and apparatus for recovery of silicon and silicon carbide from spent wafer-sawing slurry
JP4369095B2 (en) Slurry regeneration method
JP5722601B2 (en) Silicon cutting waste treatment method
JP2007246367A (en) Method for recovering silicon-containing material
JP4966938B2 (en) Silicon regeneration method
JP4520331B2 (en) Method for producing hydrogen gas
JP2009196849A (en) Silicon recovery method and silicon recovery apparatus
KR100776966B1 (en) Apparatus for recycling the disposed slurry produced in the manufacturing process of the silicon wafer
KR101194188B1 (en) A method and an apparatus for recovering the active ingredient from wasted sludge of semiconductor and solar-silicon wafer manufacturing process
CN106006629B (en) A kind of sapphire method and product that diamond is reclaimed in grinding slug
CN106241794B (en) It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire
WO2009081725A1 (en) Silicon reclamation method
CN107902659A (en) A kind of method that recycling purification boron carbide in waste material is ground from sapphire
JP2009084069A (en) Apparatus and method for regenerating silicon
JP2007246366A (en) Method for recovering silicon-containing material
CN106829953B (en) A kind of method and product that diamond is recycled and recycled
JP4414364B2 (en) Method for recovering silicon-containing material
KR101045815B1 (en) Separation method of high purity silicon from backgrinding silicon waste
JP2011116605A (en) Method and apparatus for producing high-purity silica and high-purity silicon
JP2009292656A (en) Method for manufacturing silicon ingot
CN106672948A (en) Graphene dry-state conical grinding stripping complete plant
JP2005007541A (en) Reusing system of slurry waste liquid for slicing hard/brittle material

Legal Events

Date Code Title Description
A201 Request for examination
N231 Notification of change of applicant
A302 Request for accelerated examination
A302 Request for accelerated examination
N231 Notification of change of applicant
E902 Notification of reason for refusal
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20150708

Year of fee payment: 4

FPAY Annual fee payment

Payment date: 20160801

Year of fee payment: 5

FPAY Annual fee payment

Payment date: 20170829

Year of fee payment: 6

FPAY Annual fee payment

Payment date: 20180827

Year of fee payment: 7