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KR940008898B1 - Firing liguid and soaking method of tantal condenser - Google Patents

Firing liguid and soaking method of tantal condenser Download PDF

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Publication number
KR940008898B1
KR940008898B1 KR1019920006579A KR920006579A KR940008898B1 KR 940008898 B1 KR940008898 B1 KR 940008898B1 KR 1019920006579 A KR1019920006579 A KR 1019920006579A KR 920006579 A KR920006579 A KR 920006579A KR 940008898 B1 KR940008898 B1 KR 940008898B1
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South Korea
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firing
solution
tantalum
manganese nitrate
mold
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KR1019920006579A
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Korean (ko)
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KR930022413A (en
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김용주
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대우전자부품 주식회사
석진철
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Priority to KR1019920006579A priority Critical patent/KR940008898B1/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004Details
    • H01G9/04Electrodes or formation of dielectric layers thereon
    • H01G9/042Electrodes or formation of dielectric layers thereon characterised by the material

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)

Abstract

The mold/impregnating liquor for increasing the impregnating ratio, and impuring loss characteristic and the capacitance uses a mixed solution with Mn(NO3)2 of 20 %, and NH4NO3 of 2-6 % as the first mold/impregnating liquor, and the Mn(NO3)2 liquid of 60 % as the second mold/impregnating liquor. The tantal element is dipped into the first mold/impregnating liquor 3 times, and into the second mold/impregnating liquor 7 times continuously.

Description

탄탈 전해콘덴서의 소성 함침액 및 그 침적방법Plastic Impregnation Solution for Tantalum Electrolytic Capacitors

제1도는 본 발명에 따른 소자의 정전용량 변화율 특성도.1 is a characteristic diagram of the capacitance change rate of the device according to the present invention.

제2도는 본 발명에 따른 소자의 손실각 정접 특성도.2 is a loss angle tangent characteristics of the device according to the present invention.

제3도는 종래 소자의 정전용량 변환율 특성도.3 is a capacitance conversion rate characteristic diagram of a conventional device.

제4도는 종래 소자의 손실각 정접 특성도.4 is a loss angle tangent characteristics of a conventional device.

본 발명은 탄탈 전해콘덴서의 소성 함침액 및 그 침적방법에 관한 것으로, 특히 탄탈 콘덴서의 제조공정중 콘덴서의 전기적 특성 즉 누설전류(Leakage Current, μA), 정전용량 변화율(△C,%), 손실각의 정접(tanδ,%)을 결정짓는 소성공정 있어서, 탄탈피막(Ta2O5)상에 전해질층을 형성하기 위해 소자를 질산망간(Mn(no3)2〕액과 질산(NH4NO3)액의 혼합액중에 3회 침적하고 다시 질산망간액에 7회 침적함으로써 함침율 향상에 따른 소자의 전기적 특성과 생산성향상에 기여하기 위한 것이다.The present invention relates to a plastic impregnation solution of tantalum electrolytic capacitors and their deposition method, in particular the electrical characteristics of the capacitor during the manufacturing process of the tantalum capacitor, that is, leakage current (μA), capacitance change rate (ΔC,%), loss In the firing step of determining the tangent tangent (tan δ,%), the element is manganese nitrate (Mn (no 3 ) 2 ) solution and nitric acid (NH 4 NO) to form an electrolyte layer on the tantalum coating (Ta 2 O 5 ). 3 ) It is to contribute to the improvement of the electrical properties and productivity of the device by improving the impregnation rate by immersing three times in the liquid mixture and immersing seven times in the manganese nitrate solution.

일반적으로 탄탈 전해콘덴서를 얻기 위하여 탄탈 분말파우더를 접합제(Binder)와 혼합하여 금형에 의해 펠릿(Pellet)으로 성형하는 성형공정과, 펠릿을 진공소결로에 넣고 열을 가하여 펠릿내의 접합제와 불순물제거로 순수한 탄탈파우더만 소결시키는 소결공정과, 전반적으로 양호한 화학처리 공정작업성을 부여하기 위하여 펠릿을 알루미늄 벨트에 용접하는 소자용접 공정과, 용접된 펠릿을 인산 수용액에서 전기분해 시켜 탄탈표면에 탄탈피막(Ta2O)(유전체)을 형성시키는 화성공정과, 탄탈피막위에 전핸질층을 형성하기 위해 소자를 질산망간액 중에 침적시킨후 소성로에서 열분해 시켜 이산화망간(MnO2)고체 전해질층을 형성하기 위한 소성공정으로 순차 이어지는 바, 상기 소성공전에서 소자를 침적시키는 과정중 종래의 경우에는 10~20%의 질산망간액[Mn(NO3)2]에 소자를 3회 침적하고 다시 60~75%의 질산망간액에 소자를 9회 침적하였는데 이때의 소송온도는 상기 전자의 침적 상태에서 290℃를 유지하였고 후자인 경우에는 260℃를 유지하였다. 또한 여기서는 침적시간은 4분이었다.In general, in order to obtain a tantalum electrolytic capacitor, a molding process in which a tantalum powder powder is mixed with a binder and formed into pellets by a mold, and the pellets are put into a vacuum sintering furnace and heated to apply a binder and impurities in the pellets. Sintering process to sinter only pure tantalum powder by removal, Device welding process for welding pellets to aluminum belt to give good chemical treatment process overall, Tantalum on tantalum surface by electrolysis of the welded pellet in aqueous phosphate solution A chemical conversion process for forming a coating layer (Ta 2 O) (dielectric), and a device for immersion in a manganese nitrate solution to form an all-handling layer on a tantalum coating, followed by thermal decomposition in a kiln to form a manganese dioxide (MnO 2 ) solid electrolyte layer The sequential process is followed by a sintering process. In the conventional process of depositing devices in the firing process, 10-20% of manganese nitrate [Mn (NO 3) 2] a were immersed three times the device and immersed 9 times element in manganese nitrate solution of 60% to 75% re-action temperature at this time was maintained at 290 ℃ in the deposition condition of the electron when the latter Was maintained at 260 ° C. Here, the deposition time was 4 minutes.

그러나 이와같은 종래의 침적방법에 의한 경우 소성횟수는 도합 12회를 실시하면서도 함침율이 불량하였고 이는 제3도 및 제4도에서 보는 바와같이 CHIP 16V-10㎌에서 정전용량 변화율(Δc)과 손실각의 정접(tjan δ나)주파수특성이 각각 -7%,4%로 나타나고 있음을 알 수 있어 용량미달과 손실특성이 불량한 것 임을 나타내고 있는 것이다.However, in the case of the conventional immersion method, the firing times were 12 times in total, but the impregnation rate was poor. As shown in FIGS. 3 and 4, the change rate of capacitance (Δc) and loss at CHIP 16V-10㎌ It can be seen that the frequency characteristics of the tangent tangent (tjan δ) are -7% and 4%, respectively, indicating that the capacity and loss characteristics are poor.

정전용량 변화율 즉, 용량감소율은 0의 범위체 근접할수록 용량특성이 향상되고 손실각의 정접은 최저치로 내려갈수록 양호한 것인바, 종래의 경우에 있어서는 이러한 특성에 근접하지 못하는 결과를 보이고 있다.The capacitance change rate, that is, the capacity reduction rate is improved as the near range of zero improves the capacity characteristic, and the loss angle tangent decreases to the lowest value. Thus, in the conventional case, the result is not close to this characteristic.

또한 소성횟수가 증가됨으로 인한 생산성저하의 결과르 초래하고 있는 것이다.It also results in a decrease in productivity due to the increased firing frequency.

본 발명은 소성공정의 침적횟수를 경감하면서 함침율을 향상시킴은 물론 손실특성과 용량특성 대폭 향상시키고 생산성 향상에 기여하고자 하는 것인바, 이하 첨부도면과 관련하여 본 발명을 상세히 설명하면 다음과 같다.The present invention is to improve the impregnation rate while reducing the number of depositions in the firing process, as well as to significantly improve the loss characteristics and capacity characteristics and to improve the productivity. Hereinafter, the present invention will be described in detail with reference to the accompanying drawings. .

소성공정에서 탄탈피막(Ta2O5)상에 이산화망간(MnO2)고체 전해질층을 형성하기 위한 함침액으로써 1차함침액을 20%의 질산망간[Mn(NO3)2]과 2~6%의 질산암모늄(NH4NO3)혼합액으로 하고, 2차 함침액은 60%의 질산망간액으로 하여 소자를 상기 20% Mn(NO3)2+2~6% NH4NO3의 혼합액중에 3회 침적하고 다시 60% Mn(NO3)2액중에 소자를 7회 침적시킨 다음, 소성로에서 열분해시켜 이산화망간(MnO2)의 고체 전해질층을 소자의 탄탈피막에 형성케 하는 바, 이때의 1,2차 소성온도는 각 290℃와 260℃로써 공히 종래와 동일하며 침적시간 역시 4분으로 종래와 동일 하게 실시하였다.In the firing process, 20% of manganese nitrate [Mn (NO 3 ) 2 ] and 2 ~ 6 were used as the impregnation solution to form the manganese dioxide (MnO 2 ) solid electrolyte layer on the tantalum coating (Ta 2 O 5 ). % Ammonium nitrate (NH 4 NO 3 ) mixture, the secondary impregnation solution is 60% manganese nitrate solution and the device is placed in the mixture of 20% Mn (NO 3 ) 2 + 2-6% NH 4 NO 3 After immersion three times, the device was immersed seven times in a 60% Mn (NO 3 ) 2 liquid, and then pyrolyzed in a kiln to form a solid electrolyte layer of manganese dioxide (MnO 2 ) on the tantalum film of the device. The secondary firing temperature was 290 ° C. and 260 ° C., respectively, and the same as before, and the deposition time was 4 minutes.

상기한 바에 의거한 본 발명의 실시결과 함침율 향상에 따른 안정된 고체 전해질층 형성으로 제1,2도에서 보는 바와 같이 정전용량 변화율(Δc)은 -3.5%를 나타내었고 손실각의 정점(tanδ)은 2%를 나타내고 있는바, 각각의 특성은 종래 대비 50%의 상승효과를 얻게 되었다.As a result of the implementation of the present invention based on the above, a stable solid electrolyte layer was formed according to the improvement of the impregnation rate. Silver represents 2%, and each characteristic has a synergistic effect of 50%.

이와 같이 본 발명에 의한 소자의 정전용량 변화율 즉, 용량 감소율은 0에 대폭 근접하고 있고 손실특성은 대폭 저하됨으로써 양호한 전기적 특성을 입증하는 것이라 하겠다.As described above, the capacitance change rate, that is, the capacitance decrease rate of the device according to the present invention is substantially close to zero, and the loss characteristic is greatly reduced, thereby demonstrating good electrical characteristics.

이상에서와 같이 본 발명은 함침율을 향상시키면서 소선공정의 침전회수를 경감시켰고 아울러 생상성 향상에 기여하게 되었음은 물론 궁극적으로 전기적 특성인 정전용량 변화율과 손실각의 정점 특성을 크게 개선한 발명인 것이다.As described above, the present invention is to improve the impregnation rate, to reduce the settling frequency of the wire burning process and to contribute to the improvement in productivity, as well as to ultimately improve the electrical characteristics of the capacitance change rate and the peak angle of the loss angle.

Claims (2)

탄탈소자의 1차 소성함침액을 20% 질산망간[Mn(NO3)2] +2~6% 질산(NH4NO3)의 혼합액으로 하고 2차 소성함침액을 60% 질산망간액으로 하여서 된 것을 특징으로 하는 탄탈전해콘덴서의 소성함침액.The primary firing impregnation solution of tantalum element is a mixture of 20% manganese nitrate [Mn (NO 3 ) 2 ] + 2 ~ 6% nitric acid (NH 4 NO 3 ), and the secondary firing impregnation solution is 60% manganese nitrate solution. Plastic impregnation liquid of tantalum electrolytic capacitor, characterized in that the. 탄탈소자의 상기 20% 질산망간 +2~6% 질산암모늄의 혼합액에서 3회 침적하고 상기 60% 질산망간액에서 7회 침적하는 것을 특징으로 하는 탄탈 전해콘덴서의 침적방법.And depositing three times in the mixed solution of 20% manganese nitrate + 2-6% ammonium nitrate of the tantalum element and seven times in the 60% manganese nitrate solution.
KR1019920006579A 1992-04-20 1992-04-20 Firing liguid and soaking method of tantal condenser KR940008898B1 (en)

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KR940008898B1 true KR940008898B1 (en) 1994-09-28

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