KR100254896B1 - Impregnating liquor for baking tantalum condenser and preparing method of tantalum condenser having a good loss and esr properties using it - Google Patents
Impregnating liquor for baking tantalum condenser and preparing method of tantalum condenser having a good loss and esr properties using it Download PDFInfo
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- KR100254896B1 KR100254896B1 KR1019970068582A KR19970068582A KR100254896B1 KR 100254896 B1 KR100254896 B1 KR 100254896B1 KR 1019970068582 A KR1019970068582 A KR 1019970068582A KR 19970068582 A KR19970068582 A KR 19970068582A KR 100254896 B1 KR100254896 B1 KR 100254896B1
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- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 25
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 13
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000011572 manganese Substances 0.000 claims description 29
- 238000005470 impregnation Methods 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- 239000003990 capacitor Substances 0.000 claims description 20
- 238000010304 firing Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 229910003206 NH4VO3 Inorganic materials 0.000 abstract 2
- 230000008021 deposition Effects 0.000 abstract 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract 2
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
Description
본 발명은 탄탈 콘덴서 소성용 함침액에 관한 것으로, 보다 상세하게는 함침액에 첨가제를 사용하여 탄탈 콘덴서의 손실 및 등가 직렬 저항(ESR)값이 개선된 탄탈 콘덴서 제조 방법에 관한 것이다.The present invention relates to an impregnation liquid for tantalum capacitor firing, and more particularly, to a method of manufacturing a tantalum capacitor in which the loss of tantalum capacitor and the equivalent series resistance (ESR) are improved by using an additive in the impregnation liquid.
기존의 탄탈 콘덴서 제조 공정중에서 소성 공정은 핵심 공정으로써 화성 공정을 거쳐 형성된 유전체(Ta2O5)위에 음극층인 MnO2를 형성시키기 위해 질산 망간 수용액을 주로 하는 함침액을 열분해시켜 왔다.In the conventional tantalum capacitor manufacturing process, the sintering process is a core process that has thermally decomposed an impregnating solution mainly composed of manganese nitrate solution to form a cathode layer MnO 2 on a dielectric (Ta 2 O 5 ) formed through a chemical conversion process.
상기 질산 망간 수용액으로는 Mn(NO3)2, HNO3, NH4NO3및 H2O를 적절히 배합하여 Mn(NO3)2의 농도가 각각 20%, 40%, 60% 및 72%인 함침액을 제조한 다음, 먼저 유전체(Ta2O5)를 20% 농도의 Mn(NO3)2수용액에 함침시키고 고온 소성하여 MnO2층을 형성한 다음 그위에 다시 40% 농도의 Mn(NO3)2수용액을 함침시키고 고온 소성하여 MnO2층을 형성하고, 그 위에 또다시 60% 농도의 Mn(NO3)2수용액을 함침시키고 저온 소성시켜 MnO2층을 형성한 다음 최종적으로 72% 농도의 Mn(NO3)2수용액을 함침시키고 저온 소성시켜 MnO2층을 형성하는 공정으로 이루어져 있다.As the aqueous manganese nitrate solution, Mn (NO 3 ) 2 , HNO 3 , NH 4 NO 3, and H 2 O may be appropriately blended so that the concentrations of Mn (NO 3 ) 2 are 20%, 40%, 60%, and 72%, respectively. After the impregnation solution was prepared, the dielectric (Ta 2 O 5 ) was first impregnated in a 20% aqueous solution of Mn (NO 3 ) 2 , and calcined at high temperature to form an MnO 2 layer, followed by 40% concentration of Mn (NO 3 ) Impregnating 2 aqueous solution and calcining at high temperature to form MnO 2 layer, and then impregnating 60% concentration of Mn (NO 3 ) 2 aqueous solution and calcining at low temperature to form MnO 2 layer, and finally 72% concentration It is impregnated with an aqueous solution of Mn (NO 3 ) 2 and calcined at low temperature to form a MnO 2 layer.
상기 MnO2형성 과정은 다음 반응식으로 나타낼 수 있다:The MnO 2 formation process can be represented by the following scheme:
Mn(NO3)2ㆍxH2O → Mn(NO3)2+ xH2O↑Mn (NO 3 ) 2 ㆍ xH2O → Mn (NO 3 ) 2 + xH 2 O ↑
Mn(NO3)2→ MnONO3+ NO2↑Mn (NO 3 ) 2 → MnONO 3 + NO 2 ↑
MnONO3→ MnO2+ NO2↑MnONO 3 → MnO 2 + NO 2 ↑
그러나 상기 MnO2는 비저항이 약 100Ωㆍcm으로 그 생성 정도 및 상태에 따라 콘덴서의 특성이 좌우된다. 또한 고용량 및 소형화 추세에 따라 탄탈 콘덴서의 손실 및 ESR 특성이 더욱 중요시되고 있다.However, the MnO 2 has a specific resistance of about 100 Ω · cm, and the characteristics of the capacitor depend on the generation degree and state. In addition, the loss and ESR characteristics of tantalum capacitors are becoming more important according to the trend of high capacity and miniaturization.
이에 본 발명의 목적은 기존의 질산망간 수용액에 NH4VO3를 첨가함으로써 전도성을 향상시킨 탄탈 콘덴서 제조용 함침액을 제공하려는데 있다.Accordingly, an object of the present invention is to provide an impregnation solution for manufacturing tantalum capacitors having improved conductivity by adding NH 4 VO 3 to an existing aqueous solution of manganese nitrate.
본 발명의 또다른 목적은 상기 함침액을 이용하여 기존의 라인을 그대로 이용하면서 손실 및 ESR이 개선된 탄탈 콘덴서를 제공하려는데 있다.Another object of the present invention is to provide a tantalum capacitor with improved loss and ESR while using an existing line as it is using the impregnation solution.
도 1은 본 발명에 의해 제조된 탄탈 콘덴서의 손실각(tan δ)를 도시한 그래프,및1 is a graph showing a loss angle tan δ of a tantalum capacitor manufactured according to the present invention, and
도 2는 본 발명에 의해 제조된 탄탈 콘덴서의 등가 직렬 저항(ESR)을 도시한 그래프이다.2 is a graph showing an equivalent series resistance (ESR) of a tantalum capacitor manufactured by the present invention.
본 발명의 제1견지에 의하면,According to the first aspect of the present invention,
Mn(NO3)2, HNO3, NH4NO3및 H2O로 이루어진 탄탈 콘덴서 소성용 질산 망간 수용액에 있어서,In the aqueous solution of manganese nitrate for firing tantalum capacitors composed of Mn (NO 3 ) 2 , HNO 3 , NH 4 NO 3 and H 2 O,
NH4VO3를 Mn(NO3)2농도 대비 0.009-0.011%몰 첨가한Add 0.009-0.011% mole of NH 4 VO 3 to Mn (NO 3 ) 2 concentration
탄탈 콘덴서 소성용 함침액이 제공된다.An impregnation solution for firing tantalum capacitors is provided.
본 발명의 제2 견지에 의하면,According to the second aspect of the present invention,
탄탈 콘덴서 제조시 MnO2층을 형성하는데 있어서,In forming MnO 2 layer in manufacturing tantalum capacitor,
상기 제1견지의 함침액을 Mn(NO3)2농도가 각각 10%, 20%, 40%, 60% 및 72%이도록 제조하고 10, 20 및 40% 농도에서는 NH4NO3를 제거한 함침액을 제조하는 제1단계,The impregnation liquid of the first finding was prepared such that the concentration of Mn (NO 3 ) 2 was 10%, 20%, 40%, 60%, and 72%, respectively, and the NH 4 NO 3 was removed at 10, 20, and 40% concentrations. To prepare a first step,
상기 10% 농도 함침액을 화성 공정을 거쳐 생성된 유전체 Ta2O5상에 침적한 다음 꺼내어 고온 소성하는 제2 단계,A second step of depositing the 10% concentration impregnating solution on the dielectric Ta 2 O 5 generated through the chemical conversion process and then removing the same;
이어서 20% 및 40% 농도 함침액으로 상기 제2 단계를 순차적으로 수행하는 제3 단계,A third step of sequentially performing the second step with 20% and 40% concentration impregnation solution,
상기 60% 농도 함침액을 화성 공정을 거쳐 생성된 유전체 Ta2O5상에 침적한 다음 꺼내고 저온 소성하는 제4 단계, 및A fourth step of depositing the 60% concentration impregnation solution on the dielectric Ta 2 O 5 produced through the chemical conversion process, taking out the material, and baking at a low temperature; and
이어서 72% 농도 함침액으로 상기 제5 단계를 수행하는 단계,로 이루어지는And then performing the fifth step with a 72% strength concentration impregnation solution.
손실 및 ESR 특성이 개선된 탄탈 콘덴서 제조 방법이 제공된다.A method of manufacturing tantalum capacitors with improved loss and ESR characteristics is provided.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명에서는 기존의 탄탈 콘덴서 소성용 질산망간 함침액에 NH4VO3를 첨가한 함침액을 제조하고 이를 이용하여 손실 및 ESR이 개선된 탄탈 콘덴서를 제조한다.In the present invention, the impregnation solution of NH 4 VO 3 is added to the conventional manganese nitrate impregnation solution for firing tantalum capacitors, and a tantalum capacitor with improved loss and ESR is prepared using the impregnation solution.
NH4VO3를 첨가하는 경우, 그 반응식은 다음과 같다:When NH 4 VO 3 is added, the reaction is as follows:
NH4VO3→ NH4 ++ VO3 - NH 4 VO 3 → NH 4 + + VO 3 -
(상기 VO3 -는 V2O5형태로 안정하다)(The above VO 3 - is stable in the form of V 2 O 5 )
V2O5→ 2VMn+ 2e- + 4O2+ 1/2O2↑V 2 O 5 → 2V Mn + 2e- + 4O 2 + 1 / 2O 2 ↑
여기서 종래의 MN(NO3)2로 부터 생성되는 Mn4+가 보다 가수가 큰 V5+이온 금속으로 치환되면서 전자수가 늘어나 음극의 전도성이 향상된다.Herein, Mn 4+ generated from the conventional MN (NO 3 ) 2 is substituted with a larger valence V 5+ ion metal, thereby increasing the number of electrons and improving the conductivity of the negative electrode.
상기 NH4VO3는 MN(NO3)2농도 대비하여 0.009-0.011%몰을 첨가하는 것이 적절하다. NH4VO3양이 너무 과량이면 급격한 반응으로 인해 소성후 펠릿 표면이 상당히 거칠어지게 되어 바람직하지 않다.The NH 4 VO 3 is appropriate to add 0.009-0.011% mol relative to the concentration of MN (NO 3 ) 2 . If the amount of NH 4 VO 3 is too large, it is not preferable because the pellet surface becomes rough after the firing due to the rapid reaction.
실시예Example
시편으로는 10/100펠릿을 이용하였다. 시험 패턴에 따라 각각 2벨트(56EA)개를 사용하였다. Mn(NO3)2농도가 10%, 20%, 40%, 60%, 72%인 함침액을 제조하고 하기표 1에 기술된 바와 같이 각 시료를 제조하였다.10/100 pellets were used as the specimen. Two belts (56EA) each were used according to the test pattern. An impregnation solution with Mn (NO 3 ) 2 concentrations of 10%, 20%, 40%, 60%, 72% was prepared and each sample was prepared as described in Table 1 below.
각 시료를 실험용 VAT를 이용하여 화성한 다음 소성하였다.Each sample was chemically converted using an experimental VAT and then fired.
상기 함침액중 10%, 20% 및 40% 농도의 경우에는 고온 소성(125-205℃)한 다음 60% 및 72%의 농도에 대하여는 저온 소성(95-180℃)하고 그 특성값을 측정하였다.In the case of 10%, 20% and 40% concentration in the impregnation solution, high temperature firing (125-205 ° C.) was followed by low temperature firing (95-180 ° C.) for 60% and 72%. .
각각 제조된 실시예 1-7에 대하여 정전 용량(C), 손실각(tan δ), 등가 직렬 저항(ESR), 누설 전류(LC) 및 파괴 전압(BDV)등을 측정하고 그 결과를 하기표 2에 기재하였다.The capacitance (C), loss angle (tan δ), equivalent series resistance (ESR), leakage current (LC), breakdown voltage (BDV), etc. of each manufactured Example 1-7 were measured and the results are shown in the following table. 2 is described.
또한 손실각의 측정값은 도 1에 그리고 등가 직렬 저항의 측정값은 도 2에 도시하였다.In addition, the measured value of the loss angle is shown in FIG. 1, and the measured value of the equivalent series resistance is shown in FIG.
상기표 2 및 도 1∼2에 의하면, 각 농도에 대해 Nn(NO4)3대비 0.01%몰 NH4VO3를 첨가하고, 이중 10, 20 및 40%의 농도에서는 NH4NO3를 제거한 실시예 5의 경우에 손실각은 19.68%, ESR 특성은 11.3%정도 개선되었다.According to Table 2 and FIGS. 1 and 2, 0.01% mole NH 4 VO 3 was added to Nn (NO 4 ) 3 for each concentration, and NH 4 NO 3 was removed at concentrations of 10, 20, and 40%. In Example 5, the loss angle is improved by 19.68% and the ESR characteristic is 11.3%.
나아가 모든 농도에서 NH4NO3를 제거한 실시예 4 및 6의 경우 역시 손실각 및 ESR이 개선된 것을 알 수 있다.Furthermore, in Examples 4 and 6 in which NH 4 NO 3 was removed at all concentrations, the loss angle and the ESR were also improved.
상기한 바에 따르면, 기존 라인을 그대로 이용가능하면서 손실각 및 등가 직렬 저항(ESR)이 개선된 탄탈 콘덴서를 제조할 수 있다.According to the above, it is possible to manufacture a tantalum capacitor which can use the existing line as it is and improve the loss angle and equivalent series resistance (ESR).
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| KR1019970068582A KR100254896B1 (en) | 1997-12-13 | 1997-12-13 | Impregnating liquor for baking tantalum condenser and preparing method of tantalum condenser having a good loss and esr properties using it |
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| KR1019970068582A KR100254896B1 (en) | 1997-12-13 | 1997-12-13 | Impregnating liquor for baking tantalum condenser and preparing method of tantalum condenser having a good loss and esr properties using it |
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