KR940006687B1 - Manufacturing method of thick film semiconductor oxygen sensor - Google Patents
Manufacturing method of thick film semiconductor oxygen sensor Download PDFInfo
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- KR940006687B1 KR940006687B1 KR1019910020838A KR910020838A KR940006687B1 KR 940006687 B1 KR940006687 B1 KR 940006687B1 KR 1019910020838 A KR1019910020838 A KR 1019910020838A KR 910020838 A KR910020838 A KR 910020838A KR 940006687 B1 KR940006687 B1 KR 940006687B1
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000004065 semiconductor Substances 0.000 title claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 title claims description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 25
- 239000001301 oxygen Substances 0.000 title claims description 25
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 101100522123 Caenorhabditis elegans ptc-1 gene Proteins 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000007598 dipping method Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 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
- 238000010438 heat treatment Methods 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 18
- 230000035945 sensitivity Effects 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 229910052763 palladium Inorganic materials 0.000 description 5
- 229910052703 rhodium Inorganic materials 0.000 description 5
- 239000000446 fuel Substances 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
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- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Ceramic Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
Description
제1도 내지 제3도는 본 발명에 의한 산소센서의 특성을 보인 그래프로서, 제1도는 900℃에서 1시간 열처리된 산소센서의 동작온도 400℃에서의 Ta2O5첨가량에 따른 감도 의존성 그래프.1 to 3 is a graph showing the characteristics of the oxygen sensor according to the present invention, Figure 1 is a graph of sensitivity dependence according to the amount of Ta 2 O 5 added at 400 ℃ operating temperature of the oxygen sensor heat-treated at 900 ℃ for 1 hour.
제2도는 여러가지 함량의 산소센서의 Pco/PO2비에 의존하는 소자 저항값 변화도.2 is a diagram showing the change in device resistance value depending on the Pco / PO 2 ratio of various oxygen sensors.
제3도는 동작온도 400℃, 500℃에서 공연비 λ에 의존하는 소자 저항값 변화도.3 is a diagram showing the change in device resistance value depending on the air-fuel ratio λ at the operating temperature of 400 ° C and 500 ° C.
본 발명은 백금(Pt)이 미량 첨가된 티타니아(TiO2: anatase)에 Ta2O5를 소량 첨가하고, 침적법(dippingmathod)에 의하여 후막형 공연비 제어용 산소센서를 제조하는 제조방법에 관한 것으로 특히 낮은 동작온도에서 고감도와 안정된 특성을 가지는 산화물 반도제 산소센서의 제조방법에 관한 것이다.The present invention relates to a manufacturing method for producing a thick film-type air-fuel ratio control oxygen sensor by adding Ta 2 O 5 to Titania (TiO 2 : anatase) to which a small amount of platinum (Pt) is added, and by dipping mathod. A method of manufacturing an oxide semiconductor oxygen sensor having high sensitivity and stable characteristics at low operating temperatures.
종래 자동차나 대형보일러에 이용되고 있는 산소센서의 원료물질로는 ZrO2과 TiO2가 있는 바, 이중 ZrO2를 원료로한 산소센서는 구조가 복잡하고 고가이나 TiO2를 원료로한 산소센서는 비교적 구조가 간단하고 소형화할 수 있어서 제조비용을 줄일 수 있으므로 TiO2를 주성분으로 하는 산소센서의 개발이 많이 진행되고 있다.The raw materials of oxygen sensors used in automobiles and large boilers are ZrO 2 and TiO 2. Among them, oxygen sensors based on ZrO 2 are complicated and expensive, but oxygen sensors based on TiO 2 are expensive. since the structure is relatively simple and reduce the manufacturing cost can be reduced in size in a lot of development has been going on of the oxygen sensor comprising mainly TiO 2.
그리고 이러한 TiO2산소센서의 구조는 후막형이 주가 된다.The main structure of the TiO 2 oxygen sensor is a thick film.
종래 후막형 TiO2산소센서의 경우 감지막의 형성은 주로 스크린 인쇄법(Screen printing method)에 의해 이루어지며 이때, Pt, Pd 그리고 Rh등의 귀금속 촉매물질이 소량 첨가된다.In the case of the conventional thick film type TiO 2 oxygen sensor, the formation of the sensing film is mainly performed by a screen printing method. At this time, a small amount of noble metal catalyst materials such as Pt, Pd and Rh are added.
보다 구체적으로 설명하면 스크린 인쇄법에 의한 후막형 TiO2반도제 산화물 산소센서의 제작은 TiO2분말에 Pt, Pd 그리고 Rh를 소량 첨가하여 일정한 점도를 갖는 페이스트(paste)를 만든후 이 페이스트를 스크린위에 올린후 스크린 고무로 눌러서 후막을 형성하며 이렇게 형성된 후막은 1200℃이상의 고온에서 소결하는 과정으로 이루어진다.More specifically, the fabrication of a thick film type TiO 2 semiconductor oxide oxygen sensor by screen printing method is performed by adding a small amount of Pt, Pd and Rh to the TiO 2 powder to form a paste having a constant viscosity, and then screening the paste. After lifting on the screen by pressing the screen rubber to form a thick film is formed by sintering at a high temperature of more than 1200 ℃.
상기한 바와 같이 스크린 인쇄법에 의하여 후막형 TiO2산소센서를 제조하면, 스크린의 메쉬(mesh)와 TiO2및 귀금속 촉매물질인 Pt, Pd 그리고 Rh 등의 입도사이에는 메칭(matching)의 어려움이 상존하여 균일한 조성의 막을 형성하기 어렵고 또한 페이스트의 일정점도를 조절하기 의해 사용되는 유기물(organic)이나, 글래스 플릿(glass frit)이 산소에 대한 감도에 영향을 미친다.When the thick film type TiO 2 oxygen sensor is manufactured by screen printing as described above, there is a difficulty in matching between the mesh of the screen and the particle sizes of TiO 2 and the precious metal catalyst materials Pt, Pd and Rh. It is difficult to form a film having a uniform composition at all times, and an organic material or glass frit used by adjusting a constant viscosity of the paste affects the sensitivity to oxygen.
뿐만 아니라 형성된 막의 소결이 1200℃이상의 고온에서 이루어지기 때문에 막에 크랙(crack)이 생겨 특성이 불안정하며, 500℃이상의 동작온도에서 연속적으로 사용될 정우 Pt, Pd 그리고 Rh등이 산화물을 형성하여 막의 감도가 떨어지는 것이었다.In addition, since the sintering of the formed film is performed at a high temperature of more than 1200 ℃, cracks are generated in the film and its characteristics are unstable, and Pt, Pd and Rh, which are used continuously at an operating temperature of 500 ℃ or more, form an oxide, so that the sensitivity of the film is formed. Was falling.
본 발명은 상기한 바와 같은 종래의 결함을 해소하기 위하여 창안한 것으로 이하에 구체적으로 설명하면 다음과 같다.The present invention has been made to solve the above-mentioned conventional defects and will be described in detail below.
본 발명은 TiO2와 Pt의 혼합분말에 Ta2O5를 0∼10중량% 혼합하고, 이 혼합물을 Pt전극이 형성된 알루미나 기판에 코팅하는 것을 특징으로 하고 있다.The present invention is characterized in that 0 to 10% by weight of Ta 2 O 5 is mixed with a mixed powder of TiO 2 and Pt, and the mixture is coated on an alumina substrate having a Pt electrode.
보다 자세히 설명하면 혼합물은 ( TiO2+Pt) : Ta2O5가 중량비로 95 : 5가 되도록 혼합하여 슬러리(slurry)를 형성하고, 이러한 TiO2+Pt+Ta2O5의 혼합물에 알루미나 기판을 침적법(dipping method)으로 침적시켜 후막을 형성하며, 알루미나 기판에 후막을 코팅한 후에는 종래 소결온도에 비하여 저온인 800℃∼1100℃에서 소결하는 것으로 되어 있다.In more detail, the mixture is mixed so that (TiO 2 + Pt): Ta 2 O 5 is 95: 5 by weight to form a slurry, and an alumina substrate is added to the mixture of TiO 2 + Pt + Ta 2 O 5 . Is deposited by a dipping method to form a thick film. After the thick film is coated on the alumina substrate, the film is sintered at 800 ° C to 1100 ° C, which is lower than the conventional sintering temperature.
본 발명은 상기한 과정으로 행하여 지며, 공언비 λ는 Q2와 CO표준가스를 이용하여 Pco/PO2의 분압비를 이용하였다.The present invention is carried out in the above-described process, the azeotropy ratio λ used a partial pressure ratio of Pco / PO 2 using Q 2 and CO standard gas.
그리고 산소센서의 동작온도의 콘트롤을 위하여 센서를 전기로(electric furnace)내에 위치시켰으며, 센서의 양단에 Pt선을 연결하여 저항변화를 관찰하였다.In order to control the operating temperature of the oxygen sensor, the sensor was placed in an electric furnace, and the resistance change was observed by connecting Pt lines at both ends of the sensor.
이러한 본 발명의 산소센서에 따르는 특성은 다음의 실시예와 함께 첨부도면 제1도 내지 제3도에 의하여 보다 구체적으로 설명될 것이다.This characteristic according to the oxygen sensor of the present invention will be described in more detail with reference to the accompanying drawings, FIGS.
[실시예]EXAMPLE
먼저 Pt를 H2PtCl6.6H2O의 형태로 TiO에 1중량% 혼합시키고, 이 혼합분말에 Ta2O5를 0∼l0중량% 정도 혼합하며, 탈이온수(deionized water)로 혼합한 후 110℃에서 1시간 건조시킨다.First mixing 1% by weight of Pt in the form of TiO 2 PtCl 6 .6H 2 O and H, the Ta 2 O 5 and mix approximately 0~l0% by weight in the powder mixture, were mixed with deionized water (deionized water) Dry at 110 ° C. for 1 hour.
이와 같이 하여 건조된 분말을 600∼630℃에서 1시간 동안 하소(calcing)한후 미분쇄기(agate motar등)로 미분쇄시키고 탈이온수로 점도를 맞추어서 슬러리를 만든다.The dried powder is calcined (calculated) for 1 hour at 600 to 630 ° C. and then pulverized with a pulverizer (agate motar, etc.) to make a slurry by adjusting the viscosity with deionized water.
이와 같이된 상기 혼합물 슬러리에 전극이 부착된 알루미나 기판을 약 0.5초간 담근후 꺼내어 다시 천천히 승온시켜, 110℃에서 완전히 건조시키고나서 소결온도 800∼l100℃에서 한시간 소결하여 센서를 완성한다.After dipping the alumina substrate with the electrode in the mixture slurry for about 0.5 seconds and taking it out again, slowly increasing the temperature, completely drying at 110 ° C, and sintering at sintering temperature of 800 to 100 ° C for one hour to complete the sensor.
한편 상기 과정에서 이용되는 알루미나 기판은 아세톤 용액내에서 5∼10분간 초음파 세척한 후 Pt전극(전극사이거리 1mm)을 스크린 인쇄법으로 형성한 후 110℃에서 건조시키고, 대기중 1300℃에서 5분간 소결하여 완성한 것이다.Meanwhile, the alumina substrate used in the above process was ultrasonically cleaned in acetone solution for 5 to 10 minutes, and then Pt electrodes (1 mm between electrodes) were formed by screen printing and dried at 110 ° C. for 5 minutes at 1300 ° C. in air. It is completed by sintering.
첨부도면 제1 내지 제3도는 상기와 같이 하여 제조된 후막형 산소센서의 성능을 보인 그래프로서, 제1도는 900℃에서 1시간 열처리된 TiO2산소센서 소자의 동작온도 400℃에서의 Ta2O5첨가량에 따른 TiO2소자의 감도 의존성 그래프이고, 감도 S는 표준가스 1000ppm CO/N2및 250ppm O2/N2가 혼합된 혼합가스내에서의 소자 저항값 R gas와 250ppm O2/N2가스내에서의 소자 저항값 Ro와의 저항비 Ro/R gas로 나타낸 것이다.1 to 3 are graphs showing the performance of the thick-film oxygen sensor manufactured as described above, and FIG. 1 is Ta 2 O at an operating temperature of 400 ° C. of the TiO 2 oxygen sensor element heat-treated at 900 ° C. for 1 hour. a sensitivity dependence graph of the TiO 2, the device according to the fifth addition level, the sensitivity S is a standard gas 1000ppm CO / N 2 and 250ppm O 2 / N 2 mixed device resistance values in the mixed gas R gas and 250ppm O 2 / N 2 It is shown by the resistance ratio Ro / R gas with element resistance value Ro in gas.
상기와 같이 하여 제조된 후막형 TiO2산소센서는 동작온도 400℃의 경우 소결온도 900℃에서 한시간 소결한 소자의 감도가 가장 우수하있으며, 특히 산소희박 영역인 Pco/Po2=4일때 제1도에서 알 수 있듯이 Ta2O5함량이 5중량%일 경우 센서의 감도가 우수함을 알 수 있었다.The thick film type TiO 2 oxygen sensor manufactured as described above has the highest sensitivity of the device sintered at 900 ° C for one hour at the operating temperature of 400 ° C, especially when Pco / Po 2 = 4, the oxygen lean region. As can be seen from the Ta 2 O 5 content of 5% by weight it was found that the sensitivity of the sensor is excellent.
그리고 제2도는 여러가지 함량의 TiO2소자의 Pco/Po2비에 의존하는 소자 저항값의 변화를 보인 그래프이고, 도면에서 RFg는 1000ppm CO/N2와 O2/N2와의 분압비를 보인것으로, Pco/Po2=0∼4일때 TiO2에 Pt나 Ta2O5를 첨가한 후 900℃에서 1시간 소결한 소자의 동작온도 400℃에서의 저항변화를 대비하여 보면 TiO2+Ta2O5+Pt가 중량비로 94 : 5 : 1일때 감도가 가장 큼을 보이고 있다.FIG. 2 is a graph showing the change of device resistance value depending on the Pco / Po 2 ratio of various contents of TiO 2 device, and R Fg shows the partial pressure ratio between 1000 ppm CO / N 2 and O 2 / N 2. When Pco / Po 2 = 0 to 4, TiO 2 + Ta 2 was added to TiO 2 when Pt or Ta 2 O 5 was added and then the resistance changed at 400 ° C in the operating temperature of the device sintered at 900 ° C for 1 hour. The sensitivity is the greatest when O 5 + Pt is 94: 5: 1 by weight.
또한 제3도는 동작온도 400, 500℃에서 공연비에 의존하는 소자 저항값의 변화를 보인 그래프이고, 도면에 λ는 N2분위기내에서 CO와 O2의 분압비에 의해 표현되는 공연비를 보인 것으로 공연비를 λ=로 정의할 때 TiO2+Ta2O5+Pt가 중량비로 94 : 5 : 1의 비율로 제조된 센서소자의 동작온도 400, 500℃에서의 λ에 따른 저항의 변화는 도시된 바와 같다.3 is a graph showing the change in device resistance value depending on the air-fuel ratio at the operating temperature 400, 500 ℃, λ in the figure shows the air-fuel ratio expressed by the partial pressure ratio of CO and O 2 in the N 2 atmosphere Λ = When defined as a change in the resistance according to λ at the operating temperature of 400, 500 ℃ of the sensor device manufactured TiO 2 + Ta 2 O 5 + Pt in a weight ratio of 94: 5: 1 as shown.
이상에서 설명한 바와 같이 본 발명은 후막 산소센서의 소결온도가 900℃정도로 낮고 간편한 제조방법으로 균일한 막을 얻을 수 있기 때문에 제조 비용을 줄일 수 있으며, 동작온도(400℃∼500℃)와 소결온도의 감소로 Pt, Pd, Rh등의 귀금속 촉매물질의 산화를 다소 억제하여 막의 열화를 방지할 수 있는 이점이 있다.As described above, the present invention can reduce the manufacturing cost because the sintering temperature of the thick film oxygen sensor is as low as 900 ° C. and the uniform film can be obtained by a simple manufacturing method, and the operating temperature (400 ° C. to 500 ° C.) and the sintering temperature By reducing the oxidation of the precious metal catalyst materials such as Pt, Pd, Rh to some extent there is an advantage that can prevent the degradation of the film.
그리고 Ta2O5첨가에 의해 감도를 크게 개선할 수 있다.In addition, the sensitivity can be greatly improved by adding Ta 2 O 5 .
이와 같이 본 발명은 제조가 간단하고 제조원가가 절감되며 감도가 좋기 때문에 자동차나 대형 보일러는 말할 것도 없고 가정용 보일러나 팬히터에 유리하게 적용할 수 있다.As such, the present invention can be advantageously applied to household boilers or fan heaters, not to mention automobiles and large boilers, because the manufacturing is simple, the manufacturing cost is reduced, and the sensitivity is good.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019910020838A KR940006687B1 (en) | 1991-11-21 | 1991-11-21 | Manufacturing method of thick film semiconductor oxygen sensor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019910020838A KR940006687B1 (en) | 1991-11-21 | 1991-11-21 | Manufacturing method of thick film semiconductor oxygen sensor |
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| Publication Number | Publication Date |
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| KR930011276A KR930011276A (en) | 1993-06-24 |
| KR940006687B1 true KR940006687B1 (en) | 1994-07-25 |
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| KR1019910020838A KR940006687B1 (en) | 1991-11-21 | 1991-11-21 | Manufacturing method of thick film semiconductor oxygen sensor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100352483B1 (en) * | 1998-12-30 | 2002-09-11 | 삼성전기주식회사 | Method for fabricating piezoelectric/electrostrictive thick film using seeding layer |
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| KR930011276A (en) | 1993-06-24 |
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