KR20090075036A - Sensing materials of plate type catalytic combustion sensor and its synthesis method for hydrogen detector - Google Patents
Sensing materials of plate type catalytic combustion sensor and its synthesis method for hydrogen detector Download PDFInfo
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- 238000007084 catalytic combustion reaction Methods 0.000 title abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title description 7
- 239000001257 hydrogen Substances 0.000 title description 7
- 229910052739 hydrogen Inorganic materials 0.000 title description 7
- 239000011540 sensing material Substances 0.000 title 1
- 238000001308 synthesis method Methods 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 62
- 239000011230 binding agent Substances 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 20
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 20
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 8
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 8
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 8
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 8
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 7
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims description 54
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 25
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 18
- 239000000567 combustion gas Substances 0.000 claims description 17
- 229910052697 platinum Inorganic materials 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 12
- KJSFDFNERNEFET-UHFFFAOYSA-L O[Pt]Cl Chemical compound O[Pt]Cl KJSFDFNERNEFET-UHFFFAOYSA-L 0.000 claims description 10
- 238000002485 combustion reaction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- NFOHLBHARAZXFQ-UHFFFAOYSA-L platinum(2+);dihydroxide Chemical compound O[Pt]O NFOHLBHARAZXFQ-UHFFFAOYSA-L 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 2
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 210000002615 epidermis Anatomy 0.000 abstract description 2
- 150000004683 dihydrates Chemical class 0.000 abstract 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 2
- 239000010931 gold Substances 0.000 abstract 2
- 229910052737 gold Inorganic materials 0.000 abstract 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 230000009849 deactivation Effects 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 description 9
- 229910006404 SnO 2 Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 101150003085 Pdcl gene Proteins 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002076 thermal analysis method Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000001444 catalytic combustion detection Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000012926 crystallographic analysis Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
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- G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
- G01N27/16—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature caused by burning or catalytic oxidation of surrounding material to be tested, e.g. of gas
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/12—Silica and alumina
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Abstract
Description
본 발명은 수소, 메탄, 프로판 가스 등 가연성의 가스 누설 탐지기에 사용되는 접촉연소식 가스센서를 구성하는데 핵심적으로 사용되는 가스 검지물질 페이스트에 관한 것이다. 본 발명은 또한 가스 검지물질 페이스트로부터 제조된 접촉연소식 가스센서에 관한 것이다.The present invention relates to a gas detection material paste, which is used for the core of the contact combustion gas sensor used in a flammable gas leak detector such as hydrogen, methane, propane gas. The present invention also relates to a contact combustion gas sensor made from a gas detector paste.
접촉연소식 가스검지물질은 알루미나의 작은 분말을 모물질로 하고, 반도체성 금속산화물 분말, 촉매작용의 백금종류에 유무기 바인더가 첨가된 페이스트를 말한다. 이 페이스트는 혼합물질의 선정, 조성 및 구성 비율이 센서의 검지특성에 영향이 크므로 대단히 중요하며, 센서제조공정상에서는 페이스트에 첨가되는 유무기 바인더가 큰 역할을 한다. The catalytic combustion gas detection material refers to a paste in which a small powder of alumina is used as the parent material, and an organic-inorganic binder is added to a semiconducting metal oxide powder and a catalytic platinum type. This paste is very important because the selection, composition and composition ratio of the mixture have a great influence on the detection characteristics of the sensor, and the organic-inorganic binder added to the paste plays a big role in the sensor manufacturing process.
종래의 접촉연소식 가스센서는 알루미나 하나만 사용하여 페이스트를 만들 고, 이를 도포하여 비드의 둥근형 지지체를 먼저 형성하는데 사용하고, 그 위층에 촉매층이 형성하도록 촉매가 들어있는 용액이나 묽은 페이스트에 지지체를 담궈서 열처리로 감지소자를 만든다.Conventional catalytic combustion gas sensors use only one alumina to make a paste, apply it to form a rounded support of beads first, and immerse the support in a solution or thin paste containing catalyst to form a catalyst layer on the upper layer. Heat treatment makes the sensing element.
위의 방법으로 제조된 검지물질은 센서를 대량생산하는데 2차에 걸쳐 작업을 해야 하므로 대량생산이 어렵다. 센서 특성 면에서는 수소검출 반응속도가 1에서 5초정도이라야 실용성이 우수한데, 기존의 센서는 20초 이상으로 느리고, 최저 측정범위가 약 0.1%정도로 감도가 둔하다는 단점을 가지고 있다. 기계적 특성 면에서는 표피층의 박리 가능성이 있고, 촉매열화가 빨리 진행된다.The detection material produced by the above method is difficult to mass-produce because the work must be performed twice in the mass production of the sensor. In terms of sensor characteristics, the hydrogen detection reaction rate is about 1 to 5 seconds, which is excellent in practicality. However, the conventional sensor has a disadvantage of being slower than 20 seconds and having a low sensitivity of about 0.1%. In terms of mechanical properties, there is a possibility of peeling of the skin layer, and the catalyst deterioration proceeds quickly.
본 발명은 센서의 반응속도가 상당히 빠르며, 미량의 피검물질을 감지할 수 있고, 센서 표피증의 박리가 없으며, 촉매열화가 현저하게 개선된 접촉연소식 가스센서를 제공하고자 한다. The present invention is to provide a contact-combustion gas sensor that the reaction rate of the sensor is considerably fast, can detect a small amount of test material, there is no peeling of the sensor epidermis, and the catalyst deterioration is remarkably improved.
상기와 같은 문제점을 해결하기 위한 본 발명의 목적은, 검지물질을 구성하는 분말재료를 알루미나 분말 외에 이산화주석산 분말이나 티타니아와 같은 금속산화물 반도체를 적정량을 첨가하여 완전 절연재료인 알루미나로 된 기존의 가스검지 지지체보다 열전도 특성을 개선하고, 백금 등의 촉매를 처음부터 혼합사용함으로 검지소자의 내외층의 박리현상을 없애며, 검지체의 내부 깊숙한 곳까지 촉매가 골고루 분산하여 작용함으로 감도와 반응속도를 획기적으로 향상을 이룩할 수 있고, 유무기 바인더를 잘 선택하여 사용함으로써 센서 제조작업의 수월성을 향상시키고, 검지체의 기계적 강도를 개선하고, 신뢰성 향상에도 기여한다. 특히 유기 바인더는 검지체 형성 후, 가열연소에 의해 모두 물과 이산화탄소로 날아가므로 내부 깊숙한 곳까지 기공이 생겨서 촉매연소반응 면적을 넓히는데 기여한다.An object of the present invention for solving the above problems is, by adding an appropriate amount of a metal oxide semiconductor such as tin dioxide powder or titania to the powder material constituting the detection material in addition to the alumina powder, the existing gas made of alumina as a completely insulating material It improves the thermal conduction characteristics than the detection support, eliminates the delamination of the inner and outer layers of the detection element by using a catalyst such as platinum from the beginning, and evenly distributes the catalyst evenly deep into the inside of the detection body, thereby dramatically improving sensitivity and reaction speed. It is possible to achieve an improvement, and by selecting and using an organic-inorganic binder well, it improves the ease of manufacturing a sensor, improves the mechanical strength of a detector, and contributes to the improvement of reliability. In particular, since the organic binders are all blown into water and carbon dioxide by heating and burning after the formation of the detector, pores are formed deep inside, contributing to widening the catalytic combustion reaction area.
알루미나 지지체 및 촉매를 하나의 페이스트로 만들므로 센서를 대량생산이 보다 용이하게 하고, 검지체의 표면과 내부 깊숙히 접촉연소가 일어남으로 감도가 10배이상 민감하며, 반응속도가 3초까지로 아주 빠른 장점을 갖는다. 유기 바인더는 페이스트의 점도 조절이 적절하도록 하고, 둥근형 표면체 형성, 내부의 깊은 기공형성에 도움을 준다. 무기 바인더는 검지체의 기계적 강도를 향상시키고, 금속산화물분말은 검지체의 열전도도 개선과 결합제로 작용한다.The paste is made of alumina support and catalyst, which makes the sensor easier to mass-produce, and the combustion occurs deeply in contact with the surface of the detector, which is more than 10 times more sensitive, and the reaction rate is very fast up to 3 seconds. Has an advantage. The organic binder allows proper viscosity control of the paste, and helps to form a rounded surface and form deep pores therein. The inorganic binder improves the mechanical strength of the detector, and the metal oxide powder acts as a binder and improves the thermal conductivity of the detector.
이로써, 수소, 도시가스, 프로판 등의 폭발 위험성이 높은 가스누출을 미량검출가능하며, 신속히 검지하므로 청정에너지 보급확대, 가스연료의 안전사용, 편리성 향상에 기여한다. As a result, traces of high explosion risks such as hydrogen, city gas, and propane can be detected in a small amount, and quickly detected, contributing to the expansion of clean energy supply, safe use of gas fuel, and improvement of convenience.
본 발명은 접촉연소식 가스센서를 제조하기 위한 검지물질 페이스트로서, 감마 알루미나 분말, 금속산화물 분말, 수산화염화백금 촉매, 염화팔라듐 촉매, 무기 바인더 및 유기 바인더를 포함하는 검지물질 페이스트를 제공한다. The present invention provides a detection material paste including a gamma alumina powder, a metal oxide powder, a platinum hydroxide chloride catalyst, a palladium chloride catalyst, an inorganic binder, and an organic binder as a detection material paste for manufacturing a catalytic combustion gas sensor.
본 발명은 상기된 바와 같은 검지물질 페이스트를 사용하여 제조된 접촉연소식 가스센서를 제공한다. The present invention provides a contact combustion gas sensor manufactured using the detection material paste as described above.
본 발명의 접촉연소식 가스센서를 제조하기 위한 검지물질 페이스트는 다음과 같은 물질을 혼합하여 제조한다. The detection material paste for manufacturing the contact combustion gas sensor of the present invention is prepared by mixing the following materials.
1. 백금촉매 용액으로 수산화염화백금(H2PtCl6H2O)과 물의 중량비를 10 : 1로 혼합하여 완전 용해한다.1. As a platinum catalyst solution, dissolve completely by mixing 10: 1 weight ratio of platinum hydroxide (H 2 PtCl 6 H 2 O) and water.
2. 제2의 촉매용액으로 염화팔라듐과 물과 염산의 중량비를 10 : 5 : 1의 무게비로 만든다. 2. With a second catalyst solution, the weight ratio of palladium chloride, water, and hydrochloric acid is 10: 5: 1.
3. 유기 바인더는 먼저 n-부탄올 30ml에 에틸 셀룰로오즈 1g을 넣고 50℃에서 90℃의 열을 가하며 저어주면서 용해시킨다. 이 용액에 폴리비닐알콜 수지를 중량비 1 : 1로 취하여 용액으로 만든다.3. Firstly, 1 g of ethyl cellulose is added to 30 ml of n-butanol, and dissolved by stirring with heat of 50 ° C. to 90 ° C. Polyvinyl alcohol resin is added to this solution in a weight ratio of 1: 1 to make a solution.
4. 무기 바인더는 알루미나 젤 분말과 물을 10 : 3 중량비로 혼합하여 만든다.4. The inorganic binder is made by mixing alumina gel powder and water in a 10: 3 weight ratio.
이상의 복합물질에 감마 알루미나 분말 및 금속산화물 반도체 분말, 즉, 이산화주석이나 티타니아, 인듐산화물, 텅스텐옥사이드 등을 준비한다.A gamma alumina powder and a metal oxide semiconductor powder, that is, tin dioxide, titania, indium oxide, tungsten oxide, and the like are prepared in the above composite material.
이상의 물질을 다음의 무게비로 평량하여 혼합한다. The above materials are weighed and mixed in the following weight ratio.
1) 감마 알루미나 분말(감마 Al2O3) : 10-40 wt.% 1) Gamma Alumina Powder (Gamma Al 2 O 3 ): 10-40 wt.%
2) 금속산화물 분말(SnO2 등): 10-45 wt.% 2) metal oxide powder (SnO 2 etc.): 10-45 wt.%
3) 수산화염화백금 촉매용액(H2PtCl6H2O) : 5-25wt.%3) Platinum Hydroxide Chloride Catalyst Solution (H 2 PtCl 6 H 2 O): 5-25wt.%
4) 염화팔라듐 촉매용액(PdCl2): 10-25wt.% 4) Palladium chloride catalyst solution (PdCl 2 ): 10-25wt.%
5) 무기 바인더 : 5-30 wt.% 5) inorganic binder: 5-30 wt.%
6) 유기 바인더 : 2-15 wt.%6) Organic Binder: 2-15 wt.%
평량을 함에 있어서 전체 합이 100이 되도록 하며, 이 재료를 알루미나 사발에서 넣고 골고루 분쇄 혼합을 30분에서 2시간 반 동안 한다.The basis weight is to add up to 100. Add this material in an alumina bowl and evenly grind and mix for 30 minutes to 2 and a half hours.
이렇게 하여 얻어진 수소검출용 접촉연소식 검지물질은 촉매가 포함되고 적 절한 점도를 갖으며, 큰 표면 장력에 의해 쉽게 구형을 형성한다.The thus-obtained hydrogen-detecting catalytic combustion detection material contains a catalyst, has an appropriate viscosity, and easily forms a sphere by a large surface tension.
이 검지물질 페이스트는 전극과 백금히터가 형성된 알루미나의 소형평판 기판에 도포하고 20℃ - 100℃에서 10분에서 2시간동안 건조하고, 500-1000℃로 10분에서 2시간 열을 가해서 소성과 소결한다.The detection material paste is applied to a small flat plate of alumina on which electrodes and platinum heaters are formed, dried at 20 ° C-100 ° C for 10 minutes to 2 hours, and calcined and sintered by heating at 500-1000 ° C for 10 minutes to 2 hours. do.
본 발명의 검지물질 페이스트를 제조하기 위해서 사용되는 감마 알루미나 분말(감마 Al2O3)은 검지물질 페이스트의 전체 중량을 기준으로 10-40 wt.%의 양으로 함유된다. 감마 알루미나의 양이 상기 범위를 벗어나는 경우에는, 상기 페이스트에 의해서 제조된 가스센서에서 감마 알루미나가 지지체로서의 역할을 적합하게 수행하지 못하여, 가스센서의 감도가 저하된다. 바람직하게는 감마 알루미나 분말은 24.5wt.%의 양으로 검지물질 페이스트에 함유될 수 있다. The gamma alumina powder (gamma Al 2 O 3 ) used to prepare the detector paste of the present invention is contained in an amount of 10-40 wt.% Based on the total weight of the detector paste. When the amount of gamma alumina is out of the above range, gamma alumina does not suitably serve as a support in the gas sensor manufactured by the paste, and the sensitivity of the gas sensor is lowered. Preferably the gamma alumina powder may be contained in the detector paste in an amount of 24.5 wt.%.
본 발명의 검지물질 페이스트를 제조하기 위해서 사용되는 금속산화물 분말(SnO2 등)은 검지물질 페이스트의 전체 중량을 기준으로 10-45 wt.%의 양으로 함유된다. 금속산화물 분말의 양이 10wt.% 미만으로 함유되는 경우에는 상기 페이스트로부터 제조된 사스센서의 감지 속도가 현저하게 저하되고 45wt.%를 초과하는 경우에는 센서가 쉽게 열화되는 경향이 있다. 바람직하게는, 금속산화물 분말은 30.0wt.%의 양으로 점지물질 페이스트에 함유될 수 있다. 한편, 이러한 금속산화물 분말은 이산화주석, 티타니아, 인듐산화물, 텅스텐산화물, 및 이의 혼합물로 이루어진 군으로부터 선택된다. The metal oxide powder (SnO 2, etc.) used to prepare the detector paste of the present invention is contained in an amount of 10-45 wt.% Based on the total weight of the detector paste. When the amount of the metal oxide powder is less than 10 wt.%, The sensing speed of the SARS sensor manufactured from the paste is significantly lowered, and when the amount exceeds 45 wt.%, The sensor tends to be easily degraded. Preferably, the metal oxide powder may be contained in the paste material in an amount of 30.0 wt.%. On the other hand, the metal oxide powder is selected from the group consisting of tin dioxide, titania, indium oxide, tungsten oxide, and mixtures thereof.
본 발명의 검지물질 페이스트를 제조하기 위해서 사용되는 수산화염화백금 촉매용액은 검지물질 페이스트의 전체 중량을 기준으로 5-25wt.%의 양으로 함유되는데, 5wt.% 미만의 양으로 함유되는 경우에는 촉매로서의 역할이 불량하고, 25wt.% 초과의 양에서는 촉매작용의 증가가 미약하다. 상기 수산화염화백금 촉매용액은 바람직하게는 15.0wt.%의 양으로 검지물질 페이스트에 함유될 수 있다. 본 발명에서는 수산화염화백금(H2PtCl6H2O)과 물을 10 : 1의 중량비로 혼합하여 수산화염화백금 용액을 제조하여 본 발명의 검지물질 페이스트를 제조하는데 사용한다. Platinum hydroxide chloride catalyst solution used to prepare the detection material paste of the present invention is contained in an amount of 5-25wt.% Based on the total weight of the detection material paste, if the content is less than 5wt.% Its role is poor, and the increase in catalysis is weak in amounts above 25 wt.%. The platinum hydroxide catalyst solution may be contained in the detection material paste in an amount of preferably 15.0 wt.%. In the present invention, a platinum hydroxide solution is prepared by mixing platinum hydroxide (H 2 PtCl 6 H 2 O) and water in a weight ratio of 10: 1, and used to prepare the detection material paste of the present invention.
본 발명의 검지물질 페이스트를 제조하기 위해서 사용되는 염화팔라듐 촉매(PdCl2) 용액은 검지물질 페이스트의 전체 중량을 기준으로 10-25wt.%의 양으로 함유되는데, 10wt.% 미만의 양으로 함유되는 경우에는 촉매로서의 역할이 불량하고, 25wt.% 초과의 양에서는 촉매작용의 증가가 미약하다. 바람직하게는, 염화팔라듐 촉매 용액은 15.0wt.%의 양으로 검지물질 페이스트에 함유될 수 있다. 본 발명에서는 염화팔라듐 촉매(PdCl2)와 물과 염산을 10: 5 : 1의 중량비로 혼합하여 염화팔라듐 촉매 용액을 제조하여 본 발명의 검지물질 페이스트를 제조하는데 사용한다. The palladium chloride catalyst (PdCl 2 ) solution used to prepare the detector paste of the present invention is contained in an amount of 10-25wt.%, Based on the total weight of the detector paste, in an amount of less than 10wt.%. In the case, the role as a catalyst is poor, and in the amount of more than 25 wt.%, The increase in catalysis is weak. Preferably, the palladium chloride catalyst solution may be contained in the detector paste in an amount of 15.0 wt.%. In the present invention, a palladium chloride catalyst (PdCl 2 ), water and hydrochloric acid are mixed at a weight ratio of 10: 5: 1 to prepare a palladium chloride catalyst solution, which is used to prepare the detection material paste of the present invention.
본 발명의 검지물질 페이스트를 제조하기 위해서 사용되는 무기 바인더는 검지물질 페이스트의 전체 중량을 기준으로 5-30wt.%의 양으로 함유되는데, 5wt.% 미만의 양으로 함유되는 경우에는 검지물질 페이스트로부터 제조된 가스센서의 기계적 강도가 불량하고 30wt.% 초과의 양으로 함유되는 경우에는 가스센서에서 요구되는 기계적 강도 이상의 강도를 유발시킨다. 바람직하게는, 무기 바인더는 10.5wt.% 의 양으로 검지물질 페이스트에 함유될 수 있다. 본 발명의 검지물질 페이스트를 제조하는데 사용되는 무기 바인더는 알루미나 젤과 물을 10 : 3의 중량비로 혼합함으로써 제조될 수 있다. The inorganic binder used to prepare the detector paste of the present invention is contained in an amount of 5-30 wt.% Based on the total weight of the detector paste, and when it is contained in an amount of less than 5 wt.% From the detector paste. If the mechanical strength of the manufactured gas sensor is poor and contained in an amount of more than 30wt.%, It causes the strength beyond the mechanical strength required for the gas sensor. Preferably, the inorganic binder may be contained in the detector paste in an amount of 10.5 wt.%. The inorganic binder used to prepare the detection material paste of the present invention can be prepared by mixing alumina gel and water in a weight ratio of 10: 3.
본 발명의 검지물질 페이스트를 제조하기 위해서 사용되는 유기 바인더는 검지물질 페이스트의 전체 중량을 기준으로 2-15wt.%의 양으로 함유되는데, 2wt.% 미만의 양으로 함유되는 경우에는 검지물질 페이스트로부터 제조된 가스센서의 기공형성이 충분하지 않으며, 15wt.% 초과의 양으로 함유되는 경우에는 가스센서에 너무 많은 기공을 형성시켜서 가스센서의 기계적 강도를 불량하게 한다. 바람직하게는, 유기 바인더는 5.0wt.%의 양으로 검지물질 페이스트에 함유될 수 있다. 본 발명의 검지물질 페이스트를 제조하는데 사용되는 유기 바인더는 부탄올 30ml에 에틸 셀룰로오즈 1g을 넣고 교반하면서 가열한 후에 얻은 용액과 폴리비닐알콜 1:1의 중량비로 혼합함으로써 제조되며, 유기 바인더를 제조하는데 사용되는 성분들의 양은 제조되는 검지물질 페이스트의 점도 및 검지물질로부터 제조되는 가스센서의 기공도에 따라서 적절히 조정될 수 있다. The organic binder used to prepare the detection material paste of the present invention is contained in an amount of 2-15 wt.% Based on the total weight of the detection material paste, and when it is contained in an amount of less than 2wt.% From the detection material paste Pore formation of the manufactured gas sensor is not sufficient, and when it is contained in an amount of more than 15wt.%, Too much pores are formed in the gas sensor, thereby deteriorating the mechanical strength of the gas sensor. Preferably, the organic binder may be contained in the detector paste in an amount of 5.0 wt.%. The organic binder used to prepare the detection material paste of the present invention is prepared by mixing 1 g of ethyl cellulose in 30 ml of butanol and heating with stirring in a weight ratio of polyvinyl alcohol 1: 1 and used to prepare an organic binder. The amount of the components to be prepared may be appropriately adjusted according to the viscosity of the detection material paste to be produced and the porosity of the gas sensor produced from the detection material.
바람직하게는, 본 발명은 접촉연소식 가스센서를 제조하는데 사용하기 위한 검지물질 페이스트로서, 1) 감마 알루미나 분말(감마 Al2O3) 10 내지 40 wt.%, Preferably, the present invention is a detection material paste for use in the manufacture of a contact combustion gas sensor, 1) gamma alumina powder (gamma Al 2 O 3 ) 10 to 40 wt.%,
2) 이산화주석, 티타니아, 인듐산화물, 텅스텐산화물 및 이들이 혼합물로 이루어진 군으로부터 선택금속산화물 분말 10 내지 45 wt.%, 3) 수산화염화백금(H2PtCl6H2O) : 물을 10 : 1의 중량비로 혼합하여 제조한 수산화염화백금 촉매용 액 5 내지 25wt.%, 4) 염화팔라듐(PdCl2) : 물 : 염산을 10 : 5 : 1의 중량비로 혼합하여 제조한 염화팔라듐 촉매용액 10 내지 25wt.%, 5) 알루미나 젤 분말 : 물을 10 : 3의 중량비로 혼합하여 제조한 무기 바인더 5 내지 30 wt.%, 및 6) n-부탄올 30ml에 에틸 셀룰로오즈 1g이 용해된 용액에 폴리비닐알콜 수지를 1:1의 중량비로 용해시켜 제조한 유기 바인더 2 내지 15 wt.%를 포함하는 검지물질 페이스트를 제공한다. 2) tin dioxide, titania, indium oxide, tungsten oxide and metal oxide powder selected from the group consisting of 10 to 45 wt.%, 3) platinum hydroxide chloride (H 2 PtCl 6 H 2 O): water 10: 1 5 to 25 wt.% Of a platinum hydroxide chloride catalyst solution prepared by mixing in a weight ratio of 4, palladium chloride (PdCl 2 ): water:
더욱 바람직하게는, 본 발명은 접촉연소식 가스센서를 제조하는데 사용하기 위한 검지물질 페이스트로서, 1) 감마 알루미나 분말(감마 Al2O3) 24.5wt.%, 2) 이산화주석, 티타니아, 인듐산화물, 텅스텐산화물 및 이들이 혼합물로 이루어진 군으로부터 선택금속산화물 분말 30.0wt.%, 3) 수산화염화백금(H2PtCl6H2O) : 물을 10 : 1의 중량비로 혼합하여 제조한 수산화염화백금 촉매용액 15.0wt.%, 4) 염화팔라듐(PdCl2) : 물 : 염산을 10 : 5 : 1의 중량비로 혼합하여 제조한 염화팔라듐 촉매용액 15.0wt.%, 5) 알루미나 젤 분말 : 물을 10 : 3의 중량비로 혼합하여 제조한 무기 바인더 5 내지 10.5wt.%, 및 6) n-부탄올 30ml에 에틸 셀룰로오즈 1g이 용해된 용액에 폴리비닐알콜 수지를 1:1의 중량비로 용해시켜 제조한 유기 바인더 5.0wt.%를 포함하는 검지물질 페이스트를 제공한다. More preferably, the present invention provides a detection material paste for use in the manufacture of a catalytic combustion gas sensor, comprising: 1) gamma alumina powder (gamma Al 2 O 3 ) 24.5 wt.%, 2) tin dioxide, titania, indium oxide , Metal oxide powder selected from the group consisting of tungsten oxide and mixtures thereof 30.0 wt.%, 3) platinum hydroxide chloride (H 2 PtCl 6 H 2 O): platinum hydroxide catalyst prepared by mixing water in a weight ratio of 10: 1 Solution 15.0 wt.%, 4) palladium chloride (PdCl 2 ): water: hydrochloric acid in a weight ratio of 10: 5: 1 palladium chloride catalyst solution 15.0 wt.%, 5) alumina gel powder: water 10: 5 to 10.5 wt.% Of an inorganic binder prepared by mixing in a weight ratio of 3, and 6) an organic binder prepared by dissolving polyvinyl alcohol resin in a weight ratio of 1: 1 in a solution of 1 g of ethyl cellulose in 30 ml of n-butanol. It provides a detection material paste containing 5.0wt.%.
상기 본 발명의 검지물질 페이스트에 함유되는 금속산화물은 이산화주석이 바람직하다. The metal oxide contained in the detection material paste of the present invention is preferably tin dioxide.
본 발명은 또한 상기 본 발명의 검지물질 페이스트를 접촉연소식 기판이나 백금코일에 도포한 후, 공기 중의 20℃-100℃에서 10분에서 2시간 동안 건조하고, 500-1000℃로 10분에서 2시간 열처리함으로써 소성 및 소결함을 포함하여 접촉연소식 가스센서를 제조하는 방법을 제공한다. The present invention is also applied to the detection material paste of the present invention on a contact combustion substrate or a platinum coil, and then dried in air at 20 ° C.-100 ° C. for 10 minutes to 2 hours, and at 500-1000 ° C. for 10 minutes to 2 hours. It provides a method for producing a contact combustion gas sensor including firing and sintering by time heat treatment.
상기 본 발명의 접촉연소식 가스센서를 제조하는데 사용되는 접촉연소식 기판은 전극과 백금히터가 형성된 알루미나 기판일 수 있다. The contact combustion substrate used to manufacture the contact combustion gas sensor of the present invention may be an alumina substrate having an electrode and a platinum heater.
상기 본 발명의 접촉연소식 가스센서를 제조하는데 있어서, 열처리는 650℃로 30분간 수행되는 것이 바람직하다. In manufacturing the contact combustion gas sensor of the present invention, the heat treatment is preferably performed for 30 minutes at 650 ℃.
본 발명은 또한 상기 본 발명의 방법에 따라서 제조되어, 접촉연소식 기판 또는 백금코일, 및 상기 접촉연소식 기판 또는 백금코일에 본 발명의 검지물질 페이스트가 도포되어 소성 및 소결된 가스 검지물질 부분을 포함하는 접촉연소식 가스센서를 제공한다. The present invention is also prepared according to the method of the present invention, and the gas detecting material portion which is fired and sintered by contact burning substrate or platinum coil, and the detection material paste of the present invention is applied to the contact burning substrate or platinum coil. It provides a contact combustion gas sensor comprising.
이하 본 발명의 바람직한 양태를 구체적으로 실시예로 설명하고 있는데, 이는 본 발명을 예시하고자 하는 것이며, 이로써 본 발명을 제한하고자 하는 것은 아니다. Preferred embodiments of the present invention are described below in detail by way of example, which is intended to illustrate the present invention and is not intended to limit the present invention.
실시예Example 1 One
먼저, 검지물질 페이스트에 함유되는 무기 바인더를 제조하기 위해서 알루미나 젤과 물을 10 : 3비율로 혼합하였다. 이와 같이 제조된 무기 바인더를 10.5 wt.%의 양으로 취하였다. 이어서, 유기 바인더를 제조하기 위해서, 부탄올 30ml(N-butanol)에 에틸 셀룰로오즈 1g을 넣고 60℃의 온도에서 20분간 가하면서 교반시켰다. 얻은 용액을 폴리비닐알콜과 1:1비율로 혼합한 후, 5.0wt.%를 취하였다. First, in order to prepare an inorganic binder contained in the detection material paste, alumina gel and water were mixed at a ratio of 10: 3. The inorganic binder thus prepared was taken in an amount of 10.5 wt.%. Subsequently, to prepare an organic binder, 1 g of ethyl cellulose was added to 30 ml (N-butanol) of butanol and stirred for 20 minutes at a temperature of 60 ° C. The obtained solution was mixed with polyvinyl alcohol in a 1: 1 ratio, and 5.0 wt.% Was taken.
상기된 바와 같이 제조한 무기 바인더와 유기 바인더를 그 외 성분과 함께 하기된 바와 같은 중량비로 혼합하여 검지물질 페이스트를 제조하였다. The inorganic binder and the organic binder prepared as described above were mixed with the other components in a weight ratio as described below to prepare a detection material paste.
1) 감마 알루미나 분말 : 24.5 wt.%1) Gamma Alumina Powder: 24.5 wt.%
2) 금속산화물 분말(SnO2) : 30.0 wt.% 2) Metal Oxide Powder (SnO 2 ): 30.0 wt.%
3) 수산화염화백금(H2PtCl6H2O)용액 : 15.0wt.% 3) Platinum hydroxide chloride (H 2 PtCl 6 H 2 O) solution: 15.0 wt.%
4) 염화팔라듐 (PdCl2)용액 : 15.0wt.% 4) Palladium chloride (PdCl 2 ) solution: 15.0wt.%
5) 무기바인더 : 10.5 wt.% 5) Inorganic Binder: 10.5 wt.%
6) 유기바인더 : 5.0%6) Organic Binder: 5.0%
상기된 양으로 혼합된 검지물질 페이스트의 전체 합은 100중량%가 되도록 했으며, 이 재료를 알루미나 사발에서 넣고 골고루 분쇄 혼합을 1시간 30 동안 수행하였다. The total sum of the detection agent pastes mixed in the amounts described above was 100% by weight, and the material was placed in an alumina bowl and evenly ground for 1
상기 제조된 검지물질 페이스트를 전극과 백금히터가 형성된 알루미나의 소형평판 기판에 도포하고, 80℃에서 30분 동안 건조하고, 650℃로 30분간 열처리함으로써 가스센서를 제조하였다. The gas detector was prepared by applying the prepared detection material paste to a small flat plate of alumina on which electrodes and platinum heaters were formed, dried at 80 ° C. for 30 minutes, and heat-treated at 650 ° C. for 30 minutes.
이와 같이 제조된 가스센서의 검지물질 표면의 전자 현미경 사진을 도 1에 나타냈다. 또한, 상기 제조된 가스센서의 검지물질 부분의 XRD 분석 결과를 도 2에 나타내고 있으며, 이러한 XRD 분석으로부터 각 피크의 높이가 높고 폭이 좁게 나타남으로 결정화도가 우수함을 알 수 있다. 상기 실시예 1에서 제조된 검지물질 페이스트의 열분석법에 의한 무게 감량 및 상변화도를 도 3에 나타내고 있다. 이 열분 석특성곡선으로부터 약160℃까지는 흡열반응으로 수분의 증발이 하여 중량감소가 5%가량 발생하며, 그 다음은 약 450℃까지 발열반응으로 약 6%정도의 유기바인더 등이 날아가는 과정이고, 더 이상의 온도에서는 약간의 잔류물이 제거되며 2%정도의 무게감소를 보인다.An electron micrograph of the surface of the detection material of the gas sensor thus manufactured is shown in FIG. 1. In addition, the XRD analysis results of the detection material portion of the gas sensor manufactured as shown in Figure 2, it can be seen that the crystallinity is excellent because the height of each peak is narrow and the width is shown from the XRD analysis. Figure 3 shows the weight loss and phase change by the thermal analysis method of the detection material paste prepared in Example 1. From this thermal analysis characteristic curve, up to about 160 ℃, the endothermic reaction causes evaporation of water, resulting in a weight loss of about 5%, followed by an exothermic reaction up to about 450 ℃, about 6% of organic binder, etc. At further temperatures, some residue is removed and the weight is reduced by 2%.
상기 제조된 가스센서의 수소에 대한 감도 특성을 도 5에 그래프로 나타내고 있다이 그림에서 보듯이 센서의 감도특성이 약 100ppm에서 4%까지 우수한 감도와 직진성을 나타낸다.The sensitivity characteristic of hydrogen of the manufactured gas sensor is shown graphically in FIG. 5. As shown in this figure, the sensitivity characteristic of the sensor shows excellent sensitivity and straightness up to about 4% at about 100 ppm.
실시예Example 2 2
실시예 1에서 제조된 무기 바인더와 유기 바인더 및 그 외 물질을 하기 중량비로 혼합하여 검지물질 페이스트를 제조하였다. The inorganic binder, the organic binder, and other materials prepared in Example 1 were mixed in the following weight ratio to prepare a detection material paste.
1) 감마 알루미나 분말 : 24.5 wt.%1) Gamma Alumina Powder: 24.5 wt.%
2) 금속산화물 분말(SnO2) : 37.0 wt.% 2) Metal Oxide Powder (SnO 2 ): 37.0 wt.%
3) 수산화염화백금(H2PtCl6H2O)용액 : 7.0wt.% 3) Platinum hydroxide (H 2 PtCl 6 H 2 O) solution: 7.0wt.%
4) 염화팔라듐 (PdCl2)용액 : 12.0wt.% 4) Palladium chloride (PdCl 2 ) solution: 12.0wt.%
5) 무기바인더 : 7.5 wt.% 5) Inorganic Binder: 7.5 wt.%
6) 유기바인더 : 12.0%6) Organic Binder: 12.0%
상기된 양으로 혼합된 검지물질 페이스트의 전체 합은 100중량%가 되도록 했으며, 이 재료를 알루미나 사발에서 넣고 골고루 분쇄 혼합을 1시간 30 동안 수행하였다. The total sum of the detection agent pastes mixed in the amounts described above was 100% by weight, and the material was placed in an alumina bowl and evenly ground for 1
상기 제조된 검지물질 페이스트를 전극과 백금히터가 형성된 알루미나의 소형평판 기판에 도포하고, 80℃에서 30분 동안 건조하고, 650℃로 30분간 열처리함으로써 가스센서를 제조하였다.The gas detector was prepared by applying the prepared detection material paste to a small flat plate of alumina on which electrodes and platinum heaters were formed, dried at 80 ° C. for 30 minutes, and heat-treated at 650 ° C. for 30 minutes.
상기 제조된 가스센서의 실시예 1에서와 같은 수소에 대한 감도 측정 결과는 도 5에서 나타내고 있는 바와 유사하게 우수한 결과를 나타냈다. Sensitivity measurement results for hydrogen as in Example 1 of the manufactured gas sensor showed excellent results similar to those shown in FIG. 5.
실시예Example 3 3
실시예 1에서 제조된 무기 바인더와 유기 바인더 및 그 외 물질을 하기 중량비로 혼합하여 검지물질 페이스트를 제조하였다. The inorganic binder, the organic binder, and other materials prepared in Example 1 were mixed in the following weight ratio to prepare a detection material paste.
1) 감마 알루미나 분말 : 24.5 wt.%1) Gamma Alumina Powder: 24.5 wt.%
2) 금속산화물 분말(SnO2) : 20.0 wt.% 2) Metal Oxide Powder (SnO 2 ): 20.0 wt.%
3) 수산화염화백금(H2PtCl6H2O)용액 : 20.0wt.% 3) Platinum hydroxide chloride (H 2 PtCl 6 H 2 O) solution: 20.0wt.%
4) 염화팔라듐 (PdCl2)용액 : 12.0wt.% 4) Palladium chloride (PdCl 2 ) solution: 12.0wt.%
5) 무기바인더 : 15.5 wt.% 5) Inorganic Binder: 15.5 wt.%
6) 유기바인더 : 8.0%6) Organic Binder: 8.0%
상기된 양으로 혼합된 검지물질 페이스트의 전체 합은 100중량%가 되도록 했으며, 이 재료를 알루미나 사발에서 넣고 골고루 분쇄 혼합을 1시간 30 동안 수행하였다. The total sum of the detection agent pastes mixed in the amounts described above was 100% by weight, and the material was placed in an alumina bowl and evenly ground for 1
상기 제조된 검지물질 페이스트를 전극과 백금히터가 형성된 알루미나의 소형평판 기판에 도포하고, 80℃에서 30분 동안 건조하고, 650℃로 30분간 열처리함 으로써 가스센서를 제조하였다. The gas detector was prepared by applying the prepared detection material paste to a small flat substrate of alumina on which electrodes and platinum heaters were formed, dried at 80 ° C. for 30 minutes, and heat-treated at 650 ° C. for 30 minutes.
상기 제조된 가스센서의 실시예 1에서와 같은 수소에 대한 감도 측정 결과는 도 5에서 나타내고 있는 바와 유사하게 우수한 결과를 나타냈다.Sensitivity measurement results for hydrogen as in Example 1 of the manufactured gas sensor showed excellent results similar to those shown in FIG. 5.
도 1은 본 발명의 검지물질 전자현미경 사진이다.1 is an electron micrograph of the detection material of the present invention.
도 2는 본 발명의 X-선 회절법에 의한 검지물질 결정화도 분석 자료그림이다. Figure 2 is a crystallographic analysis data of the detection material by the X-ray diffraction method of the present invention.
도 3은 본 발명의 열분석법에 의한 무게감량 및 상변화도 분석 자료그림이다.Figure 3 is a weight loss and phase change analysis data by the thermal analysis method of the present invention.
도 4는 본 발명으로 제작된 접촉연소식 평판형 기판에 양면으로 둥글게 검지물질이 도포된 접촉연소식 수소가스센서의 사진이다.4 is a photograph of a contact combustion type hydrogen gas sensor coated with a detection material rounded on both sides on a contact combustion type plate type substrate manufactured according to the present invention.
도 5는 본 발명으로 제작된 평판형 접촉연소식 수소가스센서의 감도 특성 그래프이다.5 is a sensitivity characteristic graph of the plate-type contact combustion hydrogen gas sensor manufactured by the present invention.
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| KR20150089291A (en) * | 2014-01-27 | 2015-08-05 | 울산대학교 산학협력단 | Hydrogen sensor based on nickel/palladium-graphene nanocomposite and method of fabricating the same |
| US11415537B2 (en) * | 2017-06-01 | 2022-08-16 | Robert Bosch Gmbh | MEMS gas sensor having a media-sensitive material |
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| KR100810120B1 (en) | 2006-11-28 | 2008-03-06 | 한국에너지기술연구원 | Catalytic combustion type flammable gas sensor using uv led and uv-catalyst |
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| KR20150089291A (en) * | 2014-01-27 | 2015-08-05 | 울산대학교 산학협력단 | Hydrogen sensor based on nickel/palladium-graphene nanocomposite and method of fabricating the same |
| US11415537B2 (en) * | 2017-06-01 | 2022-08-16 | Robert Bosch Gmbh | MEMS gas sensor having a media-sensitive material |
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