KR20230094239A - Composition for hydrogen sensing tape, tape and manufacturing method thereof - Google Patents
Composition for hydrogen sensing tape, tape and manufacturing method thereof Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 title description 13
- 239000001257 hydrogen Substances 0.000 title description 12
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 36
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 26
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 26
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 26
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 239000010457 zeolite Substances 0.000 claims description 23
- 229910021536 Zeolite Inorganic materials 0.000 claims description 22
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 22
- 238000002845 discoloration Methods 0.000 claims description 19
- -1 Polydimethylsiloxane Polymers 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 239000000945 filler Substances 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
- 238000002156 mixing Methods 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000004678 hydrides Chemical class 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 239000002318 adhesion promoter Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 229910052681 coesite Inorganic materials 0.000 claims 1
- 229910052906 cristobalite Inorganic materials 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 abstract description 15
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 abstract description 13
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 19
- 229910003445 palladium oxide Inorganic materials 0.000 description 12
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 description 12
- 238000001514 detection method Methods 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 239000004971 Cross linker Substances 0.000 description 3
- 101150003085 Pdcl gene Proteins 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C08G77/04—Polysiloxanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
Description
본 발명은 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법에 관한 것으로,The present invention relates to a silicone tape composition for detecting hydrogen gas, a silicone tape for detecting hydrogen gas, and a method for manufacturing the same,
보다 상세하게는 단순하게 접착 또는 점착성 테이프 형태로 제조될 수 있어 현장적용성이 뛰어나고, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법에 관한 것이다.More specifically, a silicone tape composition for detecting hydrogen gas, which can be simply manufactured in the form of an adhesive or adhesive tape, is excellent in field applicability, and has excellent tensile strength and color change visibility, the hydrogen gas sensing silicon tape, and a method for manufacturing the same will be.
수소 연료 전지 에너지원이나 수소차, 다양한 산업분야에서 사용되는 수소가스를 감지하는 수소센서와 관련하여 특허등록 제10-1015088호(2011년02월09일) [초 고감도 수소 센서에 사용되는 환원된 ＰｄＯ 박막과 그것을 제조하기 위한 방법]이 있는데,Patent registration No. 10-1015088 (February 9, 2011) related to a hydrogen sensor that detects hydrogen gas used in hydrogen fuel cell energy sources, hydrogen vehicles, and various industries There is a PDO thin film and a method for manufacturing it],
이 등록특허는 리액티브 스퍼터링 기법(reactive DC magnetron sputtering system)을 이용하여 인위적으로 PdO 박막을 제작하는 단계와, 상기 PdO 박막을 환원반응시켜 나노크랙이 형성된 Pd 박막을 얻는 단계를 포함하며, This registered patent includes the steps of artificially producing a PdO thin film using a reactive DC magnetron sputtering system, and obtaining a Pd thin film with nanocracks by reducing the PdO thin film,
상기 나노크랙이 형성된 Pd 박막은 수소검지특성이 향상되어 수소검지 센서에 사용되기 적합한 기술을 제시하고 있다.The Pd thin film in which the nanocrack is formed has improved hydrogen detection characteristics, suggesting a technology suitable for use in a hydrogen detection sensor.
또 특허등록 제10-1269510호(2013년05월24일) [수소 농도 측정이 가능한 수소 감지 센서]가 있는데,In addition, there is a patent registration No. 10-1269510 (May 24, 2013) [Hydrogen detection sensor capable of measuring hydrogen concentration],
이 등록특허는 수소 가스의 농도 변화에 상응하여 저항값이 변함으로써 연속적으로 수소 가스의 농도 변화를 측정할 수 있는 수소 감지 센서에 관한 것으로 This registered patent relates to a hydrogen detection sensor that can continuously measure the change in concentration of hydrogen gas by changing the resistance value corresponding to the change in concentration of hydrogen gas.
구체적으로 수소 가스와 접촉시 수소화되는 수소 감지부를 포함하되, 상기 수소 감지부가 수소화될 때, 상기 수소 감지부의 저항값이 변하고, 수소 가스의 제1농도에서 제1 저항값 변화율를 갖고, 상기 제1 농도와 다른 수소 가스의 제2 농도에서 상기 제1 저항값 변화율과 다른 제2 저항값 변화율을 갖는 것을 특징으로 한다.Specifically, it includes a hydrogen sensing unit that is hydrogenated when in contact with hydrogen gas, when the hydrogen sensing unit is hydrogenated, the resistance value of the hydrogen sensing unit changes, has a first resistance value change rate at a first concentration of hydrogen gas, and the first concentration It is characterized in that it has a second resistance value change rate different from the first resistance value change rate at a second concentration of hydrogen gas different from .
그러나 이 두 특허를 비롯한 종래문헌은 즉자적인 현장적용성 부분이나 색변화 시인성을 향상하여 이상 상태를 즉각적으로 감지할 수 있도록 하는 기술과는 무관하다.However, the prior literature including these two patents has nothing to do with the immediate field applicability or the technology for immediately detecting an abnormal state by improving color change visibility.
이에 본 발명은 단순하게 접착 또는 점착성 테이프 형태로 제조될 수 있어 현장적용성이 뛰어나고, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법을 제공하는 것을 목적으로 한다.Therefore, the present invention provides a silicone tape composition for detecting hydrogen gas, which can be simply manufactured in the form of an adhesive or adhesive tape, which is excellent in field applicability and has excellent tensile strength and color change visibility, the hydrogen gas sensing silicon tape, and a manufacturing method thereof. aims to do
상기와 같은 목적을 달성하기 위하여 본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물은 In order to achieve the above object, the silicone tape composition for detecting hydrogen gas according to the present invention
수소가스 감지제와, PDMS와, 백금촉매를 포함하여 이루어진다.It consists of a hydrogen gas sensing agent, PDMS, and a platinum catalyst.
또 본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물에서In addition, in the silicone tape composition for detecting hydrogen gas according to the present invention
상기 수소가스 감지제 30 중량부에 대하여 PDMS 600~1200 중량부 및 백금촉매 0.5~3 중량부로 구성되고,It consists of 600 to 1200 parts by weight of PDMS and 0.5 to 3 parts by weight of a platinum catalyst based on 30 parts by weight of the hydrogen gas sensing agent,
테이프의 변색 시인성 향상제가 더 첨가되며,A discoloration visibility improver of the tape is further added,
상기 변색 시인성 향상제는 알루미나이고,The discoloration visibility improver is alumina,
경화지연제가 더 첨가되고,A curing retardant is further added,
상기 경화지연제는 메틸비닐시클로실록산(MVC)인 것을 특징으로 한다.The curing retardant is characterized in that methylvinylcyclosiloxane (MVC).
나아가 본 발명에 따른 수소가스 감지 실리콘 테이프 및 그 제조방법은 상기 조성물을 이용하여 이루어진다.Furthermore, the hydrogen gas sensing silicone tape and method for manufacturing the same according to the present invention are made using the above composition.
본 발명은 현장적용성이 뛰어난 테이프 형태이면서도, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법을 제공할 수 있다.The present invention can provide a silicone tape composition for detecting hydrogen gas, a silicone tape for detecting hydrogen gas, and a method for manufacturing the same, which are in the form of a tape having excellent field applicability and also have excellent tensile strength and color change visibility.
도 1은 본 발명에 따른 수소가스 감지 실리콘 테이프의 수소가스 노출 전후 비교사진.1 is a comparative photograph of a hydrogen gas sensing silicon tape before and after exposure to hydrogen gas according to the present invention.
이하 본 발명을 상세히 설명하도록 한다. Hereinafter, the present invention will be described in detail.
본 발명은 다양한 변경을 가할 수 있고 여러 가지 형태를 가질 수 있는 바, 구현예(態樣, aspect)(또는 실시예)들을 본문에 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 개시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. Since the present invention can have various changes and various forms, the implementation examples (or embodiments) will be described in detail in the text. However, this is not intended to limit the present invention to a specific form disclosed, and should be understood to include all modifications, equivalents, or substitutes included in the spirit and scope of the present invention.
본 명세서에서 사용한 용어는 단지 특정한 구현예(태양, 態樣, aspect)(또는 실시예)를 설명하기 위해 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다. 본 출원에서, ~포함하다~ 또는 ~이루어진다~ 등의 용어는 명세서 상에 기재된 특징, 숫자, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.Terms used in this specification are only used to describe a specific embodiment (aspect, aspect, aspect) (or embodiment), and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, terms such as ~comprising~ or ~consisting of are intended to designate that there is a feature, number, step, operation, component, part, or combination thereof described in the specification, but one or more other features It should be understood that it does not preclude the possibility of the presence or addition of numbers, steps, operations, components, parts, or combinations thereof.
다르게 정의되지 않는 한, 기술적이거나 과학적인 용어를 포함해서 여기서 사용되는 모든 용어들은 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에 의해 일반적으로 이해되는 것과 동일한 의미를 가지고 있다. 일반적으로 사용되는 사전에 정의되어 있는 것과 같은 용어들은 관련 기술의 문맥 상 가지는 의미와 일치하는 의미를 가지는 것으로 해석되어야 하며, 본 출원에서 명백하게 정의하지 않는 한, 이상적이거나 과도하게 형식적인 의미로 해석되지 않는다.Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs. Terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the related art, and unless explicitly defined in the present application, they should not be interpreted in an ideal or excessively formal meaning. don't
본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법은 기본 조성물로 The silicone tape composition for detecting hydrogen gas according to the present invention, the silicone tape for detecting hydrogen gas, and the manufacturing method thereof include a basic composition
수소가스 감지제와, PDMS와, 백금촉매를 포함하여 이루어진다.It consists of a hydrogen gas sensing agent, PDMS, and a platinum catalyst.
구체적으로 수소가스 감지제 30 중량부에 대하여 PDMS 600~1200 중량부 및 백금촉매 0.5~3 중량부로 구성되는 것이 바람직하다.Specifically, it is preferably composed of 600 to 1200 parts by weight of PDMS and 0.5 to 3 parts by weight of a platinum catalyst based on 30 parts by weight of the hydrogen gas sensing agent.
또 테이프의 변색 시인성 향상제가 더 첨가되는 것이 바람직한데,In addition, it is preferable that a discoloration visibility improver of the tape is further added.
이 변색 시인성 향상제는 알루미나인 것이 바람직하며, 이 경우 알루미나는 테이프의 인장강도 향상에도 일조한다.It is preferable that the discoloration visibility improving agent is alumina, and in this case, alumina also contributes to improving the tensile strength of the tape.
아울러 본 발명은 경화지연제가 더 첨가되는 것을 좋고, 이 경화지연제는 메틸비닐시클로실록산(MVC)일 수 있다.In addition, in the present invention, it is preferable that a curing retardant is further added, and the curing retardant may be methylvinylcyclosiloxane (MVC).
기초적으로 수소가스 감지제는 PdO(Palladium Oxide)를 사용하는 것이 바람직하다.Basically, it is preferable to use PdO (Palladium Oxide) as the hydrogen gas sensing agent.
또 수소가스 감지제는 조작 용이성, 물질 안정성, 보존성 등을 고려하여 담체에 수용된 것이 바람직하며, 그 담체의 예로는 제올라이트(Zeolite), TiO2, SiO2, ZnO, Al2O3 등의 다공성 물질(이 중 하나, 일부 또는 모두일 수 있다)을 활용할 수 있고, 이중 제올라이트가 적합하다.In addition, the hydrogen gas sensing agent is preferably accommodated in a carrier in consideration of ease of operation, material stability, preservation, etc. Examples of the carrier are porous materials such as zeolite, TiO 2 , SiO 2 , ZnO, Al 2 O 3 (which may be one, some or all of these) may be utilized, and dual zeolites are suitable.
즉, PdCl2를 담체인 제올라이트에 혼합하여 담지한다.That is, PdCl 2 is mixed and supported on zeolite as a carrier.
나아가 수소가스 감지 원리는 아래와 같으며, 본 발명에 따른 테이프를 이용한 수소가스 감지 전후의 변색은 도 1의 비교 사진에서 확인할 수 있다.Furthermore, the principle of detecting hydrogen gas is as follows, and discoloration before and after detecting hydrogen gas using the tape according to the present invention can be confirmed in the comparative photograph of FIG.
PdO (Brown) + H2 → Pd (Gray)+ H2OPdO (Brown) + H 2 → Pd (Gray) + H 2 O
[조성물의 성분에 대한 설명][Description of the components of the composition]
본 발명에 따른 수소가스 감지 실리콘 테이프는 특히 다양한 분야에 안정적으로 적용되도록 실리콘 테이프를 채용하는 것이 바람직하며, 실리콘 테이프는 비닐(Vinyl)기, 수소(H)기, 수산(OH)기가 부여된 실리콘을 사용하여 기능성 향상을 도모하였다. 또 실리콘의 경화반응은 부가반응형으로 백금(Pt)촉매를 채용하는 것이 바람직하다.The hydrogen gas sensing silicone tape according to the present invention is particularly preferably employed so that it can be stably applied to various fields. was used to improve functionality. In addition, it is preferable to employ a platinum (Pt) catalyst in an addition reaction type for the curing reaction of silicon.
○ 말단 비닐기를 갖는 폴리디메틸실록산(Vinyl terminated Polydimethylsiloxane(이하 'PDMS'로 함)○ Polydimethylsiloxane having a terminal vinyl group (Vinyl terminated Polydimethylsiloxane (hereinafter referred to as 'PDMS')
실리콘의 기재(Back-bone) 역할을 한다.It serves as the back-bone of silicon.
○ 말단 수소기를 갖는 PDMS(Hydride terminated PDMS)○ PDMS (Hydride terminated PDMS) with terminal hydrogen groups
가교제 (Cross-linker) 역할을 한다.It acts as a cross-linker.
○ 말단 수산기를 갖는 PDMS(Hydroxyl terminated PDMS)○ PDMS having terminal hydroxyl groups (Hydroxyl terminated PDMS)
수산기 특유의 점착 특성을 부여한다(부가경화에 참여하지 않는 -OH를 부여하여 피착물에 대한 점착력을 확보할 수 있다).Gives unique adhesive properties to hydroxyl groups (adhesion to adherends can be secured by adding -OH, which does not participate in additional curing).
○ Pt 촉매○ Pt catalyst
실리콘의 경화반응을 유도한다.Induces the curing reaction of silicone.
<Silicone 반응 예> <Silicone reaction example>
Hydride terminated PDMS + Vinyl terminated PDMS (Pt 촉매 사용) Hydride terminated PDMS + Vinyl terminated PDMS (Pt catalyst used)
{Source: Gelest社 카탈로그}{Source: Gelest catalog}
아울러 수소가스 감지를 위한 필러는 다음과 같다.In addition, the filler for detecting hydrogen gas is as follows.
○ PdO/담체○ PdO/carrier
PdO는 수소가스와 반응하여 변색 특성을 나타내며, 제올라이트, TiO2, SiO2, ZnO, Al2O3는 PdO의 담체 역할을 하며, 제올라이트가 적합하다.PdO reacts with hydrogen gas to exhibit discoloration, and zeolite, TiO 2 , SiO 2 , ZnO, and Al 2 O 3 serve as a carrier for PdO, and zeolite is suitable.
○ 알루미나(Al22O3)○ Alumina (Al 2 2O 3 )
PdO의 색변화의 시인성(색 대비 효과)을 극대화하며(즉, 변색 시인성 향상제로 기능한다) 아울러 테이프의 인장강도 증가에도 일조한다.It maximizes the visibility (color contrast effect) of the color change of PdO (that is, functions as a color change visibility improver) and also contributes to the increase in the tensile strength of the tape.
○ 경화지연제(inhibitor)○ Curing retardant (inhibitor)
경화지연제인 Inhibitor MVC(메틸비닐시클로실록산)를 사용한다.Inhibitor MVC (methylvinylcyclosiloxane), a curing retardant, is used.
이하 본 발명은 구체 실시예 및 비교예를 통하여 더 잘 이해될 수 있다.Hereinafter, the present invention can be better understood through specific examples and comparative examples.
[실시예 및 비교예][Examples and Comparative Examples]
adhesion promoter MS-
adhesion promoter
adhesion promoter MS-
adhesion promoter
*VTP = Vinyl Terminated Polydimethylsiloxane* VTP = Vinyl Terminated Polydimethylsiloxane
*hTPS = Hydride Terminated Polydimethylsiloxane* hTPS = Hydride Terminated Polydimethylsiloxane
*HTPS = Hydroxyl Terminated Polydimethylsiloxane* HTPS = Hydroxyl Terminated Polydimethylsiloxane
*MS = Methacylate Silane* MS = Methacylate Silane
[제조예 : 수소가스 감지 실리콘 테이프를 제조하기 위한 전체 조성물 제조][Manufacturing Example: Preparation of entire composition for manufacturing hydrogen gas sensing silicone tape]
○ 수소가스 감지제 제조○ Manufacture of hydrogen gas detection agent
1. Substrate(담체)(제올라이트(Zeolite), TiO2, SiO2 또는 ZnO)와 함께 PdCl2 및 물(H2O)을 혼합하여 제조한다.1. It is prepared by mixing PdCl 2 and water (H 2 O) with a substrate (Zeolite, TiO 2, SiO 2 or ZnO).
PdCl2는 담체 대비 2~4 phr로 투입한다. PdCl 2 is added at 2 to 4 phr compared to the carrier.
2. 10분간 교반하며, 반응온도는 상온(RT)~60 ℃이다.2. Stir for 10 minutes, and the reaction temperature is room temperature (RT) ~ 60 ℃.
3. pH Control; 묽은염산을 이용하여 용액의 pH를 7로 조절한다.3. pH Control; Adjust the pH of the solution to 7 using dilute hydrochloric acid.
4. 60분간 교반하며, 반응온도는 상온~60 ℃이다.4. Stir for 60 minutes, the reaction temperature is room temperature ~ 60 ℃.
5. 필터를 이용하여 가압 필터링 한다.(0.2 ㎛ Membrane filter with washing).5. Filter under pressure using a filter (0.2 ㎛ Membrane filter with washing).
6. 12시간 동안 건조하여(건조온도: 120 ℃) PdO/담체 분말 수득한다.6. Drying for 12 hours (drying temperature: 120° C.) to obtain PdO/carrier powder.
○ 원료 배합비 ○ Raw material mixing ratio
수소가스 감지제인 PdO/Zeolite 100 중량부를 기준으로Based on 100 parts by weight of PdO/Zeolite, a hydrogen gas detecting agent
각 실시예 및 비교예의 나머지 조성물을 2,000~4,000 중량부, 바람직하기로는 2,500~3,800 중량부, 보다 바람직하기로는 2,800~3,500 배합한다.2,000 to 4,000 parts by weight, preferably 2,500 to 3,800 parts by weight, more preferably 2,800 to 3,500 parts by weight of the remaining compositions of each Example and Comparative Example are blended.
또 상기 말단 비닐기를 갖는 PDMS(VTP)는 서로 다른 점도를 갖는 것을 혼합하여 사용하여 수소가스 감지제(Detector)인 PdO/담체에 대한 분산 특성을 확보하는 데 일조할 수 있다. 예를 들어 1000 cps 점도의 VTP 100 중량부에 대하여 20000 cps 점도의 VTP 90~120 중량부, 65000 cps 점도의 VTP 40~60 중량부를 혼합하여 사용하는 것이 적합하다.In addition, PDMS (VTP) having a terminal vinyl group may help to secure dispersion characteristics for PdO/carrier, which is a hydrogen gas detector, by mixing and using those having different viscosities. For example, it is appropriate to mix and use 90 to 120 parts by weight of VTP of 20000 cps viscosity and 40 to 60 parts by weight of VTP of 65000 cps viscosity to 100 parts by weight of VTP of 1000 cps viscosity.
○ 혼합(Planetary Mixing)○ Planetary Mixing
실시예 및 비교예별 조성물을 믹서(Planetary Mixer) 장비를 이용하여 혼합하는데,The compositions of Examples and Comparative Examples are mixed using a planetary mixer equipment,
공전 블레이드 기준 60 rpm으로 설정(자전 블레이드 120 rpm)하여 10분간 혼합한다.Set to 60 rpm based on the revolving blade (rotating blade 120 rpm) and mix for 10 minutes.
○ 밀링(Three Roll Milling)○ Milling (Three Roll Milling)
상기 혼합된 조성물내 존재하는 입자(필러)들을 분쇄/분산하는 공정으로,In the process of grinding / dispersing the particles (fillers) present in the mixed composition,
실리콘 레진이 투입되는 롤의 갭을 20 ㎛, 토출되는 롤의 갭을 5 ㎛로 하여 밀링한다.Milling is performed by setting the gap of the roll into which the silicone resin is injected to 20 μm and the gap of the roll through which the silicone resin is ejected to 5 μm.
○ 후공정; 필름화하여 수소가스 변색 관찰 ○ post-process; Observation of hydrogen gas discoloration by filming
PET 기재에 300 ㎛ 습도막 두께로 코팅하여 120 ℃에서 10분간 경화하고, 경화된 필름은 수소가스에 노출하여 변색을 관찰한다.The PET substrate was coated with a wet film thickness of 300 μm, cured at 120° C. for 10 minutes, and the cured film was exposed to hydrogen gas to observe discoloration.
[실험예-변색 측정][Experimental Example - Measurement of Discoloration]
경화된 필름은 수소가스에 노출하여 변색을 관찰한다.The cured film is exposed to hydrogen gas to observe discoloration.
수소가스 노출 조건으로 4 % H2 가스에 1 mL/min의 유량으로 5분간 노출시켰다.(노출 전후 변색은 도 1 참조)As a hydrogen gas exposure condition, it was exposed to 4% H 2 gas at a flow rate of 1 mL/min for 5 minutes. (See Figure 1 for discoloration before and after exposure.)
본 발명의 실시예와 같이 수소가스 감지를 위한 필러로 알루미나(Al 2 O 3 )를 사용한 것이 아니라, 비교예와 같이 SiO 2 를 사용한 경우에는 아래 비교 사진에서 확인할 수 있는 바와 같이, 실시예(알루미나(Al 2 O 3 ))가 더 시인성이 더 뛰어남을 확인할 수 있다.As can be seen in the comparative photos below, when alumina (Al 2 O 3 ) is not used as a filler for detecting hydrogen gas as in the example of the present invention, but SiO 2 is used as in the comparative example, the example (alumina It can be seen that (Al 2 O 3 )) has better visibility.
[실시예들의 변색 사진][Photographs of discoloration of Examples]
{좌측-브라운(변색 전), 우측-그레이(변색 후)}{Left-brown (before discoloration), right-grey (after discoloration)}
[비교예 4의 변색 사진][Photograph of discoloration of Comparative Example 4]
{좌측-라이트 브라운 또는 아이보리(변색 전), 우측-라이트 그레이 (변색 후)}{Left-light brown or ivory (before discoloration), right-light gray (after discoloration)}
[실험예-인장강도 측정][Experimental Example-Tensile strength measurement]
이상의 설명에서 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법과 관련한 통상의 공지된 기술은 생략되어 있으나, 당업자라면 용이하게 이를 추측 및 추론하고 재현할 수 있다.In the above description, the commonly known technology related to the silicone tape composition for detecting hydrogen gas, the silicon tape for detecting hydrogen gas, and the manufacturing method thereof is omitted, but those skilled in the art can easily guess, infer, and reproduce them.
Claims (14)
상기 PDMS는 VTP(Vinyl Terminated Polydimethylsiloxane)와 함께
hTPS(Hydride Terminated Polydimethylsiloxane) 또는 HTPS(Hydroxyl Terminated Polydimethylsiloxane), 또는 hTPS 및 HTPS 둘 모두의 혼합으로 구성된 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to claim 1,
The PDMS is combined with VTP (Vinyl Terminated Polydimethylsiloxane)
A silicone tape composition for detecting hydrogen gas, characterized in that it consists of hydride terminated polydimethylsiloxane (hTPS) or hydroxyl terminated polydimethylsiloxane (HTPS), or a mixture of both hTPS and HTPS.
상기 PDMS는 VTP 100 중량부에 대하여 hTPS 10~80 중량부, HTPS 0~120 중량부의 혼합으로 구성된 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to claim 2,
The PDMS is a silicone tape composition for detecting hydrogen gas, characterized in that composed of a mixture of 10 to 80 parts by weight of hTPS and 0 to 120 parts by weight of HTPS based on 100 parts by weight of VTP.
상기 VTP는 서로 다른 점도를 갖는 것을 혼합하여 사용하는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to claim 2 or 3,
The VTP is a silicone tape composition for detecting hydrogen gas, characterized in that used by mixing those having different viscosities.
상기 VTP는 1000 cps 점도의 VTP 100 중량부에 대하여 20000 cps 점도의 VTP 90~120 중량부, 65000 cps 점도의 VTP 40~60 중량부를 혼합하여 사용하는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to claim 4,
The VTP is used by mixing 90 to 120 parts by weight of VTP of 20000 cps viscosity and 40 to 60 parts by weight of VTP of 65000 cps viscosity with respect to 100 parts by weight of VTP of 1000 cps viscosity Silicone tape composition for detecting hydrogen gas.
상기 수소가스 감지제 100 중량부에 대하여 PDMS 1,000~2,000 중량부 및 백금촉매 0.5~5 중량부로 구성되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that composed of 1,000 to 2,000 parts by weight of PDMS and 0.5 to 5 parts by weight of a platinum catalyst based on 100 parts by weight of the hydrogen gas sensing agent.
테이프의 변색 시인성 향상제가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that an agent for improving the discoloration and visibility of the tape is further added.
상기 변색 시인성 향상제는 알루미나인 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to claim 7,
The discoloration visibility improver is a silicone tape composition for detecting hydrogen gas, characterized in that alumina.
경화지연제가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that a curing retardant is further added.
상기 경화지연제는 메틸비닐시클로실록산(MVC)인 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to claim 9,
The curing retardant is a silicone tape composition for detecting hydrogen gas, characterized in that methylvinylcyclosiloxane (MVC).
접착성 향상제(adhesion promoter)가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that an adhesion promoter is further added.
인장강도 향상제(Filler)가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that a tensile strength improver (Filler) is further added.
상기 수소가스 감지제는 PdO를 사용하고, 담체는 제올라이트, TiO2, SiO2, ZnO, Al2O3 중 일부 또는 모두인 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.According to any one of claims 1 to 3,
The hydrogen gas sensing agent is PdO, and the carrier is a silicone tape composition for detecting hydrogen gas, characterized in that some or all of zeolite, TiO2, SiO2, ZnO, Al 2 O 3 .
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020210183010A KR20230094239A (en) | 2021-12-20 | 2021-12-20 | Composition for hydrogen sensing tape, tape and manufacturing method thereof |
| PCT/KR2021/019758 WO2023120778A1 (en) | 2021-12-20 | 2021-12-23 | Silicone tape composition for sensing hydrogen gas, hydrogen-gas-sensing silicone tape thereof, and production method for same |
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020210183010A KR20230094239A (en) | 2021-12-20 | 2021-12-20 | Composition for hydrogen sensing tape, tape and manufacturing method thereof |
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| KR20230094239A true KR20230094239A (en) | 2023-06-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7449146B2 (en) * | 2002-09-30 | 2008-11-11 | 3M Innovative Properties Company | Colorimetric sensor |
| KR101701928B1 (en) * | 2015-10-06 | 2017-02-02 | 울산대학교 산학협력단 | A foldable hydrogen sensor and method for manufacturing the same |
| JP6669601B2 (en) * | 2016-07-05 | 2020-03-18 | 東京瓦斯株式会社 | Hydrogen gas detection tape |
| JP7181192B2 (en) * | 2017-02-17 | 2022-11-30 | 日東電工株式会社 | Gas sensing element and method for manufacturing gas sensing element |
| KR101953295B1 (en) * | 2017-06-07 | 2019-02-28 | 울산과학기술원 | Hydrogen gas sensor |
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