KR101956093B1 - Light absorber comprising composite of dielectric-metal nanoparticle, preparing method thereof and comprising the same - Google Patents
Light absorber comprising composite of dielectric-metal nanoparticle, preparing method thereof and comprising the same Download PDFInfo
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- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 42
- 239000006096 absorbing agent Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims 9
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 19
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- JQOAQUXIUNVRQW-UHFFFAOYSA-N hexane Chemical compound CCCCCC.CCCCCC JQOAQUXIUNVRQW-UHFFFAOYSA-N 0.000 claims description 2
- 239000007908 nanoemulsion Substances 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
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- 238000010521 absorption reaction Methods 0.000 description 7
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 229910021446 cobalt carbonate Inorganic materials 0.000 description 2
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 2
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 description 2
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 description 2
- WEZJBAOYGIDDLB-UHFFFAOYSA-N cobalt(3+);borate Chemical compound [Co+3].[O-]B([O-])[O-] WEZJBAOYGIDDLB-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 238000000675 plasmon resonance energy transfer Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
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- 239000002028 Biomass Substances 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000127225 Enceliopsis nudicaulis Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004577 artificial photosynthesis Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- VXWSFRMTBJZULV-UHFFFAOYSA-H iron(3+) sulfate hydrate Chemical compound O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VXWSFRMTBJZULV-UHFFFAOYSA-H 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
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- 230000000243 photosynthetic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
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- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
- B32B2037/243—Coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
Abstract
본 발명은 유전체-금속 나노입자 복합체를 포함하는 광 흡수체, 이의 제조방법 및 이를 포함하는 물분해 광전극에 관한 것으로, 보다 상세하게는 금속기판; 상기 금속기판 상에 증착된 유전체 및 금속 나노입자로 이루어진 광흡수 필름; 및 상기 광흡수 필름 상에 증착된 조촉매 층;을 포함하는, 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제공한다.
본 발명에 따른 유전체-금속 나노입자 복합체를 포함하는 광 흡수체는 유전체와 금속 나노입자의 분율 조절을 통해 광특성 및 광전류 특성을 조절할 수 있는 장점이 있다.The present invention relates to a light absorber comprising a dielectric-metal nano-particle composite, a method for producing the same, and a water-decomposable photoelectrode comprising the same. More particularly, A light absorbing film composed of dielectric and metal nanoparticles deposited on the metal substrate; And a co-catalyst layer deposited on the light absorbing film. The present invention also provides a light absorber comprising a dielectric-metal nanoparticle composite.
The light absorber including the dielectric-metal nanoparticle composite according to the present invention has an advantage in that it can control optical characteristics and photocurrent characteristics by controlling the fraction of dielectric and metal nanoparticles.
Description
본 발명은 유전체에 금속 나노입자를 혼합한 나노 이멀젼을 금속기판에 코팅함으로써 흡수도 및 광전류를 개선할 수 있는 유전체-금속 나노입자 복합체를 포함하는 광 흡수체, 이의 제조방법 및 이를 포함하는 물분해 광전극에 관한 것이다.The present invention relates to a light absorber comprising a dielectric-metal nano-particle composite capable of improving absorption and photocurrent by coating a metal substrate with nanoimulsion mixed with dielectric nanoparticles, a method for producing the same, and a water decomposition To a photoelectrode.
수소는 다양한 에너지원과 기술을 통하여 생산할 수 있는데, 기존의 화석연료나 재생에너지, 원자력, 바이오매스, 인공광합성광촉매를 이용하여 이산화탄소 배출 없이 물분해를 통해 생산할 수 있다. Hydrogen can be produced through a variety of energy sources and technologies, which can be produced using conventional fossil fuels, renewable energy, nuclear power, biomass, artificial photosynthetic photocatalysts, and water decomposition without CO2 emissions.
이산화 티타늄(TiO2)을 기반으로 개발된 인공광합성에 이용되는 광 흡수체는 대부분이 자외선에 반응하는 것으로 태양광선의 경우 자외선은 약 4%이므로 태양광선 중 약 43%를 차지하는 가시광선에 반응하는 고효율의 광 흡수체의 개발이 중요하다. Most of the light absorbers used for artificial photosynthesis developed on the basis of titanium dioxide (TiO 2 ) react with ultraviolet light. In the case of sunlight, ultraviolet light is about 4%. Therefore, It is important to develop a light absorber.
종래 가시광에서 작동하는 광 흡수체로 Fe2O3, BiVO4, CdSe 등을 이용하였으나, 태양광을 조사할 경우 광전화학작용으로 인해 광 흡수체가 부식되는 특성이 있어, 수명 및 신뢰성에 문제점이 지적되고 있다.Conventionally, Fe 2 O 3 , BiVO 4 , and CdSe are used as light absorbers that operate in visible light. However, when solar light is irradiated, the light absorber is corroded due to photoelectric effect, have.
상기 문제점으로 인하여 가시광선에서 물 분해나 고효율의 활성이 실현되고 있지만 아쉽게도 현 단계에서는 수명의 문제로 인해 아직 실용화 단계에 이르지 못하고 있다.Due to the above problems, water decomposition or high-efficiency activity is realized in visible light, but unfortunately it has not been put to practical use due to the problem of life at the present stage.
신뢰성을 가지는 물질로는 대표적으로 TiO2가 있지만 가시광을 거의 흡수하지 않아 태양광에서 낮은 효율을 가져, Fe2O3, BiVO4, ZnO, 및 WO3 등과 복합구조를 이뤄 사용하여 가시광에서 동작하는 광전극 제조에 관한 연구가 활발하게 진행되고 있으며, p-n 접합형 다이오드 구조 등 복합광촉매를 이용하여 전자/정공 쌍을 효율적으로 분리하고 재결합함으로서 광촉매 활성을 얻는 연구 결과가 주목받고 있으나 아직 가시광선 영역에서의 빛의 흡수율이 낮아 solar-to-hydrogen 변환 효율이 낮으며 대체적으로 2% 내외의 효율을 보여주고 있는 문제점이 있다.Reliable materials include TiO 2 , but it absorbs almost no visible light and has low efficiency in solar light. It has a complex structure with Fe 2 O 3 , BiVO 4 , ZnO, WO 3, etc., Research on the fabrication of photoelectrodes has been actively carried out, and studies have been focused on the photocatalytic activity by efficiently separating and recombining electron / hole pairs using a composite photocatalyst such as a pn junction type diode structure. However, To-hydrogen conversion efficiency is low due to a low absorption rate of light of about 2%.
최근 TiO2 소재에 금속 나노입자를 결합한 형태로 플라즈몬 효과를 유도하여 낮은 포톤 에너지에서도 전자/정공이 생성이 될 수 있는 플라즈모닉 광전극에 대한 연구가 진행되고 있으며, 플라즈모닉 효과에 대한 실험적 증명 결과를 보여주고 있기 때문에 고효율 광 흡수체 제조에 있어 필수적으로 고려되고 있다.Recently, plasmonic photoelectrodes capable of generating electrons / holes at low photon energy by inducing plasmon effect in the form of metal nanoparticles bonded to TiO 2 material are being studied. Experimental results of the plasmonic effect Which is considered to be essential for the production of high efficiency light absorbers.
본 발명의 목적은 넓은 밴드 갭을 가지고 가시광 영역에서 동작하지 않는 유전체에, 금속 나노입자를 혼합하여 얻어진 나노 이멀젼을 이용하여 플라즈모닉 현상을 유도하고 흡수된 빛으로 여기된 전자를 효율적으로 광 흡수체에 전달함으로써 태양광선 영역 뿐만 아니라 가시광선 영역의 빛을 통해 수소 및 산소를 생산할 수 있는 유전체-금속 나노입자 복합체를 포함하는 광 흡수체, 이의 제조방법 및 이를 포함하는 물분해 광전극을 제공하는 데에 있다.SUMMARY OF THE INVENTION An object of the present invention is to provide a dielectric substance which has a wide bandgap and does not operate in a visible light region, induces a plasmonic phenomenon by using nanoimulsion obtained by mixing metal nanoparticles, efficiently excites electrons excited by the absorbed light, Metal nanoparticle complex capable of producing hydrogen and oxygen through light in the visible ray region as well as in the sun ray region by transferring the water-decomposable polymer to the water-decomposing electrode, a method for producing the same, and a water decomposition photo- have.
상기 목적을 달성하기 위하여, 본 발명은 금속기판; 상기 금속기판 상에 증착된 유전체 및 금속 나노입자로 이루어진 광흡수 필름; 및 상기 광흡수 필름 상에 증착된 조촉매 층;을 포함하는, 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제공한다.In order to achieve the above object, the present invention provides a semiconductor device comprising: a metal substrate; A light absorbing film composed of dielectric and metal nanoparticles deposited on the metal substrate; And a co-catalyst layer deposited on the light absorbing film. The present invention also provides a light absorber comprising a dielectric-metal nanoparticle composite.
또한 본 발명은 상기 광 흡수체를 포함하는, 물분해 광전극을 제공한다.The present invention also provides a water-decomposable photo-electrode comprising the light absorber.
또한 본 발명은 금속기판을 준비하는 단계; 유기용매에 유전체를 분산시킨 후 금속 나노입자(Metal NPs)를 혼합하여 나노 이멀젼을 준비하는 단계; 상기 나노 이멀젼을 금속기판 상에 코팅한 후 열처리 하여 유전체 및 금속 나노입자로 이루어진 광흡수 필름을 적층하는 단계; 및 상기 적층된 광흡수 필름 상에 조촉매 층을 코팅하는 단계;를 포함하는, 유전체-금속 나노입자 복합체를 포함하는 광 흡수체 제조방법을 제공한다.According to another aspect of the present invention, Preparing a nanoimulsion by dispersing a dielectric material in an organic solvent and then mixing metal nanoparticles (Metal NPs); Coating the nanoimage on a metal substrate and then heat-treating the laminate to form a light absorbing film comprising a dielectric and metal nanoparticles; And coating a cocatalyst layer on the laminated light absorbing film. The present invention also provides a method of manufacturing a light absorbing body including a dielectric-metal nanoparticle composite.
본 발명에 따른 유전체-금속 나노입자 복합체를 포함하는 광 흡수체는 유전체와 금속 나노입자의 분율 조절을 통해 광특성 및 광전류 특성을 조절할 수 있는 장점이 있다.The light absorber including the dielectric-metal nanoparticle composite according to the present invention has an advantage in that it can control optical characteristics and photocurrent characteristics by controlling the fraction of dielectric and metal nanoparticles.
도 1은 본 발명인 유전체-금속 나노입자 복합체를 포함하는 광 흡수체 제조방법을 나타낸 순서도이고;
도 2는 본 발명인 유전체-금속 나노입자 복합체를 포함하는 광 흡수체 제조방법을 나타낸 모식도이며;
도 3은 유전체와 금속 나노입자의 중량비에 따라 제조된 나노 이멀젼을 나타낸 도면이고;
도 4는 나노 이멀젼을 금속기판 상에 코팅한 후 열처리 하여 유전체-금속 광흡수 필름을 적층하는 단계를 개략적으로 나타낸 모식도이며;
도 5는 실시예 1 내지 실시예 4 및 비교예 1에 따라 제조된 광 흡수체의 흡수도를 나타낸 도면이고;
도 6은 실시예 1 내지 실시예 4 및 비교예 1에 따라 제조된 광 흡수체의 광전류를 나타낸 도면이다.1 is a flowchart illustrating a method of manufacturing a light absorber including a dielectric-metal nano-particle composite according to the present invention;
2 is a schematic view showing a method of manufacturing a light absorber including the dielectric-metal nano-particle composite according to the present invention;
3 is a view showing a nanoimage prepared according to a weight ratio of a dielectric material and metal nanoparticles;
4 is a schematic view schematically showing a step of laminating a dielectric-metal light absorbing film by coating a nanoimage on a metal substrate and then performing heat treatment;
FIG. 5 is a view showing the absorption degree of the light absorber produced according to Examples 1 to 4 and Comparative Example 1; FIG.
Fig. 6 is a view showing the photocurrent of the light absorber produced according to Examples 1 to 4 and Comparative Example 1. Fig.
이하, 본 발명인 유전체-금속 나노입자 복합체를 포함하는 광 흡수체, 이의 제조방법 및 이를 포함하는 물분해 광전극을 보다 상세하게 설명한다.Hereinafter, a light absorber including a dielectric-metal nano-particle composite according to the present invention, a method for producing the same, and a water decomposition photo-electrode including the same will be described in detail.
본 발명의 발명자들은 유전체에 금속 나노입자를 혼합함으로써 얻어진 유전체-금속 광흡수 필름을 광 흡수체에 포함할 경우, 종래 광 흡수체에 비해 광흡수가 증가되고, 광전류 특성을 향상시킬 수 있음을 밝혀내어 본 발명을 완성하였다.The inventors of the present invention have found that when a dielectric-metal light absorbing film obtained by mixing metal nanoparticles in a dielectric material is included in the light absorbing material, the light absorption can be increased and the photocurrent characteristic can be improved compared to the conventional light absorbing material Thereby completing the invention.
본 발명은 금속기판; 상기 금속기판 상에 증착된 유전체 및 금속 나노입자로 이루어진 광흡수 필름; 및 상기 광흡수 필름 상에 증착된 조촉매 층;을 포함하는, 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제공한다.The present invention relates to a metal substrate, A light absorbing film composed of dielectric and metal nanoparticles deposited on the metal substrate; And a co-catalyst layer deposited on the light absorbing film. The present invention also provides a light absorber comprising a dielectric-metal nanoparticle composite.
상기 광흡수 필름은 평균 두께가 450 내지 550 nm일 수 있으며, 이에 제한되는 것은 아니다.The light absorbing film may have an average thickness of 450 to 550 nm, but is not limited thereto.
상기 광흡수 필름은 이산화 티타늄(TiO2) 및 금 나노입자(Au NPs)로 이루어진 것일 수 있으며, 이에 제한되는 것은 아니다.The light absorbing film may be made of titanium dioxide (TiO 2 ) and gold nanoparticles (Au NPs), but is not limited thereto.
상기 조촉매 층은 평균 두께가 200 내지 500 nm일 수 있으며, 이에 제한되는 것은 아니다.The co-catalyst layer may have an average thickness of 200 to 500 nm, but is not limited thereto.
상기 조촉매 층은 코발트포스페이트(Cobalt phosphate, CoPi), 코발트카보네이트(Cobalt carbonate, CoCi), 코발트보레이트(Cobalt borate, CoBi), 및 NiOOH/FeOOH로 이루어진 군에서 선택된 어느 하나일 수 있으며, 이에 제한되는 것은 아니다.The co-catalyst layer may be any one selected from the group consisting of cobalt phosphate (CoPi), cobalt carbonate (CoCi), cobalt borate (CoBi), and NiOOH / FeOOH, It is not.
또한 본 발명은 상기 광 흡수체를 포함하는, 물분해 광전극을 제공한다.The present invention also provides a water-decomposable photo-electrode comprising the light absorber.
또한 본 발명은 금속기판을 준비하는 단계; 유기용매에 유전체를 분산시킨 후 금속 나노입자(Metal NPs)를 혼합하여 나노 이멀젼을 준비하는 단계; 상기 나노 이멀젼을 금속기판 상에 코팅한 후 열처리 하여 유전체 및 금속 나노입자로 이루어진 광흡수 필름을 적층하는 단계; 및 상기 적층된 광흡수 필름 상에 조촉매 층을 코팅하는 단계;를 포함하는, 유전체-금속 나노입자 복합체를 포함하는 광 흡수체 제조방법을 제공한다.According to another aspect of the present invention, Preparing a nanoimulsion by dispersing a dielectric material in an organic solvent and then mixing metal nanoparticles (Metal NPs); Coating the nanoimage on a metal substrate and then heat-treating the laminate to form a light absorbing film comprising a dielectric and metal nanoparticles; And coating a cocatalyst layer on the laminated light absorbing film. The present invention also provides a method of manufacturing a light absorbing body including a dielectric-metal nanoparticle composite.
상기 금속기판은 ITO 기판, FTO 기판, 및 스테인리스 스틸 기판으로 이루어진 군에서 선택된 어느 하나일 수 있으며, 이에 제한되는 것은 아니다.The metal substrate may be any one selected from the group consisting of an ITO substrate, an FTO substrate, and a stainless steel substrate, but is not limited thereto.
상기 유기용매는 이소프로필알코올(IPA) 및 헥산(Hexane)을 1 : (1 ~ 9)의 중량비로 혼합한 것 일 수 있으며, 이에 제한되는 것은 아니다.The organic solvent may be a mixture of isopropyl alcohol (IPA) and hexane at a weight ratio of 1: (1 to 9), but is not limited thereto.
상기 유전체는 이산화 규소(SiO2), 또는 이산화 티타늄(TiO2) 중 어느 하나일 수 있으며, 이에 제한되는 것은 아니다.The dielectric may be any one of silicon dioxide (SiO 2 ), or titanium dioxide (TiO 2 ), but is not limited thereto.
상기 유전체는 평균 직경이 10 내지 100 nm인 나노입자일 수 있으며, 이에 제한되는 것은 아니다.The dielectric may be nanoparticles having an average diameter of 10 to 100 nm, but is not limited thereto.
상기 금속 나노입자는 구리(Cu) 나노입자, 철(Fe) 나노입자, 금(Au) 나노입자, 알루미늄(Al) 나노입자, 및 은(Ag) 나노입자로 이루어진 군에서 선택된 어느 하나일 수 있으며, 이에 제한되는 것은 아니다.The metal nanoparticles may be any one selected from the group consisting of copper (Cu) nanoparticles, iron (Fe) nanoparticles, gold (Au) nanoparticles, aluminum (Al) nanoparticles, and silver , But is not limited thereto.
상기 금속 나노입자는 평균 직경이 5 내지 20 nm일 수 있으며, 이에 제한되는 것은 아니다.The metal nanoparticles may have an average diameter of 5 to 20 nm, but are not limited thereto.
상기 나노 이멀젼을 준비하는 단계는 유기용매에 95.0 내지 99.9995 중량%의 유전체를 분산시킨 후 0.0005 내지 5.0 중량%의 금속 나노입자를 혼합할 수 있으며, 이에 제한되는 것은 아니다.The step of preparing the nanomigration may include mixing 0.000005 to 5.0% by weight of metal nanoparticles after dispersing 95.0 to 99.9995% by weight of a dielectric material in an organic solvent, but is not limited thereto.
상기 광흡수 필름을 적층하는 단계는 40 내지 80 μL/cm2의 나노 이멀젼을 금속기판 상에 드랍(drop)하여 2 내지 4회 코팅한 후 열처리 할 수 있으며, 이에 제한되는 것은 아니다.In the step of laminating the light absorbing film, the nanoimulsion of 40 to 80 L / cm 2 may be dropped on the metal substrate and coated 2 to 4 times, followed by heat treatment, but is not limited thereto.
상기 광흡수 필름을 적층하는 단계는 나노 이멀젼을 금속기판 상에 코팅한 후 450 내지 550℃에서 2 내지 4분 동안 열처리 할 수 있으며, 이에 제한되는 것은 아니다.The step of laminating the light absorbing film may be performed by heat-treating the nanoimulsion at 450 to 550 ° C for 2 to 4 minutes after coating the metal substrate, but is not limited thereto.
상기 조촉매 층은 코발트포스페이트(Cobalt phosphate, CoPi), 코발트카보네이트(Cobalt carbonate, CoCi), 코발트보레이트(Cobalt borate, CoBi), 및 NiOOH/FeOOH로 이루어진 군에서 선택된 어느 하나일 수 있으며, 이에 제한되는 것은 아니다.The co-catalyst layer may be any one selected from the group consisting of cobalt phosphate (CoPi), cobalt carbonate (CoCi), cobalt borate (CoBi), and NiOOH / FeOOH, It is not.
이하, 하기 실시예에 의해 본 발명인 유전체-금속 나노입자 복합체를 포함하는 광 흡수체, 이의 제조방법 및 이를 포함하는 물분해 광전극을 보다 상세하게 설명한다. 다만, 이러한 실시예에 의해 본 발명이 한정되는 것은 아니다.Hereinafter, a light absorber including a dielectric-metal nanoparticle composite according to the present invention, a method for producing the same, and a water-decomposable photo-electrode including the dielectric-metal nano-particle composite will be described in more detail with reference to the following examples. However, the present invention is not limited by these examples.
<실시예 1> 유전체-금속 나노입자 복합체를 포함하는 광 흡수체의 제조≪ Example 1 > Fabrication of light absorber including dielectric-metal nanoparticle composite
1. 스티엔리스 스틸(Stainless still) 기판의 준비1. Preparation of Stainless Still Substrate
스티엔리스 스틸 기판을 아세톤, 이소프로필알코올(IPA), 및 증류수(DI water) 순으로 세척하여 준비하였다.The styreness steel substrate was prepared by washing with acetone, isopropyl alcohol (IPA), and distilled water (DI water) in this order.
2. 이산화 티타늄(TiO2. Titanium dioxide (TiO 22 )-금(Au) 나노 이멀젼 준비) - Preparation of gold (Au) nanoimulsion
이소프로필알코올(IPA) : 헥산(Hexane)을 1 : 6의 중량비로 혼합한 유기용매에 20 nm의 일정한 크기로 합성한 이산화 티타늄 나노입자(TiO2 NPs, 99.9995 중량%) 25 mM을 분산시킨 후, 염화금산(HAuCl4)의 구연산염 환원법(citrate reduction)을 이용하여 준비한 5 nm 크기의 금 나노입자(Au NPs, 0.0005 중량%)를 혼합하여 Ti02-Au 나노 이멀젼을 준비하였다.25 mM of titanium dioxide nanoparticles (TiO 2 NPs, 99.9995% by weight) synthesized with a constant size of 20 nm was dispersed in an organic solvent mixed with isopropyl alcohol (IPA): hexane (Hexane) in a weight ratio of 1: 6 Au nano-particles (Au NPs, 0.0005 wt%) prepared by citrate reduction of HAuCl 4 were mixed to prepare TiO 2 -Au nanomigration.
3. 스티엔리스 스틸 기판 상에 Ti03. On the styreness steel substrate, TiO 22 및 Au 나노입자로 이루어진 광흡수 필름의 적층 And a light absorbing film composed of Au nanoparticles
60 μL/cm2에 해당하는 양의 Ti02-Au 나노 이멀젼을 드랍한 후, 아르곤(Ar) 분위기에서 건조시켜 스티엔리스 스틸 기판 상에 Ti02 및 Au 나노입자로 이루어진 광흡수 필름을 코팅하였고, 상기 코팅 과정을 3번 반복한 후 500℃의 Vacuum RTA 조건에서 3분 동안 열처리 하여 평균 두께가 500 nm의 광흡수 필름을 스테인리스 스틸 기판 상에 적층하였다.After dropping TiO 2 -Au nanoimulsion in an amount corresponding to 60 μL / cm 2 , it was dried in an argon (Ar) atmosphere to coat a light absorbing film made of TiO 2 and Au nanoparticles on a Styreness steel substrate The coating process was repeated three times and then heat-treated for 3 minutes under a vacuum RTA condition at 500 ° C. to deposit a light absorbing film having an average thickness of 500 nm on a stainless steel substrate.
4. 광흡수 필름 상에 NiOOH/FeOOH 층 코팅4. NiOOH / FeOOH layer coating on light absorbing film
0.7 V(vs Ag/AgCl) 조건하에서, Ti02 및 Au 나노입자로 이루어진 광흡수 필름을 0.1 M Fe2(SO4)3(iron(Ⅲ) sulfate hydrate) 용액에 15분 동안 전착시켰다. 이후, 0.45 V(vs Ag/AgCl) 조건하에서, 0.1 M 황산니켈·6수화물 용액(Nickel sulfate hexahydrate)에 8분 동안 전착하여 광흡수 필름 상에 NiOOH/FeOOH 층을 코팅시켜 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제조하였다.The light absorbing film consisting of TiO 2 and Au nanoparticles was electrodeposited in 0.1 M Fe 2 (SO 4 ) 3 (iron (III) sulfate hydrate) solution for 15 minutes under 0.7 V (vs Ag / AgCl) conditions. Then, the NiOOH / FeOOH layer was coated on the light absorbing film by electrodeposition in a 0.1 M nickel sulfate hexahydrate solution under 0.45 V (vs Ag / AgCl) condition for 8 minutes to form a dielectric-metal nano-particle complex Was prepared.
<실시예 2> 유전체-금속 나노입자 복합체를 포함하는 광 흡수체의 제조Example 2: Fabrication of a light absorber including a dielectric-metal nanoparticle composite
이산화 티타늄 나노입자(TiO2 NPs, 99.995 중량%) 및 금 나노입자(Au NPs, 0.005 중량%)를 이용한 것을 제외하고는, 상기 실시예 1과 동일한 조건으로 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제조하였다.Metal nanoparticle composite was prepared under the same conditions as in Example 1 except that titanium dioxide nanoparticles (TiO 2 NPs, 99.995 wt%) and gold nanoparticles (Au NPs, 0.005 wt%) were used. An absorber was prepared.
<실시예 3> 유전체-금속 나노입자 복합체를 포함하는 광 흡수체의 제조Example 3: Fabrication of a light absorber including a dielectric-metal nanoparticle composite
이산화 티타늄 나노입자(TiO2 NPs, 99.5 중량%) 및 금 나노입자(Au NPs, 0.5 중량%)를 이용한 것을 제외하고는, 상기 실시예 1과 동일한 조건으로 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제조하였다.Metal nanoparticle composite was prepared under the same conditions as in Example 1 except that titanium dioxide nanoparticles (TiO 2 NPs, 99.5 wt%) and gold nanoparticles (Au NPs, 0.5 wt%) were used. An absorber was prepared.
<실시예 4> 유전체-금속 나노입자 복합체를 포함하는 광 흡수체의 제조Example 4: Fabrication of a light absorber including a dielectric-metal nano-particle composite
이산화 티타늄 나노입자(TiO2 NPs, 95 중량%) 및 금 나노입자(Au NPs, 5 중량%)를 이용한 것을 제외하고는, 상기 실시예 1과 동일한 조건으로 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제조하였다.Metal nanoparticle composite was prepared under the same conditions as in Example 1 except that titanium dioxide nanoparticles (TiO 2 NPs, 95 wt%) and gold nanoparticles (Au NPs, 5 wt%) were used. An absorber was prepared.
<비교예 1> 유전체를 포함하는 광 흡수체의 제조≪ Comparative Example 1 > Production of a light absorber including a dielectric
금 나노입자를 포함하지 않고, 100 중량%의 이산화 티타늄 나노입자를 이용한 것을 제외하고는, 상기 실시예 1과 동일한 조건으로 유전체-금속 나노입자 복합체를 포함하는 광 흡수체를 제조하였다. A light absorber comprising a dielectric-metal nano-particle composite was prepared under the same conditions as in Example 1 except that gold nanoparticles were not included and 100 weight% titanium dioxide nanoparticles were used.
<실험예 1> 광 흡수도 분석≪ Experimental Example 1 >
도 5는 실시예 1 내지 실시예 4 및 비교예 1에 따라 제조된 광 흡수체의 흡수도를 나타낸 도면이다.Fig. 5 is a diagram showing the absorption of a light absorber produced according to Examples 1 to 4 and Comparative Example 1. Fig.
도면을 참조하면, 가시광 효율은 실시예 1에 따라 제조된 광 흡수체가 가장 높지만 태양광에서 가장 높은 효율을 보이는 것은 실시예 2에 따라 제조된 광 흡수체 임을 알 수 있으며, 더 많은 태양광을 흡수할 수록 더 높은 효율로 광전극의 구동이 가능해진다.Referring to the drawings, it can be seen that the visible light efficiency is the highest in the light absorber produced according to Example 1, but the light absorber produced according to Example 2 shows the highest efficiency in the sunlight, It becomes possible to drive the photoelectrode with higher efficiency.
구체적으로, Au NPs에서 생성된 플라즈몬(Plasmon)이 플라즈몬 공명 에너지 전이 메카니즘(Plasmon Resonance Energy Transfer mechanism; 이하 'PRET 메카니즘')에 의해 Au NPs가 TiO2에 광전하를 생성할 에너지를 건내 주기 때문이다.Specifically, Plasmon generated from Au NPs donates energy that Au NPs generate photoelectrons to TiO 2 by a plasmon resonance energy transfer mechanism (PRET mechanism) .
먼저 Au NPs의 함량 비율이 증가할수록, 즉 실시예 1에서 실시예 4로 변화할 수록 태양광, 및 가시광에서의 광전류 값이 모두 줄어드는 것을 확인할 수 있었다. 이는 트랩사이트 소멸현상(trap site quenching)에 의해, Au NPs가 TiO2 또는 다른 Au NPs에서 생성된 광전하를 소멸시키는 역할을 수행하므로 태양광, 및 가시광에서의 빛을 효과적으로 흡수할 수 없다. First, it was confirmed that as the content ratio of Au NPs increases, that is, the photocurrent values in sunlight and visible light decrease as the concentration of Au NPs changes from Example 1 to Example 4. This is because the trap site quenching causes Au NPs to extinguish light charges generated in TiO 2 or other Au NPs, and thus can not effectively absorb light in sunlight and visible light.
광흡수도에서 볼 수 있듯이 진공 열처리에 의해 TiO2에는 가시광에 해당하는 에너지를 받아들일 donor level이 생성된 것을 기반으로, 비교예 1에 따라 제조된 광 흡수체는 흡수도가 393nm에서, 실시예 1 내지 실시예 4에 따라 제조된 광 흡수체는 400 nm이상에서 x축과 만남을 알 수 있다. As can be seen from the optical absorption, based on the fact that the donor level to receive the energy corresponding to the visible light was generated in the TiO 2 by the vacuum heat treatment, the optical absorber produced according to Comparative Example 1 had an absorption of 393 nm, The optical absorber prepared according to Example 4 can find the x-axis contact at 400 nm or more.
<< 실험예Experimental Example 2> 광전류 분석 2> Photocurrent analysis
도 6은 실시예 1 내지 실시예 4 및 비교예 1에 따라 제조된 광 흡수체의 광전류를 나타낸 도면이다.Fig. 6 is a view showing the photocurrent of the light absorber produced according to Examples 1 to 4 and Comparative Example 1. Fig.
도면을 참조하면, 실시예 1에 따라 제조된 광 흡수체는 Au NPs의 함량이 적어 Au NPs에 의해 생성된 플라즈몬이 Au NPs 주위의 TiO2를 충분히 여기시키지 못하는 것으로 판단할 수 있다. 이러한 결과는 태양광 영역의 흡수도가 실시예 1 내지 실시예 3 및 비교예 1에 따라 제조된 광 흡수체에 비해 가장 작은 값을 나타냈음을 통해 뒷받침된다. Referring to the drawings, it can be concluded that the light absorber produced according to Example 1 has a low content of Au NPs, so that plasmons produced by Au NPs do not sufficiently excite TiO 2 around Au NPs. This result is supported by the fact that the absorption of the solar region is the smallest value compared with the light absorber produced according to Examples 1 to 3 and Comparative Example 1. [
실시예 2에 따라 제조된 광 흡수체는 가시광 영역의 광전류는 감소하였으나, 이는 앞서 설명한 trap site의 증가와 동시에 더 많은 양의 광전하를 TiO2 내부에 여기시킬 수 있기 때문이다. 이에 따라 Au NPs 주변에 얼마나 많은 TiO2가 존재하는지 여부가 효율적인 광전극을 제작하는데 중요한 요인이 됨을 확인하였고, 상기 실험예들을 통해 실시예 1 및 실시예 2 사이의 Ti02와 Au NPs의 분율 조건에서 가장 높은 광전극 효율을 얻을 수 있음을 확인하였다.The light absorber prepared according to Example 2 showed a decrease in photocurrent in the visible light region because it can excite a larger amount of photo charge into the TiO 2 simultaneously with the increase of the trap site described above. Accordingly, it was confirmed that how much TiO 2 is present around the Au NPs is an important factor for forming an efficient photoelectrode. Through the above-mentioned experimental examples, the fraction of TiO 2 and Au NPs between Examples 1 and 2 It is confirmed that the highest photoelectrode efficiency can be obtained.
이상과 같이, 본 발명은 비록 한정된 실시예와 도면에 의해 설명되었으나, 본 발명은 이것에 의해 한정되지 않으며 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에 의해 본 발명의 기술 사상과 아래에 기재될 청구범위의 균등 범위 내에서 다양한 수정 및 변형이 가능함은 물론이다.While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. It is to be understood that various modifications and changes may be made without departing from the scope of the appended claims.
Claims (17)
상기 금속기판 상에 증착된 이산화 티타늄(TiO2) 및 금 나노입자(AuNPs)로 이루어진 광흡수 필름; 및
상기 광흡수 필름 상에 증착되며, NiOOH/FeOOH로 이루어진 조촉매 층;을 포함하며,
상기 광흡수 필름은 99.995 중량%의 이산화 티타늄(TiO2) 및 0.005 중량%의 금 나노입자(AuNPs)로 이루어진 것을 특징으로 하는, 광 흡수체.A metal substrate;
A light absorbing film composed of titanium dioxide (TiO 2 ) and gold nanoparticles (AuNPs) deposited on the metal substrate; And
And a co-catalyst layer deposited on the light absorbing film and made of NiOOH / FeOOH,
Characterized in that the light absorbing film comprises 99.995% by weight of titanium dioxide (TiO 2 ) and 0.005% by weight of gold nanoparticles (AuNPs).
상기 광흡수 필름은,
평균 두께가 450 내지 550 nm인 것을 특징으로 하는, 광 흡수체.The method according to claim 1,
The light-
And an average thickness of 450 to 550 nm.
상기 조촉매 층은,
평균 두께가 200 내지 500 nm인 것을 특징으로 하는, 광 흡수체.The method according to claim 1,
The co-
And an average thickness of 200 to 500 nm.
유기용매에 99.995 중량%의 이산화 티타늄(TiO2)을 분산시킨 후 0.005 중량%의 금(Au) 나노입자를 혼합하여 나노 이멀젼을 준비하는 단계;
상기 나노 이멀젼을 금속기판 상에 코팅한 후 열처리 하여 이산화 티타늄(TiO2) 및 금(Au) 나노입자로 이루어진 광흡수 필름을 적층하는 단계; 및
상기 적층된 광흡수 필름 상에 NiOOH/FeOOH로 이루어진 조촉매 층을 코팅하는 단계;를 포함하는, 광 흡수체 제조방법.Preparing a metal substrate;
Dispersing 99.995% by weight of titanium dioxide (TiO 2 ) in an organic solvent, and mixing 0.005% by weight of gold (Au) nanoparticles to prepare a nanoimulsion;
Laminating a light absorbing film made of titanium dioxide (TiO 2 ) and gold (Au) nanoparticles by coating the metal nanoparticles on a metal substrate and then performing heat treatment; And
And coating a co-catalyst layer made of NiOOH / FeOOH on the laminated light absorbing film.
상기 금속기판은,
ITO 기판, FTO 기판, 및 스테인리스 스틸 기판으로 이루어진 군에서 선택된 어느 하나인 것을 특징으로 하는, 광 흡수체 제조방법.The method of claim 7,
Wherein the metal substrate comprises:
An ITO substrate, an FTO substrate, and a stainless steel substrate.
상기 유기용매는,
이소프로필알코올(IPA) 및 헥산(Hexane)을 1 : (1 ~ 9)의 중량비로 혼합한 것을 특징으로 하는, 광 흡수체 제조방법.The method of claim 7,
The organic solvent may include,
Isopropyl alcohol (IPA), and hexane (Hexane) at a weight ratio of 1: (1 to 9).
상기 이산화 티타늄(TiO2)은,
평균 직경이 10 내지 100 nm인 나노입자인 것을 특징으로 하는, 광 흡수체 제조방법.The method of claim 7,
The titanium dioxide (TiO 2 )
Wherein the nanoparticles are nanoparticles having an average diameter of 10 to 100 nm.
상기 금(Au) 나노입자는,
평균 직경이 5 내지 20 nm인 것을 특징으로 하는, 광 흡수체 제조방법.The method of claim 7,
The gold (Au) nano-
Wherein the average diameter is 5 to 20 nm.
상기 광흡수 필름을 적층하는 단계는,
40 내지 80 μL/cm2의 나노 이멀젼을 금속기판 상에 드랍(drop)하여 2 내지 4회 코팅한 후 열처리 하는 것을 특징으로 하는, 광 흡수체 제조방법.The method of claim 7,
Wherein the step of laminating the light absorbing film comprises:
40 drops (drop) the nano-emulsion of this to 80 μL / cm 2 on the metal substrate, characterized in that the heat treatment after the coating 2 to 4 times, the light absorber manufacturing method.
상기 광흡수 필름을 적층하는 단계는,
나노 이멀젼을 금속기판 상에 코팅한 후 450 내지 550℃에서 2 내지 4분 동안 열처리 하는 것을 특징으로 하는, 광 흡수체 제조방법.
The method of claim 7,
Wherein the step of laminating the light absorbing film comprises:
Characterized in that the nanoimulsion is coated on a metal substrate and then heat-treated at 450 to 550 DEG C for 2 to 4 minutes.
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