KR101296811B1 - Method of surface treatment of semiconductor powder - Google Patents
Method of surface treatment of semiconductor powder Download PDFInfo
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- KR101296811B1 KR101296811B1 KR1020110126219A KR20110126219A KR101296811B1 KR 101296811 B1 KR101296811 B1 KR 101296811B1 KR 1020110126219 A KR1020110126219 A KR 1020110126219A KR 20110126219 A KR20110126219 A KR 20110126219A KR 101296811 B1 KR101296811 B1 KR 101296811B1
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- 239000000843 powder Substances 0.000 title claims abstract description 102
- 239000004065 semiconductor Substances 0.000 title claims abstract description 70
- 238000004381 surface treatment Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007822 coupling agent Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 239000011787 zinc oxide Substances 0.000 claims description 12
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(i) oxide Chemical compound [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 8
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- -1 methacryloxy, acryloxy, amino group Chemical group 0.000 claims description 4
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 150000004645 aluminates Chemical class 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000008117 polysulfides Polymers 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- FWZLXRFUDMNGDF-UHFFFAOYSA-N [Co].[Cu]=O Chemical compound [Co].[Cu]=O FWZLXRFUDMNGDF-UHFFFAOYSA-N 0.000 claims description 2
- PBAJOOJQFFMVGM-UHFFFAOYSA-N [Cu]=O.[Sr] Chemical compound [Cu]=O.[Sr] PBAJOOJQFFMVGM-UHFFFAOYSA-N 0.000 claims description 2
- QMVMBRVXQLUKPF-UHFFFAOYSA-N [Rh]=O.[Zn] Chemical compound [Rh]=O.[Zn] QMVMBRVXQLUKPF-UHFFFAOYSA-N 0.000 claims description 2
- UNRNJMFGIMDYKL-UHFFFAOYSA-N aluminum copper oxygen(2-) Chemical compound [O-2].[Al+3].[Cu+2] UNRNJMFGIMDYKL-UHFFFAOYSA-N 0.000 claims description 2
- CDZGJSREWGPJMG-UHFFFAOYSA-N copper gallium Chemical compound [Cu].[Ga] CDZGJSREWGPJMG-UHFFFAOYSA-N 0.000 claims description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 2
- KYKLWYKWCAYAJY-UHFFFAOYSA-N oxotin;zinc Chemical compound [Zn].[Sn]=O KYKLWYKWCAYAJY-UHFFFAOYSA-N 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- 125000005504 styryl group Chemical group 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000010409 thin film Substances 0.000 abstract description 16
- 239000000203 mixture Substances 0.000 abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000002411 thermogravimetry Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 108091006146 Channels Proteins 0.000 description 1
- 108090000699 N-Type Calcium Channels Proteins 0.000 description 1
- 108010075750 P-Type Calcium Channels Proteins 0.000 description 1
- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SLIUAWYAILUBJU-UHFFFAOYSA-N pentacene Chemical compound C1=CC=CC2=CC3=CC4=CC5=CC=CC=C5C=C4C=C3C=C21 SLIUAWYAILUBJU-UHFFFAOYSA-N 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
Abstract
본 발명은 반도체 분말의 표면처리방법에 관한 것으로, 유기용매에 산화물 반도체 분말 100중량부와, 커플링제 1 내지 50 중량부를 혼합하고 초음파분산기 또는 교반기를 이용하여 산화물 반도체 분말과 커플링제를 반응시켜 산화물 반도체 분말의 표면을 처리시키는 제1공정과; 상기 제1공정 후에 원심분리기를 이용하여 표면처리된 분말과 유기용매를 분리시켜 표면처리된 분말을 회수시키는 제2공정과; 상기 제2공정후에 상기 표면처리된 분말에 포함된 미반응 커플링제 및 반응잔여물을 제거시키기 위해 상기 표면처리된 분말을 유기용매에 첨가하여 초음파 세척기나 교반기를 통하여 3번~10번 세정시키는 제3공정과; 상기 제3공정후에 진공여과장치를 이용하여 상기 표면처리된 분말을 회수시키는 제4공정; 그리고, 상기 제4공정을 거친 상기 표면처리된 분말을 건조시키는 제5공정;을 포함하여 구성되는 반도체 분말의 표면처리방법을 기술적 요지로 한다. 이에 따라, 투명박막트랜지스터용 유무기 나노하이브리드 조성물에 사용되는 산화물 반도체 분말을 커플링제를 이용하여 표면 처리시킴에 의해 유기물 반도체 용액에 균일하게 분산가능하고, 미반응 커플링제 및 반응잔여물은 효율적으로 제거시키는 이점이 있다.The present invention relates to a method for treating a surface of a semiconductor powder, wherein 100 parts by weight of an oxide semiconductor powder and 1 to 50 parts by weight of a coupling agent are mixed with an organic solvent, and the oxide semiconductor powder and the coupling agent are reacted with an ultrasonic disperser or agitator to produce an oxide. A first step of treating the surface of the semiconductor powder; A second step of recovering the surface treated powder by separating the surface treated powder and the organic solvent using a centrifugal separator after the first step; After the second process, the surface-treated powder is added to the organic solvent to remove the unreacted coupling agent and the reaction residue contained in the surface-treated powder 3 to 10 times through an ultrasonic cleaner or agitator to wash 3 step; A fourth step of recovering the surface-treated powder using a vacuum filtration device after the third step; In addition, a fifth step of drying the surface-treated powder that has passed through the fourth step; and a surface treatment method of the semiconductor powder comprising a technical gist. Accordingly, the oxide semiconductor powder used in the organic-inorganic nanohybrid composition for transparent thin film transistors is surface-treated using a coupling agent to uniformly disperse the organic semiconductor solution, and the unreacted coupling agent and the reaction residue are efficiently There is an advantage to eliminate.
Description
본 발명은 반도체 분말의 표면처리 방법에 관한 것으로, 더욱 상세하게는, 투명박막트랜지스터용 유무기 나노하이브리드 조성물에 사용되는 산화물 반도체 분말을 커플링제를 이용하여 표면 처리시킴에 의해 유기물 반도체 용액에 균일하게 분산가능하고, 미반응 커플링제 및 반응잔여물은 효율적으로 제거되는 반도체 분말의 표면처리방법을 기술적 요지로 한다. The present invention relates to a surface treatment method of a semiconductor powder, and more particularly, to an organic semiconductor solution by uniformly treating the oxide semiconductor powder used in the organic-inorganic nanohybrid composition for transparent thin film transistors with a coupling agent. It is a technical point of the surface treatment method of the semiconductor powder which is dispersible and unreacted coupling agent and reaction residue are efficiently removed.
일반적으로 투명박막트랜지스터(TFT)는 투명한 유기물(organics)을 활성반도체로 이용하는 OTFT(Organic TFT)와 투명한 산화물 반도체를 이용하는 ITFT(Inorganic TFT)가 있다.In general, transparent thin film transistors (TFTs) include OTFTs (Organic TFTs) using transparent organics as active semiconductors and ITFTs (Inorganic TFTs) using transparent oxide semiconductors.
도 1은 기존의 투명박막트랜지스터의 구조를 나타낸 것으로, 일반적으로 Si 기판 상층에 게이트 전극과 소스 전극 및 드레인 전극이 형성되고, 게이트 전극 및 소스 전극과 드레인 전극과의 절연을 위해서 게이트 절연층이 형성되며, 게이트 절연층 상층의 소스 전극과 드레인 전극 사이에 또는 게이트 절연층 상층의 소스 전극과 드레인 전극 하측에 상기의 활성반도체 또는 투명한 산화물 반도체를 이용하는 n 또는 p 타입의 채널층이 형성된다.1 illustrates a structure of a conventional transparent thin film transistor, in which a gate electrode, a source electrode, and a drain electrode are generally formed on an Si substrate, and a gate insulating layer is formed to insulate the gate electrode, the source electrode, and the drain electrode. The n or p type channel layer using the active semiconductor or the transparent oxide semiconductor is formed between the source electrode and the drain electrode on the gate insulating layer or below the source electrode and the drain electrode on the gate insulating layer.
상기 OTFTs는 용매에 녹는 물질의 개발이 가능하여 습식공정의 적용과 비교적 저온(<250℃)에서 제조가 가능하며 유연성이 ITFTs에 비해 뛰어난 장점이 있는 반면, 특성이 ITFTs에 비하여 낮다는 단점과 함께, 우수한 성능의 n-type 재료 개발이 미진하여 complementary TFT 회로를 구성하는데 어려움이 있다.The OTFTs can be developed in a solvent-soluble material, can be applied to wet process and manufactured at a relatively low temperature (<250 ℃), and the flexibility is superior to ITFTs, while the characteristics are lower than that of ITFTs. As a result, the development of high performance n-type materials is insufficient, making it difficult to construct a complementary TFT circuit.
그리고, ZnO 등의 투명 산화물 반도체를 이용하는 ITFTs는 펜타센 등과 같은 투명 유기 반도체를 이용한 OTFTs에 비해 전계효과 이동도가 높은 장점은 있으나 우수한 특성을 얻기 위해서는 비교적 고온(>250℃)의 열처리가 필요하며 습식도포공정을 도입한 경우 더욱 높은 온도에서의 열처리가 필요한 단점과 ITFT는 p-채널 구현이 어려운 단점이 있다. In addition, ITFTs using transparent oxide semiconductors such as ZnO have a higher field effect mobility than OTFTs using transparent organic semiconductors such as pentacene, but heat treatment at a relatively high temperature (> 250 ° C) is required to obtain excellent characteristics. The introduction of the wet coating process has the disadvantage of requiring heat treatment at a higher temperature and the ITFT has a disadvantage of difficult p-channel implementation.
따라서, 낮은 온도에서도 제작 가능하며 우수한 성능을 나타내는 박막 트랜지스터 제작을 위해서 용액 공정 적용이 가능한 하이브리드 반도체 용액 제조기술이 필요하다. 즉, 하이브리드 반도체 용액 제조에 있어 산화물 반도체를 유기물 반도체 용액에 균일하게 분산시킬 수 있는 기술의 개발이 필요한데 이를 위해서는 산화물 반도체 표면의 표면처리 기술 개발이 필요하다. Therefore, a hybrid semiconductor solution manufacturing technology capable of applying a solution process is required for fabricating a thin film transistor that can be manufactured at low temperature and exhibits excellent performance. That is, in the manufacture of a hybrid semiconductor solution, it is necessary to develop a technology capable of uniformly dispersing an oxide semiconductor in an organic semiconductor solution. This requires developing a surface treatment technology for an oxide semiconductor surface.
이를 더욱 상세히 설명하면, 용액 공정을 이용하여 박막트랜지스터의 채널층을 형성하기 위해서는 하이브리드 반도체 용액 제조가 필요하다. 하이브리드 반도체 용액 제조를 위해서는 산화물 반도체를 유기물 반도체 용액에 분산시키는 기술이 필요하다. 즉, 산화물 반도체는 분말 형태로 유기물 반도체가 용해되어있는 용액에 분산시키게 된다. In more detail, in order to form the channel layer of the thin film transistor using a solution process, it is necessary to manufacture a hybrid semiconductor solution. In order to manufacture a hybrid semiconductor solution, a technique for dispersing an oxide semiconductor in an organic semiconductor solution is required. That is, the oxide semiconductor is dispersed in a solution in which the organic semiconductor is dissolved in powder form.
그런데, 산화물 반도체인 산화물 분말의 표면에는 하드록시기(-OH)가 다량 존재한다. By the way, a large amount of hydroxy group (-OH) exists in the surface of the oxide powder which is an oxide semiconductor.
상기 하이드록시기에는 수분이 쉽게 흡착되는데, 이는 유기 용매에서의 산화물 분말의 분산을 저해하는 요인이 된다. 또한 박막트랜지스터로 제작되었을 경우 하이드록시기가 캐리어의 트랩(trap)으로 작용하여 소자의 성능을 저해하게 된다.Water is easily adsorbed to the hydroxy group, which becomes a factor of inhibiting the dispersion of the oxide powder in an organic solvent. In addition, when a thin film transistor is manufactured, a hydroxyl group acts as a trap of a carrier, thereby impairing device performance.
따라서, 소자의 성능을 개선하고 산화물 분말의 효과적인 분산을 위한 하이브리드 반도체 용액 제조를 위한 산화물 분말의 표면처리 기술이 필요한 실정이다. Accordingly, there is a need for a surface treatment technique of an oxide powder for producing a hybrid semiconductor solution for improving the performance of the device and effective dispersion of the oxide powder.
상기 용액공정을 이용한 종래기술은 본 출원인이 선출하여 등록받은 대한민국특허청 공개특허공보 공개번호 10-2011-0064180호에 "유무기 나노하이브리드 투명박막트랜지스터용 재료 및 이를 이용한 유무기 나노하이브리드 투명박막트랜지스터"로 소개되어 있다. The prior art using the solution process is disclosed in Korean Patent Application Publication No. 10-2011-0064180, filed by the applicant of the present invention, "Material for organic-inorganic nano-hybrid transparent thin film transistor and organic-inorganic nano-hybrid transparent thin film transistor using the same" It is introduced as.
상기 종래기술은 투명박막트랜지스터의 재료를 형성시키기 위해 투명 무기물 반도체 입자를 투명 유기물 반도체 매트릭스(matrix)에 균일하게 분산시킨 하이브리드 반도체 잉크를 제조하되, 상기 투명 무기물 반도체 입자는 미리 커플링제(coupling agent)를 이용하여 투명 무기물 반도체 입자를 표면 처리하여 투명 유기물 반도체에 분산시키거나, 상기 하이브리드 반도체 잉크 제조시에 커플링제를 첨가하여 표면 개질하여 사용한다. 그리고 미반응 커플링제는 에탄올을 이용하여 린싱과정을 거쳐 유무기 나노하이브리드 조성물을 형성시킨다. The prior art manufactures a hybrid semiconductor ink in which transparent inorganic semiconductor particles are uniformly dispersed in a transparent organic semiconductor matrix to form a material of a transparent thin film transistor, wherein the transparent inorganic semiconductor particles are prepared in advance with a coupling agent. The surface-treated transparent inorganic semiconductor particles are dispersed in a transparent organic semiconductor by using a compound, or a surface modified by adding a coupling agent in the hybrid semiconductor ink production. The unreacted coupling agent is then rinsed with ethanol to form an organic-inorganic nanohybrid composition.
그러나 상기 종래기술은 미반응 커플링제의 제거가 완전하지 못할 뿐만 아니라 반응잔여물이 잔존하게 되어 상기 유무기 나노하이브리드 조성물을 이용하여 투명박막트랜지스터를 형성하는 경우 성능저하의 요인이 되는 등의 문제점이 있다. However, the prior art is not only complete removal of the unreacted coupling agent but also the reaction residues remain, such as problems of performance degradation when forming a transparent thin film transistor using the organic-inorganic nano-hybrid composition have.
따라서, 본 발명은 상기한 종래기술들의 문제점을 해결하기 위해 안출된 것으로, 투명박막트랜지스터용 유무기 나노하이브리드 조성물에 사용되는 산화물 반도체 분말을 커플링제를 이용하여 표면 처리시킴에 의해 유기물 반도체 용액에 균일하게 분산가능하고, 미반응 커플링제 및 반응잔여물은 효율적으로 제거되는 반도체 분말의 표면처리방법을 제공하는 것을 목적으로 한다. Accordingly, the present invention has been made to solve the above problems of the prior art, uniformity in the organic semiconductor solution by surface-treating the oxide semiconductor powder used in the organic-inorganic nanohybrid composition for transparent thin film transistor using a coupling agent. It is an object of the present invention to provide a method for treating a surface of a semiconductor powder that is dispersible and unreacted coupling agent and reaction residue are efficiently removed.
상기한 목적을 달성하기 위한 본 발명은, 유기용매에 산화물 반도체 분말 100중량부와, 커플링제 1 내지 50 중량부를 혼합하고 초음파분산기 또는 교반기를 이용하여 산화물 반도체 분말과 커플링제를 반응시켜 산화물 반도체 분말의 표면을 처리시키는 제1공정과; 상기 제1공정 후에 원심분리기를 이용하여 표면처리된 분말과 유기용매를 분리시켜 표면처리된 분말을 회수시키는 제2공정과; 상기 제2공정후에 상기 표면처리된 분말에 포함된 미반응 커플링제 및 반응잔여물을 제거시키기 위해 상기 표면처리된 분말을 유기용매에 첨가하여 초음파 세척기나 교반기를 통하여 3번~10번 세정시키는 제3공정과; 상기 제3공정후에 진공여과장치를 이용하여 상기 표면처리된 분말을 회수시키는 제4공정; 그리고, 상기 제4공정을 거친 상기 표면처리된 분말을 건조시키는 제5공정;을 포함하여 구성되는 반도체 분말의 표면처리방법을 기술적 요지로 한다. The present invention for achieving the above object, the oxide semiconductor powder by mixing 100 parts by weight of the oxide semiconductor powder and 1 to 50 parts by weight of the coupling agent in the organic solvent and reacting the oxide semiconductor powder and the coupling agent using an ultrasonic disperser or agitator. A first step of treating the surface of the; A second step of recovering the surface treated powder by separating the surface treated powder and the organic solvent using a centrifugal separator after the first step; After the second process, the surface-treated powder is added to the organic solvent to remove the unreacted coupling agent and the reaction residue contained in the surface-treated powder 3 to 10 times through an ultrasonic cleaner or agitator to wash 3 step; A fourth step of recovering the surface-treated powder using a vacuum filtration device after the third step; In addition, a fifth step of drying the surface-treated powder that has passed through the fourth step; and a surface treatment method of the semiconductor powder comprising a technical gist.
상기 산화물 반도체 분말은 ZnO(zinc oxide), SnO2(tin oxide), IGZO(indium gallium zinc oxide), In2O3(indium oxide), ZIO(zinc indium oxide), IGO(indium gallium oxide), IZO(indium zinc oxide), ZTO(zinc tin oxide), Cu2O(copper(Ⅰ) oxide), CuO(copper(Ⅱ) oxide), CuAlO2(delafossite copper aluminum oxide), Cr2O3(copper(Ⅰ) oxide), ZnO-Rh2O3 (zinc rhodium oxide), Cu2O-CoO(copper cobalt oxide), CuGaO2(copper gallium oxide), SrCu2O2(strontium copper oxide) 중 하나가 되는 것이 바람직하다. The oxide semiconductor powder is ZnO (zinc oxide), SnO 2 (tin oxide), IGZO (indium gallium zinc oxide), In 2 O 3 (indium oxide), ZIO (zinc indium oxide), IGO (indium gallium oxide), IZO (indium zinc oxide), ZTO ( zinc tin oxide), Cu 2 O (copper (ⅰ) oxide), CuO (copper (ⅱ) oxide), CuAlO 2 (delafossite copper aluminum oxide), Cr 2 O 3 (copper (ⅰ ) oxide), ZnO-Rh 2 O 3 (zinc rhodium oxide), Cu 2 O—CoO (copper cobalt oxide), CuGaO 2 (copper gallium oxide), or SrCu 2 O 2 (strontium copper oxide).
상기 커플링제는 비닐계(vinyl), 에폭시계(epoxy group), 스티릴계(styryl group), 메타크릴록시계(methacryloxy group), 아크릴록시계(acryloxy), 아미노계(amino group), 클로로프로필계(chloropropyl group), 폴리술피도계(polysulfide group), 이소시아네이트계(isocyanate group)를 포함한 실란(silane), 티타네이트(titanate), 알루미네이트(aluminate) 중 하나가 되는 것이 바람직하다.The coupling agent is vinyl, epoxy, styryl, methacryloxy, acryloxy, amino, chloropropyl (chloropropyl group), polysulfide group (polysulfide group), isocyanate group (silane) including the (silane), titanate (titanate), it is preferable to be one of aluminate (aluminate).
상기 제1공정은, 10분 내지 30분 진행되는 것이 바람직하다.It is preferable that the said 1st process advances for 10 to 30 minutes.
상기 제2공정은, 원심분리기의 회전속도 5000rpm 내지 16000rpm에서 10분 내지 1시간 진행되는 것이 바람직하다.The second step is preferably 10 minutes to 1 hour at a rotational speed of 5000rpm to 16000rpm of the centrifuge.
상기 제3공정은, 각각의 세정이 10분 내지 30분 진행되는 것이 바람직하다.It is preferable that each washing | cleaning advances for said 3rd process for 10 to 30 minutes.
상기 제5공정은 60℃~150℃온도에서 1시간 내지 3시간 진행되는 것이 바람직하다. The fifth step is preferably performed for 1 hour to 3 hours at 60 ℃ ~ 150 ℃ temperature.
이에 따라, 투명박막트랜지스터용 유무기 나노하이브리드 조성물에 사용되는 산화물 반도체 분말을 커플링제를 이용하여 표면 처리시킴에 의해 유기물 반도체 용액에 균일하게 분산가능하고, 미반응 커플링제 및 반응잔여물은 효율적으로 제거시키는 이점이 있다. Accordingly, the oxide semiconductor powder used in the organic-inorganic nanohybrid composition for transparent thin film transistors is surface-treated using a coupling agent to uniformly disperse the organic semiconductor solution, and the unreacted coupling agent and the reaction residue are efficiently There is an advantage to eliminate.
상기의 구성에 의한 본 발명은, 투명박막트랜지스터용 유무기 나노하이브리드 조성물에 사용되는 산화물 반도체 분말을 커플링제를 이용하여 표면 처리시킴에 의해 유기물 반도체 용액에 균일하게 분산가능하고, 미반응 커플링제 및 반응잔여물은 효율적으로 제거시키는 효과가 있다. According to the present invention, the oxide semiconductor powder used in the organic-inorganic nanohybrid composition for transparent thin film transistors can be uniformly dispersed in an organic semiconductor solution by surface treatment using a coupling agent, and an unreacted coupling agent and Reaction residues are effective in removing them.
도1은 기존의 투명박막트랜지스터의 구조를 나타낸 도이고,
도2는 본 발명의 제1실시예에 따른 표면처리전 분말의 전계방출형주사현미경(FE-SEM) 이미지(a) 와 표면처리된 분말의 전계방출형주사현미경(FE-SEM) 이미지(b)를 나타낸 도이고,
도3은 본 발명의 제1실시에에 따른 표면처리전 분말의 열중량분석(a) 과 표면처리된 분말의 열중량분석(b)를 나타낸도이고,
도4는 본 발명의 제2실시예에 따른 표면처리전 분말의 전계방출형주사현미경(FE-SEM)이미지(a) 와 표면처리된 분말의 전계방출형주사현미경(FE-SEM)이미지(b)를 나타낸 도이고,
도5는 본 발명의 제2실시예에 따른 표면처리전 분말의 분광광도계 분석스펙트럼(a)과 표면처리된 분말의 분광광도계 분석스펙트럼(b)을 나타낸 도이다.1 is a view showing the structure of a conventional transparent thin film transistor,
Figure 2 is a field emission scanning microscope (FE-SEM) image (a) of the powder before the surface treatment according to the first embodiment of the present invention and the field emission scanning microscope (FE-SEM) image (b) of the surface treated powder (b ),
Figure 3 is a diagram showing the thermogravimetric analysis (a) and the thermogravimetric analysis (b) of the surface-treated powder before the surface treatment according to the first embodiment of the present invention,
Figure 4 is a field emission scanning microscope (FE-SEM) image of the powder before the surface treatment according to a second embodiment of the present invention (a) and the field emission scanning microscope (FE-SEM) image of the surface-treated powder (b ),
5 is a view showing a spectrophotometer analysis spectrum (a) of the powder before the surface treatment and a spectrophotometer analysis spectrum (b) of the surface treated powder according to the second embodiment of the present invention.
이하 첨부된 도면을 참조로 본 발명의 바람직한 실시예를 상세히 설명하기로 한다.Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
도시된 바와 같이, 본 발명에 따른 반도체 분말의 표면처리방법은, 유기용매에 산화물 반도체 분말 100중량부와, 커플링제 1 내지 50 중량부를 혼합하고 초음파분산기 또는 교반기를 이용하여 산화물 반도체 분말과 커플링제를 반응시켜 산화물 반도체 분말의 표면을 처리시키는 제1공정과; 상기 제1공정 후에 원심분리기를 이용하여 표면처리된 분말과 유기용매를 분리시켜 표면처리된 분말을 회수시키는 제2공정과; 상기 제2공정후에 상기 표면처리된 분말에 포함된 미반응 커플링제 및 반응잔여물을 제거시키기 위해 상기 표면처리된 분말을 유기용매에 첨가하여 초음파 세척기나 교반기를 통하여 3번~10번 세정시키는 제3공정과; 상기 제3공정후에 진공여과장치를 이용하여 최종적으로 표면처리된 분말을 회수시키는 제4공정; 그리고, 상기 제4공정을 거친 표면처리된 분말을 건조시키는 제5공정;으로 구성된다. As shown, the surface treatment method of the semiconductor powder according to the present invention, the oxide semiconductor powder and the coupling agent by mixing 100 parts by weight of the oxide semiconductor powder and 1 to 50 parts by weight of the coupling agent in an organic solvent and using an ultrasonic disperser or agitator Reacting the surface of the oxide semiconductor powder to react with the first step; A second step of recovering the surface treated powder by separating the surface treated powder and the organic solvent using a centrifugal separator after the first step; After the second process, the surface-treated powder is added to the organic solvent to remove the unreacted coupling agent and the reaction residue contained in the surface-treated powder 3 to 10 times through an ultrasonic cleaner or agitator to wash 3 step; A fourth step of recovering the powder finally surface treated using the vacuum filtration device after the third step; And a fifth step of drying the surface-treated powder which has undergone the fourth step.
상기 제1공정은, 10분 내지 30분 진행되고, 상기 제2공정은, 원심분리기의 회전속도 5000rpm 내지 16000rpm에서 10분 내지 1시간 진행되고, 상기 제3공정은, 각각의 세정이 10분 내지 30분 진행되며, 제5공정은 60℃~150℃온도에서 1시간 내지 3시간 진행된다. The first step proceeds from 10 minutes to 30 minutes, the second step proceeds from 10 minutes to 1 hour at a rotational speed of 5000 rpm to 16000 rpm of the centrifuge, and the third step includes 10 minutes to each cleaning. The process proceeds for 30 minutes, and the fifth process is performed for 1 hour to 3 hours at a temperature of 60 ° C to 150 ° C.
이하 본 발명의 구체적인 실시예를 상세히 설명한다.
Hereinafter, specific embodiments of the present invention will be described in detail.
< 제1실시예 >≪ Embodiment 1 >
본 발명의 제1실시예는 He 분위기 산화로에서 500℃에서 2시간 열처리를 한 50㎚ 크기의 ZnO 분말 1g을 용매 n-헥산(n-hexane)에 혼합하고, 티타네이트(titanate)계 커플링제인 이소프로필트리아이소테라로일티나네이트(isopropyl triisoteraroyl titanate, 이하 KR-TTS라 함) 0.1을 혼합한다. In a first embodiment of the present invention, 1 g of a 50 nm size ZnO powder obtained by heat treatment at 500 ° C. for 2 hours in a He atmosphere oxidation furnace is mixed with a solvent n-hexane, and a titanate-based coupling. Jane isopropyl triisoteraroyl titanate (isopropyl triisoteraroyl titanate, hereinafter referred to as KR-TTS) 0.1 is mixed.
그리고, 초음파 분산기에서 30분 정도 처리하게 되면 KR-TTS와 ZnO의 혼합되고, KR-TTS는 ZnO 분말 표면에서의 반응을 일으키게 된다. After 30 minutes of treatment in the ultrasonic disperser, KR-TTS and ZnO are mixed, and KR-TTS causes a reaction on the surface of the ZnO powder.
반응을 마친 용액을 원심분리기에서 회전속도 10000rpm에서 30분간 회전시켜 분말과 용액을 분리한다. 회전 후 분리된 용액과 분말에서 용액을 제거한다. After the reaction, the solution is spun at a rotational speed of 10000 rpm for 30 minutes in a centrifuge to separate the powder and the solution. After rotation, the solution is removed from the separated solution and powder.
분리된 분말에 다시 n-헥산(n-hexane)을 첨가하여 초음파 세척기에서 30분간 처리하여 준다. 이러한 세정공정을 3회 이상 실시한다. 최종적으로 표면처리된 분말의 회수를 위하여 진공여과장치를 이용하여 분말을 회수한다. 이때 포어 사이즈(pore size) 20㎚의 알루미나 필터를 이용하여 분말을 회수한다. N-hexane was added to the separated powder and treated in an ultrasonic cleaner for 30 minutes. This washing step is performed three times or more. In order to recover the surface-treated powder, the powder is recovered using a vacuum filtration device. At this time, the powder is recovered using a pore size 20 nm alumina filter.
회수한 분말을 80℃ 진공 오븐에서 2시간 이상 건조하여 최종적으로 표면처리된 분말이 수득 된다. The recovered powder is dried in a vacuum oven at 80 ° C. for at least 2 hours to obtain a final surface treated powder.
상기 실시예1에서 수득된 표면처리된 분말에 대한 물성측정을 하였는바, 도2는 표면처리전 분말의 전계방출형주사현미경(FE-SEM)이미지(a) 와 표면처리된 분말의 전계방출형주사현미경(FE-SEM)이미지(b)를 나타내었다. The physical properties of the surface treated powders obtained in Example 1 were measured. FIG. 2 shows the field emission scanning microscope (FE-SEM) image (a) of the powder before the surface treatment and the field emission type of the surface treated powders. Scanning microscope (FE-SEM) image (b) is shown.
도2에서 50㎚ 크기의 ZnO 나노 입자 크기는 표면처리 후에도 변화가 없으며, 표면처리후에는 분말의 엉김 현상도 나타나지 않는다. 이는 상기 표면처리된 분말을 이용하여 유무기하이브리드 반도체 용액 제조를 하는 경우, 산화물 반도체를 유기물 반도체 용액에 균일하게 분산시킬 수 있다는 것을 의미한다. In FIG. 2, the size of the ZnO nanoparticles having a size of 50 nm does not change even after the surface treatment, and no powder entanglement occurs after the surface treatment. This means that when the organic-inorganic hybrid semiconductor solution is prepared using the surface-treated powder, the oxide semiconductor can be uniformly dispersed in the organic semiconductor solution.
도3은 본 발명의 제1실시에에 따른 표면처리전 분말의 열중량분석(a) 과 표면처리된 분말의 열중량분석(b)를 나타낸도이다.Figure 3 is a diagram showing the thermogravimetric analysis (a) and the thermogravimetric analysis (b) of the surface-treated powder before the surface treatment according to the first embodiment of the present invention.
도시된 바와 같이, 표면처리 전, 후 열중량 분석 결과에서 ZnO의 온도에 따른 중량변화를 살펴보면 표면처리 후가 표면처리 전보다 중량 변화가 큰 것을 알 수 있다. 이것은 표면처리에 의해 반도체 분말에 대체된 탄화수소가 온도에 따라 분해되면서 표면처리 전보다 큰 중량변화를 나타낸 것을 의미하는바, 표면처리에 의해 하이드록시기가 대부분 대체됨을 의미한다.
As shown, the weight change according to the temperature of ZnO in the thermogravimetric analysis results before and after the surface treatment shows that the weight change after the surface treatment is greater than before the surface treatment. This means that hydrocarbons replaced in the semiconductor powder by the surface treatment show a greater weight change than before the surface treatment as the hydrocarbon is decomposed with temperature, which means that most of the hydroxyl groups are replaced by the surface treatment.
< 제2실시예 >≪ Embodiment 2 >
본 발명의 제2실시예는 p-type 5㎛ 크기의 Cu2O 분말 1g을 용매 n-헥산(n-hexane)에 혼합하고, 여기에 티타네이트(titanate)계 커플링제인 Isopropyl tri(dioctylpyrophosphate) titanate (이하 'KR-38S'라 함) 0.1을 혼합한다. In a second embodiment of the present invention, 1 g of p-type 5 μm Cu 2 O powder is mixed in a solvent n-hexane, and a titanate-based coupling agent isopropyl tri (dioctylpyrophosphate). Mix 0.1 titanate (hereinafter referred to as KR-38S).
초음파 분산기에서 30분 가량 처리하게 되면 KR-38S와 Cu2O 가 혼합되고 KR-38S는 Cu2O 분말 표면에서의 반응을 일으키게 된다. After 30 minutes of treatment in the ultrasonic disperser, KR-38S and Cu 2 O are mixed and KR-38S reacts on the surface of Cu 2 O powder.
반응을 마친 용액을 원심분리기에서 회전속도 10000rpm에서 30분간 회전시켜 분말과 용액을 분리한다. After the reaction, the solution is spun at a rotational speed of 10000 rpm for 30 minutes in a centrifuge to separate the powder and the solution.
회전 후 분리된 용액과 분말에서 용액을 제거한다. After rotation, the solution is removed from the separated solution and powder.
분리된 분말에 다시 n-헥산(n-hexane)을 첨가하여 초음파 세척기에서 30분간 처리하여 준다. 이러한 세정공정을 3회 이상 실시한다. N-hexane was added to the separated powder and treated in an ultrasonic cleaner for 30 minutes. This washing step is performed three times or more.
최종적으로 표면처리된 분말의 회수를 위하여 진공여과장치를 이용하여 분말을 회수한다. 이때 포어사이즈(pore size) 20㎚의 알루미나 필터를 이용하여 분말을 회수한다. In order to recover the surface-treated powder, the powder is recovered using a vacuum filtration device. At this time, the powder is recovered using a pore size 20 nm alumina filter.
회수한 분말을 80℃ 진공 오븐에서 2시간 이상 건조시켜 최종적으로 표면처리된 분말이 수득 된다. The recovered powder is dried in an 80 ° C. vacuum oven for at least 2 hours to obtain a final surface treated powder.
상기 실시예2에서 수득된 표면처리된 분말에 대한 물성측정을 하였는바, 도4는 표면처리전 분말의 전계방출형주사현미경(FE-SEM)이미지(a) 와 표면처리된 분말의 전계방출형주사현미경(FE-SEM)이미지(b)를 나타내었다. The physical properties of the surface treated powders obtained in Example 2 were measured. FIG. 4 shows the field emission scanning microscope (FE-SEM) image (a) of the powder before the surface treatment and the field emission type of the surface treated powders. Scanning microscope (FE-SEM) image (b) is shown.
도4에서 5㎛ 크기의 Cu2O 입자 크기는 표면처리 후에도 변화가 없으며, 표면처리후에는 분말의 엉김 현상도 나타나지 않는다. 이는 상기 표면처리된 분말을 이용하여 유무기하이브리드 반도체 용액 제조를 하는 경우, 산화물 반도체를 유기물 반도체 용액에 균일하게 분산시킬 수 있다는 것을 의미한다. In FIG. 4, the Cu 2 O particle size having a size of 5 μm is unchanged even after the surface treatment, and no powder entanglement occurs after the surface treatment. This means that when the organic-inorganic hybrid semiconductor solution is prepared using the surface-treated powder, the oxide semiconductor can be uniformly dispersed in the organic semiconductor solution.
도5는 본 발명의 제2실시에에 따른 표면처리전 분말의 분광광도계 분석스펙트럼(a) 과 표면처리된 분말의 분광광도계 분석스펙트럼(b)을 나타낸도이다.5 is a view showing a spectrophotometer analysis spectrum (a) of the powder before the surface treatment and a spectrophotometer analysis spectrum (b) of the surface treated powder according to the second embodiment of the present invention.
도시된 바와 같이, 표면처리 전, 후 분광광도계 분석 결과를 통해 알킬기(-CxHy)의 스트레칭 진동(stretching vibration)과 벤딩 진동 (bending vibration)에 의해 나타나는 2800~3000cm- 1와 1200~1400cm- 1 의 피크가 표면처리 전에 Cu2O의 스펙트럼에서는 관찰되지 않지만 표면처리 후에는 나타나는 것을 알 수 있다. 이것을 통해 KR-38S가 Cu2O 분말 표면에 처리된 것을 알 수 있다. As shown, 2800 ~ 3000cm - 1 and 1200 ~ 1400cm, which are indicated by stretching vibration and bending vibration of alkyl group (-C x H y ) through spectrophotometric analysis before and after surface treatment. - a peak of 1, but not observed in the spectrum of Cu 2 O prior to surface treatment after the surface treatment can be seen to appear. This shows that KR-38S was treated on the surface of the Cu 2 O powder.
이상에서와 같이, 본 발명은 투명박막트랜지스터용 유무기 나노하이브리드 조성물에 사용되는 산화물 반도체 분말을 커플링제를 이용하여 표면 처리시킴에 의해 유기물 반도체 용액에 균일하게 분산가능하고, 미반응 커플링제 및 반응잔여물은 효율적으로 제거시키는 이점이 있다.As described above, the present invention is uniformly dispersed in the organic semiconductor solution by surface treatment of the oxide semiconductor powder used in the organic-inorganic nanohybrid composition for transparent thin film transistor with a coupling agent, unreacted coupling agent and reaction The residue has the advantage of removing it efficiently.
Claims (7)
상기 제1공정 후에 원심분리기를 이용하여 표면처리된 분말과 유기용매를 분리시켜 표면처리된 분말을 회수시키는 제2공정과;
상기 제2공정후에 상기 표면처리된 분말에 포함된 미반응 커플링제 및 반응잔여물을 제거시키기 위해 상기 표면처리된 분말을 유기용매에 첨가하여 초음파 세척기나 교반기를 통하여 3번~10번 세정시키는 제3공정과;
상기 제3공정후에 진공여과장치를 이용하여 상기 표면처리된 분말을 회수시키는 제4공정; 그리고,
상기 제4공정을 거친 상기 표면처리된 분말을 건조시키는 제5공정;을 포함하여 구성됨을 특징으로 하는 반도체 분말의 표면처리방법.A first step of mixing 100 parts by weight of an oxide semiconductor powder with 1 to 50 parts by weight of an organic solvent and reacting the oxide semiconductor powder with a coupling agent using an ultrasonic disperser or agitator to treat the surface of the oxide semiconductor powder;
A second step of recovering the surface treated powder by separating the surface treated powder and the organic solvent using a centrifugal separator after the first step;
After the second process, the surface-treated powder is added to the organic solvent to remove the unreacted coupling agent and the reaction residue contained in the surface-treated powder 3 to 10 times through an ultrasonic cleaner or agitator to wash 3 step;
A fourth step of recovering the surface-treated powder using a vacuum filtration device after the third step; And,
And a fifth step of drying the surface-treated powder after the fourth step.
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