CN101246952A - Preparation of organic-inorganic ordered compound device for ultraviolet detection - Google Patents
Preparation of organic-inorganic ordered compound device for ultraviolet detection Download PDFInfo
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- CN101246952A CN101246952A CN 200810059558 CN200810059558A CN101246952A CN 101246952 A CN101246952 A CN 101246952A CN 200810059558 CN200810059558 CN 200810059558 CN 200810059558 A CN200810059558 A CN 200810059558A CN 101246952 A CN101246952 A CN 101246952A
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- 238000000825 ultraviolet detection Methods 0.000 title claims description 21
- 238000002360 preparation method Methods 0.000 title claims description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 41
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000010410 layer Substances 0.000 claims abstract description 13
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 12
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000012044 organic layer Substances 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 48
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 48
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 30
- 238000007738 vacuum evaporation Methods 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000003792 electrolyte Substances 0.000 claims description 20
- 229910052697 platinum Inorganic materials 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 16
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 10
- -1 phenylhydrazone Chemical compound 0.000 claims description 10
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- DCZNSJVFOQPSRV-UHFFFAOYSA-N n,n-diphenyl-4-[4-(n-phenylanilino)phenyl]aniline Chemical compound C1=CC=CC=C1N(C=1C=CC(=CC=1)C=1C=CC(=CC=1)N(C=1C=CC=CC=1)C=1C=CC=CC=1)C1=CC=CC=C1 DCZNSJVFOQPSRV-UHFFFAOYSA-N 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000011698 potassium fluoride Substances 0.000 claims description 6
- 235000003270 potassium fluoride Nutrition 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 239000011135 tin Substances 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 238000010422 painting Methods 0.000 claims description 4
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 claims description 4
- DNXIASIHZYFFRO-UHFFFAOYSA-N pyrazoline Chemical compound C1CN=NC1 DNXIASIHZYFFRO-UHFFFAOYSA-N 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
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- 239000011775 sodium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 230000001680 brushing effect Effects 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
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- 238000003618 dip coating Methods 0.000 claims description 3
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910000480 nickel oxide Inorganic materials 0.000 description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
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- 238000003745 diagnosis Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 208000017520 skin disease Diseases 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
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- 238000001514 detection method Methods 0.000 description 1
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- BXNFVPMHMPQBRO-UHFFFAOYSA-N magnesium nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Mg++].[Ni++] BXNFVPMHMPQBRO-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The present invention discloses a method for producing organic-inorganic ordered compound device for UV exploration. Firstly, oxidizing partially high pure metal substrates or high pure metal deposited on substrate by electrochemistry anodic oxidation, obtaining tube shape metal oxide array, and then coating organic layer and electrode layer in turn. Controlling length of tube shape metal oxide array and thickness of organic layer and electrode layer by appropriate technique. The present invention has merits of low price, adjustable structure, producing in large area of organic material and good stability of inorganic material by combination of organic and inorganic semiconductor material, and improves the responsivity using the array inorganic semiconductor material. The techinics of present invention is simple and easy to operation.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection.
Technical background
As far back as the 1950's, people have just begun the ultraviolet detection Study on Technology.The ultraviolet detection technology is the another dual-use detecting technique that grows up after infrared and laser acquisition technology.Only with regard to military aspect, such as electrooptical countermeasures, the infrared counteraction and oppose reaching its maturity of anti-technology of continuing, ultraviolet countermeasure and oppose that anti-technology also more and more is subjected to the attention of the military.The later stage eighties 20th century has begun the military research of ultraviolet technology abroad, and has obtained certain progress.First ultraviolet alarm device AAR-47 in the world just arranged on the C-130S of USN helicopter and the P-3S transporter.The aircraft of states such as thousands of covers are equipped on American and Britain respectively, add, Australia is just arranged soon, in the Gulf War, once threw the people under battle conditions in 1991.The ultraviolet detection technology is also having a wide range of applications aspect medical science, the biology, particularly in recent years unique effect is being arranged aspect the skin disease diagnosis.Utilize the ultraviolet detection technology when detecting the diagnosis skin disease, can directly see the pathology details.Also available it detect cancer cell, microbe, hemochrome, red blood cell, white blood cell, nucleus etc., this detection is not only rapidly, accurately, and is and directly perceived, clear.
According to the mechanism of ultraviolet detection process, ultraviolet detector can be divided into thermal detector and photon detector.Wherein photon detector is divided into photoemissive detector again, photovoltaic detector and optical waveguide detector.The principle of photoemissive detector is: when radiation irradiation during at some metal, metal oxide or semiconductor material surface, if this photon energy is enough big, then is enough to make in the material some electronics to break away from material fully and overflows from the surface.This phenomenon is called photoelectron emissions, and the detector that utilizes this effect to make is exactly the photoelectron emissions detector.The principle of photovoltaic detector is: p-n junction or p-i-n knot are added reverse biased, and then after the interface absorbed the enough big photon of energy, reverse current will increase.This situation is similar to photoconductive phenomenon.This class photovoltaic detector is called semiconductor photo diode usually.The principle of optical waveguide detector is: after semiconductor absorbs the enough big photon of energy, can be activated to the free state that to conduct electricity to some electronics or hole wherein from original nonconducting bound state, thereby conductivity semiconductor is increased, and this phenomenon is called photoconductive effect.Device according to the photoconductive effect probe radiation is called photoconduction (PC) detector.Present this device kind is maximum, most widely used.Chinese patent CN1684275A has narrated a kind of preparation method of nickel magnesium oxide day blind region ultraviolet detector device.U.S. Pat 6326654 has been narrated a kind of ultraviolet detector of inorganic, inorganic composite type.People such as J.Yamaura have made a kind of organic UV detector based on inorganic substrates.
Inorganic-organic ordered compound ultraviolet detector that the present invention makes by a kind of simple method, the inorganic semiconductor material array response that can make full use of ordering is fast, good stability and transmit advantages such as fast, and advantages such as organic material is cheap, the easy accent of structure, save cost effectively, make performance more superior.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection.
Comprise the steps:
1) purity is that 95～99.8% high pure metal sheet or the substrate that deposits 95～99.8% high pure metal use acetone, isopropyl alcohol, methyl alcohol supersound washing after 1～20 minute successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing, obtain basal electrode;
2) with platinized platinum as negative electrode, basal electrode is as anode, in electrolyte, antianode carries out oxidation, and voltage is 2～30 volts, and the time is 5～120 minutes, behind deionized water rinsing, place 180～680 ℃ of air or oxygen environment heat treatments cooling naturally after 3-9 hour, take out, obtain tubular metal oxide array;
3) applying a layer thickness on tubular metal oxide array is the organic layer of 2nm～200nm;
4) applying a layer thickness on organic layer is the electrode layer of 2～60nm.
Described high pure metal sheet is titanium, zinc, nickel, magnesium, aluminium or tin.Substrate is simple glass, electro-conductive glass, silicon chip or macromolecule resin, and high pure metal adopts vacuum evaporation or magnetically controlled sputter method to be deposited in the substrate, and thickness is 1 μ m～100 μ m.Electrolyte is one or more the mixture in sulfuric acid, acetic acid, hydrochloric acid, phosphoric acid, potassium fluoride aqueous solution, sodium fluoride aqueous solution, the niter cake aqueous solution, and electrolyte ph is 1～6.5.The pipe range of tubular metal oxide array is that 0.02 μ m～10 μ m, caliber are 10nm～120nm.Organic layer is that triphenylamine, alkyl replace triphenylamine, phenylhydrazone, naphthalene phenylhydrazone, tetraphenyl benzidine, alkyl replacement tetraphenyl benzidine, Polyvinyl carbazole, bipyridine, pyrazoline, polyphenylene ethylene or alkyl replacement polyphenylene ethylene.Electrode layer is gold, silver, aluminium, magnesium, calcium, platinum or carbon paste.The painting method of organic layer is solution spin coating, dip-coating or vacuum evaporation.The painting method of electrode layer is magnetron sputtering, vacuum evaporation or brushing.
The present invention is by the cooperative effect of inorganic material and organic material, and utilize the inorganic material array of ordering, made the ultraviolet detector that performance is better than single component material and common composite organic-inorganic material.Its technology is simple, is easy to realize, increases under the condition of limited at cost to have increased substantially performance.
Description of drawings
Fig. 1 is the structural representation that is used for the organic-inorganic ordered compound device of ultraviolet detection of the present invention; From top to bottom successively by electrode layer, organic layer, tubular metal oxide array and substrate are formed;
Fig. 2 is the ESEM picture of tubular metal oxide array; This loose structure helps the infiltration of organic molecule, thereby increases the contact area between inorganic, the organic material, makes more light induced electron-holes to separating, and strengthens photoresponse;
Fig. 3 is the UV absorption spectrogram that is used for the organic-inorganic ordered compound device of ultraviolet detection of the present invention; As can be seen, this detector has very strong absorption to the light of 280～420nm from spectrogram, shows the characteristics that it is surveyed in the ultra-violet (UV) band;
Fig. 5 is the organic-inorganic ordered compound device that is used for ultraviolet detection of the present invention I-V curve when bright attitude and dark attitude under ultraviolet light irradiation.The ratio of 2V time/dark current can reach 400.The enhancing of electric current derives from contact area big between tubular metal oxide array and the organic film and the quick transmission of charge carrier in tube array.
Embodiment
The present invention is described in further detail by following embodiment:
Embodiment 1:
High-purity zinc metal sheet (purity 95%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 10 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the aqueous sulfuric acid of pH=6.5, adopts two electrode systems, and platinized platinum is as negative electrode, and zinc metal sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 30V.Reaction carries out taking out after 120 minutes the zinc metal sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 9 hours in 380 ℃ of air ambients, obtain the tubulose zinc oxide array, the triphenylamine film of vacuum evaporation 200nm on above-mentioned array, the thick gold electrode of magnetron sputtering one deck 60nm on the triphenylamine film at last.
Embodiment 2:
High-purity magnesium sheet (purity 99.8%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 20 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the aqueous acetic acid of pH=1, adopts two electrode systems, and platinized platinum is as negative electrode, and magnesium sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 2V.Reaction carries out taking out after 5 minutes the magnesium sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 3 hours in 680 ℃ of oxygen atmospheres, obtain tubulose magnesium oxide array, the bipyridine film of vacuum evaporation 2nm on above-mentioned array, the thick silver electrode of magnetron sputtering one deck 20nm on the bipyridine film at last.
Embodiment 3:
High purity titanium sheet (purity 99.8%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 1 minute successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the hydrochloric acid of pH=3, adopts two electrode systems, and platinized platinum is as negative electrode, and the titanium sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 10V.Reaction carries out taking out after 15 minutes the titanium sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 4 hours in 280 ℃ of oxygen atmospheres, obtain the tubular titanium oxide array, the Polyvinyl carbazole film of spin coating 20nm on above-mentioned array, the thick aluminium electrode of vacuum evaporation one deck 20nm on the Polyvinyl carbazole film at last.
Embodiment 4:
High purity nickel sheet (purity 96%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 5 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the hydrochloric acid of pH=4, adopts two electrode systems, and platinized platinum is as negative electrode, and the nickel sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 20V.Reaction carries out taking out after 10 minutes the nickel sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 6 hours in 480 ℃ of oxygen atmospheres, obtain tubulose nickel oxide array, the phenylhydrazone film of vacuum evaporation 100nm on above-mentioned array, the thick magnesium electrode of magnetron sputtering one deck 40nm on the phenylhydrazone film at last.
Embodiment 5:
High-purity aluminium flake (purity 97%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 15 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the potassium fluoride aqueous solution of pH=3.3, adopts two electrode systems, and platinized platinum is as negative electrode, and the tin sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 25V.Reaction carries out taking out after 70 minutes the nickel sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 5.6 hours in 500 ℃ of oxygen atmospheres, obtain tubulose tin oxide array, the tetraphenyl benzidine film of dip-coating 73nm on above-mentioned array, the thick calcium electrode of magnetron sputtering one deck 15nm on tetraphenyl benzidine film at last.
Embodiment 6:
High purity tin sheet (purity 99.8%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 6 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with potassium fluoride, the acetic acid mixed aqueous solution of pH=4.8, adopts two electrode systems, and platinized platinum is as negative electrode, and the tin sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 25V.Reaction carries out taking out after 70 minutes the nickel sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 8.8 hours in 300 ℃ of air ambients, obtain tubulose tin oxide array, the polyphenylene ethylene film of solution spin coating 47nm on above-mentioned array, the thick platinum electrode of vacuum evaporation one deck 15nm on the polyphenylene ethylene film at last.
Embodiment 7:
Vacuum evaporation has the substrate of glass of high purity titanium to use acetone, isopropyl alcohol, methyl alcohol supersound washing after 3 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with potassium fluoride, acetic acid, sulfuric acid, the mixed in hydrochloric acid aqueous solution of pH=5.2, adopts two electrode systems, and platinized platinum is as negative electrode, and the glass that deposits high purity titanium is as anode, the constant distance of two interpolars, and oxidation voltage is 18V.Reaction is carried out taking out after 55 minutes, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 7.2 hours in 570 ℃ of air ambients, obtain the tubular titanium oxide array, the pyrazoline film of solution spin coating 155nm on above-mentioned array, the last thick carbon paste electrode of one deck 28nm of on the pyrazoline film, brushing.
Embodiment 8:
Vacuum evaporation has the electro-conductive glass substrate of 99.8% high-purity magnesium to use acetone, isopropyl alcohol, methyl alcohol supersound washing after 13 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the phosphate aqueous solution of pH=2, adopts two electrode systems, and platinized platinum is as negative electrode, and the electro-conductive glass that deposits high-purity magnesium is as anode, the constant distance of two interpolars, and oxidation voltage is 15V.Reaction is carried out taking out after 30 minutes, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 3 hours in 480 ℃ of oxygen atmospheres, obtain tubulose magnesium oxide array, on above-mentioned array 4 of vacuum evaporation 2nm, 4-benzidine film, at last 4, the thick gold electrode of magnetron sputtering one deck 60nm on the 4-benzidine film.
Embodiment 9:
Vacuum evaporation has the silicon chip of 95% high purity zinc to use acetone, isopropyl alcohol, methyl alcohol supersound washing after 18 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with sodium fluoride, acetic acid, sulfuric acid, the mixed in hydrochloric acid aqueous solution of pH=4.5, adopts two electrode systems, and platinized platinum is as negative electrode, and the silicon chip that deposits high purity zinc is as anode, the constant distance of two interpolars, and oxidation voltage is 12V.Reaction is carried out taking out after 5 minutes, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 9 hours in 380 ℃ of air ambients, obtain the tubulose zinc oxide array, the naphthalene phenylhydrazone film of vacuum evaporation 200nm on above-mentioned array, the thick silver electrode of magnetron sputtering one deck 20nm on naphthalene phenylhydrazone film at last.
Embodiment 10:
Magnetron sputtering has the macromolecule resin of 99.8% high purity titanium to use acetone, isopropyl alcohol, methyl alcohol supersound washing after 8 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with phosphoric acid, acetic acid, sodium fluoride, the niter cake of pH=5, adopts two electrode systems, and platinized platinum is as negative electrode, and the macromolecule resin that deposits high purity titanium is as anode, the constant distance of two interpolars, and oxidation voltage is 10V.Reaction is carried out taking out after 25 minutes, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 4.5 hours obtains the tubular titanium oxide array in 180 ℃ of oxygen atmospheres, on above-mentioned array 4 of vacuum evaporation 20nm, 4 ', 4 " triphenylamine film-three-(3-aminomethyl phenyl anilino-) is at last 4; 4 ', 4 " the thick gold electrode of vacuum evaporation one deck 30nm on-three-(3-aminomethyl phenyl anilino-) the triphenylamine films.
Embodiment 11:
High purity titanium sheet (purity 99.8%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 10 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is with the hydrochloric acid of pH=2.3, and potassium fluoride is an electrolyte, adopts two electrode systems, and platinized platinum is as negative electrode, and the titanium sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 24V.Reaction carries out taking out after 35 minutes the titanium sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 4 hours in 380 ℃ of oxygen atmospheres, obtain the tubular titanium oxide array, the alkyl of spin coating 20nm replaces the polyphenylene ethylene film on above-mentioned array, replaces the thick aluminium electrode of vacuum evaporation one deck 20nm on the polyphenylene ethylene film at alkyl at last.
Embodiment 12:
High purity nickel sheet (purity 99.8%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 9 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the phosphoric acid of pH=4.3, adopts two electrode systems, and platinized platinum is as negative electrode, and the nickel sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 17V.Reaction carries out taking out after 8 minutes the nickel sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 6 hours in 360 ℃ of oxygen atmospheres, obtain tubulose nickel oxide array, the alkyl of vacuum evaporation 100nm replaces tetraphenyl benzidine film on above-mentioned array, replaces the thick magnesium electrode of magnetron sputtering one deck 40nm on the tetraphenyl benzidine film at alkyl at last.
Embodiment 13:
High purity nickel sheet (purity 96%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 19 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the phosphoric acid of pH=4.3, adopts two electrode systems, and platinized platinum is as negative electrode, and the nickel sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 17V.Reaction carries out taking out after 8 minutes the nickel sheet of partial oxidation, rinses well with deionized water, places Ma Fulu, insulation cooling naturally after 6 hours obtains tubulose nickel oxide array, the N of vacuum evaporation 100nm on above-mentioned array in 360 ℃ of oxygen atmospheres, N '-diphenyl-N, N '-two-(1-naphthyl-1,1 '-biphenyl)-4,4 '-diamines film, at last at N, N '-diphenyl-N, N '-two-(1-naphthyl-1,1 '-biphenyl)-4, the thick magnesium electrode of magnetron sputtering one deck 40nm on 4 '-diamines film.
Embodiment 14:
High-purity magnesium sheet (purity 98%) uses acetone, isopropyl alcohol, methyl alcohol supersound washing after 10 minutes successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing.Anode oxidation process is an electrolyte with the phosphoric acid of pH=4.3, adopts two electrode systems, and platinized platinum is as negative electrode, and the nickel sheet is as anode, the constant distance of two interpolars, and oxidation voltage is 17V.Reaction carries out taking out after 8 minutes the nickel sheet of partial oxidation, rinse well with deionized water, place Ma Fulu, insulation cooling naturally after 6 hours in 360 ℃ of oxygen atmospheres, obtain tubulose nickel oxide array, the N of vacuum evaporation 100nm on above-mentioned array, N '-diphenyl-N, N '-two-(3-aminomethyl phenyl)-1,1 '-biphenyl-4,4 '-diamines film, at last at N, N '-diphenyl-N, N '-two-(3-aminomethyl phenyl)-1,1 '-biphenyl-4, the thick magnesium electrode of magnetron sputtering one deck 40nm on 4 '-diamines film.
Claims (9)
1. a preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection is characterized in that comprising the steps:
1) purity is that 95～99.8% high pure metal sheet or the substrate that deposits 95～99.8% high pure metal use acetone, isopropyl alcohol, methyl alcohol supersound washing after 1～20 minute successively, with rinsed with deionized water and oven dry, again it is carried out chemical polishing, obtain basal electrode;
2) with platinized platinum as negative electrode, basal electrode is as anode, in electrolyte, antianode carries out oxidation, and voltage is 2～30 volts, and the time is 5～120 minutes, behind deionized water rinsing, place 180～680 ℃ of air or oxygen environment heat treatments cooling naturally after 3-9 hour, take out, obtain tubular metal oxide array;
3) applying a layer thickness on tubular metal oxide array is the organic layer of 2nm～200nm;
4) applying a layer thickness on organic layer is the electrode layer of 2～60nm.
2. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1 is characterized in that described high pure metal sheet is titanium, zinc, nickel, magnesium, aluminium or tin.
3. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1, it is characterized in that described substrate is simple glass, electro-conductive glass, silicon chip or macromolecule resin, high pure metal adopts vacuum evaporation or magnetically controlled sputter method to be deposited in the substrate, and thickness is 1 μ m～100 μ m.
4. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1, it is characterized in that described electrolyte is one or more the mixture in sulfuric acid, acetic acid, hydrochloric acid, phosphoric acid, potassium fluoride aqueous solution, sodium fluoride aqueous solution, the niter cake aqueous solution, electrolyte ph is 1～6.5.
5. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1, the pipe range that it is characterized in that described tubular metal oxide array is that 0.02 μ m～10 μ m, caliber are 10nm～120nm.
6. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1 is characterized in that described organic layer is that triphenylamine, alkyl replace triphenylamine, phenylhydrazone, naphthalene phenylhydrazone, tetraphenyl benzidine, alkyl replacement tetraphenyl benzidine, Polyvinyl carbazole, bipyridine, pyrazoline, polyphenylene ethylene or alkyl replacement polyphenylene ethylene.
7. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1 is characterized in that electrode layer is gold, silver, aluminium, magnesium, calcium, platinum or carbon paste.
8. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1, the painting method that it is characterized in that organic layer is solution spin coating, dip-coating or vacuum evaporation.
9. a kind of preparation method who is used for the organic-inorganic ordered compound device of ultraviolet detection according to claim 1, the painting method that it is characterized in that electrode layer is magnetron sputtering, vacuum evaporation or brushing.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101916827A (en) * | 2010-06-29 | 2010-12-15 | 浙江大学 | Preparation method of organic/titanium dioxide composite ultraviolet detector |
| CN101976728A (en) * | 2010-09-29 | 2011-02-16 | 昆明物理研究所 | Photovoltaic organic ultraviolet semiconductor detector |
| CN103280340A (en) * | 2013-05-23 | 2013-09-04 | 华南理工大学 | Nickel-based electrode material and preparation method thereof |
| CN103311439A (en) * | 2013-05-17 | 2013-09-18 | 中国科学院化学研究所 | Thin film photoconductive detector and manufacturing method and application thereof |
| CN103700770A (en) * | 2013-12-13 | 2014-04-02 | 浙江大学 | Solar blind type organic-inorganic composite ultraviolet detector |
| CN103700771A (en) * | 2013-12-13 | 2014-04-02 | 浙江大学 | Sodium tantalum oxide/organic composite active layer-based solar blind ultraviolet photodetector |
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2008
- 2008-01-31 CN CN 200810059558 patent/CN101246952A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101916827A (en) * | 2010-06-29 | 2010-12-15 | 浙江大学 | Preparation method of organic/titanium dioxide composite ultraviolet detector |
| CN101916827B (en) * | 2010-06-29 | 2012-05-02 | 浙江大学 | Preparation method of organic/titanium dioxide composite ultraviolet detector |
| CN101976728A (en) * | 2010-09-29 | 2011-02-16 | 昆明物理研究所 | Photovoltaic organic ultraviolet semiconductor detector |
| CN101976728B (en) * | 2010-09-29 | 2012-07-04 | 昆明物理研究所 | Photovoltaic organic ultraviolet semiconductor detector |
| CN103311439A (en) * | 2013-05-17 | 2013-09-18 | 中国科学院化学研究所 | Thin film photoconductive detector and manufacturing method and application thereof |
| CN103311439B (en) * | 2013-05-17 | 2015-07-15 | 中国科学院化学研究所 | Thin film photoconductive detector and manufacturing method and application thereof |
| CN103280340A (en) * | 2013-05-23 | 2013-09-04 | 华南理工大学 | Nickel-based electrode material and preparation method thereof |
| CN103280340B (en) * | 2013-05-23 | 2015-12-02 | 华南理工大学 | A kind of nickel base electrode material and preparation method thereof |
| CN103700770A (en) * | 2013-12-13 | 2014-04-02 | 浙江大学 | Solar blind type organic-inorganic composite ultraviolet detector |
| CN103700771A (en) * | 2013-12-13 | 2014-04-02 | 浙江大学 | Sodium tantalum oxide/organic composite active layer-based solar blind ultraviolet photodetector |
| CN103700771B (en) * | 2013-12-13 | 2016-05-04 | 浙江大学 | Sun blind UV detector based on sodium tantalate/organic composite active layer |
| CN103700770B (en) * | 2013-12-13 | 2016-05-04 | 浙江大学 | Day blind type organic and inorganic composite ultraviolet detector device |
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