CN102110735B - Semiconductor ultraviolet detection sensor and preparation method thereof - Google Patents
Semiconductor ultraviolet detection sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a semiconductor sensor for ultraviolet detection and a preparation method of the sensor. The semiconductor ultraviolet detection sensor comprises a baseplate, electrodes loaded on the baseplate and zinc oxide nanowires which are positioned between the electrodes, connected in parallel and integrated, wherein the electrodes are two comb tooth-shaped electrodes which are arranged oppositely, one comb tooth of one electrode is inserted between two comb teeth of the other electrode so as to form the tooth insertion shape, and the zinc oxide nanowires are respectively connected in parallel and integrated on the adjacent two comb teeth. The light response current of the semiconductor ultraviolet detection sensor can achieve the milliamp magnitude, thereby significantly reducing the ultraviolet detection difficulty and the characterization difficulty of the strength thereof.
Description
Technical field
The present invention discloses a kind of preparation method who is used for the semiconductor transducer and this transducer of ultraviolet detection, the invention belongs to ultraviolet detector technology category.Semiconductor ultraviolet detection transducer of the present invention is a kind of integrated ultraviolet light detector of zinc oxide nano-wire array of using.
Background technology
Ultraviolet detection is as a kind of dual-use technology that broad prospect of application is arranged, and the later stage eighties 20th century has just begun a large amount of research and application.At military aspect, first ultraviolet alarm device AAR-47 in the world just arranged on the C-130S of USN helicopter that in the Gulf War, came into operation in 1991 and the P-3S transporter, and the U.S. also researches and develops the Ultraviolet sensor technology in the lasting manpower and materials that drop into energetically.In the recent period, only Flos micheliae Albae Optical Technology Corp. is used for the research of this respect with regard to the funds that obtained 1,250,000 dollars, referring to Ke limit, and " aerospace electron antagonism " (2), 47,2001.Aspect civilian; The ultraviolet transducing technology is widely used in medical science and field of biology; Especially in the skin disease context of detection of medical science, utilize the ultraviolet detection technology 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 rapid, accurate, and directly perceived, clear.Referring to: Chen Peng, Jiang offers, Int J Dermatol Venereol, January 2007, and Vol 33, No.1; Xu Yiqing, Wang Ying, Shanghai Nursing, Jul.2009, Vol.9, No.4; Zhang Ruili, Dong Yan, high lily feet, J Clin Dermatol, October 2006, Vol.35, NO.10; Zhang Hongming Bi Zhi is firm, 2003 the 29th the 3rd phases of volume of foreign medical science skin cypridology fascicle.
The ultraviolet detection of broad research technology mainly is based on ultraviolet light the influence of semiconductor carrier concentration is developed at present.When the UV-irradiation semiconductor, the valence band electronics is excited to conduction band, makes carrier concentration rise, and semiconductor resistor descends, thereby measures change in current, realizes a kind of technology to ultraviolet detector with this.
As the Ultraviolet sensor of photon detection technology category, main difficulty has three broad aspect at present.At first,, need to use expensive tiny signal detection system to realize the detection of photoresponse electric current, cause his limitation on large-scale application because the photoresponse electric current that ultraviolet light produced is very little.Secondly, ultraviolet lighting is mapped to after the sample surfaces, and the response and the turnaround time of detector are longer, make on detectivity, to have difficulties.Moreover; Nano wire has big specific area with respect to traditional material; When nano wire is exposed to airborne the time for a long time; Airborne steam and carbon dioxide can make the surface state of zinc oxide change gradually, thereby cause the degeneration of ultraviolet light detector to the ultraviolet light response ability, make the life-span of device have problems.Moreover, if device is made up of the destruction fully that can cause entire device in case nano wire damages, so it has problems aspect reliability single nano-wire.For first difficulty, the method that solves at present mainly contains two types, and first kind method is that the surface of single nano-wire is handled, and makes it have higher response.Such as, human CdTe quantum dot modification zinc oxide nanowire surface such as S.Aga.Jr make photoresponse curve roughly improve near 5nA; Though the photoresponse electric current rises to some extent; Need very expensive instrument but survey other electric current of nA level, referring to R.S.Aga, Jr et.al; Appl.Phys.Lett.91,232108 (2007).People such as J.H.He have carried out functionalization with the zinc-oxide nano belt surface, and make electrical signal intensity increase substantially 100 times of baseline, but because baseline is almost nil; So the postradiation signal of telecommunication of actual photon is still very faint; And the flow process of functionalization is loaded down with trivial details, is unfavorable for large-scale application, referring to J.H.He; J.Appl.Phys.102,084303 (2007).Second class methods are to carry out integrated to nano wire; People such as Yanbo Li utilize the mutual bridge joint between finger-inserting type electrode direct growth zinc oxide nanowire and the zinc oxide nanowire to realize the raising of photoresponse electric current; Referring to Yanbo Li et.al, Nanotechnology 20 (2009) 045501.For second difficulty, after having used the ultraviolet photon detector of Schottky contacts, significant improvement can be arranged, exist when still can't avoid first difficult equally.
Chinese invention patent application 201010190839.8 discloses a kind of transducer that is used for ultraviolet detection and preparation method thereof.Semiconductor transducer of the present invention is made up of two electrodes and the parallelly connected integrated zinc oxide nanowire between two electrodes.The preparation method of this semiconductor transducer of the present invention is: at first on first substrate, grow the zinc oxide nano-wire array of one deck perpendicular to substrate surface; Then zinc oxide nano-wire array is transferred to the surface of second substrate; Again with mask plate top electrode figure place glue-coated surface perpendicular to the two ends of the nano wire that orientation is arranged and the position that can cover the nano wire end sections make public, development, photoetching; Process electrode through physical method at least a conducting metal of deposition in the electrode zone that photoetching forms then; Again electrode and nano wire are peeled off from second substrate, on electrode, connected lead, obtain required device.I can reach several microamperes through its photoresponse electric current Δ of the disclosed device of this patent application of test shows.Visible from this patent application document; Prolong the length of electrode theoretically; More integrated zinc oxide nano wire possibly further improve the photoresponse current value on electrode; But in fact this way is impracticable, because receive the restriction of device size to make integrated more zinc oxide nanowire between electrode by unconfined prolongation electrode length.Should technology exist zinc oxide nanowire to be exposed to airborne deficiency for a long time equally on the other hand.
Summary of the invention
The present invention provides a kind of prior art deficiency that overcomes; Can improve the photoresponse current value by a larger margin; For example improve one even several orders of magnitude on the basis of existing technology, and can thoroughly overcome the zinc oxide nanowire that existing device exists and be exposed to semiconductor ultraviolet detection transducer of airborne deficiency and preparation method thereof for a long time.
Semiconductor ultraviolet detection transducer of the present invention is made up of substrate, the electrode and the parallelly connected integrated zinc oxide nanowire between electrode that are carried on the substrate; Electrode wherein is two electrodes that respectively are the broach shape and arrange in opposite directions; The broach of one of them electrode inserts between two broach of another electrode; Form tooth and insert shape, between two adjacent broach all parallel connection integrated zinc oxide nanowire.
In semiconductor ultraviolet detection transducer of the present invention; Electrode and above the zinc oxide nanowire with below be respectively equipped with substrate with the encapsulation sheet material; But and having at least one to be the material of ultraviolet light in substrate and the encapsulation sheet material, substrate seals with insulating cement with the edge of encapsulation sheet material.
Semiconductor ultraviolet detection transducer of the present invention is owing to adopted two electrodes that respectively are the broach shape and arrange in opposite directions; Between two broach of corresponding another electrode of insertion of each broach of one of them electrode; Form tooth and insert shape; Parallel connection is integrated with zinc oxide nanowire between two adjacent broach; This technical scheme has solved in the prior art effectively can't prolong electrode length, the deficiency of integrated more Donna rice noodles between electrode, and adopt this structure can improve the photoresponse current value when surveying greatly.On the other hand; Semiconductor ultraviolet detection transducer of the present invention electrode and above the zinc oxide nanowire with below respectively be provided with substrate with the encapsulation sheet material; And two-layer edge seals with insulating cement; Make in zinc oxide nanowire is closed in, this has just been avoided the influence of external environment to the line nanometer, the useful life of director's device greatly fully.
The preparation method of semiconductor ultraviolet detection transducer grows the zinc oxide nano-wire array of one deck perpendicular to substrate surface on substrate; Then on-chip zinc oxide nano-wire array is shifted the surface as the sheet material of substrate; And make nano wire be parallel to the surface of substrate sheet material; Perhaps prepared beforehand has the slotting mutually comb teeth shape electrode of broach on this substrate sheet material, perhaps after zinc oxide nanowire being transferred on the substrate sheet material, prepares the comb teeth shape electrode that broach is inserted mutually more above that, on two electrodes, connects lead respectively; On described substrate sheet material, cover an encapsulation sheet material then; Again the edge of substrate sheet material with the encapsulation sheet material solidified with the insulating cement sealing, obtain required device, have at least one to be the material that can see through ultraviolet light in used substrate sheet material and the encapsulation sheet material.
Specific practice of the present invention is following:
Substrate sheet surface spin coating last layer flexible polymer with clean dry is baked to and solidifies; On substrate, grow the zinc oxide nano-wire array of one deck perpendicular to substrate surface; There is the one side of zinc oxide nanowire to be covered in the one side that has flexible polymer on the substrate sheet material substrate length; On substrate and substrate film face, apply normal pressure greater than 100Pa; Along same direction substrate being slipped over simultaneously is coated in the flexible polymer surface on the substrate sheet material, zinc oxide nanowire is transferred to be coated with on the substrate sheet material of flexible polymer; Get an encapsulation sheet material and clean and dried,, with mask aligner photoresist is made public after the photoresist drying at one surface spin coating one deck photoresist; Obtaining two respectively is comb teeth shape and electrode pattern that broach is inserted mutually; On electrode pattern, form metal electrode through physics or chemical method then,, have in load on the substrate sheet material then to cover the encapsulation sheet material on the face of zinc oxide nanowire through on electrode, connecting lead behind the stripping photoresist respectively; And the metal electrode on the encapsulation sheet material is contacted with zinc oxide nanowire; On substrate sheet material and encapsulation sheet material, apply a normal pressure, make between substrate sheet material and encapsulation sheet material to be adjacent to, the substrate sheet material is sealed with insulating cement with the edge that encapsulates sheet material solidify again; Obtain required device, have at least one to be the material that can see through ultraviolet light in used substrate sheet material and the encapsulation sheet material;
Or, the substrate sheet material cleaned dry up spin coating one deck photoresist on one surface; With mask aligner photoresist is made public after the photoresist drying; Obtain two and respectively be comb teeth shape and electrode pattern that broach is inserted mutually, on electrode pattern, form metal electrode through physics or chemical method then, behind the stripping photoresist; Obtaining a load on it has the substrate sheet material of two strip electrodes, on electrode, connects lead respectively; On substrate, grow the zinc oxide nano-wire array of one deck perpendicular to substrate surface; With resulting on it growth have one deck that the one side of finger-inserting type electrode is arranged over against the load of substrate sheet material perpendicular to the substrate of the zinc oxide nano-wire array on surface; On substrate and substrate sheet material, apply normal pressure again greater than 100Pa; Make first substrate slip over the substrate sheet surface along same direction simultaneously; Zinc oxide nanowire is transferred on the substrate sheet material, and the two ends of zinc oxide nanowire are positioned on the tooth that refers to intercalative electrode; After getting clean the drying up of a slice encapsulation sheet material; Again at its surperficial spin coating last layer flexible polymer and be baked to and solidify; The one side that will be coated with flexible polymer then places on the substrate sheet material there to be on the face of zinc oxide nanowire load; On substrate sheet material and encapsulation sheet material, apply a normal pressure, make between substrate sheet material and encapsulation sheet material to be adjacent to, the substrate sheet material is sealed with insulating cement with the edge that encapsulates sheet material solidify again; Obtain required device, have at least one to be the material that can see through ultraviolet light in used substrate sheet material and the encapsulation sheet material;
Or, on substrate, grow the zinc oxide nano-wire array of one deck perpendicular to substrate surface; The substrate sheet material cleaned dry up; With the resulting substrate product face that growth has zinc oxide nanowire on it over against the substrate sheet material; On substrate and substrate sheet material, apply normal pressure again greater than 100Pa; Make substrate slip over the surface of substrate sheet material along same direction simultaneously, on-chip zinc oxide nanowire is transferred on the substrate sheet material; Load has surperficial spin coating one deck photoresist of zinc oxide nanowire on the substrate sheet material again; With mask aligner photoresist is made public after the photoresist drying, obtain two and respectively be comb teeth shape and electrode pattern that broach is inserted mutually, on electrode pattern, form metal electrode through physics or chemical method then; Behind the stripping photoresist; On electrode, connect lead respectively, get an encapsulation sheet material and be covered in the one side that the load of substrate sheet material has zinc oxide nanowire and electrode, on substrate sheet material and encapsulation sheet material, apply a normal pressure; Make between substrate sheet material and encapsulation sheet material and be adjacent to; Again the edge of substrate sheet material with the encapsulation sheet material solidified with the insulating cement sealing, obtain required device, have at least one to be the material that can pass through ultraviolet light in used substrate sheet material and the encapsulation sheet material.
The method that on substrate, grows zinc oxide nanowire that adopts among the above-mentioned described preparation method can be a chemical vapour deposition technique, also can be chemical liquid phase reaction.
A kind of preparation method of semiconductor ultraviolet detection transducer of the present invention is: spin coating one deck photoresist on the substrate sheet material; After preceding baking, at the mask aligner microscopically mask plate top electrode pattern alignment substrate sheet material is made public again; Obtain an electrode pattern that is comb teeth shape; Magnetron sputtering one deck zinc-oxide film on electrode pattern; The metal barrier of sputter one deck forming core growth above that on zinc-oxide film again, obtaining behind stripping photoresist that load has below one is to be the substrate sheet material of metal electrode above the zinc oxide, and this sheet material is adopted the sidewall orthotropic zinc oxide nano-wire array of chemical liquid phase reaction at the zinc oxide strip electrode of sheet material; And then spin coating one deck photoresist; After preceding baking, make public again with the other end of mask aligner microscope alignment zinc oxide nanowire, again through after baking and develop after obtain the electrode pattern that second is comb teeth shape, and the second broach that is the electrode of comb teeth shape is inserted into article one and is between the broach of electrode of comb teeth shape; Form the gear shaping shape; On the second electrode pattern, form metal electrode through physics or chemical method then,, obtain required device through on first and second strip electrodes, connecting lead respectively behind the stripping photoresist.
The another kind of preparation method of semiconductor ultraviolet detection transducer of the present invention is: spin coating one deck photoresist on the substrate sheet material; After preceding baking, at the mask aligner microscopically mask plate top electrode pattern alignment substrate sheet material is made public again; Obtain an electrode pattern that is comb teeth shape; Magnetron sputtering one deck zinc-oxide film on electrode pattern, again on zinc-oxide film sputter one deck not with the metal barrier of chemical liquid phase reactant reaction, obtaining behind stripping photoresist that load has below one is to be the substrate sheet material of metal electrode above the zinc oxide; This sheet material is adopted the sidewall orthotropic zinc oxide nano-wire array of chemical liquid phase reaction at the zinc oxide strip electrode of sheet material; And then spin coating one deck photoresist, after preceding baking, make public again with the other end of mask aligner microscope alignment zinc oxide nanowire, again through after baking back obtain the electrode pattern that second is comb teeth shape after developing; And the broach that second is the electrode of comb teeth shape is inserted into article one and is between the broach of electrode of comb teeth shape; Form the gear shaping shape, on the second electrode pattern, form metal electrode through physics or chemical method then, through on first and second strip electrodes, connecting lead respectively behind the stripping photoresist; Getting an encapsulation sheet material is covered in the load of substrate sheet material and has on the one side of zinc oxide nanowire and electrode; On substrate sheet material and encapsulation sheet material, apply a normal pressure, make between substrate sheet material and encapsulation sheet material to be adjacent to, the substrate sheet material is sealed with insulating cement with the edge that encapsulates sheet material solidify again; Obtain required device, have at least one to be the material that can see through ultraviolet light in used substrate sheet material and the encapsulation sheet material.
Relevant experiment shows, when adopting transducer of the present invention, the integrated quantity of semiconductor nanowires is very big in the transducer, and the photoresponse electric current can reach a milliampere magnitude, makes the detection of ultraviolet light characterize difficulty with its intensity and significantly descends.
The invention has the advantages that:
1. the ultraviolet light transducer that is made up of semiconductor nanowires of the present invention, cheap, good reproducibility has good bio-compatibility, totally nontoxic, no environment public hazards.
2. have high optical response signal intensity, can roll up owing to integrated semiconductor nanowires number simultaneously, therefore can be so that the photoresponse electric current of transducer reaches the degree that the common electrical flowmeter can be surveyed.Thereby make the cost of detector to reduce greatly.
3. semiconductor transducer preparation method of the present invention is comparatively easy, and technology is simple relatively.
Description of drawings
Accompanying drawing 1 is the zinc oxide nano-wire array ESEM vertical view of preparation.
Accompanying drawing 2 is the zinc oxide nano-wire array ESEM sectional drawing of preparation.
Accompanying drawing 3 is the zinc oxide nano-wire array X-ray diffractogram of preparation.
Accompanying drawing 4 is first kind of device preparation method's a sketch map.Among the figure: 1 is substrate, and 2 is zinc oxide nanowire, and 3 is the sheet material as substrate, and 4 is flexible polymer, and 5 is two comb teeth shape metal electrodes of inserting shape mutually for tooth, and 6 are the encapsulation sheet material.Scheme clearly visible two square each other positions of putting of electrode that are comb teeth shape by this.
Accompanying drawing 5 is second kind of device preparation method's a sketch map.Among the figure: 1 is substrate.2 is zinc oxide nanowire.3 sheet materials as substrate.4 is flexible polymer.5 is two comb teeth shape metal electrodes of inserting shape mutually for tooth.6 are the encapsulation sheet material.
Accompanying drawing 6 is the third device preparation method's a sketch map.Among the figure: 1 is substrate.2 is zinc oxide nanowire.3 is first sheet material as substrate.4 is two comb teeth shape metal electrodes of inserting shape mutually for tooth.
Accompanying drawing 7 is for for the device I-V curve, and is as shown in the figure, and device is the ohm-type contact.
Accompanying drawing 8 is the I-t curve of device, and is as shown in the figure, and when UV-irradiation, the photoresponse electric current reaches 4.4mA.
Accompanying drawing 9 is under the 3V bias voltage, the photoresponse curve of varying strength ultraviolet light.From top to bottom, ultraviolet ray intensity is followed successively by 100 μ w/cm
2, 500 μ w/cm
2, 1mw/cm
2, 1.8mw/cm
2
Accompanying drawing 11 is under the 3V bias voltage, the photoresponse curve of varying strength ultraviolet light.From top to bottom, ultraviolet ray intensity is followed successively by 100nw/cm
2, 500nw/cm
2, 1 μ w/cm
2
Accompanying drawing 12: the sketch map of the another kind of preparation process of device of the present invention.Among the figure: 1 is the sheet material of substrate, and 2 are one deck zinc-oxide film under the comb teeth shape metal electrode, and 3 is a comb teeth shape metal electrode that is made up of the crome metal barrier layer, and 4 is the zinc oxide nanowire perpendicular to 2, and 5 is another comb teeth shape metal electrode.
Embodiment
Accompanying drawing is a most preferred embodiment of the present invention, below in conjunction with the embodiment explanation:
Device architecture of the present invention can be referring to a nethermost width of cloth in accompanying drawing 4 and the accompanying drawing 5; It is to have substrate sheet material, the parallel connection of two electrodes that respectively are the broach shape and arrange in opposite directions to be integrated in the zinc oxide nanowire between each broach by: load; And the encapsulation sheet material that covers on it constitutes; Wherein: each broach of an electrode inserts between each two broach of another electrode, forms the position that tooth is inserted the shape interaction arrangement, sees Fig. 4 or Fig. 5; Zinc oxide nanowire then parallel connection is integrated between each broach; Load has the substrate sheet material of broach shape electrode and the edge that covers encapsulation sheet material on it to seal with insulating cement, and electrode, zinc oxide nanowire are closed between two sheet materials.But substrate sheet material of the present invention or encapsulation have at least one be the transparent material layer of ultraviolet light in the sheet material, and the sheet material requirement that sees through ultraviolet light of the present invention and material that can satisfy the temperature of corresponding baking in processing technology less to the absorption of ultraviolet light gets final product.The material that the present invention recommends is a sheet glass.
Below be preparation of devices method instance of the present invention and test case, the concrete liquid chemical method that is used to form zinc oxide nano-wire array that adopts is a hydro thermal method in following embodiment.
Embodiment 1:
1. at first adopt high temperature chemical vapor deposition method or hydro thermal method on substrate, to grow zinc oxide nano-wire array perpendicular to substrate; The used substrate of the present invention is a silicon chip, and the form of the zinc oxide nanowire that on substrate, grows and sign are referring to accompanying drawing 1, accompanying drawing 2 and accompanying drawing 3.
When adopting high temperature chemical vapor deposition to prepare, with the 0.81g zinc oxide that grinds and the mixture of 0.12g graphite powder, put into the reaction boat earlier, the reaction boat is put into the blind end of single radial cut sleeve pipe.Burnishing surface is cut into the small pieces of 0.5cm * 0.8cm for the silicon chip of (100) crystal face, successively use each ultrasonic cleaning 20 minutes successively of HF, acetone, absolute ethyl alcohol and distilled water, take out the back and dries up silicon chip surface, put into 175 degrees centigrade of bakings of baking oven 1 hour with nitrogen.Silicon chip is placed on from the mouth of pipe inside 1 to 5cm interval the placement, burnishing surface upwards again.The bobbin seal end is placed on the flat-temperature zone, and openend feeds 190sccm argon gas and 10sccm oxygen over against the gas approach axis; The system vacuum is to 200Pa; Begin to be warmed up to 1050 degrees centigrade from room temperature, heating rate is 50 degrees celsius/minute, and 1050 degrees centigrade are incubated 1.5 hours.Reaction naturally cools to room temperature after finishing, and on silicon chip, obtains the membranaceous product of canescence, through characterizing, is the zinc oxide nano-wire array perpendicular to silicon chip.
When adopting the Hydrothermal Growth zinc oxide nano-wire array, earlier at any substrate surface, magnetron sputtering one deck zinc-oxide film; Then substrate is put into the hexamethylenetetramine mixed liquor of 2.5mM zinc nitrate and 2.5mM; Substrate was coated with the placed face down of zinc-oxide film, is heated to 80 degrees centigrade, whenever changed reactant liquor at a distance from 2.5 hours; Reaction in 10 hours finishes, and obtains zinc oxide nano-wire array.
When adopting the Hydrothermal Growth zinc oxide nano-wire array; Also earlier at any substrate surface; Magnetron sputtering one deck zinc-oxide film is put into the 25mM zinc nitrate with substrate then, the 12.5mM hexamethylenetetramine; The 5mM molecular weight is in the mixed solution formed of 800 polymine and 0.35M ammoniacal liquor, is heated to 87.5 degrees centigrade.Whenever changed reactant liquor at a distance from 2.5 hours, reaction in 10 hours finishes, and takes out substrate, 450 degrees centigrade of calcinations 3 hours, obtains zinc oxide nano-wire array.
2. preparation zinc oxide nanowire ultraviolet light detector.
The first method of fabricate devices of the present invention is:
Get two sheets; A slice is as substrate; Another sheet (is annotated: also we can say this two sheet material substrate and encapsulation sheet material each other in the method as the encapsulation sheet material; Because wherein one piece material is the substrate of load zinc oxide nanowire, and another sheet is the encapsulation sheet material, and the latter is the substrate of load electrode).With a sheet glass, clean dry up after, at its surperficial spin coating last layer flexible polymer, sheet glass is put in 30-110 degree centigrade the baking oven, be baked to and solidify.Growth there is zinc oxide nanowire silicon chip product face over against the glass sheet surface that is coated with flexible polymer; And apply a certain size normal pressure (being generally normal pressure) greater than 100Pa; Along same direction silicon chip is slipped over simultaneously and be coated in the flexible polymer surface on the sheet glass; Flexible polymer and nano-wire array produce shearing force in this process; Zinc oxide nanowire is transferred to be coated with on the sheet glass of flexible polymer, after the friction, that the flexible polymer surface on sheet glass obtains lying low and almost parallel each other nano wire.
An other sheets cleaned dry up, at glass sheet surface spin coating one deck photoresist, the photoresist spinner rotating speed from slow to fast, final rotating speed is 3000 rev/mins, keeps this rotating speed 60 seconds.Baking is 40 minutes before subsequently in 90 degrees centigrade of baking ovens; With mask aligner photoresist is made public then, obtain electrode pattern, temperature is heightened after 110 degrees centigrade dried by the fire 30 minutes again; Obtain litho pattern after the development; Through two aluminium electrodes of magnetron sputtering sputter, after peeling off, obtain the sheet glass that a load has two finger-inserting type aluminium electrodes then.
The one side that then load on the sheet glass is had zinc oxide nanowire, load has the one side of aluminium electrode on the other sheets, under the static relatively situation of two sheets, applies a normal pressure, and two sheets are adjacent to.Keeping under the situation of pressure,,, after the curing, remove pressure with the glue encapsulation at the edge of two sheets.
Above preparation process is referring to accompanying drawing 4.
The second method of fabricate devices of the present invention is:
With a sheets clean dry up after, at its surperficial spin coating last layer flexible polymer, sheet glass is put in 30-110 degree centigrade the baking oven, be baked to and solidify.
An other sheets cleaned dry up, at glass sheet surface spin coating one deck photoresist, the photoresist spinner rotating speed from slow to fast, final rotating speed is 3000 rev/mins, keeps this rotating speed 60 seconds.Baking is 40 minutes before subsequently in 90 degrees centigrade of baking ovens; With mask aligner photoresist is made public then, obtain electrode pattern, temperature is heightened after 110 degrees centigrade dried by the fire 30 minutes again; Obtain litho pattern after the development; Through two aluminium electrodes of magnetron sputtering sputter, after peeling off, obtain the sheet glass that a load has two finger-inserting type aluminium electrodes then.The glass sheet surface that silicon chip product face is had the finger-inserting type electrode over against load; And apply a certain size normal pressure, and be generally normal pressure greater than 100Pa, make silicon chip slip over glass sheet surface along same direction simultaneously; In this process, produce shearing force between sheet glass and nano-wire array; Zinc oxide nanowire is transferred on the electrode, after the friction on electricity level obtain lying low and almost parallel each other nano wire, nano wire axially becomes 90 to spend angles with the comb-tooth-like portion of electrode.
The one side that then load on the sheet glass is had zinc oxide nanowire is coated with the one side of flexible polymer on the other sheets, under the static relatively situation of two sheets, applies a normal pressure, and two sheets are adjacent to.Keeping under the situation of pressure,,, after the curing, remove pressure with the glue encapsulation at the edge of two sheets.
Above preparation process is referring to accompanying drawing 5.
The third method of fabricate devices of the present invention is:
With a sheets clean dry up after; Silicon chip product face over against sheet glass, and is applied a certain size normal pressure, be generally normal pressure greater than 100Pa; Make silicon chip slip over glass sheet surface along same direction simultaneously; In this process, produce shearing force between sheet glass and silicon chip, zinc oxide nanowire is transferred on the sheet glass, obtaining lying low on sheet glass and almost parallel each other nano wire in glass sheet surface after the friction.Spin coating one deck photoresist on this sheet glass, photoresist spinner rotating speed from slow to fast, final rotating speed is 3000 rev/mins, keeps this rotating speed 60 seconds.Baking is 40 minutes before subsequently in 90 degrees centigrade of baking ovens; At the mask aligner microscopically made public perpendicular to the nano wire that orientation is arranged in mask plate top electrode pattern alignment sheet glass upper edge then, obtain electrode pattern, temperature is heightened after 110 degrees centigrade dried by the fire 30 minutes again; Obtain finger-inserting type electrode litho pattern after the development; Through two aluminium electrodes of magnetron sputtering sputter, after peeling off, obtain the ultraviolet light detector that nano wire and electrode are ohmic contact then.Whole process of preparation is referring to seeing accompanying drawing 6.
3. the test of device
Device with the present invention's preparation is surveyed ultraviolet light as detector.Adding under the 3V bias voltage, letting ultraviolet lighting be mapped on the detector, recording photoresponse electric current Δ I, its measured value is about 12mA.Can know by this instance; The zinc oxide nanowire integrated level is very big in the device of the present invention; Make device have high ultraviolet response, its measured value can break away from accurate measuring instrument fully, uses common current measurement just can realize the detection of ultraviolet photon.Measured result is seen accompanying drawing 7 and Fig. 8.Can reach 4.4 milliamperes by the visible device photoresponse electric current of the present invention of figure.
Under the 3V bias voltage, with shining ultraviolet ray intensity on this detector from 100nw/cm
2To 1.8mw/cm
2Change, obtained excursion from 2 μ A to 4.4mA, and with intensity photoresponse electric current one to one..Ultraviolet ray intensity is demarcated with commercial ultraviolet light detector respectively, is respectively 100nw/cm
2, 500nw/cm
2, 1 μ w/cm
2, 5 μ w/cm
2, 10 μ w/cm
2, 50 μ w/cm
2, 100 μ w/cm
2, 500 μ w/cm
2, 1mw/cm
2, 1.8mw/cm
2Measured result is seen accompanying drawing 8,9 and 10.
Embodiment 2: the preparation of the height response ultraviolet light transducer of non-close press seal dress ohmic contact
On sheet glass, spin coating one deck photoresist, photoresist spinner rotating speed from slow to fast, final rotating speed is 3000 rev/mins, keeps this rotating speed 60 seconds.Baking is 40 minutes before subsequently in 90 degrees centigrade of baking ovens; At the mask aligner microscopically mask plate top electrode pattern alignment sheet glass is made public then; Dried by the fire 30 minutes the back under 110 degrees centigrade then, and making width after the development is half litho pattern of the finger-inserting type electrode of 10 μ m.Magnetron sputtering one deck zinc-oxide film, thickness greatly between 300～4000nm, on zinc-oxide film again sputter one deck chromium barrier layer (can also be not with Zn (NO
3)
2Other metals with the HMTA reaction), thickness is about 10～100nm.Obtain after peeling off below one is to be the broach shape electrode of Cr above the zinc oxide.
It is 2.5mmol/L Zn (NO that sheet glass is put into concentration
3)
2In the mixed-culture medium of 2.5mmol/L HMTA; Sheet glass is fixed with the plastics holder, and facing down of figure arranged, in the floating immersion nutrient solution; (60～100 degrees centigrade) reaction is 5～12 hours under certain reaction temperature, obtains at the orthotropic zinc oxide nano-wire array of zinc oxide strip electrode sidewall.
And then spin coating one deck photoresist, the photoresist spinner rotating speed from slow to fast, final rotating speed is 3000 rev/mins, keeps this rotating speed 60 seconds.Baking is 40 minutes before subsequently in 90 degrees centigrade of baking ovens; Make public with the other end of mask aligner microscope alignment zinc oxide nanowire, temperature is heightened after 110 degrees centigrade dried by the fire 30 minutes again, obtain litho pattern after the development; Obtain the detector of ohmic contact if desired; Then can aluminium electrode of sputter, to peel off the back and on electrode, connect lead, transducer promptly prepares completion.Whole process of preparation is referring to accompanying drawing 12.
Claims (10)
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| CN103441180A (en) * | 2013-08-21 | 2013-12-11 | 中国石油大学(北京) | Nanometer wire ultraviolet light detector and preparing method and application thereof |
| WO2015081665A1 (en) * | 2013-12-06 | 2015-06-11 | 纳米新能源（唐山）有限责任公司 | Zinc oxide nano structure based sensor and preparation method thereof |
| CN104701404B (en) * | 2013-12-06 | 2017-06-16 | 纳米新能源（唐山）有限责任公司 | Ultraviolet light sensor based on nano structure of zinc oxide and preparation method thereof |
| CN103868951B (en) * | 2014-02-24 | 2016-12-07 | 北京大学 | A kind of method of dry process nano-wire array gas sensor |
| CN104779314B (en) * | 2014-06-27 | 2017-02-08 | 纳米新能源（唐山）有限责任公司 | Ultraviolet photosensitive sensor based on zinc oxide and preparation method of ultraviolet photosensitive sensor |
| US9865766B2 (en) | 2015-07-28 | 2018-01-09 | Carrier Corporation | Ultraviolet photodetectors and methods of making ultraviolet photodetectors |
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| US9806125B2 (en) | 2015-07-28 | 2017-10-31 | Carrier Corporation | Compositionally graded photodetectors |
| US10126165B2 (en) | 2015-07-28 | 2018-11-13 | Carrier Corporation | Radiation sensors |
| US10336017B2 (en) * | 2016-06-30 | 2019-07-02 | Boeing Company, The | Microwire array devices and methods for fabricating polymeric sheets containing microwires |
| CN106054425B (en) * | 2016-08-03 | 2019-07-23 | 深圳市华星光电技术有限公司 | The preparation method of display panel and display panel |
| CN107359170A (en) * | 2017-06-19 | 2017-11-17 | 北京邮电大学 | A kind of ultraviolet detector array structure based on interdigital electrode |
| CN108183138A (en) * | 2017-12-15 | 2018-06-19 | 中山大学 | A kind of photoelectric device based on two-dimentional micro belt and preparation method thereof |
| CN108493268B (en) * | 2018-04-28 | 2019-10-01 | 西安交通大学 | A kind of diamond ultraviolet detector three-diemsnional electrode structure and preparation method thereof |
| CN113130683B (en) * | 2021-04-15 | 2022-11-22 | 北京工业大学 | A high-speed and high-sensitivity ZnO nanowire array radio frequency ultraviolet detector |
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