CN101476111A - Transparent conductive film and preparation thereof - Google Patents
Transparent conductive film and preparation thereof Download PDFInfo
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- CN101476111A CN101476111A CNA2009100605766A CN200910060576A CN101476111A CN 101476111 A CN101476111 A CN 101476111A CN A2009100605766 A CNA2009100605766 A CN A2009100605766A CN 200910060576 A CN200910060576 A CN 200910060576A CN 101476111 A CN101476111 A CN 101476111A
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Abstract
The invention relates to a composite transparent conductive film of a indium tin aluminum zinc oxide which has characteristics that an indium tin alloy target and metal adulterating zinc oxide conductive ceramics form a composite target by using magnetic control sputter technique, wherein, component of the indium tin alloy target is In90%wt and Sn10%wt. The transparent conductive film of the indium tin aluminum zinc oxide can be prepared by sputter in room temperature. The technique has advantages that a base piece needs not to be heated; the film can deposit with large area; an electrode has better electrical conductivity; the film has better light transmission; the film can be prepared on a flexible underlay; the film surface has better planeness and stabile electricity capability. The technique is suitable for preparing the transparent electrode such as various field effect transistor, thin-film solar cell, thin-film luminescent device, other photoelectron device and electronic device with poor high temperature tolerance.
Description
Technical field
The present invention relates to that a kind of (InSn In/Sn=9/1wt%) and the transparent conductive film that makes of metal doped zinc oxide conductivity ceramics reaction cosputtering and preparation method thereof, had both belonged to the thin-film material field, also belonged to optical device, field of electronic devices by indium stannum alloy.
Background technology
Transparent conductive film is with its electric conductivity near metal, high-transmission rate in the visible-range, infrared high reflectance with and characteristic of semiconductor, be widely used in the window of solar cell, indicating meter, luminescent device, gas sensor, antistatic coating and semiconductor/insulator/semi-conductor (SIS) heterojunction, modern opportunity of combat and cruise missile etc.The electrode materials that needs high conductivity in a lot of indicating meters to reduce driving voltage and power consumption, improves the homogeneity of response resume speed and display device.The kind of transparent conductive film has a lot, but sull is occupied an leading position.The sull of mainly being studied has at present: tindioxide (SnO
2) base film, indium trioxide (In
2O
3) base film and zinc oxide (ZnO) base film.In these several oxide semiconductor thin-films, In
2O
3Base is (as In
2O
3: Sn) film and SnO
2Base is (as SnO
2: F) film all exists poisonous, cost than problems such as height.
The zno-based film not only has with above sull comparable electricity and optical characteristics, and it is with low cost, nontoxic, be easy to big area production, more stable in hydrogen plasma, make it become the more favourable replacer of above-mentioned film.
Adopt two discrete ITO (indium tin oxide), AZO (Al-Doped ZnO pottery) target, target radio frequency (direct current) sputtering technology is prepared the existing report of laminated film of electrically conducting transparent.But adopt the target sputtering technology is not suitable for the depositing large-area film.
Wherein, adopt InSn-AZO Planar Compound target, indium tin aluminium zinc oxide (ITAZO) film that preparation has high conductivity yet there are no report.
Summary of the invention
For reducing the usage quantity of rare metal In, guarantee its conduction and light transmission simultaneously, the invention provides a kind of method for preparing the ITAZO transparent conductive film based on InSn/AZO composition target technology.But the transparent conductive film of preparation has advantages such as good conductivity, transmittance height normal temperature deposition.
Technical scheme of the present invention is: a kind of transparent conductive film, it is characterized in that: form composition target by indium tin (InSn) alloys target and aluminium-doped zinc oxide (AZO) conductivity ceramics, adopt the magnetron sputtering technique cosputtering to form, the structure of described composition target is the aura district (sputtering zone) that the aluminium-doped zinc oxide conductivity ceramics is placed the indium stannum alloy target, wherein, conductivity ceramics is 5～10% with the area ratio of indium stannum alloy target.
Described indium tin (InSn) alloys target consist of In90wt% and Sn10wt%.
Described aluminium-doped zinc oxide conductivity ceramics is to take by weighing ZnO powder and Al according to Zn/Al atomic ratio 97:3
2O
3Powder, 1400 ℃ of following sintering made in 5 hours.
Described aluminium-doped zinc oxide (AZO) conductivity ceramics can use dysprosium doping zinc-oxide (DZO), yttrium doping zinc-oxide (YZO), Ga-doped zinc oxide (GZO) or indium doping zinc-oxide (IZO) conductivity ceramics to replace.
Above-mentioned film is to prepare on simple glass, silica glass or transparent plastic substrate, and wherein, described transparent plastics is PET or PI.
The preparation method of described transparent conductive film is characterized in that: adopt the magnetically controlled sputter method preparation, reaction conditions is as follows:
(1) the base vacuum degree 3 * 10
-3～1 * 10
-4Pa;
(2) operating air pressure 0.1～1.0Pa;
(3) sputtering power is 80～120W;
(4) sputtering pressure 0.1-1Pa;
(5) sputter temperature is 0～35 ℃;
(6) sputter O
2/ (Ar+O
2) throughput ratio is 14～22%.
Preparation method provided by the invention can prepare the ITAZO compound transparent electricity conductive film on substrates such as flexiplast.Prepared film can be used as the electrode materials of preparation solar cell, and the compound thin-film solar cells performance of prepared organic-inorganic can compare favourably as the Solar cell performance of electrode materials preparation with the ITO that adopts commerce, FTO film.
The advantage of this technology is: substrate does not need heating; But film big area deposition; Electrode conductivuty is good; Light transmission is preferably arranged; Can on flexible substrate, prepare; Film surface has good planeness and stable electrical properties.And this technology is applicable to the transparency electrode preparation of the relatively poor opto-electronic device of various field-effect transistors, thin-film solar cells, thin-film light emitting device and other high temperature tolerances, electron device.
Embodiment
The preparation of 1 target:
(1) takes by weighing ZnO powder (97at%, purity is 99.99%) and Al according to Zn/Al atomic ratio 97:3
2O
3Powder (3at%, purity is 99.99%).
(2) these two kinds of mixed powders are poured in the sealed can that an amount of agate ball is housed, poured into an amount of acetone or ethanol, be placed on and carry out ball milling on the ball mill, the ball milling time is 12 hours.The purpose of ball milling is by two: at first be for ZnO and Al
2O
3Powder mixes is even, with the homogeneity of the target that guarantees to prepare; Secondly, be for powder fining, be beneficial to the moulding and the sintering of mixed powder subsequently.
(3) after ball milling finishes, with powder pressing forming.The block that suppresses is that diameter is 8mm, and thickness is the disk of 1mm.
(4) block that suppresses is carried out sintering, sintering temperature is 1400 ℃, and the time is 5 hours, and AZO (ZnO:Al) ceramic target has just completed like this.
(5) preparation technology of DZO, YZO, GZO, IZO, ZnO pottery is the same.
2 substrate processing:
The substrate that adopts in the test is simple glass (wave carrier piece) and silica glass, before test substrate is cleaned.At first sheet glass is cut into suitable shape size, putting in the potassium bichromate washing lotion soaks more than 24 hours again, with deionized water glass surface is rinsed well then, place it in again and use alcohol on the ultrasonic cleaner successively, each ultrasonic cleaning of acetone 10 minutes dries up the glass substrate that can obtain surface cleaning with deionized water rinsing at last.
3 thin film deposition processes processes:
(1) target and clean glass substrate are put into the corresponding position of sediment chamber, adjusted the specimen holder position, make it to aim at, and keep the distance of about 5cm with target surface.Adopt general plane magnetic control reactive sputtering process.The structure of composition target as shown in Figure 1.The diameter of InSn alloys target is 50mm, and AZO conduction block (little first sheet) evenly is placed on the aura district of InSn alloys target.
(2) vacuum system is vacuumized.At first open water coolant.Open mechanical pump and take out rough vacuum, after the system vacuum degree is lower than 10Pa, open the molecular pump pumping high vacuum, reach more than the 10-3Pa until the system vacuum degree.
(3) in the sediment chamber, feed an amount of gas, make air pressure reach required deposition pressure.
(4) high-purity Ar and O
2Gas is respectively as sputter and reactant gases.The flow-ratio control of oxygen in the whole process/(oxygen+argon gas) is 14～22%.During sputter sputtering pressure is controlled at (1 * 10
-1Pa-1.0Pa), sputtering power (80-120W), underlayer temperature (0-35 ℃), deposition finishes, and treats to take out behind the sample naturally cooling.
By AZO/InSn area ratio in the modulation target, the content ratio of the In in the may command film, Sn, Al, Zn.In order to study of the influence of each experiment parameter, and obtain optimum growth parameter(s), change various processing parameters and carry out a series of experiments the ITAZO film characteristics.By depositing time control film thickness, depend on area fraction and the sputtering power of AZO in the target, the film thickness that obtains is between between the 200nm to 400nm.
(5) after thin film deposition is finished, close shielding power supply.
(6) close the substrate heating power supply, allow substrate reduce to room temperature naturally with furnace temperature.Close slide valve, close valve and all gas circuit valves of gas cylinder.The closure molecule pump, the molecular pump speed drop is closed mechanical pump again after zero.
4 material properties tests:
For electric property and the optical property of estimating the ITAZO film, film has been carried out a series of test from electricity and optics equal angles:
(1) the UV, visible light photothermal spectroscopic analyzer is measured with the Cary 5000 of VARIAN company;
(2) resistivity of usefulness vanderburg method MEASUREMENTS OF THIN, carrier concentration and Hall coefficient;
(3) film thickness is measured with the FORM TALYSURF SERLES II of Taylor Hoboson Precision company.
Because the present invention prepares composite transparent conductive film with InSn-AZO composition target cosputtering, can realize the preparation of big area pipeline system, reduce the content of In as much as possible, thereby reduced cost.Realized that simultaneously normal temperature prepares the ITAZO compound transparent electricity conductive film on the flexible transparent plastic substrate, the performance of the ITO of resulting film and commercial usefulness, FTO film can match in excellence or beauty.Therefore, aspect photoelectricity,, has the potential using value as aspects such as solar cell (as shown in Figure 2), information display, thin film transistor, semiconductor laser and LED.
Description of drawings
Accompanying drawing 2 adopts the J-V curve of the ITAZO film of prepared of the present invention as the organic solar batteries (ITAZO/PEDOT:PSS/P3HT:PCBM/A1) of electrode preparation.
Specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described in further detail.
As shown in Figure 1, provided by the invention based on the preparation of InSn-doping zinc-oxide composition target reaction cosputtering Indium tin aluminium zinc oxide composite transparent conductive film.
Embodiment 1:
Below to change one of parameter among the preparation technology: power illustrates preparation process as example.
(1) clean sheet glass and PET: used substrate has two kinds in this example, and one is 2cm * 2cm * 1mm Slide, it two is the transparent plastic substrate of 3cm * 2cm * 0.1mm. The cleaning step of slide For: earlier slide is put into the solution that fills cleaning agent and soaked 10 minutes, clear after repeatedly cleaning then Water rinses; Then carry out polishing with polishing powder; Put into respectively then acetone and alcohol are housed Priority is ultrasonic 20 minutes in the vessel; Put at last behind twice of the deionized water rinsing ultrasonic 10 minutes again into, Dry up with nitrogen gun and to get final product. The plastic supporting base cleaning step: similar with the glass slide cleaning step, earlier with cleaning Ji is cleaned, and is rear with alcohol and ultrasonic 10 minutes (without acetone) of deionized water difference, last nitrogen gun Dry up and put into baking oven 80 degree oven dry.
(2) preparation of ITAZO composite membrane in the situation that changes sputtering power: with the composition target that will use (InSn+AZO, the Area Ratio of AZO conductivity ceramics and indium stannum alloy target is 10%) and substrate are packed into In the magnetron sputtering apparatus, carry out sputter with radio-frequency power supply. Condition of work is: base vacuum: 1 * 10-3
Pa；O
2/(Ar+O
2)=18%; Underlayer temperature: 20 ℃; Sputtering pressure: 0.5Pa; Power is at 80W Change to the 120W scope, stepping 10W, sputtering time changes to protect with the variation of power It is consistent demonstrate,proving each on-chip thickness.
(3) quality of forming film explanation: the film of making take 80W--12min is as example, and thickness is 320nm, and sheet resistance is 259 Ω/sq., the average transmittance between the 420nm-800nm are 89.6%. Become with 120W-4min Film is example, and thickness is 318nm, and sheet resistance is 6.16k Ω/sq., between the 420nm-800nm average thoroughly The light rate is 54.3%. In 80W to 120W excursion, take 90W as best power, its one-tenth The film parameter is: thickness is 300nm, and sheet resistance is 26.4 Ω/sq., and resistivity is 8.8 * 10-4Ω .cm, Average transmittance between the 420nm-800nm is 87.5%.
(4) the ITAZO film of the sputtering power preparation of employing 90W is as the organic solar batteries of electrode preparation (ITAZO/PEDOT:PSS/P3HT:PCBM/A1), adopt simultaneously commercial ito thin film as electricity The utmost point prepares organic solar batteries under the same conditions (ITO/PEDOT:PSS/P3HT:PCBM/A1). Get rid of 10 nanometers at ITO and ITAZO PEDOT:PSS gets rid of the P3HT:PCBM of 100 nanometers again. Again excellent on P3HT:PCBM In 10-3Evaporation aluminium electrode 200nm under the Pa vacuum. Record the J-V curve of battery as shown in Figure 2.
Embodiment 2:
Below to change one of parameter among the preparation technology: oxygen content illustrates preparation process as example.
(1) cleans: with example one. Substrate (substrate) is slide.
(2) preparation of ITAZO composite membrane in the situation that changes oxygen content: with the composition target that will use ((InSn+AZO, the Area Ratio of AZO conductivity ceramics and indium stannum alloy target is 10%)) and the substrate magnetic of packing into In the control sputtering equipment, carry out sputter with radio-frequency power supply. Condition of work is: base vacuum: 1 * 10-3Pa, Sputtering power: 90W, underlayer temperature: 23 ℃, sputtering pressure: 0.5Pa, oxygen content 14% to 22% scope changes, stepping 2%, and the variation that sputtering time is pressed with oxygen changes to guarantee each substrate On thickness be consistent.
(3) quality of forming film explanation: the film of making take 14%O--2min is as example, and thickness is 318nm, and sheet resistance is 2.95k Ω/sq., the average transmittance between the 420nm-800nm are 54.3%. With 22% O2-15min film forming is example, and thickness is 318nm, and sheet resistance is greater than 107Ω/sq., the average printing opacity between the 420nm-800nm Rate is 98.6%. Press from 14% to 22% excursion at oxygen, press to best its film forming take 18% oxygen Parameter is: thickness is 315nm, and sheet resistance is 30 Ω/sq., the average transmittance between the 420nm-800nm Be 86.8%.
Embodiment 3:
Below to change one of parameter among the preparation technology: the time illustrates preparation process as example.
(1) clean: the quartz glass substrate, clean with example one.
(2) preparation of ITAZO composite membrane in the situation that changes sputtering time: with the composition target that will use (InSn+AZO, the Area Ratio of AZO conductivity ceramics and indium stannum alloy target is 10%) and the substrate magnetic control of packing into In the sputtering equipment, with the sputter of radio-frequency power supply reason row. Condition of work is: base vacuum: 1 * 10-3Pa spatters Penetrate power: 90W, underlayer temperature: 0 ℃, sputtering pressure: 0.5Pa, oxygen content: 18%, sputter Time changes from 4min to 12min, stepping 2min. The thickness time to time change of film forming.
(3) quality of forming film explanation: 4min:150 Ω/square, the average transmittance 90% between the 420nm-800nm; 6min:90 Ω/square, the average transmittance 89% between the 420nm-800nm; 8min:80 Ω/square, Average transmittance 88% between the 420nm-800nm; 10min:50 Ω/square, 420nm-800nm Between average transmittance 87%; 12min:30 Ω/square, the average printing opacity between the 420nm-800nm Rate 86%.
Embodiment 4:
Below to change one of parameter among the preparation technology: the time illustrates preparation process as example.
1. clean: with example one. Substrate (substrate) is slide.
2. (InSn+DZO, the Area Ratio of DZO conductivity ceramics and indium stannum alloy target is with the composition target that will use 8%) and substrate pack in the magnetron sputtering apparatus, with the sputter of radio-frequency power supply reason row. Condition of work is: background Vacuum: 5 * 10-4Pa, sputtering power: 90W, underlayer temperature: 35 ℃, sputtering pressure: 1Pa, oxygen Gas content: 18%, sputtering time changes from 4min to 12min, stepping 2min. The thickness of film forming with Time and changing.
3. quality of forming film explanation: 4min: square resistance 140 Ω/square, the average transmittance 90% between the 420nm-800nm; 10min: square resistance 30 Ω/square, the average transmittance 87%. between the 420nm-800nm
Embodiment 5:
1. clean: with example one.Substrate (substrate) is a slide glass.
2. the composition target (InSn+GZO, the GZO conductivity ceramics is 10% with the area ratio of indium stannum alloy target) that will use and substrate are packed in the magnetron sputtering equipment, with the sputter of radio-frequency power supply reason row.Working conditions is: base vacuum: 3 * 10
-3Pa, sputtering power: 90W; Underlayer temperature: 23 ℃, sputtering pressure: 0.1Pa, oxygen content: 18%, sputtering time 12min.
3. quality of forming film explanation: 12min:30 Ω/square, the average transmittance 88% between the 420nm-800nm.
Embodiment 6:
1. clean: with example one.Substrate (substrate) is a slide glass.
2. the composition target (InSn+ZnO, the ZnO pottery is 8% with the area ratio of indium stannum alloy target) that will use and substrate are packed in the magnetron sputtering equipment, carry out sputter with radio-frequency power supply.Working conditions is: base vacuum: 1 * 10
-3Pa, sputtering power: 90W, underlayer temperature: 30 ℃, sputtering pressure: 0.5Pa, oxygen content: 18%, sputtering time 10min.
3. quality of forming film explanation: square resistance 80 Ω/square, the average transmittance 90% between the 420nm-800nm.
Embodiment 7:
1. clean: with example one.Substrate (substrate) is a slide glass.
2. the composition target (InSn+AZO+DZO, the AZO+DZO conductivity ceramics is 5% with the area ratio of indium stannum alloy target) that will use and substrate are packed in the magnetron sputtering equipment, carry out sputter with radio-frequency power supply.Working conditions is: base vacuum: 1 * 10
-4Pa, sputtering power: 90W, underlayer temperature: 23 ℃, sputtering pressure: 0.5Pa, oxygen content: 18%, sputtering time 12min.
3. quality of forming film explanation: square resistance 32 Ω/square, the average transmittance 89% between the 420nm-800nm.
Claims (6)
1. transparent conductive film, it is characterized in that: form composition target by indium stannum alloy target and aluminium-doped zinc oxide conductivity ceramics, adopt the magnetron sputtering technique cosputtering to form, the structure of described composition target is the aura district that the aluminium-doped zinc oxide conductivity ceramics is placed the indium stannum alloy target, wherein, conductivity ceramics is 5～10% with the area ratio of indium stannum alloy target.
2. transparent conductive film as claimed in claim 1 is characterized in that: described indium stannum alloy target consist of In90wt% and Sn10wt%.
3. transparent conductive film as claimed in claim 1 or 2 is characterized in that: described aluminium-doped zinc oxide conductivity ceramics is to take by weighing ZnO powder and Al at 97: 3 according to the Zn/Al atomic ratio
2O
3Powder, 1400 ℃ of following sintering made in 5 hours.
4. transparent conductive film as claimed in claim 1 or 2 is characterized in that: described aluminium-doped zinc oxide conductivity ceramics can use dysprosium doping zinc-oxide, yttrium doping zinc-oxide, Ga-doped zinc oxide or indium doping zinc-oxide conductivity ceramics to replace.
5. transparent conductive film as claimed in claim 3 is characterized in that: described film is to prepare on simple glass, silica glass or transparent plastic substrate, and wherein, described transparent plastics is PET or PI.
6. the preparation method of a transparent conductive film as claimed in claim 1 is characterized in that: adopt the magnetically controlled sputter method preparation, reaction conditions is as follows:
(1) the base vacuum degree 3 * 10
-3～1 * 10
-4Pa;
(2) operating air pressure 0.1～1.0Pa;
(3) sputtering power is 80～120W;
(4) sputtering pressure 0.1-1Pa;
(5) sputter temperature is 0～35 ℃;
(6) sputter O
2/ (Ar+O
2) throughput ratio is 14～22%.
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|---|---|---|---|
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|---|---|---|---|
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