CN1718840A - Preparation method of gallium adulterated zinc oxide transparent conductive film - Google Patents
Preparation method of gallium adulterated zinc oxide transparent conductive film Download PDFInfo
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- CN1718840A CN1718840A CN 200510043865 CN200510043865A CN1718840A CN 1718840 A CN1718840 A CN 1718840A CN 200510043865 CN200510043865 CN 200510043865 CN 200510043865 A CN200510043865 A CN 200510043865A CN 1718840 A CN1718840 A CN 1718840A
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Abstract
A process for preparing the electrically conductive transparent film of Ga doped zinc oxide used for photoelectronic devices includes such steps as providing ZnO film and doping Ga in the ZnO film by magnetically controlled bias RF sputter to prepare said ZnO:Ga film. The ceramic target for sputter is composed of ZnO and Ga2O3. The sputtering parameters are also disclosed.
Description
(1) technical field
The present invention relates to the preparation method of the adulterated electrically conducting transparent oxide film of a kind of gallium, belong to the optoelectronic information technical field of function materials.
(2) background technology
The oxidic transparent conducting film is important optoelectronic information material, and this thin-film material not only has very high transmitance at visible region, and has very high reflectivity at infrared region, and its specific conductivity is near the numerical value of metal.Nesa coating is mainly used in: the transparency electrode of thin film solar cell, flat-panel monitor and luminescent device, the window well heater of infra-red heat reflective film, touch sensitive overlays and aircraft etc.
The problem of current nesa coating commonly used and existence is as follows:
(1) tin-doped indium oxide (ITO) film is current most popular nesa coating, fields such as main using planar demonstration.There is the problem of indium diffusion during as the transparency electrode of photoelectric device in ITO.The diffusion of indium can influence the performance of device, particularly causes the decay of thin film solar cell performance.People prepare blocking layer or buffer layer on ito thin film, to improve the performance of device.Indium is a noble metal, so the ito thin film cost is higher.
(2) aluminium-doped zinc oxide (ZnO:Al) nesa coating photoelectric properties are good.With ITO and SnO
2Compare, ZnO film has better stability in plasma body, and low price.Yet the atomic radius of aluminum and zinc differs bigger, can cause lattice distortion during heavy doping, influences the photoelectric property of nesa coating.
(3) stannic oxide (SnO
2) film is to obtain the commercial transparent conductive material that uses the earliest.This film photoelectric excellent property, stability is high, has extremely strong erosion resistance.The subject matter that exists is that film is difficult to etching, has therefore limited the range of application of electrically conducting transparent stannic oxide film.In addition, SnO
2Film-forming temperature higher relatively, on the organic materials substrate, be not easy to obtain high-quality transparent conductive film.
Compare the ordination number that ZnO:Ga has significant advantage: Ga (ordination number 31) and Zn (30) with the ZnO:Al film and only differ 1, atomic radius is more or less the same, and the bond distance of Ga-O key and Zn-O key is also very approaching, be respectively 1.92 and 1.97 , therefore even under than higher doping content situation, the lattice distortion of ZnO is also very little.In addition, in the developmental process of film, aluminium shows very high reactivity, oxidation easily, and gallium is not easy oxidation with respect to aluminium, and this is gallium another advantage as doping agent.
Nesa coating with respect to rigid substrate, organic film substrate nesa coating has many distinct advantages, for example can around bent, in light weight, shock-resistant, be easy to big area production, to be convenient to transportation and facility investment few etc., thereby be widely used in organic electro-optic device, plastic liquid crystal indicating meter, transparency electromagnetic wave shield material and folding hot mirror etc.Because the hot ability to bear of organic materials substrate is poor, need sputter prepare the ZnO:Ga film under lower underlayer temperature, but low excessively preparation temperature is unfavorable for film growth.
(3) summary of the invention
The present invention is directed to organic semiconductor device, plastic liquid crystal indicating meter etc. needs low temperature to prepare the requirement of nesa coating, a kind of preparation method of gallium adulterated zinc oxide transparent conductive film is proposed, room temperature preparation gallium adulterated zinc oxide transparent conductive film on the organic polymer substrate, prepared material photoelectric properties are good, stability is high, and adhesion property is good, and price is low and nontoxic simultaneously, range of application is big, has a extensive future.
Gallium of the present invention is mixed the preparation method of zinc oxide transparent conductive film, be in ZnO film, to carry out gallium to mix, under vacuum condition, room temperature preparation goes out to have the ZnO:Ga nesa coating of polycrystalline structure on the organic polymer thin film substrate with the bias voltage radiofrequency magnetron sputtering technology.Sputter is as follows with the ceramic target component, is a mole deal:
1 part in zinc oxide,
0.01～0.08 part of Gallium trioxide.
Processing condition are: partial pressure of ar gas 0.5-5Pa, and sputtering power 50-200W, sputtering bias-voltage 0～-100V.
It is one of following that above-mentioned organic polymer thin film substrate is selected from: polypropylene second diester (Polypropylene adipate, abbreviation PPA) substrate, polyethylene terephthaldehyde ester (Polyethylene terephthalate is called for short PET) substrate, polypropylene (Polypropylene) or polyimide (Polyimide).
Above-mentioned sputter with each component raw material of ceramic target by mechanically mixing evenly after, be pressed into embryo, generate ceramic target through 1100～1250 ℃ of high temperature sinterings.
Above-mentioned sputter is preferably as follows with the component of ceramic target, is a mole deal:
1 part in zinc oxide, 0.03 part of Gallium trioxide.
The room temperature preparation processing condition of above-mentioned ZnO:Ga nesa coating are preferably:
Argon partial pressure 1Pa, sputtering power 150W, bias voltage-75V.
In order to reduce ZnO:Ga film growth temperature, improve film quality, the present invention adopts the bias sputtering technology.On substrate, use the film that negative bias can attract the positively charged ion bombardment in the plasma body growing, and this bombardment provides an additional energy for the molecule on the substrate and cluster, the molecule that bonding in the film is more weak peels off in film, and what stay in film then is the strong molecule of bonding.
Under preferred processing condition, the carrier concentration that makes film is 1.2 * 10
21Cm
-3, mobility is 13.5cm2V
-1S
-1, resistivity is 4.6 * 10
-4Ω cm, square resistance 6.2 Ω/mouths, the transmitance of visible-range surpasses 83%.The influence of deduction organic materials substrate, the average transmittances of film can reach 90% in visible-range.Performance is better than the ZnO:Al film, therefore can substitute existing electrically conducting transparent mould material in fields such as organic flat pannel display and organic optoelectronic devices.
It is as follows that the ZnO:Ga nesa coating of the inventive method preparation and existing nesa coating are compared excellent results:
1, under identical doping content situation, the lattice distortion of ZnO:Ga film is littler than ZnO:Al.
2, gallium is not easy oxidation with respect to aluminium, and therefore under identical doping content situation, ZnO:Ga is higher than ZnO:Al doping efficiency, so carrier concentration is higher.
3, under identical underlayer temperature condition, the crystalline texture that substrate adds negative bias growth ZnO:Ga film is better than the not film of biasing growth of substrate.
4. at ambient temperature, under identical doping content situation, the mobility of ZnO:Ga nesa coating is apparently higher than the ZnO:Al film, so the conductivity of ZnO:Ga film is better.
Organic polymer thin film substrate ZnO:Ga transparent conductive film material of the present invention, its photoelectric properties are good, can substitute a large amount of at present ito thin films that use, and can save a large amount of noble metal indiums, can reduce the nesa coating cost again.
(4) description of drawings
Fig. 1 is the resistivity p of PPA film-substrate ZnO:Ga nesa coating and the carrier concentration n change curve with sputtering power, and Fig. 2 is the change curve of ZnO:Ga nesa coating hall mobility with sputtering power.Carrier concentration and hall mobility all increase with the increase of sputtering power as can be seen, and film resiativity reduces along with the increase of sputtering power.Can cause damage to organic substrate material when but sputtering power is excessive.
Fig. 3 is the visible light transmissivity spectrum of the PPA substrate ZnO:Ga film of preparation under the different bias voltages.ZnO:Ga film transmitance is along with the variation of substrate bias.(a)0V；(b)-40V；(c)-75V。Thickness is respectively: (a) 380nm, (b) 430nm and (c) 440nm..The increase of negative bias makes crystallization degree improve, and grain-size strengthens, and grain boundary reduces, so visible light transmissivity improves.
The X-ray diffraction spectrum of preparation PPA substrate ZnO:Ga nesa coating under the different bias condition of Fig. 4.The pairing bias voltage of spectral line is respectively (a) 0V, (b)-50V, (c)-75V and (d)-100V.Bias voltage is-and the X-ray diffraction peak is the strongest during 75V, and the crystal grain that prepare film this moment is big, and structure is good.
(5) embodiment
Embodiment 1: the bias voltage radiofrequency magnetron sputtering technology prepares the gallium adulterated zinc oxide transparent conductive film material.
Sputter with the ceramic target component is: 1 part of ZnO, Ga
2O
30.03 part, be molar part.With ZnO and Ga
2O
3The powder stock ball milling was rolled into base with hydropress after mixing in 2 hours under the pressure of 60Mpa, then at 1200 ℃ of following sintered heat insulatings after 2 hours, chargedly be cooled to 800 ℃, naturally cooling behind the powered-down.
With polypropylene second diester (PPA) film is substrate material, and the diameter of target is 6.5cm, and target is 5cm to the distance of substrate.At argon partial pressure 2Pa, sputtering power 150W, bias voltage 0V, underlayer temperature are that the ZnO:Ga nesa coating of room temperature condition preparation is a polycrystal film, and growth for Thin Film speed is 19nm/min, and the resistivity of film is 8.7 * 10
-4Ω cm, the average transmitance relatively of visible-range surpasses 82%.
Embodiment 2:
The bias voltage radiofrequency magnetron sputtering technology prepares ZnO:Ga electrically conducting transparent mould material, and sputter is identical with embodiment 1 with the ceramic target component.With polypropylene second diester (PPA) film is substrate material, at argon partial pressure 1Pa, and sputtering power 150W, bias voltage-75V, underlayer temperature is that the ZnO:Ga nesa coating of room temperature condition preparation is a polycrystal film, and growth for Thin Film speed is 21nm/min, and the resistivity of film is 4.6 * 10
-4Ω cm, square resistance 6.2 Ω/, the average transmitance relatively of visible-range surpasses 83%.
Embodiment 3:
Sputter with the ceramic target component is, 1 part of ZnO, and, Ga
2O
3, 0.05 part, be molar part, ceramic target preparation method with
Embodiment 1 is identical.
Substrate material is a polyethylene terephthaldehyde ester film, and the film preparation condition is identical with embodiment 2.Gained ZnO:Ga nesa coating has polycrystalline structure, and the resistivity of film is 5.1 * 10
-4Ω cm, the average transmitance relatively of visible-range surpasses 81%.
Embodiment 4:
The bias voltage radiofrequency magnetron sputtering technology prepares ZnO:Ga electrically conducting transparent mould material, and sputter is identical with embodiment 1 with the ceramic target component.With the Kapton is substrate material, and at argon partial pressure 1Pa, sputtering power 150W, bias voltage-100V, underlayer temperature are that the ZnO:Ga nesa coating of room temperature condition preparation is a polycrystal film, and growth for Thin Film speed is 16nm/min, and the resistivity of film is 1.03 * 10
-3Ω cm,, the average transmitance relatively of visible-range is 80%.
Comparative Examples:
Sputter is identical with embodiment 2 with the component of ceramic target, and ceramic target preparation method is identical with embodiment 1.
With the simple glass is substrate material, and the preparation condition of ZnO:Ga nesa coating is: argon partial pressure 1Pa, sputtering power 175W, bias voltage-75V, underlayer temperature are room temperature, preparation ZnO:Ga nesa coating, growth for Thin Film speed is 21nm/min, and the resistivity of film is 3.6 * 10
-4Ω cm, square resistance 3.9 Ω/, the average transmitance relatively of visible-range surpasses 84%.
Claims (5)
1. the preparation method of the adulterated electrically conducting transparent oxide film of gallium, it is characterized in that it being in ZnO film, to carry out gallium to mix, with the bias voltage radiofrequency magnetron sputtering technology under vacuum condition, room temperature preparation goes out to have the ZnO:Ga nesa coating of polycrystalline structure on the organic polymer thin film substrate, sputter is as follows with the ceramic target component, is a mole deal:
1 part in zinc oxide,
0.01～0.08 part of Gallium trioxide,
Processing condition are: partial pressure of ar gas 0.5-5Pa, and sputtering power 50-200W, sputtering bias-voltage 0～-100V.
2. the preparation method of the adulterated electrically conducting transparent oxide film of gallium as claimed in claim 1, it is one of following to it is characterized in that described organic polymer thin film substrate is selected from: polypropylene second diester, polyethylene terephthaldehyde ester, polypropylene or polyimide.
3. the preparation method of the adulterated electrically conducting transparent oxide film of gallium as claimed in claim 1, it is characterized in that described sputter with each component raw material of ceramic target by mechanically mixing evenly after, be pressed into embryo, generate ceramic target through 1100～1250 ℃ of high temperature sinterings.
4. the preparation method of the adulterated electrically conducting transparent oxide film of gallium as claimed in claim 1 is characterized in that described sputter is as follows with the component of ceramic target, is a mole deal:
1 part in zinc oxide, 0.03 part of Gallium trioxide.
5. the preparation method of doping multivariant oxide transparent conductive film material as claimed in claim 1 is characterized in that described ZnO:Ga nesa coating preparation process condition is:
Partial pressure of ar gas 1Pa, sputtering power 150W, bias voltage-75V.
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| CN102191466A (en) * | 2010-03-18 | 2011-09-21 | 中国科学院福建物质结构研究所 | Gallium doped zinc oxide target and preparation method of transparent conductive film thereof |
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