CN102312201A - Preparation method of Al-doped zinc oxide transparent conductive thin film - Google Patents

Preparation method of Al-doped zinc oxide transparent conductive thin film Download PDF

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CN102312201A
CN102312201A CN2010102144127A CN201010214412A CN102312201A CN 102312201 A CN102312201 A CN 102312201A CN 2010102144127 A CN2010102144127 A CN 2010102144127A CN 201010214412 A CN201010214412 A CN 201010214412A CN 102312201 A CN102312201 A CN 102312201A
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transparent conductive
conductive film
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CN102312201B (en
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刘学超
陈之战
宋力昕
施尔畏
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention belongs to the field of transparent conductive thin films, relates to a preparation method of an Al-doped ZnO transparent conductive thin film, and in particular relates to an inductively coupled plasma reinforced physical vapour deposition (ICP-PVD) method. The ICP-PVD method comprises the following steps of: firstly preparing a Zn1-xAlxO (x is more than or equal to 0.01 and is less than or equal to 0.05) target material; and placing a clean and dry substrate into an ICP-PVD system, and controlling all the technological parameters of the ICP-PVD system to carry out thin film deposition, so as to obtain the Al-doped ZnO transparent conductive thin film. The method provided by the invention adopts simple equipment, is easy to operate and can realize large-area and mass production of coating films. Compared with the traditional thin film equipment, the ICP-PVD system realizes constrain and acceleration effects on various charged particles in plasma, thus crystallization quality of the thin film and controllability of doping of a donor are improved, a ZnO thin film with low resistivity, high transmissivity and good repeatability and stability can be easily obtained, and the thin film can be applied to photoelectronic devices.

Description

The preparation method of the adulterated zinc oxide transparent conductive film of a kind of Al
Technical field
The invention belongs to the transparent conductive film field, relate to the preparation method of the adulterated zinc oxide transparent conductive film of a kind of Al, relate in particular to a kind of inductively coupled plasma and strengthen physical vaporous deposition.
Background technology
The electrically conducting transparent membrane technique started from for 20 beginnings of the century; Along with the development of electronics technology, the nineties begins to be widely used on optics, electronics and the photoelectric devices such as flat-panel screens, transparent heating component, antistatic film, electromagnetic wave proof film, solar cell transparency electrode, anti-reflective coating and hot mirror.Show that on the plane field, liquid-crystal display become now and the leading product of future market, its market output value will be how much magnitudes and increase, and global whole liquid-crystal display industry production value in 2015 will reach 1,480 hundred million dollars according to estimates.At energy field, sun power is more and more paid attention to as pollution-free, a reproducible energy, thereby makes the demand of solar film battery also increasing.Nesa coating demand as one of important raw and processed materials in the solar film battery is corresponding also in increase.Global solar photovoltaic market will be expanded 1,500 hundred million dollars in 2015 from 1,000,000,000 dollars in 2000 to according to estimates, and the shared market share of hull cell maybe be with rising to 52% from 2%, and surmounting crystal silicon solar energy battery becomes main flow.At present, transparent conductive film is mainly taken as the leading factor by tin indium oxide (ITO), and the major ingredient of ITO rete is a tin indium oxide.The ito thin film transmitance is high, and conductive capability is strong, a kind of just conductive film glass that is coated with high permeability of ito glass that liquid-crystal display is used.Though ITO occupies an leading position in the transparent conductive film field,,, require also higher to safety production condition so cost is higher because the shortcoming of himself belongs to rare noble metal and severe toxicity is arranged like indium among the ITO and tin; ITO has very strong water-absorbent, absorbs airborne moisture content and carbonic acid gas easily and produces chemical reaction and go bad; The ito thin film layer is prone to produce the ion exchange reaction in active nominal price solion, forms other conduction and not good RM of transmitance, and complete processing is had relatively high expectations.For this reason, people are seeking always and can reduce production costs by the alternate material, enhance product performance.
Zinc oxide (ZnO) has hexagonal prism shape wurtzite and zincblende lattce structure as one of representative of third generation wide bandgap semiconductor, and band gap is 3.3eV under the room temperature, and exciton binding energy is 60meV, has the good characteristic that sees through in the visible region.Because ZnO has characteristics such as good photoelectricity, piezoelectricity, acousto-optic, luminous, gas sensor and chemical catalysis, be novel material research and one of focus of Application Areas always.Prepare the film of low-resistivity, high transparent through suitable adulterated ZnO, have the potential using value in transparent demonstration and new energy field.The photoelectric characteristic of Al doping ZnO (AZO) nesa coating has received widely and having paid attention in recent years, can be used as solar cell window electrode like AZO, and its anti-plasma performance is good, can improve solar cell properties; Also can be used as the good material of liquid-crystal display and photo-sensor, electroluminescence device.Compare with traditional nesa coating ITO, AZO has the unrivaled photoelectric properties of ITO, and the ZnO raw material resources are abundant; Low price is prone to lithography process, and stability is better than ito thin film in hydrogen plasma; Complete processing is to the environment nontoxic pollution-free, and stable performance, so extremely pay attention to.In transparent conducting ZnO film field, common following several method, the pulsed laser deposition (PLD) of mainly containing; Molecular beam epitaxy (MBE), vapour deposition (CVD), sputter (comprising RF and DC sputter); Reactive evaporation, ultrasonic spray pyrolysis (USP) and sol-gel (Sol-Gel) method etc.Though PLD and MBE can prepare high-quality film, be unfavorable for the mass-producing application; The common surface quality of film of sputter or evaporation preparation is relatively poor, and rough degree is higher, and the conductivity difference is bigger; USP and Sol-Gel belong to chemical preparation, and film quality is relatively low, also are unfavorable for large-scale production.Except that chemical vapor deposition (CVD) method, additive method does not all reach the level (suitability for industrialized production) of the even plated film of big area, but the main drawback of CVD method is complex equipments and costliness, and used organic zinc source costs an arm and a leg and be poisonous, and the thin film deposition underlayer temperature is high.Therefore, seek the technology of preparing that a kind of technology is simple, cost is low and prepare the AZO film, with the commercial application that more helps advancing the AZO film.
Summary of the invention
The preparation method who the purpose of this invention is to provide the adulterated zinc oxide transparent conductive film of a kind of high-quality Al is to overcome the deficiency of prior art.
In order to solve the problems of the prior art, the invention discloses a kind of inductively coupled plasma and strengthen physical vaporous deposition, promptly the ICP-PVD method adopts the Al doping ZnO, meets chemical formula Zn with chemical ingredients 1-xAl xThe target of O (0.01≤x≤0.05) prepares the adulterated ZnO semiconductor film of Al of high quality, low-resistivity, high transparent.But this preparing method's big area large-scale production, technology is simple, cost is low, and heavy metal free is poisoned or phenomenons such as pollution take place in the preparation process.
The preparation method of the adulterated ZnO transparent conductive film of a kind of Al, said preparation method strengthens physical vaporous deposition for inductively coupled plasma, and promptly the ICP-PVD method specifically comprises the steps:
(1), static pressure solid state reaction synthesis technique such as employing prepares chemical ingredients and meets chemical formula Zn 1-xAl xThe target of O, wherein 0.01≤x≤0.05;
Said Zn 1-xAl xElement lower right corner part is represented mol ratio among the O;
Said synthesis technique such as solid state reaction such as static pressure such as grade can be the synthesis technique such as solid state reaction such as static pressure such as grade of standard;
The preparation method of said target does, presses Zn 1-xAl xThe stoichiometric ratio of O (0.01≤x≤0.05) corresponding element takes by weighing ZnO and Al 2O 3, behind thorough mixing, first pre-molding adopts isostatic cool pressing then, places electric tube furnace to be fired into Zn at last 1-xAl xThe target of O;
Said ZnO and Al 2O 3Purity be more than 99.99%.
The condition of firing in the said electric tube furnace can be for progressively being warming up to 1000 ℃, and be incubated 48 hours.
(2), the substrate of clean dry is put into ICP-PVD system response chamber;
Said substrate is selected from silica glass substrate or Si substrate; Said substrate is dry, like available N 2Dry up drying.
(3) ICP-PVD system base vacuum is evacuated to P≤1 * 10 -7Torr, heated substrate then, underlayer temperature is 300～400 ℃;
(4) in step (3) system with Ar as carrier gas and plasma source; Reaction chamber pressure is 20～100Torr; Radio-frequency sputtering power is 150～200W; The lashing wire loop current is 0.3～0.5A, and adding positive bias between substrate and target is 250～300V, carries out thin film deposition and obtains the adulterated ZnO transparent conductive film of Al.
The purity of Ar is more than 99.9995% in the said step (4).
Also can sneak into part oxygen, the intrinsic standoff ratio V of said oxygen and argon gas in the argon gas that said ICP-PVD system feeds O: V Ar≤1: 10.
Said reaction chamber pressure is preferably 50～100Torr.
The thickness of the adulterated ZnO transparent conductive film of said Al can be through regulating the control of preparation technology parameter or depositing time.
The resistivity of said film can be controlled through Al content and the oxygen partial pressure in the preparation process regulated in the target, like the throughput ratio through regulating oxygen and argon gas to control the oxygen partial pressure in the sediment chamber.
Said radio-frequency sputtering power lower (as＜film deposition rate is slow 150W) time, power higher (as＞can increase the roughness of film surface 200W) time; The growth temperature of said substrate is the optimum temps that obtains the better quality film, and the crystalline quality of this film and c axle crystalline orientation property are not good during lower growth temperature (as＜300 ℃); Said positive bias helps improving the stoichiometric ratio of Zn in this film: O, reduces the defective in the film.
A kind of high-quality Al doping ZnO transparent conductive film is for ICP-PVD method according to the present invention makes.
The chemical ingredients of said thin-film material meets chemical formula Zn 1-xAl xO, wherein 0.01≤x≤0.05.
The surfacing of the adulterated ZnO transparent conductive film of said Al, its surface average roughness is 4.0 ± 0.5nm; Said thin film crystallization is fine and close, and homogeneous grain size has the high C-axis preferred orientation; The resistivity of said film is≤8 * 10 -4Ω cm, visible spectrum average transmittances>=90%.
The Al doping ZnO transparent conductive film of ICP-PVD method preparation of the present invention; The gas ions enhanced system of introducing can make the neutral particle ionize that sputters out; It is active that the charged particle that sputters out is increased, and promotes to decompose or dissociate, and promptly can strengthen the degree of ionization of particle; Improve sedimentation rate, reduce the film growth temperature.This magnetic confinement system can confining plasma, thereby improves uniformity of thin film deposition and compactness.In addition, it is simple, easy to operate that this method also has equipment, is fit to launch advantages such as big area large-scale production.ICP-PVD method of the present invention makes the Al ion evenly be doped among the ZnO; The introducing of Al can significantly reduce the resistivity of film; Improve current carrier (electronics) concentration in the ZnO film, and obtain high-quality film, for the application of opto-electronic device provides the excellent material basis.
But preparing method's big area of the present invention large-scale production, technology is simple, cost is low; Phenomenons such as heavy metal free poisoning or pollution in the preparation process; The surfacing of prepared Al doping ZnO transparent conductive film, compact crystallization, homogeneous grain size; Have the high C-axis preferred orientation, this film has low-resistivity, high transparent, repeatability and stability.
Description of drawings
Fig. 1 ICP-PVD system sputter equipment synoptic diagram
The XRD figure of the ZnO thin film doped sample of Al spectrum among Fig. 2 embodiment 1
The ZnO thin film doped surface topography stereoscan photograph of Al among Fig. 3 embodiment 1
The ZnO thin film doped surfaceness atomic power of Al AFM photo among Fig. 4 embodiment 1
The ZnO thin film doped optical transmittance of Al (ultraviolet-visible spectrum) collection of illustrative plates among Fig. 5 embodiment 1
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1
With 2% mole of ZnO thin film doped Zn of Al 0.98Al 0.02O is an example:
(1) adopt the static pressure solid state reaction synthesis technique that waits of standard to prepare Zn 0.98Al 0.02The O target.Press Zn with electronic balance 0.98Al 0.02The stoichiometric ratio of the corresponding element of O takes by weighing the ZnO (40.695g) and the Al of high-purity (>=99.99%) 2O 3(0.520g), behind thorough mixing, first pre-molding (50MPa) adopts isostatic cool pressing (200MPa) then, places electric tube furnace progressively to be warming up to 1000 ℃ at last, and is incubated 48 hours.
(2) the silica glass substrate is cleaned, with N 2Dry up and put into the ICP-PVD reaction chamber.
(3) ICP-PVD system base vacuum is extracted into 1 * 10 -7Torr, heated substrate then, underlayer temperature is 400 ℃.
(4) with high-purity (>=99.9995%) Ar as carrier gas and plasma source; Reaction chamber pressure is 100Torr, and radio-frequency sputtering power is 150W, and the lashing wire loop current is 0.5 ampere; Add 300 volts of positive biases between substrate and target, carry out thin film deposition and obtain the adulterated ZnO transparent conductive film of Al.
Fig. 1 is an ICP-PVD system sputter equipment synoptic diagram, and this device is a kind of composite system, and the plasma enhanced system has been introduced physical vapor deposition device, can fully utilize the advantage of plasma body and PVD, effectively improves film quality and sedimentation effect.The inductively coupled plasma enhanced system that this ICP-PVD system and conventional films apparatus in comparison are introduced can the article on plasma body in the film preparation process in various charged particles play constraint and booster action; Thereby improved the crystalline quality of film; Improved the controllability of donor doping, be easy to obtain to have that resistivity is low, transmitance is high, the transparent conductive film of repeatability and good stability.
Obtain Fig. 2-Fig. 5 through detecting
Fig. 2 is the XRD figure spectrum of the ZnO thin film doped sample of Al among the embodiment 1, and the Al doping ZnO transparent conductive film of visible gained has the high C-axis preferred orientation, has good crystallization property;
Fig. 3 is the ZnO thin film doped surface topography stereoscan photograph of Al among the embodiment 1, the Al doping ZnO transparent conductive film homogeneous grain size of visible gained;
Fig. 4 is the ZnO thin film doped surfaceness atomic power of an Al AFM photo among the embodiment 1, the Al doping ZnO transparent conductive film surfacing of visible gained, and average surface roughness is 4.0nm, compact crystallization;
Fig. 5 is the ZnO thin film doped optical transmittance of Al (ultraviolet-visible spectrum) collection of illustrative plates among the embodiment 1, and visible average transmittances in visible-range reaches 90%;
Conductivity under detection gained film room temperature is shown in Table I, and the resistivity of film is low to moderate 2.18 * 10 -4Ω cm, electron density is up to 9.2 * 10 20Cm -3, electronic mobility is up to 31.0cm 2V -1s -1, this high-quality film has very high repetition rate.
Embodiment 2
With 1% mole of ZnO thin film doped Zn of Al 0.99Al 0.01O is an example:
(1) adopt the static pressure solid state reaction synthesis technique that waits of standard to prepare Zn 0.99Al 0.01The O target.Press Zn with electronic balance 0.99Al 0.01The stoichiometric ratio of the corresponding element of O takes by weighing the ZnO (40.695g) and the Al of high-purity (>=99.99%) 2O 3(0.257g), behind thorough mixing, first pre-molding (50MPa) adopts isostatic cool pressing (200MPa) then, places electric tube furnace progressively to be warming up to 1000 ℃ at last, and is incubated 48 hours.
(2) the Si substrate is cleaned, with N 2Dry up and put into the ICP-PVD reaction chamber.
(3) ICP-PVD system base vacuum is extracted into 5 * 10 -8Torr, heated substrate then, underlayer temperature is 300 ℃.
(4) with high-purity (>=99.9995%) Ar as carrier gas and plasma source; Reaction chamber pressure is 50Torr, and radio-frequency sputtering power is 200W, and the lashing wire loop current is 0.3 ampere; Add 250 volts of positive biases between substrate and target, carry out thin film deposition and obtain the adulterated ZnO transparent conductive film of Al.
Fig. 1 is an ICP-PVD system sputter equipment synoptic diagram, and this device is a kind of composite system, and the plasma enhanced system has been introduced physical vapor deposition device, can fully utilize the advantage of plasma body and PVD, effectively improves film quality and sedimentation effect.
Through detecting, Al doping ZnO transparent conductive film (AZO film) surfacing of gained, average surface roughness is 3.9nm, compact crystallization, homogeneous grain size, has the high C-axis preferred orientation; Average transmittances in visible-range reaches 91%;
Conductivity under detection gained film room temperature is shown in Table I, and the resistivity of this film is 6.34 * 10 -4Ω cm, electron density is 1.84 * 10 20Cm -3, electronic mobility is 53.1cm 2V -1s -1, this high-quality film has very high repetition rate.
Embodiment 3
With 5% mole of ZnO thin film doped Zn of Al 0.95Al 0.05O is an example:
(1) adopt the static pressure solid state reaction synthesis technique that waits of standard to prepare Zn 0.95Al 0.05The O target.Press Zn with electronic balance 0.95Al 0.05The stoichiometric ratio of the corresponding element of O takes by weighing the ZnO (40.695g) and the Al of high-purity (>=99.99%) 2O 3(1.342g), behind thorough mixing, first pre-molding (50MPa) adopts isostatic cool pressing (200MPa) then, places electric tube furnace progressively to be warming up to 1000 ℃ at last, and is incubated 48 hours.
(2) the Si substrate is cleaned, with N 2Dry up and put into the ICP-PVD reaction chamber.
(3) ICP-PVD system base vacuum is extracted into 5 * 10 -8Torr, heated substrate then, underlayer temperature is 350 ℃.
(4) with high-purity (>=99.9995%) Ar as carrier gas and plasma source; Reaction chamber pressure is 50Torr, and radio-frequency sputtering power is 150W, and the lashing wire loop current is 0.4 ampere; Add 300 volts of positive biases between substrate and target, carry out thin film deposition and obtain the adulterated ZnO transparent conductive film of Al.
Fig. 1 is an ICP-PVD system sputter equipment synoptic diagram, and this device is a kind of composite system, and the plasma enhanced system has been introduced physical vapor deposition device, can fully utilize the advantage of plasma body and PVD, effectively improves film quality and sedimentation effect.
Through detecting, the Al doping ZnO transparent conductive film surfacing of gained, average surface roughness is 4.2nm, compact crystallization, homogeneous grain size, has the high C-axis preferred orientation; Average transmittances in visible-range reaches 90%;
Conductivity under detection gained film room temperature is shown in Table I, and the resistivity of this film is 3.05 * 10 -4Ω cm, electron density is 5.09 * 10 20Cm -3, electronic mobility is 40.2cm 2V -1s -1, this high-quality film has very high repetition rate.
Table I
Al mole doping Resistivity (Ω cm) Electron density (cm -3) Hall mobility (cm 2V -1s -1)
1％ 6.34×10 -4 1.84×10 20 53.1
2％ 2.18×10 -4 9.20×10 20 31.0
5％ 3.05×10 -4 5.09×10 20 40.2

Claims (9)

1. the preparation method of the adulterated ZnO transparent conductive film of Al, said preparation method comprises the steps: for inductively coupled plasma strengthens physical vaporous deposition
(1), static pressure solid state reaction synthesis technique such as employing prepares chemical ingredients and meets chemical formula Zn 1-xAl xThe target of O, wherein 0.01≤x≤0.05;
(2), the substrate of clean dry is put into ICP-PVD system response chamber;
(3), ICP-PVD system base vacuum is evacuated to P≤1 * 10 -7Torr, heated substrate temperature to 300～400 ℃ then;
(4), in step (3) system with Ar as carrier gas and plasma source; Reaction chamber pressure is 20～100Torr; Radio-frequency sputtering power is 150～200W; The lashing wire loop current is 0.3～0.5A, and adding positive bias between substrate and target is 250～300V, carries out thin film deposition and obtains the adulterated ZnO transparent conductive film of Al.
2. the preparation method of the adulterated ZnO transparent conductive film of a kind of Al as claimed in claim 1 is characterized in that the preparation method of said target does, presses Zn 1-xAl xThe stoichiometric ratio of O corresponding element takes by weighing ZnO and Al 2O 3, behind thorough mixing, first pre-molding adopts isostatic cool pressing then, places electric tube furnace to fire at last and forms.
3. the preparation method of the adulterated ZnO transparent conductive film of a kind of Al as claimed in claim 2 is characterized in that said ZnO and Al 2O 3Purity be more than 99.99%.
4. the preparation method of the adulterated ZnO transparent conductive film of a kind of Al as claimed in claim 1 is characterized in that, the purity of Ar is more than 99.9995% in the said step (4).
5. the preparation method of the adulterated ZnO transparent conductive film of a kind of Al as claimed in claim 1 is characterized in that said substrate is selected from silica glass substrate or Si substrate.
6. adulterated ZnO transparent conductive film of Al is for the preparation method according to the adulterated ZnO transparent conductive film of the arbitrary described Al of claim 1-5 makes.
7. the adulterated ZnO transparent conductive film of Al as claimed in claim 6 is characterized in that the chemical ingredients of said thin-film material meets chemical formula Zn 1-xAl xO, wherein 0.01≤x≤0.05.
8. like claim 6 or the adulterated ZnO transparent conductive film of 7 described Al, it is characterized in that said film surface is smooth, its surface average roughness is 4.0 ± 0.5nm; The resistivity of said film is≤8 * 10 -4Ω cm, visible spectrum average transmittances>=90%.
9. like the application of the adulterated ZnO transparent conductive film of the arbitrary described Al of claim 7-9 in opto-electronic device.
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CN103325888A (en) * 2013-06-21 2013-09-25 哈尔滨工业大学深圳研究生院 Transparent conductive thin film manufacturing method based on silicon-based thin film substrate
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CN104120323B (en) * 2013-04-27 2017-05-03 深圳光启高等理工研究院 Thin-film resistor, sputtering target material and preparation method

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US20120211355A1 (en) * 2011-02-22 2012-08-23 Korea Institute Of Science & Technology Transparent conductive composition, target, transparent conductive thin film using the target and method for fabricating the same
CN103046013A (en) * 2012-12-30 2013-04-17 青海天誉汇新能源开发有限公司 Method for preparing photovoltaic cell transparent oxide film with flexible substrate
CN104120323B (en) * 2013-04-27 2017-05-03 深圳光启高等理工研究院 Thin-film resistor, sputtering target material and preparation method
CN103325888A (en) * 2013-06-21 2013-09-25 哈尔滨工业大学深圳研究生院 Transparent conductive thin film manufacturing method based on silicon-based thin film substrate
CN103325888B (en) * 2013-06-21 2017-02-08 哈尔滨工业大学深圳研究生院 Transparent conductive thin film manufacturing method based on silicon-based thin film substrate
CN103706792A (en) * 2013-12-30 2014-04-09 北京科技大学 Al-doped ZnO texture thermoelectric material manufacturing method
CN103706792B (en) * 2013-12-30 2015-08-26 北京科技大学 A kind of preparation method of Al doping ZnO texture thermoelectric material

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