CN100485082C - Method for preparing ZnO:Al transparent conductive film by direct magnetic control co-sputtering method - Google Patents
Method for preparing ZnO:Al transparent conductive film by direct magnetic control co-sputtering method Download PDFInfo
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- CN100485082C CN100485082C CNB2006100695006A CN200610069500A CN100485082C CN 100485082 C CN100485082 C CN 100485082C CN B2006100695006 A CNB2006100695006 A CN B2006100695006A CN 200610069500 A CN200610069500 A CN 200610069500A CN 100485082 C CN100485082 C CN 100485082C
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Abstract
The present invention discloses DC magnetically controlled co-sputtering process for preparing transparent conductive ZnO:Al film in polycrystalline structure on glass substrate. The present invention has sputtering target of separated pure metal zinc target and aluminum target separated by 40-80 mm, basic vacuum lower than 1.0x10<-3> Pa in the sputtering room, sputtering gas of argon, reacted gas of oxygen, gas pressure of 0.5-3 Pa in the sputtering room, argon-to-oxygen flow rate ratio of 4-10, and substrate temperature of 100-300 deg.c. The present invention has low cost, easy target making, capacity of filming in great area, high film quality and other advantages.
Description
(1) technical field:
The present invention relates to a kind of method of the ZnO:Al of preparation transparent conductive film, relate in particular to the method that a kind of direct magnetic control co-sputtering legal system is equipped with the ZnO:Al transparent conductive film, belong to the photoelectricity information material technical field.
(2) background technology:
Transparent conductive film is a kind of important photoelectricity information material, not only has both low resistance and high visible light transmissivity, also has good film toughness and chemical stability.Good photoelectric characteristic has a wide range of applications it in electronic industry, it can be used as the transparency electrode of liquid-crystal display, electroluminescent display, non-crystal silicon solar cell; Do the antifrost antifogging film of visible observation at aspects such as automobile, locomotive, aircraft, freezer, instrument; Utilize its good micro-wave screening effect, be used for computer house, radar shielding protection etc.The domestic transparent conductive film of producing mainly concentrates on ITO (In from material at present
2O
3: Sn) film, and most target dependence on import.Ito thin film costs an arm and a leg, and forces the researchist to go to seek new film system.The photoelectric properties of finding the ZnO:Al film in the ZnO film system in recent years are suitable with the ito thin film performance, but there is bigger advantage aspects such as its cost than ito thin film.The Zn price is lower than the price of In, Sn, is that the ZnO:Al film of raw material must be lower than ito thin film cost with it; In is poisonous, and it is contaminate environment not only, but also can work the mischief to HUMAN HEALTH, and Zn is the obligato trace element of human body growth; Under special occasions such as hydrogen plasma, use the ZnO:Al film, its stable performance, ito thin film then can't be compared; Any method for preparing ito thin film can be used for preparing the ZnO:Al film.Because of ZnO:Al film aboundresources, low price, space nontoxic, further research are very big, being expected becomes substituting of ito thin film, thus the puzzlement that solves the In shortage of resources.
Find by retrieval existing document, the method for preparing the ZnO:Al transparent conductive film has rf magnetron sputtering (RF magnetron sputtering) method, " property research of the adulterated ZnO film of Al of radio-frequency magnetron sputter method preparation " referring to people such as Satoshi Kobayakawa, " nuclear instrument and physical study method " B249 (2006) 536-539 (Satoshi Kobayakawa, Yoshikazu Tanaka, Ari Ide-Ektessabi.Characteristics of Al doped zinc oxide (ZAO) thin films deposited by RF magnetronsputtering, Nuclear Instruments and Methods in Physics Research B249 (2006) 536-539); Dc magnetron reactive sputtering (dc magnetron reactive sputtering) method, referring to people's such as M.Chen " the dc magnetron reactive sputtering legal system is equipped with the adulterated ZnO film of Al ", " material wall bulletin " 48 (2001) 194-198 (M.Chen, Z.L.Pei, C.Sun, et al.Formation of Al-doped ZnO films bydc magnetron reactive sputtering, Materials Letters 48 (2001) 194-198); Pulsed laser deposition (pulsed laser deposition) method, " with the adulterated ZnO film of the brilliant Al of pulsed laser deposition growth transparent conductive nano " referring to people such as R.K.Shukla, " crystal growth " 294 (2006) 427-431 (R.K.Shukla, Anchar Srivastave, Atul Srivastava, et al.Growth of transparent conductingnanocrystalline Al doped ZnO thin films by pulsed laser deposition, Journal of CrystalGrowth 294 (2006) 427-431); Thermospray (Spray pyrolysis) method, referring to people's such as M.T.Mohammad " hot spray process prepares the ZnO film of conductive, transparent ", " materials chemistry and physics " 99 (2006) 382-387 (M.T.Mohammad, A.A.Hashim, M.H.Al-Maamory.Highly conductive andtransparent ZnO thin films prepared by spray pyrolysis technique, MaterialsChemistry and Physics 99 (2006) 382-387); Sol-gel (sol-gel) method, " anneal is to ZnO:Al film electricity and optical property influence " referring to people such as V.Musat, " solid film " 502 (2006) 219-222 (V.Musat, B.Teixeira, E.Fortunato, et al.Effect of post-heat treatment onthe electrical and optical properties of ZnO:Al thin films, Thin Solid Films 502 (2006) 219-222).
Radio-frequency magnetron sputter method ZnO/Al
2O
3The oxide ceramics target, the making trouble of oxide target, the cost height of target, target can not be recycled; Dc magnetron reactive sputtering method Zn/Al alloys target, can make resistivity under optimum process condition is 4.8 * 10
-4Ω cm and visible light transmissivity are near 90% film, and alloys target is easily manufactured than ceramic target, but the person's character of the easy oxidation of metal has determined alloys target to poison easily, and influential to sputter coating, target can not be recycled.Pulsed laser deposition can make resistivity under optimum process condition be 6 * 10
-4Ω cm and visible light transmissivity are near 85% film, but apparatus expensive is difficult to the big area film forming; Hot spray process equipment simple cheap, but under optimum process condition, make film conductivity and visible light transmissivity is respectively 0.3 (Ω cm)
-1With 70%; Sol-gel method equipment simple cheap makes film resiativity under optimum process condition and visible light transmissivity is respectively 2.9 * 10
-3Ω cm and 80%, the thickness evenness of film photoelectric performance and spin-coating is poor.
(3) summary of the invention:
The objective of the invention is to overcome the deficiency in the above-mentioned prior art and a kind of method that is equipped with the ZnO:Al transparent conductive film with the direct magnetic control co-sputtering legal system is provided, this method is with low cost, target is easily manufactured and recyclable utilization, be easy to the big area film forming, the electroconductibility of made transparent conductive film and optical transmittance height, thickness evenness is good, superior performance.
Purpose of the present invention can reach by following measure: a kind of direct magnetic control co-sputtering legal system is equipped with the method for ZnO:Al transparent conductive film, and step is as follows:
(1) highly purified Metal Zn target is installed in the negative electrode target groove of water-cooled of sputtering chamber of magnetically controlled DC sputtering device, highly purified metal A l sheet is attached to Zn target surface, the substrate that cleaned is put into substrate frame, substrate frame is inserted in the media disk of sputtering chamber, adjusting target-substrate distance (distance between target and the substrate) is 40-80mm, preferred 50mm;
(2) sputtering chamber is bled, the base vacuum that makes sputtering chamber is less than 1.0 * 10
-3Pa, preferred 4.0 * 10
-4Pa is heated to 100 ℃-300 ℃ to substrate, and the back charges into sputter gas argon gas and reactant gases oxygen respectively in sputtering chamber, and the flow ratio of argon gas and oxygen is 4-10, and sputter gas Ar gas is guided to by conduit near the metal target surface, reactant gases O
2Gas is guided near the substrate by conduit, and reduces rate of air sucked in required, and the gaseous tension that makes sputtering chamber is 0.5-3Pa, and last magnetron sputtering makes the ZnO:Al transparent conductive film.
In order further to realize purpose of the present invention, the effective area area of described metal A l sheet accounts for 2-8 part, and Zn target effective area area accounts for 92-98 part.The effective area area of preferable alloy Al sheet accounts for 4 parts, and Zn target effective area area accounts for 96 parts.
In order further to realize purpose of the present invention, the purity of described Metal Zn target is greater than 99.99wt.%, and the purity of metal A l sheet is greater than 99.99wt.%.
In order further to realize purpose of the present invention, described Metal Zn target be shaped as circle, being shaped as of metal A l sheet is fan-shaped.
In order further to realize purpose of the present invention, described Zn target diameter is 60mm, the sputtering power 20W-50W of sputtering chamber.Preferred Corning 1737F sheet glass, thickness 1.1mm.Described substrate soaks in the glass washing lotion, cleans at alcohol and deionized water for ultrasonic, dries up with nitrogen gun.
In order further to realize purpose of the present invention, described media disk can 0-360 ° of revolution.
For fear of the oxidation of metallic target, improve film deposition rate, the present invention adopts the reactive sputtering film technique, sputter gas Ar gas not only provides the ion source of bombardment metal targets, and rare gas element Ar gas shiled metallic target.
Under preferred processing condition, promptly sputtering chamber gaseous tension 1.8Pa, argon gas and oxygen flow are respectively 250 ℃ of 24sccm and 4sccm, sputtering power 46W and substrate temperatures, and the resistivity that makes film is 5.2 * 10
-4The transmitance of film is higher than 95% in the Ω cm, visible-range.
Method of the present invention compared with prior art excellent results is as follows:
1. compare with the dc magnetron reactive sputtering method with radio-frequency magnetron sputter method, the pure metal targets manufacturing is simple, and is cheap, can recycle;
2. compare with pulsed laser deposition, the equipment simple cheap, be easy to the big area film forming;
3. compare with sol-gel method with hot spray process, the electroconductibility of film and the optical transmittance of visible-range obviously improve, and thickness evenness is good.
(4) embodiment: following the specific embodiment of the present invention is elaborated:
Embodiment 1:
(1) the Metal Zn target of purity 99.99wt.%, diameter 60mm is installed in the negative electrode target groove of water-cooled of sputtering chamber of magnetically controlled DC sputtering device, the metal A l sheet of purity 99.99wt.% is attached to Zn target surface, the Zn target be shaped as circle, being shaped as of metal A l sheet is fan-shaped.The effective area area of metal A l sheet accounts for 4 parts, and Zn target effective area area accounts for 96 parts.Corning 1737F glass with thickness 1.1mm is substrate, substrate soaks in the glass washing lotion, clean at alcohol and deionized water for ultrasonic, dry up with nitrogen gun, the substrate that cleaned is put into substrate frame, substrate frame is inserted in the media disk of sputtering chamber, 0-360 ° of revolution of media disk energy, adjusting target-substrate distance (distance between target and the substrate) is 50mm;
(2) sputtering chamber is bled, the base vacuum that makes sputtering chamber is 4.0 * 10
-4Pa, be heated to 100 ℃ (being underlayer temperature) to substrate, the back charges into sputter gas argon gas and reactant gases oxygen respectively in sputtering chamber, sputter gas argon flow amount 24sccm, reactant gases oxygen flow 4sccm, the flow ratio of argon gas and oxygen is 6, and sputter gas Ar gas is guided to by conduit near the metal target surface, reactant gases O
2Gas is guided near the substrate by conduit, and reduces rate of air sucked in required, and the gaseous tension that makes sputtering chamber is 1.8Pa, the sputtering power 46W of last magnetron sputtering, and sputter 8 minutes makes the ZnO:Al transparent conductive film, makes film thickness 150nm, and the resistivity of film is 8.2 * 10
-4Ω cm, the optical transmittance of the visible-range of film surpasses 94%, and film has polycrystalline structure.
Embodiment 2:
Sputtering target is identical with embodiment 1, and different is that underlayer temperature is 250 ℃ in the step (2), and other preparation condition of film is identical with embodiment 1.The resistivity of film is 5.2 * 10
-4Ω cm, the optical transmittance of the visible-range of film surpasses 95%, and film has polycrystalline structure.
Embodiment 3.
Sputtering target is identical with embodiment 1, and different is that underlayer temperature is 300 ℃ in the step (2), and other preparation condition of film is identical with embodiment 1.The resistivity of film is 7.3 * 10
-4Ω cm, the optical transmittance of the visible-range of film surpasses 92%, and film has polycrystalline structure.
Embodiment 4
The Metal Zn target of the diameter 60mm of purity 99.999wt.% is installed in the negative electrode target groove of water-cooled, the fan-shaped metal A l sheet of purity 99.999wt.% is attached to Zn target surface, the effective area area of magnetron sputtering Al sheet accounts for 8 parts, and Zn target effective area area accounts for 92 parts.The film preparation condition is identical with embodiment 2.Film has polycrystalline structure, and the resistivity of film is 8.6 * 10
-4Ω cm, the optical transmittance of the visible-range of film surpasses 93%.
Embodiment 5
The diameter 60mm Metal Zn target of purity 99.999wt.% is installed in the negative electrode target groove of water-cooled, and the fan-shaped metal A l sheet of purity 99.99wt.% is attached to Zn target surface, and the effective area area of magnetron sputtering Al sheet accounts for 2 parts, and Zn target effective area area accounts for 98 parts.The film preparation condition is identical with embodiment 2.Film has polycrystalline structure, and the resistivity of film is 6.7 * 10
-4Ω cm, the optical transmittance of the visible-range of film surpasses 94%.
Embodiment 6
Sputtering target is identical with embodiment 1 with substrate, different is that the adjustment target-substrate distance is 40mm, 250 ℃ of substrate heating temperatures, sputter gas argon flow amount 24sccm, reactant gases oxygen flow 2.4sccm, the flow ratio of argon gas and oxygen is 10, the gaseous tension of sputtering chamber is 0.5Pa, the sputtering power 20W of last magnetron sputtering, sputtering time 18 minutes, make film thickness 150nm, other preparation condition of film is identical with embodiment 1.The resistivity of film is 6.4 * 10
-4Ω cm, the optical transmittance of the visible-range of film is greater than 87%.
Embodiment 7
Sputtering target is identical with embodiment 1 with substrate, and different is that the adjustment target-substrate distance is 80mm, and the base vacuum of sputtering chamber is 2.0 * 10
-4Pa, 250 ℃ of substrate heating temperatures, sputter gas argon flow amount 24sccm, reactant gases oxygen flow 6sccm, the flow ratio of argon gas and oxygen are 4, and the gaseous tension of sputtering chamber is 3Pa, the sputtering power 50W of last magnetron sputtering, sputtering time 10 minutes makes film thickness 150nm, and other preparation condition of film is identical with embodiment 1.The resistivity of film is 8.0 * 10
-4Ω cm, the optical transmittance of the visible-range of film surpasses 94%, and film has polycrystalline structure.
Claims (10)
1, a kind of direct magnetic control co-sputtering legal system is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that step is as follows:
(1) highly purified Metal Zn target is installed in the negative electrode target groove of water-cooled of sputtering chamber of magnetically controlled DC sputtering device, highly purified metal A l sheet is attached to Zn target surface, the substrate that cleaned is put into substrate frame, substrate frame is inserted in the media disk of sputtering chamber, the adjustment target-substrate distance is 40-80mm;
(2) sputtering chamber is bled, the base vacuum that makes sputtering chamber is less than 1.0 * 10
-3Pa is heated to 100 ℃-300 ℃ to substrate, and the back charges into sputter gas argon gas and reactant gases oxygen respectively in sputtering chamber, and the flow ratio of argon gas and oxygen is 4-10, and sputter gas Ar gas is guided to by conduit near the metal target surface, reactant gases O
2Gas is guided near the substrate by conduit, and reduces rate of air sucked in required, and the gaseous tension that makes sputtering chamber is 0.5-3Pa, and last magnetron sputtering makes the ZnO:Al transparent conductive film.
2, a kind of direct magnetic control co-sputtering legal system according to claim 1 is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that the effective area area of described metal A l sheet accounts for 2-8 part, and Zn target effective area area accounts for 92-98 part.
3, a kind of direct magnetic control co-sputtering legal system according to claim 2 is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that the effective area area of described metal A l sheet accounts for 4 parts, and Zn target effective area area accounts for 96 parts.
4, be equipped with the method for ZnO:Al transparent conductive film according to claim 1 or 2 or 3 described a kind of direct magnetic control co-sputtering legal systems, the purity that it is characterized in that described Metal Zn target is greater than 99.99wt.%, and the purity of metal A l sheet is greater than 99.99wt.%.
5, the method that is equipped with the ZnO:Al transparent conductive film according to claim 1 or 2 or 3 described a kind of direct magnetic control co-sputtering legal systems is characterized in that the circle that is shaped as of described Metal Zn target, and being shaped as of metal A l sheet is fan-shaped.
6, a kind of direct magnetic control co-sputtering legal system according to claim 5 is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that described Zn target diameter is 60mm, the sputtering power 20W-50W of sputtering chamber.
7, a kind of direct magnetic control co-sputtering legal system according to claim 1 is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that described substrate is a sheet glass.
8, a kind of direct magnetic control co-sputtering legal system according to claim 7 is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that described substrate is a Corning 1737F sheet glass, thickness 1.1mm.
9, be equipped with the method for ZnO:Al transparent conductive film according to claim 7 or 8 described a kind of direct magnetic control co-sputtering legal systems, it is characterized in that described substrate soaks in the glass washing lotion, clean, dry up with nitrogen gun at alcohol and deionized water for ultrasonic.
10, direct magnetic control co-sputtering legal system according to claim 1 is equipped with the method for ZnO:Al transparent conductive film, it is characterized in that described media disk can 0-360 ° of revolution.
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Cited By (1)
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| CN102453869A (en) * | 2010-10-28 | 2012-05-16 | 海洋王照明科技股份有限公司 | Preparation method and application of aluminum-doped zinc oxide conductive film |
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| CN102453869A (en) * | 2010-10-28 | 2012-05-16 | 海洋王照明科技股份有限公司 | Preparation method and application of aluminum-doped zinc oxide conductive film |
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