CN102560391A - Conducting film, and preparation method and application thereof - Google Patents
Conducting film, and preparation method and application thereof Download PDFInfo
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- CN102560391A CN102560391A CN2010106041454A CN201010604145A CN102560391A CN 102560391 A CN102560391 A CN 102560391A CN 2010106041454 A CN2010106041454 A CN 2010106041454A CN 201010604145 A CN201010604145 A CN 201010604145A CN 102560391 A CN102560391 A CN 102560391A
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Abstract
The invention is applicable to the technical field of semiconductor material, and provides a conducting film, and a preparation method and the application of the conducting film. The preparation method of the conducting film comprises the following steps of: mixing magnesium oxide, aluminium oxide and silicon dioxide into zinc oxide, wherein according to the mass percent, Al2O3 accounts for 0.5-3% of the total mass, SiO2 accounts for 0.5-1.5% of the total mass, MgO accounts for 5-25% of the total mass, and ZnO accounts for the balance; obtaining a mixture by stirring, sintering the obtained mixture and forming magnetron sputtering target; taking mixed gas of hydrogen and inert gas as working gas; carrying out magnetron sputtering by the magnetron sputtering target under the condition that the temperature of a substrate is 20-100 DEG C, and forming a film; and finally, obtaining the conducting film. The preparation method is simple in operation, mild in condition, low in price of raw materials, high in productivity and very suitable for industrialized production.
Description
Technical field
The invention belongs to the photoelectric semiconductor material technical field, relate in particular to a kind of conducting film preparation method, conducting film and application.
Background technology
The zinc oxide conducting film of prior art is the adulterated zinc oxide conducting film of single-element normally.There are problems for the Zinc oxide doped of single-element in preparation with in using.With single aluminium-doped zinc oxide conducting film (Al-doped ZnO, be called for short AZO) is example, is not easy to prepare low-resistance film in the production, and this also is that the AZO film is slowly failed one of reason that gets into production.AZO in use exists surface and intergranule circle oxygen to adsorb and causes conductivity to descend in addition, and resistivity is unstable.Simultaneously, utilize magnetron sputtering equipment all need underlayer temperature be promoted to more than 300 ℃ in the prior art, if deposit the film that obtains at low temperatures; It generally is the polycrystalline film; Crystal boundary and defective are many, reduce the rate of migration of electronic carrier greatly, cause the decline of conductive capability.
Summary of the invention
In view of this, the embodiment of the invention provides a kind of conducting film preparation method, and the conducting film that coldcondition prepares down in the solution prior art owing to crystal boundary and the defective high technical problems of resistivity that cause more.
A kind of conducting film preparation method comprises the steps:
Mixed oxidization magnesium, aluminium sesquioxide and silicon-dioxide in zinc oxide, this Al by mass percentage
2O
3Account for 0.5～3% of total mass, this SiO
2Account for 0.5～1.5% of total mass, this MgO accounts for 5～25% of total mass, and surplus is ZnO, stirs to obtain mixture, and sintering forms magnetic control spattering target;
At the mixed gas with hydrogen and rare gas element is that working gas, underlayer temperature are to utilize this magnetic control spattering target to carry out magnetron sputtering under the 20-100 ℃ of condition to form film, obtains conducting film.
The embodiment of the invention further provides the conducting film of above-mentioned conducting film preparation method preparation, and the thickness of this conducting film is 280-395nm.
The embodiment of the invention also provides the application of above-mentioned conducting film in electroluminescent device, solar cell or field-effect transistor.
Embodiment of the invention preparation method, simple to operate, mild condition, raw material is cheap, and productivity is high, is very suitable for suitability for industrialized production; Simultaneously, through in the magnetron sputtering step, using hydrogen and argon gas, realized under coldcondition, utilizing magnetically controlled sputter method to prepare the excellent conducting film of conductivity as working gas.Embodiment of the invention conducting film through the Natural manganese dioxide that in Zinc oxide film, mixes, utilizes mg ion to widen the optical transmission window of Zinc oxide film, and the Zinc oxide film transmittance is increased greatly; Through doped alumina and silicon-dioxide, the electric conductivity of Zinc oxide film is strengthened greatly, thereby reduce the resistivity of Zinc oxide film; Doping through above-mentioned three kinds of materials simultaneously makes this conducting film keep its resistivity stable in the course of the work.
Description of drawings
Fig. 1 is an embodiment of the invention preparation method schema;
Fig. 2 is an embodiment of the invention conducting film transmitted spectrum;
Fig. 3 is an embodiment of the invention conducting film XRD figure;
Fig. 4 is that embodiment of the invention conducting film uses the change in resistance graphic representation after 48 hours under differing temps.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
See also Fig. 1, Fig. 1 shows embodiment of the invention conducting film preparation method flow process, comprises the steps:
S01, the preparation magnetic control spattering target
Mixed oxidization magnesium, aluminium sesquioxide and silicon-dioxide in zinc oxide; This aluminium sesquioxide accounts for 0.5～3% of total mass by mass percentage; 0.5～1.5% of this silica comprises total mass, this Natural manganese dioxide accounts for 5～25% of total mass, and surplus is a zinc oxide; Stirring obtains mixture, and sintering forms magnetic control spattering target;
S02, magnetron sputtering forms film
At the mixed gas with hydrogen and rare gas element is that working gas, underlayer temperature are to utilize said magnetic control spattering target to carry out magnetron sputtering under the 20-100 ℃ of condition to form film, obtains conducting film.
Among the step S01, mixed oxidization magnesium, aluminium sesquioxide and silicon-dioxide stir in zinc oxide, and all even zinc oxide of Natural manganese dioxide, aluminium sesquioxide and silicon-dioxide is evenly mixed, and form mixture.In this mixture, the quality percentage composition of four kinds of materials is following:
Aluminium sesquioxide 0.5～3%
Silicon-dioxide 0.5～3%
Natural manganese dioxide 5～25%
Zinc oxide is surplus.
The weight percentage of preferred zinc oxide is that the quality percentage composition of 75-90%, aluminium sesquioxide is 1-2.5%; The quality percentage composition of silicon-dioxide is 0.8-1.2%; Magnesian quality percentage composition is 6-20%.The zinc oxide that the embodiment of the invention is used, aluminium sesquioxide, silicon-dioxide and Natural manganese dioxide are powder structure, and particle diameter is 50～200nm.
Particularly, in the preparation magnetic control spattering target, sintering temperature is 900-1100 ℃, and atmosphere is non-reduced atmosphere, for example inert atmosphere or air atmosphere etc.The agglomerating time is 1-24 hour.Through high-temperature calcination, aluminium sesquioxide, silicon-dioxide and Natural manganese dioxide are doped in the lattice of zinc oxide, form sputtering target material, and this sputtering target material is Ф 50mm * 2mm; This inert atmosphere is helium atmosphere, argon gas atmosphere, neon atmosphere or nitrogen atmosphere.
Among the step S02, at first this magnetic control spattering target is put to the cavity of magnetron sputtering equipment, got substrate and be positioned in the cavity of this magnetron sputtering equipment, cavity is evacuated to 1.0 * 10 with mechanical pump and molecular pump
-3More than the Pa; Regulate then that spacing is the 50-90 millimeter between substrate and the target, and the adjustment underlayer temperature is to 20-100 ℃, preferred, underlayer temperature is 30-80 ℃; In operating pressure is 0.2～1.5Pa; And carried out under gas flow 15～25sccm condition sputter 1-3 hour, obtain conducting film, particularly; The gas that feeds in the magnetron sputtering is the mixed gas of hydrogen and rare gas element; Hydrogen accounts for the 1-5% of mixed gas TV, is preferably 2-4%, and this rare gas element is argon gas, helium, neon etc.In the magnetron sputtering with the part of hydrogen as working gas; Thereby can make Wasserstoffatoms enter in the zinc oxide lattice of conducting film doped with hydrogen element in zinc oxide lattice,, thereby in zinc oxide, introduce the hydrogen proton through doped with hydrogen element in zinc oxide; Because the nucleidic mass of protium is little; Can be at crystal boundary, move and the conductivity of enhancing conducting film in atom gap and the vacancy defect, realized at the depositing temperature that do not raise; Exist in the film on the basis of a large amount of crystal boundaries and defective, the electric conductivity of film is improved.
Particularly, the substrate that uses in this magnetron sputtering step is silica glass, and this silica glass is with acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning, and dries up with high pure nitrogen; Employed magnetron sputtering equipment is restriction not, can be the magnetron sputtering equipment of various models; The purity of employed zinc oxide, Natural manganese dioxide, silicon-dioxide and aluminium sesquioxide is all at the quality percentage composition more than 99.9%.
Further, after magnetron sputtering equipment vacuumized, vacuum tightness preferred 6.0 * 10
-4Pa; Simultaneously, spacing is preferably 60 millimeters between above-mentioned substrate and the target, and underlayer temperature is preferably 85 ℃, and operating pressure is preferably 1.0Pa and gas flow is preferably 20sccm.Parameter through in the magnetron sputtering is set to above-mentioned parameter, guarantees that prepared conductive film deposits speed is very fast, and zinc oxide, Natural manganese dioxide, silicon-dioxide and aluminium sesquioxide evenly mix according to the quality percentage composition in the sputtering target material in the conducting film.
Embodiment of the invention preparation method, simple to operate, mild condition, raw material is cheap, and productivity is high, is very suitable for suitability for industrialized production.
The embodiment of the invention further provides the conducting film of above-mentioned conducting film preparation method preparation; The thickness of this conducting film is the 280-395 nanometer; Measure the not restriction of this film thickness method, for example, sample surface profiles scanner (KLA Tencor P-16+Surface profiler).
Particularly; Embodiment of the invention conducting film; Mainly form conducting film by zinc oxide, simultaneously, silicon-dioxide, Natural manganese dioxide and aluminium sesquioxide are entrained in this Zinc oxide film; This zinc oxide, silicon-dioxide, Natural manganese dioxide, and aluminium sesquioxide evenly mix, realize that the conducting film transmittance is not piled up and the disadvantageous effect that produces by this imparity (Natural manganese dioxide, aluminium sesquioxide and silicon-dioxide).
See also Fig. 2; Fig. 2 shows embodiment of the invention conducting film transmitted spectrum; As can be seen from Figure 2, the conducting film of 3% time preparation that accounts for the mixed gas TV when hydrogen at the average transmittance of visible region all greater than 80%, preferred; The transmittance of conducting film is between 80-86%, and this conducting film has excellent light transmission.
See also Fig. 3; Fig. 3 shows embodiment of the invention conducting film XRD figure, as can be seen from Figure 3, has only (002) of zinc oxide and (004) to have peak value; Can explain that thus silicon-dioxide, Natural manganese dioxide and aluminium sesquioxide all get in the lattice of zinc oxide in the embodiment of the invention conducting film.
See also Fig. 4; Fig. 4 shows that embodiment of the invention conducting film uses the change in resistance curve after 48 hours under differing temps; As can beappreciated from fig. 4; In use the change in resistance amplitude is little for embodiment of the invention conducting film, under less than 200 ℃ of situation, uses 48 hours, and change in resistance is all less than 15%.
Embodiment of the invention conducting film through the Natural manganese dioxide that in Zinc oxide film, mixes, utilizes mg ion to widen the optical transmission window of Zinc oxide film, and the Zinc oxide film transmittance is increased greatly; Through doped alumina and silicon-dioxide; Owing to contain trivalent aluminium ion in the aluminium sesquioxide, contain the tetravalence silicon ion in the silicon-dioxide, thereby in Zinc oxide film, form electronic carrier; The electric conductivity of Zinc oxide film is strengthened greatly, thereby reduce the resistivity of Zinc oxide film; Simultaneously, multiple element doping makes this conducting film keep its resistivity stable in the course of the work in Zinc oxide film.
The embodiment of the invention also provides the application of above-mentioned conducting film in electroluminescent device, solar cell or field-effect transistor.
Below in conjunction with specific embodiment embodiment of the invention preparation method is set forth in detail.
Embodiment one
With following components in weight percentage content uniform mixing, calcining is 12 hours under 1000 ℃ air ambient, forms the ceramic sputtering target material of Ф 50 * 2mm, and this sputtering target material is packed in the magnetron sputtering equipment vacuum cavity,
Account for 77.5% of total mass, Al according to mass percent ZnO
2O
3Account for 1.5% of total mass, SiO
21% and the MgO that account for total mass account for 20% of total mass;
With acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning silica glass, and dry up, put into above-mentioned magnetron sputtering equipment vacuum cavity with high pure nitrogen;
The distance of adjusting this sputtering target material and silica glass is 60mm, with mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa feeds the mixed gas of hydrogen and argon gas, and hydrogen content is 1% (mol ratio), and to adjust gas flow be 20sccm, and pressure is 1.0Pa, and the silica glass temperature is 50 ℃, carries out magnetron sputtering, deposits 2 hours, obtains conducting film.
Embodiment two
With following components in weight percentage content uniform mixing, calcining is 1 hour under 1100 ℃ air ambient, forms the ceramic sputtering target material of Ф 50 * 2mm, and this sputtering target material is packed in the magnetron sputtering equipment vacuum cavity,
Account for 90% of total mass, Al according to mass percent ZnO
2O
3Account for 2% of total mass, SiO
21% and the MgO that account for total mass account for 7% of total mass;
With acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning silica glass, and dry up, put into above-mentioned magnetron sputtering equipment vacuum cavity with high pure nitrogen;
The distance of adjusting this sputtering target material and silica glass is 90mm, with mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 1.0 * 10
-3Pa feeds the mixed gas of hydrogen and argon gas, and hydrogen content is 2% (mol ratio), and to adjust gas flow be 25sccm, and pressure is 1.5Pa, and the silica glass temperature is 30 ℃, carries out magnetron sputtering, deposits 3 hours, obtains conducting film.
Embodiment three
With following components in weight percentage content uniform mixing, calcining is 24 hours under 900 ℃ air ambient, forms the ceramic sputtering target material of Ф 50 * 2mm, and this sputtering target material is packed in the magnetron sputtering equipment vacuum cavity,
Account for 73% of total mass, Al according to mass percent ZnO
2O
3Account for 0.5% of total mass, SiO
21.5% and the MgO that account for total mass account for 25% of total mass;
With acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning silica glass, and dry up, put into above-mentioned magnetron sputtering equipment vacuum cavity with high pure nitrogen;
The distance of adjusting this sputtering target material and silica glass is 50mm, with mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa feeds the mixed gas of hydrogen and argon gas, and hydrogen content is 3% (mol ratio), and to adjust gas flow be 15sccm, and pressure is 0.2Pa, and the silica glass temperature is 60 ℃, carries out magnetron sputtering, deposits 1 hour, obtains conducting film.
Embodiment four
With following components in weight percentage content uniform mixing, calcining is 12 hours under 900 ℃ air ambient, forms the ceramic sputtering target material of Ф 50 * 2mm, and this sputtering target material is packed in the magnetron sputtering equipment vacuum cavity,
Account for 80% of total mass, Al according to mass percent ZnO
2O
3Account for 3% of total mass, SiO
21% and the MgO that account for total mass account for 16% of total mass;
With acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning silica glass, and dry up, put into above-mentioned magnetron sputtering equipment vacuum cavity with high pure nitrogen;
The distance of adjusting this sputtering target material and silica glass is 50mm, with mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa feeds the mixed gas of hydrogen and argon gas, and hydrogen content is 4% (mol ratio), and to adjust gas flow be 15sccm, and pressure is 0.2Pa, and the silica glass temperature is 100 ℃, carries out magnetron sputtering, deposits 1 hour, obtains conducting film.
Embodiment five
With following components in weight percentage content uniform mixing, calcining is 20 hours under 900 ℃ air ambient, forms the ceramic sputtering target material of Ф 50 * 2mm, and this sputtering target material is packed in the magnetron sputtering equipment vacuum cavity,
Account for 77.5% of total mass, Al according to mass percent ZnO
2O
3Account for 1.5% of total mass, SiO
21% and the MgO that account for total mass account for 20% of total mass;
With acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning silica glass, and dry up, put into above-mentioned magnetron sputtering equipment vacuum cavity with high pure nitrogen;
The distance of adjusting this sputtering target material and silica glass is 65mm, with mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 7.0 * 10
-4Pa feeds the mixed gas of hydrogen and argon gas, and hydrogen content is 3% (mol ratio), and to adjust gas flow be 18sccm, and pressure is 1.3Pa, and the silica glass temperature is 80 ℃, carries out magnetron sputtering, deposits 1.5 hours, obtains conducting film.
Embodiment six
With following components in weight percentage content uniform mixing, calcining is 16 hours under 950 ℃ air ambient, forms the ceramic sputtering target material of Ф 50 * 2mm, and this sputtering target material is packed in the magnetron sputtering equipment vacuum cavity,
Account for 73% of total mass, Al according to mass percent ZnO
2O
3Account for 0.5% of total mass, SiO
21.5% with MgO account for 25% of total mass;
With acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning silica glass, and dry up, put into above-mentioned magnetron sputtering equipment vacuum cavity with high pure nitrogen;
The distance of adjusting this sputtering target material and silica glass is 50mm, with mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 6.0 * 10
-4Pa feeds the mixed gas of hydrogen and argon gas, and hydrogen content is 5% (mol ratio), and to adjust gas flow be 21sccm, and pressure is 1.1Pa, and the silica glass temperature is 20 ℃, carries out magnetron sputtering, deposits 1.5 hours, obtains conducting film.
See also table 1 and table 2, table 1 shows the conducting film resistivity of the embodiment of the invention one to six preparation method preparation; Table 2 shows the conducting film thickness of the embodiment of the invention one to six preparation method preparation:
Table 1
Can know that from table 1 embodiment of the invention one to five prepared conducting film has excellent conductivity and light transmission.The performance of the conducting film that embodiment six preparing methods are prepared is similar with embodiment's one to five, does not repeat to set forth at this.
Table 2
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a conducting film preparation method comprises the steps:
Mixed oxidization magnesium, aluminium sesquioxide and silicon-dioxide in zinc oxide; Said by mass percentage aluminium sesquioxide accounts for 0.5～3% of total mass; 0.5～1.5% of said silica comprises total mass, said Natural manganese dioxide accounts for 5～25% of total mass, and surplus is a zinc oxide; Stirring obtains mixture, and sintering forms magnetic control spattering target;
At the mixed gas with hydrogen and rare gas element is that working gas, underlayer temperature are to utilize said magnetic control spattering target to carry out magnetron sputtering under the 20-100 ℃ of condition to form film, obtains conducting film.
2. conducting film preparation method as claimed in claim 1 is characterized in that, hydrogen volume is the 1-5% of mixed gas TV in the said mixed gas.
3. conducting film preparation method as claimed in claim 1 is characterized in that, hydrogen volume is the 2-4% of mixed gas TV in the said mixed gas.
4. conducting film preparation method as claimed in claim 1; It is characterized in that; Said magnetron sputtering step is for to put said magnetic control spattering target to the magnetron sputtering equipment cavity, gets substrate and is positioned in the said magnetron sputtering equipment cavity, and said cavity is evacuated to 1.0 * 10
-3More than the Pa, regulate that spacing is the 50-90 millimeter between said substrate and the sputtering target material, adjusting said underlayer temperature is 20-100 ℃, is 0.2～1.5Pa in operating pressure, and carries out sputter 1-3 hour under gas flow 15～25sccm condition.
5. conducting film preparation method as claimed in claim 1 is characterized in that, zinc oxide, aluminium sesquioxide, silicon-dioxide and magnesian quality percentage composition are following in the said mixture:
Aluminium sesquioxide 1～2.5%
Silicon-dioxide 0.8～1.2%
Natural manganese dioxide 6～20%,
Surplus is a zinc oxide.
6. conducting film preparation method as claimed in claim 1 is characterized in that, said underlayer temperature is 30-80 ℃.
7. conducting film preparation method as claimed in claim 1 is characterized in that, sintering temperature is 900-1100 ℃ in the said sintering formation sputtering target material step, and the time is 1-24 hour.
8. like the conducting film of each described conducting film preparation method preparation of claim 1-6, it is characterized in that the thickness of said conducting film is 280-395nm.
9. conducting film as claimed in claim 8 is characterized in that, the transmittance of said conducting film is 80-86%.
10. each described conducting film application in solar cell, electroluminescent device or field-effect transistor of claim 8-9.
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| CN104487402A (en) * | 2012-07-13 | 2015-04-01 | 吉坤日矿日石金属株式会社 | Sintered body and amorphous film |
| CN106380193A (en) * | 2016-08-29 | 2017-02-08 | 基迈克材料科技（苏州）有限公司 | Preparation method of MgO-doped ZnO sputtering target material |
| CN109147990A (en) * | 2018-08-09 | 2019-01-04 | 盐城美茵新材料有限公司 | A kind of single side jet printing type conductive film and preparation method thereof |
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| CN109147990A (en) * | 2018-08-09 | 2019-01-04 | 盐城美茵新材料有限公司 | A kind of single side jet printing type conductive film and preparation method thereof |
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Application publication date: 20120711 |