CN103993281A - Preparation method of FTO (F-doped SiO2) transparent conducting thin film - Google Patents
Preparation method of FTO (F-doped SiO2) transparent conducting thin film Download PDFInfo
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- CN103993281A CN103993281A CN201410238871.7A CN201410238871A CN103993281A CN 103993281 A CN103993281 A CN 103993281A CN 201410238871 A CN201410238871 A CN 201410238871A CN 103993281 A CN103993281 A CN 103993281A
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- preparation
- fto
- thin film
- transparent conductive
- conductive film
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Abstract
The invention discloses a preparation method of an FTO (F-doped SiO2) transparent conducting thin film. An isostatic pressing solid-phase reaction synthesis process is adopted for preparing an FTO target material, namely SnO2-0.5xFx (x is more than or equal to 0.04 and less than or equal to 0.3), a magnetron sputtering deposition technology is utilized, and Ar and O2 are adopted as sputtering gases, and an FTO transparent conducting thin film with the thickness of 200-700nm is deposited. The preparation method of the FTO transparent conducting thin film has the advantages that specific resistance of the thin film is obviously reduced, carrier concentration in the thin film is increased, large-scale production can be realized, a process is simple, cost is low, the prepared thin film has a smooth and flat surface, contains dense and uniform crystals and has low specific resistance, high transparency, repeatability and stability; transmittance of the thin film is more than or equal to 80%, and specific resistance is less than 5.0*10<-3>ohm.cm.
Description
Technical field
The invention relates to electronic information material and components and parts, particularly a kind of is the preparation method of FTO transparent conductive film with magnetron sputtering deposition legal system for the tindioxide of F doping.
Background technology
Transparent conductive oxide (TCO) film is owing to having high transmission of visible light and low resistivity, at aspects such as antistatic coating, touch display screen, solar cell, flat pannel display, calorifier, anti-icing equipment, optical coating and transparent optical electronics, have vast potential for future development, representative TCO film is wherein In
2o
3: Sn (ITO) film, has good photoelectric properties.For traditional ito thin film, tindioxide base film is cheap, nontoxic in price, and in atmospheric environment chemical stability and thermostability all fine.Pure tin dioxide thin film photoelectric property is not satisfactory, and in order to improve its optical property and electrical properties, F studied person mixes in tindioxide and is studied as impurity.The preparation method of tin dioxide thin film mainly contains: the technology such as chemical vapour deposition, pulsed laser deposition, spray pyrolysis, sol-gel.
Although pulsed laser deposition can be prepared high-quality film, is unfavorable for scale operation; Spray pyrolysis and sol-gel belong to chemical preparation process, and film quality is relatively low, are also unfavorable for large-scale production.Although chemical vapour deposition can scale operation, its shortcoming is that equipment is complicated and expensive, and F source toxicity used is larger.So, find the technology of preparing that a kind of technique is simple, cost is low and prepare FTO film, will more be conducive to advance the commercial application of FTO film.
Summary of the invention
Object of the present invention, is to prepare for overcoming prior art the shortcoming and defect that FTO film exists, and provides a kind of magnetron sputtering deposition legal system that adopts for the preparation method of F doping stannic oxide transparent conductive film.
The present invention is achieved by following technical solution.
A preparation method who prepares FTO transparent conductive film, has following steps:
(1) employing waits static pressure solid state reaction synthesis technique to prepare the target that FTO is the tindioxide of F doping
Press SnO
2-0.5xf
x, wherein the stoichiometric ratio of 0.04≤x≤0.3 corresponding element takes SnO
2and SnF
2powder, after fully mixing, first pre-molding, then adopts isostatic cool pressing, is finally placed in electric furnace in 1000 ℃ of targets that are fired into FTO;
(2) clean dry substrate is put into magnetic control sputtering system reaction chamber;
(3) the base vacuum degree of magnetic control sputtering system is evacuated to 1.0 * 10
-5t
obelow rr, heated substrate to 500～700 ℃ then;
(4), in step 3 system, use Ar and O
2as sputter gas, sputtering power is 50～200W, and the intrinsic standoff ratio of oxygen and argon gas, 0.02～0.2, deposits and obtains the FTO transparent conductive film that thickness is 200～700nm.
The SnO of described step (1)
2and SnF
2the purity of raw material is all more than 99.9%.
The firing condition of the FTO target of described step (1) is: be progressively warming up to 200 ℃ of insulations 10 hours, and then be progressively warming up to 1000 ℃ of insulations 2 hours.
The substrate of described step (2) is glass, quartz or Si substrate.
Ar and the O of described step (4)
2purity all more than 99.99%.
The film thickness of described step (4) is by regulating preparation technology parameter or depositing time to control, and the resistivity of film is by regulating the content of the F in target and the oxygen partial pressure in preparation process to control.
Beneficial effect of the present invention is as follows:
(1) magnetron sputtering method of the present invention makes F uniform ion be doped in SnO
2in, the introducing of F can significantly reduce the resistivity of film, improves the carrier concentration in film, and obtains high-quality film, for the application of opto-electronic device provides good material foundation.
(2) preparation method of the present invention can big area large-scale production, and technique is simple, and cost is low, the SnO of prepared F doping
2transparent conductive film surfacing, compact crystallization, even particle size, has low-resistivity, high transparent, repeatability and stability; Transmitance>=80% of film, resistivity <5.0 * 10
-3Ω cm.
Accompanying drawing explanation
Fig. 1 is the SnO of embodiment 1
1.92f
0.16the XRD figure spectrum of film;
Fig. 2 is the preparation of embodiment 1 SnO on silica glass substrate
1.92f
0.16the electron scanning micrograph of film;
Fig. 3 is the preparation of embodiment 1 SnO on silica glass substrate
1.92f
0.16the optical transmittance of film (ultraviolet-visible spectrum) collection of illustrative plates.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
With 16% mole of F doping SnO
2.
(1) adopt the static pressure solid state reaction synthesis technique that waits of standard to prepare SnO
1.92f
0.16target:
With electronic balance, press SnO
1.92f
0.16the stoichiometric ratio of corresponding element take SnO
2and SnF
2powder, purity is 99.9%, after sufficiently mixing, first pre-molding (50MPa), then adopts isostatic cool pressing (200MPa), is finally placed in electric furnace and is progressively warming up to 200 ℃ of insulations 10 hours, progressively be warming up to again 1000 ℃ of insulations 2 hours, make SnO
1.
92f
0.
16target.
(2) silica glass substrate is cleaned, with N
2dry up and put into magnetron sputtering preparation room.
(3) the base vacuum degree of magnetic control sputtering system is evacuated to 7.0 * 10
-6torr, then heated substrate to 700 ℃.
(4) with high-purity (99.99%) Ar and O
2as sputter gas, the throughput ratio of argon gas and oxygen is 30:1, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the F doping SnO that thickness is 200nm
2film.
Obtain after testing Fig. 1～3.
Fig. 1 is the SnO of the F doping of embodiment 1
2the XRD figure spectrum of film, the crystalline property of visible gained is good.
Fig. 2 is the preparation of embodiment 1 SnO on silica glass substrate
1.92f
0.16film scanning electron micrograph, visible resulting SnO
1.92f
0.16film surface is smooth, uniform particles.
Fig. 3 is the preparation of embodiment 1 SnO on silica glass substrate
1.92f
0.16film Optics through performance (ultraviolet-visible spectrum) collection of illustrative plates, visible average optical transmitance in visible-range reaches 85%.
The conductivity of the FTO transparent conductive film of gained is as shown in table 1 after testing, and the resistivity of film is low to moderate 2.1 * 10
-3Ω cm, carrier concentration is 1.36 * 10
20cm
-3, carrier mobility is 21.9cm
2v
-1s
-1.
Embodiment 2
With 30% mole of F doping SnO
2.
(1) adopt the static pressure solid state reaction synthesis technique that waits of standard to prepare SnO
1.85f
0.3target, presses SnO with electronic balance
1.92f
0.16the stoichiometric ratio of corresponding element take SnO
2and SnF
2powder, purity is 99.9%, after sufficiently mixing, first pre-molding (50MPa), then adopts isostatic cool pressing (200MPa), is finally placed in electric furnace and is progressively warming up to 200 ℃ of insulations 10 hours, progressively be warming up to again 1000 ℃ of insulations 2 hours, make SnO
1.85f
0.3target.
(2) silica glass substrate is cleaned, with N
2dry up and put into magnetron sputtering preparation room.
(3) the base vacuum degree of magnetic control sputtering system is evacuated to 7.0 * 10
-6torr, then heated substrate to 700 ℃.
(4) with high-purity (99.99%) Ar and O
2as sputter gas, the throughput ratio of argon gas and oxygen is 30:1, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the SnO that thickness is the F doping of 200nm
2film.
The conductivity of the FTO transparent conductive film of gained is as shown in table 1 after testing, and the resistivity of film is low to moderate 3.9 * 10
-3Ω cm, carrier concentration is 0.89 * 10
20cm
-3, carrier mobility is 18.2cm
2v
-1s
-1.
Embodiment 3
With 4% mole of F doping SnO
2.
(1) adopt the static pressure solid state reaction synthesis technique that waits of standard to prepare SnO
1.98f
0.04target, presses SnO with electronic balance
1.92f
0.16the stoichiometric ratio of corresponding element take SnO
2and SnF
2powder, purity is 99.9%.After sufficiently mixing, first pre-molding (50MPa), then adopts isostatic cool pressing (200MPa), is finally placed in electric furnace and is progressively warming up to 200 ℃ of insulations 10 hours, is then progressively warming up to 1000 ℃ of insulations 2 hours, makes SnO
1.98f
0.04target.
(2) silica glass substrate is cleaned, with N
2dry up and put into magnetron sputtering preparation room.
(3) the base vacuum degree of magnetic control sputtering system is evacuated to 7.0 * 10
-6torr, then heated substrate to 700 ℃.
(4) with high-purity (99.99%) Ar and O
2as sputter gas, the throughput ratio of argon gas and oxygen is 30:1, and sputtering pressure is 10mTorr, and sputtering power is 150W, deposits and obtains the SnO that thickness is the F doping of 700nm
2film.
The conductivity of the FTO transparent conductive film of gained is as shown in table 1 after testing, and the resistivity of film is low to moderate 4.9 * 10
-3Ω cm, carrier concentration is 0.56 * 10
20cm
-3, carrier mobility is 22.6cm
2v
-1s
-1.
Table 1
Claims (6)
1. a preparation method who prepares FTO transparent conductive film, has following steps:
(1) employing waits static pressure solid state reaction synthesis technique to prepare the target that FTO is the tindioxide of F doping
Press SnO
2-0.5xf
x, wherein the stoichiometric ratio of 0.04≤x≤0.3 corresponding element takes SnO
2and SnF
2powder, after fully mixing, first pre-molding, then adopts isostatic cool pressing, is finally placed in electric furnace in 1000 ℃ of targets that are fired into FTO;
(2) clean dry substrate is put into magnetic control sputtering system reaction chamber;
(3) the base vacuum degree of magnetic control sputtering system is evacuated to 1.0 * 10
-5below Torr, heated substrate to 500～700 ℃ then;
(4), in step 3 system, use Ar and O
2as sputter gas, sputtering power is 50～200W, and the intrinsic standoff ratio of oxygen and argon gas, 0.02～0.2, deposits and obtains the FTO transparent conductive film that thickness is 200～700nm.
2. a kind of preparation method who prepares FTO transparent conductive film according to claim 1, is characterized in that, the SnO of described step (1)
2and SnF
2the purity of raw material is all more than 99.9%.
3. a kind of preparation method who prepares FTO transparent conductive film according to claim 1, it is characterized in that, the firing condition of the FTO target of described step (1) is: be progressively warming up to 200 ℃ of insulations 10 hours, and then be progressively warming up to 1000 ℃ of insulations 2 hours.
4. a kind of preparation method who prepares FTO transparent conductive film according to claim 1, is characterized in that, the substrate of described step (2) is glass, quartz or Si substrate.
5. a kind of preparation method who prepares FTO transparent conductive film according to claim 1, is characterized in that, Ar and the O of described step (4)
2purity all more than 99.99%.
6. a kind of preparation method who prepares FTO transparent conductive film according to claim 1, it is characterized in that, the film thickness of described step (4) is by regulating preparation technology parameter or depositing time to control, and the resistivity of film is by regulating the content of the F in target and the oxygen partial pressure in preparation process to control.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338318A (en) * | 2018-09-30 | 2019-02-15 | 武汉科技大学 | On flexible substrate surface, preparation F adulterates SnO2The method of transparent conductive film |
| EP4328355A2 (en) | 2022-08-23 | 2024-02-28 | Indian Oil Corporation Limited | Process of reusing bi-facial metal substrates for photoactive semiconductor materials for solar water splitting |
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| CN101705467A (en) * | 2009-05-14 | 2010-05-12 | 上海高展金属材料有限公司 | Method for preparing rotary ceramic target |
| CN101752260A (en) * | 2008-12-09 | 2010-06-23 | 上海广电电子股份有限公司 | Method for manufacturing oxide semiconductor active layer of thin film transistor |
| CN102839348A (en) * | 2012-09-27 | 2012-12-26 | 攀枝花学院 | Method for preparing fluorine-doped tin oxide thin film |
| CN103695856A (en) * | 2013-12-24 | 2014-04-02 | 滨州学院 | Flexible F-doped SnO2 transparent conducting thin film and preparation method thereof |
-
2014
- 2014-05-30 CN CN201410238871.7A patent/CN103993281A/en active Pending
Patent Citations (6)
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| CN101175347A (en) * | 2007-11-28 | 2008-05-07 | 上海广电电子股份有限公司 | Production method for oxide luminescent layer in inorganic electroluminescence display device |
| CN101752260A (en) * | 2008-12-09 | 2010-06-23 | 上海广电电子股份有限公司 | Method for manufacturing oxide semiconductor active layer of thin film transistor |
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| CN101638772A (en) * | 2009-08-17 | 2010-02-03 | 鲁东大学 | Method for preparing fluorine doped tin oxide transparent conductive film |
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|---|---|---|---|---|
| CN109338318A (en) * | 2018-09-30 | 2019-02-15 | 武汉科技大学 | On flexible substrate surface, preparation F adulterates SnO2The method of transparent conductive film |
| EP4328355A2 (en) | 2022-08-23 | 2024-02-28 | Indian Oil Corporation Limited | Process of reusing bi-facial metal substrates for photoactive semiconductor materials for solar water splitting |
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Application publication date: 20140820 |