CN104726851A - Method for preparing p-type tin oxide film material by using sol-gel method - Google Patents
Method for preparing p-type tin oxide film material by using sol-gel method Download PDFInfo
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- CN104726851A CN104726851A CN201510143623.9A CN201510143623A CN104726851A CN 104726851 A CN104726851 A CN 104726851A CN 201510143623 A CN201510143623 A CN 201510143623A CN 104726851 A CN104726851 A CN 104726851A
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Abstract
The invention provides a method for preparing a p-type tin oxide film material by using a sol-gel method. The method comprises the following steps: mixing ethylene glycol monomethyl ether, stannous chloride dehydrate and ethanolamine in a vessel, transferring a solution in a vacuum tubular furnace, vacuumizing and inflating argon, heating, and ageing after heating; performing ultrasonic cleaning on a substrate, fixing the substrate on a spinner, instilling the sol on the substrate, carrying out spin coating and spinning to prepare a film sample; after the spinning is finished, transferring the film sample to the vacuum tubular furnace, vacuumizing and introducing argon, heating and drying the film sample; repeating above steps until the coating layer number of the substrate achieves the required layer number; and annealing, naturally cooling after the annealing is finished, thereby obtaining the p-type tin oxide film material. Through the adoption of the method, a multi-component phase can be uniformly mixed, the film-forming is uniform, the component is easy to control, the thickness of the film is thin, the cost is low, and the period is short; therefore, the method is suitable for industrial production.
Description
Technical field
The invention provides one and prepare SnO
xthe method of thin-film material, particularly relates to the p-type SnO that the preparation of a kind of sol-gel method has high mobility
xthe method of thin-film material, belongs to electronics, information, display, semiconductor film technique field.
Background technology
Along with the high speed development of information display technology, wearable technique of display is arisen at the historic moment, the important component part that transparent electron will be Future Information technique of display.Wherein, the N-shaped oxide thin film transistor bipolar thin film transistor formed that combines with p-type oxide thin film transistor is the basis realizing transparent electronics.P-type oxide film, due to hole conduction, is made thin film transistor, will advantageously in driving Organic Light Emitting Diode high aperture ratio pixel unit.Meanwhile, if the thin film transistor of p-type oxide can combine with flat panel display, screen will be made more clear.
But now studies have found that, the electric property of p-type oxide also far can cannot match with the electrology characteristic of N-shaped oxide compound, which greatly limits the development of oxide compound PN junction, transparent oxide large-scale integrated circuit.In recent years, stannic oxide and doping system thereof are considered to the huge p-type oxide of application potential.So the p-type SnO that preparation high-performance, structure and physical properties is stable
xtransparent conductive film has very large value and important meaning in p-type oxide transparent conductive film field.
Summary of the invention
The invention provides a kind of method that sol-gel method prepares p-type SnO 2 thin film material, solve the deficiency in background technology, the method has Multicomponent phase can Homogeneous phase mixing, the advantage such as film forming is even, composition is easy to control, the thinner thickness of film, cost are low, the cycle is short, is therefore suitable for suitability for industrialized production.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of sol-gel method prepares the method for p-type SnO 2 thin film material, comprise the following steps: (1), ethylene glycol monomethyl ether, stannous chloride dihydrate and the thanomin mol ratio according to 6.5 ~ 7:0.15 ~ 0.2:0.8 ~ 1 is mixed and stirs to clarify in vessel, then solution is moved in vacuum tube furnace, vacuumize and be filled with argon gas, to solution heating 1 ~ 2 hour under 80 ~ 100 DEG C of conditions, after heating, solution is continued ageing 1 ~ 2 day in argon gas atmosphere, obtained colloidal sol;
(2), with acetone, dehydrated alcohol and deionized water, ultrasonic cleaning is carried out to substrate successively;
(3), by substrate be fixed on sol evenning machine, rotate, substrate drips colloidal sol with the speed of 2000 ~ 2500 revs/min, carry out revolving Tu whirl coating, rotational time is 20 ~ 30 seconds, obtained film sample;
(4), after whirl coating terminates, moved to by film sample in vacuum tube furnace, vacuumize and pass into argon gas, then carry out heat drying to film sample, drying terminates rear naturally cooling;
(5), repeating step (3) and (4), until the number of plies that substrate applies reaches the required number of plies;
(6), film sample obtained in upper step is annealed, annealing temperature is 600 ~ 650 DEG C, and soaking time is 30 ~ 40 minutes, and the heat-up rate in annealing process is 1 ~ 2 DEG C/min, to anneal rear naturally cooling, i.e. obtained described p-type SnO 2 thin film material.
Substrate described in step (2) is insulation SiO
2/ Si substrate, substrate is of a size of 10mm × 10mm, SiO on substrate
2the thickness 500nm of layer.
In step (3), the rotating speed of sol evenning machine is 2000 revs/min, and rotational time is 20 seconds.
In step (6), annealing temperature is 600 DEG C, and soaking time is 30 minutes, and the heat-up rate in annealing process is 1 DEG C/min.
Compared with prior art, the present invention has the following advantages: 1, present invention employs sol-gel method, therefore in preparation process, Multicomponent phase can Homogeneous phase mixing, the advantage such as film forming is even, composition is easy to control, the thinner thickness of film, cost are low, the cycle is short, is therefore suitable for suitability for industrialized production.2, the square resistance of p-type SnO 2 thin film material prepared by method provided by the present invention is adopted to be 2.7 × 10
5~ 2.8 × 10
5Ω/, hall mobility is 6 ~ 12cm
2v
-1s
-1, hole is 2.0 × 10
12~ 3.6 × 10
12cm
-2.
Accompanying drawing explanation
Fig. 1 is p-type SnO prepared in the embodiment of the present invention 1
xthe XRD test result figure of thin-film material.
Embodiment
Below in conjunction with specific embodiment, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
The p-type SnO provided in the present embodiment
xthe preparation method of thin-film material is as follows: (1), by ethylene glycol monomethyl ether 0.065mol, stannous chloride dihydrate 0.002mol and thanomin 0.01mol, mix in vessel and stir to clarify, then solution is moved in vacuum tube furnace, after tube furnace internal medium being bled reach required vacuum state with mechanical pump, be filled with argon gas.Under 90 DEG C of conditions, 1.5 hours are heated to solution, after heating, solution is continued ageing 1.5 days in argon gas atmosphere, obtained colloidal sol.Because stannous chemical property is active, in atmosphere just can be oxidized very soon, so configuration sol-process must be rapid, in order to avoid Bivalent Tin is oxidized.The concentration of tin is too high, and when annealing, ion agglomeration can occur, so want concentration as far as possible little.The consumption of stablizer will be determined according to the consumption of tin, not easily forms colloidal sol very little, too much on the mobility of colloidal sol and and the matching of substrate have impact.Heating temperature and the synthesis speed of colloidal sol network can be affected heat-up time, digestion time then can affect the quality of solute particles dispersiveness and the formation of network in colloid, digestion time is too short, Bivalent Tin cannot be uniformly dispersed in solvent network, network forms poor quality, and then affects the quality of colloidal sol.
(2), with acetone, dehydrated alcohol, deionized water, ultrasonic cleaning is carried out respectively once to substrate respectively.Described substrate is insulation SiO
2/ Si substrate, substrate is of a size of 10mm × 10mm, SiO on substrate
2the thickness 500nm of layer.
(3), by substrate be fixed on sol evenning machine, rotate, substrate drips colloidal sol with the speed of 2000 revs/min, carry out revolving Tu whirl coating, rotational time is 25 seconds, obtained film sample.
(4), after whirl coating terminates, moved to by film sample in vacuum tube furnace, vacuumize and pass into argon gas, then carry out heat drying to film sample, drying terminates rear naturally cooling.Because sinter under the environment that oxygen level is few, the carbon in sample is difficult to perfect combustion, easily carbonization occurs, so extend soaking time in the cryodrying stage as far as possible, to drop to minimum by the content of carbon.
(5), repeating step (3) and (4), until the number of plies that substrate applies reaches the required number of plies.
(6), by film sample obtained in upper step anneal, annealing temperature is 600 DEG C, and soaking time is 30 minutes, and the heat-up rate in annealing process is 1 DEG C/min, rear naturally cooling of having annealed, i.e. obtained described p-type SnO 2 thin film material.P-type SnO prepared in the present embodiment
xthin-film material XRD test result figure as shown in Figure 1, SnO
xfilm has 4 obvious diffraction peaks.Four directions SnO
2characteristic peak (110), the characteristic peak (002) of cubic SnO.The diffraction peak (021) of Si and (311) in substrate.Detected by XRD and demarcate, can determine that our sample has SnO and SnO
2hybrid films, therefore we are called SnO
xfilm.
Carry out the test of electric property after sample preparation terminates, thin-film material electric property is as shown in the table:
Table 1 shows SnO of the present invention
xthe measuring result of film rectangular resistance, hole, mobility.The electric property of sample tests 6 times repeatedly, all shows p-type electrology characteristic, and prepared p-type SnO 2 thin film material square resistance is 2.7 × 10
5~ 2.8 × 10
5Ω/, hall mobility is 6 ~ 12cm
2v
-1s
-1, hole is 2.0 × 10
12~ 3.6 × 10
12cm
-2.
Embodiment 2
The p-type SnO provided in the present embodiment
xthe preparation method of thin-film material is as follows: (1), by ethylene glycol monomethyl ether 0.07mol, stannous chloride dihydrate 0.0015mol and thanomin 0.008mol, mix in vessel and stir to clarify, then solution is moved in vacuum tube furnace, after tube furnace internal medium being bled reach required vacuum state with mechanical pump, be filled with argon gas.Under 80 DEG C of conditions, 2 hours are heated to solution, after heating, solution is continued ageing 3 days in argon gas atmosphere, obtained colloidal sol.
(2), with acetone, dehydrated alcohol, deionized water, ultrasonic cleaning is carried out respectively once to substrate respectively.Described substrate is insulation SiO
2/ Si substrate, substrate is of a size of 10mm × 10mm, SiO on substrate
2the thickness 500nm of layer.
(3), by substrate be fixed on sol evenning machine, rotate, substrate drips colloidal sol with the speed of 2500 revs/min, carry out revolving Tu whirl coating, rotational time is 30 seconds, obtained film sample.
(4), after whirl coating terminates, moved to by film sample in vacuum tube furnace, vacuumize and pass into argon gas, then carry out heat drying to film sample, drying terminates rear naturally cooling.Because sinter under the environment that oxygen level is few, the carbon in sample is difficult to perfect combustion, easily carbonization occurs, so extend soaking time in the cryodrying stage as far as possible, to drop to minimum by the content of carbon.
(5), repeating step (3) and (4), until the number of plies that substrate applies reaches the required number of plies.
(6), by film sample obtained in upper step anneal, annealing temperature is 650 DEG C, and soaking time is 40 minutes, and the heat-up rate in annealing process is 2 DEG C/min, rear naturally cooling of having annealed, i.e. obtained described p-type SnO 2 thin film material.
Claims (5)
1. a sol-gel method prepares the method for p-type SnO 2 thin film material, it is characterized in that comprising the following steps: (1), ethylene glycol monomethyl ether, stannous chloride dihydrate and the thanomin mol ratio according to 6.5 ~ 7:0.15 ~ 0.2:0.8 ~ 1 is mixed and stirs to clarify in vessel, then solution is moved in vacuum tube furnace, vacuumize and be filled with argon gas, to solution heating 1 ~ 2 hour under 80 ~ 100 DEG C of conditions, after heating, solution is continued ageing 1 ~ 2 day in argon gas atmosphere, obtained colloidal sol;
(2), with acetone, dehydrated alcohol and deionized water, ultrasonic cleaning is carried out to substrate successively;
(3), by substrate be fixed on sol evenning machine, rotate, substrate drips colloidal sol with the speed of 2000 ~ 2500 revs/min, carry out revolving Tu whirl coating, rotational time is 20 ~ 30 seconds, obtained film sample;
(4), after whirl coating terminates, moved to by film sample in vacuum tube furnace, vacuumize and pass into argon gas, then carry out heat drying to film sample, drying terminates rear naturally cooling;
(5), repeating step (3) and (4), until the number of plies that substrate applies reaches the required number of plies;
(6), film sample obtained in upper step is annealed, annealing temperature is 600 ~ 650 DEG C, and soaking time is 30 ~ 40 minutes, and the heat-up rate in annealing process is 1 ~ 2 DEG C/min, to anneal rear naturally cooling, i.e. obtained described p-type SnO 2 thin film material.
2. the method preparing p-type SnO 2 thin film material according to claim 1, is characterized in that: the square resistance of prepared p-type SnO 2 thin film material is 2.7 × 10
5~ 2.8 × 10
5Ω/, hall mobility is 6 ~ 12cm
2v
-1s
-1, hole is 2.0 × 10
12~ 3.6 × 10
12cm
-2.
3. the method preparing p-type SnO 2 thin film material according to claim 1, is characterized in that: the substrate described in step (2) is insulation SiO
2/ Si substrate, substrate is of a size of 10mm × 10mm, SiO on substrate
2the thickness 500nm of layer.
4. the method preparing p-type SnO 2 thin film material according to claim 1, is characterized in that: in step (3), the rotating speed of sol evenning machine is 2000 revs/min, and rotational time is 20 seconds.
5. the method preparing p-type SnO 2 thin film material according to claim 1, is characterized in that: in step (6), annealing temperature is 600 DEG C, and soaking time is 30 minutes, and the heat-up rate in annealing process is 1 DEG C/min.
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| CN201510143623.9A CN104726851B (en) | 2015-03-30 | 2015-03-30 | A kind of method that sol-gal process prepares p-type SnO 2 thin film material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420696A (en) * | 2015-11-25 | 2016-03-23 | 中国地质大学（武汉） | Method for preparing stannic oxide-based thin film material |
| CN106531635A (en) * | 2016-12-23 | 2017-03-22 | 中国地质大学（武汉） | P-type stannous oxide thin-film material and preparation method of potassium-doped p-type stannous oxide thin-film material |
| CN106784012A (en) * | 2016-11-24 | 2017-05-31 | 安徽瑞研新材料技术研究院有限公司 | A kind of tin oxide base thin film material of high mobility |
-
2015
- 2015-03-30 CN CN201510143623.9A patent/CN104726851B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 曾凡菊: "SnO2薄膜的制备与光电性能研究", 《中国优秀硕士学位论文全文数据库 基础学科辑》 * |
| 罗文彬等: "退火温度对溶胶-凝胶法制备锌锡氧化物薄膜晶体管的影响", 《发光学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420696A (en) * | 2015-11-25 | 2016-03-23 | 中国地质大学（武汉） | Method for preparing stannic oxide-based thin film material |
| CN106784012A (en) * | 2016-11-24 | 2017-05-31 | 安徽瑞研新材料技术研究院有限公司 | A kind of tin oxide base thin film material of high mobility |
| CN106531635A (en) * | 2016-12-23 | 2017-03-22 | 中国地质大学（武汉） | P-type stannous oxide thin-film material and preparation method of potassium-doped p-type stannous oxide thin-film material |
| CN106531635B (en) * | 2016-12-23 | 2019-02-22 | 中国地质大学（武汉） | A kind of preparation method of p-type stannous oxide thin-film material and potassium doped p type stannous oxide thin-film material |
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