CN104726851B - A kind of method that sol-gal process prepares p-type SnO 2 thin film material - Google Patents
A kind of method that sol-gal process prepares p-type SnO 2 thin film material Download PDFInfo
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- CN104726851B CN104726851B CN201510143623.9A CN201510143623A CN104726851B CN 104726851 B CN104726851 B CN 104726851B CN 201510143623 A CN201510143623 A CN 201510143623A CN 104726851 B CN104726851 B CN 104726851B
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Abstract
The invention provides a kind of method that sol-gal process prepares p-type SnO 2 thin film material, comprise the following steps：EGME, stannous chloride dihydrate and monoethanolamine are mixed in vessel, during solution moved into vacuum tube furnace, argon gas is vacuumized and be filled with, heated, heating is aged after finishing；Ultrasonic wave cleaning is carried out to substrate；Substrate is fixed on sol evenning machine, colloidal sol is added dropwise on substrate, carry out revolving Tu whirl coating, film sample is obtained；After whirl coating terminates, during film sample moved into vacuum tube furnace, argon gas is vacuumized and be passed through, then film sample is thermally dried；Step in repetition is until the number of plies coated on substrate reaches the required number of plies；Annealing, natural cooling after the completion of annealing is obtained the p-type SnO 2 thin film material.The method has the advantages that Multicomponent phase can uniformly mix, film forming is uniform, composition is easy to control, film thinner thickness, low cost, cycle is short, is thus suitable for industrialized production.
Description
Technical field
SnO is prepared the invention provides one kindxA kind of method of thin-film material, more particularly to sol-gal process is prepared and had
The p-type SnO of high mobilityxThe method of thin-film material, belongs to electronics, information, display, semiconductor film technique field.
Background technology
With the high speed development of information display technology, wearable Display Technique is arisen at the historic moment, and transparent electron will be future
The important component of information display technology.Wherein, N-shaped oxide thin film transistor is mutually tied with p-type oxide thin film transistor (TFT)
The bipolar thin film transistor being combined into is the basis for realizing transparent electronics.P-type oxide film is due to hole conduction
Feature, is made thin film transistor (TFT), be would be more advantageous in driving Organic Light Emitting Diode high aperture ratio pixel unit.Meanwhile, p
If the thin film transistor (TFT) of type oxide can be combined with flat panel display, it will become apparent from screen.
However, it is existing studies have found that, the electric property of p-type oxide also far cannot be with the electrology characteristic energy of N-shaped oxide
Match, which greatly limits oxide PN junction, the development of transparent oxide large scale integrated circuit.In recent years, tin oxide and
Its doping system is considered as the huge p-type oxide of application potential.So preparing high-performance, structure and physical property stabilization
P-type SnOxTransparent conductive film has very big value and important meaning in p-type oxide transparent conductive film field.
The content of the invention
The invention provides a kind of method that sol-gal process prepares p-type SnO 2 thin film material, background technology is solved
In deficiency, the method has that Multicomponent phase can uniformly mix, film forming is uniform, composition is easy to control, film thinner thickness, cost
The advantages of low, cycle is short, it is thus suitable for industrialized production.
Realize technical scheme that above-mentioned purpose of the present invention used for：
A kind of method that sol-gal process prepares p-type SnO 2 thin film material, comprises the following steps：(1), by ethylene glycol first
Ether, stannous chloride dihydrate and monoethanolamine are according to 6.5~7：0.15~0.2:0.8~1 mol ratio mixes and stirs in vessel
Mix to clarification, during solution then moved into vacuum tube furnace, argon gas is vacuumized and be filled with, to solution under the conditions of 80~100 DEG C
Heating 1~2 hour, heating continues solution after finishing to be aged 1~2 day in argon gas atmosphere, and colloidal sol is obtained；
(2), ultrasonic wave is carried out to substrate with acetone, absolute ethyl alcohol and deionized water successively to clean；
(3), substrate is fixed on sol evenning machine, is rotated with 2000~2500 revs/min of speed, dripped on substrate
Solubilization glue, carries out revolving Tu whirl coating, and rotational time is 20~30 seconds, and film sample is obtained；
(4) after, whirl coating terminates, during film sample moved into vacuum tube furnace, argon gas is vacuumized and is passed through, then to film
Sample is thermally dried, and drying terminates rear natural cooling；
(5), repeat step (3) and (4), until the number of plies coated on substrate reaches the required number of plies；
(6), film sample obtained in upper step is annealed, annealing temperature is 600~650 DEG C, soaking time
It it is 30~40 minutes, the programming rate in annealing process is 1~2 DEG C/min, natural cooling after the completion of annealing is obtained the p
Type SnO 2 thin film material.
Substrate described in step (2) is insulation SiO2/ Si substrates, the size of substrate is 10mm × 10mm, SiO on substrate2
The thickness 500nm of layer.
The rotating speed of sol evenning machine is 2000 revs/min in step (3), and rotational time is 20 seconds.
Annealing temperature is 600 DEG C in step (6), and soaking time is 30 minutes, programming rate in annealing process for 1 DEG C/
Minute.
Compared with prior art, the present invention has advantages below：1st, present invention employs sol-gal process, therefore preparing
During Multicomponent phase can uniformly mix, film forming is uniform, composition is easy to control, film thinner thickness, low cost, cycle is short etc. are excellent
Point, is thus suitable for industrialized production.2nd, using the square of p-type SnO 2 thin film material prepared by method provided by the present invention
Resistance is 2.7 × 105~2.8 × 105Ω/, hall mobility is 6~12cm2V-1S-1, hole be 2.0 ×
1012~3.6 × 1012cm-2。
Brief description of the drawings
Fig. 1 is p-type SnO prepared in the embodiment of the present invention 1xThe XRD test result figures of thin-film material.
Specific embodiment
Detailed specific description is done to the present invention with reference to specific embodiment, but protection scope of the present invention not office
It is limited to following examples.
Embodiment 1
P-type SnO provided in the present embodimentxThe preparation method of thin-film material is as follows：(1), by EGME
0.065mol, stannous chloride dihydrate 0.002mol and monoethanolamine 0.01mol, are mixed and stirred for clarification, then in vessel
During solution moved into vacuum tube furnace, tube furnace internal environment is evacuated with mechanical pump after reaching required vacuum state, is filled with argon
Gas.Solution is heated 1.5 hours under the conditions of 90 DEG C, heating continues solution after finishing to be aged 1.5 days in argon gas atmosphere, system
Obtain colloidal sol.Because stannous chemical property is active, can just be oxidized quickly in atmosphere, so configuration sol-process must
Rapidly, in order to avoid Bivalent Tin is oxidized.The concentration of tin is too high, and in annealing, ion can occur agglomeration, so wanting concentration to use up
Amount is small.The consumption of stabilizer will be determined according to the consumption of tin, be difficult to form colloidal sol very little, too much to the mobility of colloidal sol
And all have an impact with the matching of substrate.Heating-up temperature and heat time can influence the synthesis speed of colloidal sol network, ageing
Time can then influence the formation of the quality and network of solute particles dispersiveness in colloid, and digestion time is too short, and Bivalent Tin is in solvent
Cannot be uniformly dispersed in network, network forms poor quality, and then influences the quality of colloidal sol.
(2), ultrasonic wave is carried out to substrate with acetone, absolute ethyl alcohol, deionized water respectively to clean respectively once.Described substrate
It is insulation SiO2/ Si substrates, the size of substrate is 10mm × 10mm, SiO on substrate2The thickness 500nm of layer.
(3), substrate is fixed on sol evenning machine, is rotated with 2000 revs/min of speed, be added dropwise on substrate molten
Glue, carries out revolving Tu whirl coating, and rotational time is 25 seconds, and film sample is obtained.
(4) after, whirl coating terminates, during film sample moved into vacuum tube furnace, argon gas is vacuumized and is passed through, then to film
Sample is thermally dried, and drying terminates rear natural cooling.Because being sintered under the few environment of oxygen content, in sample
Carbon is difficult to burn completely, is susceptible to carbonization, so tried one's best extension soaking time in the low temperature drying stage, by carbon
Content be preferably minimized.
(5), repeat step (3) and (4), until the number of plies coated on substrate reaches the required number of plies.
(6), film sample obtained in upper step is annealed, annealing temperature is 600 DEG C, soaking time is 30 points
Clock, the programming rate in annealing process is 1 DEG C/min, and natural cooling after the completion of annealing is obtained the p-type SnO 2 thin film
Material.P-type SnO prepared in the present embodimentxThin-film material XRD test results figure is as shown in figure 1, SnOxFilm has 4 substantially
Diffraction maximum.Cubic SnO2Characteristic peak (110), the characteristic peak (002) of cubic SnO.In substrate the diffraction maximum (021) of Si and
(311).Detected by XRD and demarcated, it may be determined that our sample is with SnO and SnO2Hybrid films, therefore we are referred to as
SnOxFilm.
Sample prepares the test that electric property is carried out after terminating, and thin-film material electric property is as shown in the table：
Table 1 shows SnO of the present inventionxFilm rectangular resistance, hole, the measurement result of mobility.Sample
Electric property test repeatedly 6 times, show p-type electrology characteristic, prepared p-type SnO 2 thin film material square resistance is
2.7×105~2.8 × 105Ω/, hall mobility is 6~12cm2V-1s-1, hole is 2.0 × 1012~
3.6×1012cm-2。
Embodiment 2
P-type SnO provided in the present embodimentxThe preparation method of thin-film material is as follows：(1), by EGME
0.07mol, stannous chloride dihydrate 0.0015mol and monoethanolamine 0.008mol, are mixed and stirred for clarification, then in vessel
During solution moved into vacuum tube furnace, tube furnace internal environment is evacuated with mechanical pump after reaching required vacuum state, is filled with argon
Gas.Solution is heated 2 hours under the conditions of 80 DEG C, heating continues solution after finishing to be aged 3 days in argon gas atmosphere, is obtained molten
Glue.
(2), ultrasonic wave is carried out to substrate with acetone, absolute ethyl alcohol, deionized water respectively to clean respectively once.Described substrate
It is insulation SiO2/ Si substrates, the size of substrate is 10mm × 10mm, SiO on substrate2The thickness 500nm of layer.
(3), substrate is fixed on sol evenning machine, is rotated with 2500 revs/min of speed, be added dropwise on substrate molten
Glue, carries out revolving Tu whirl coating, and rotational time is 30 seconds, and film sample is obtained.
(4) after, whirl coating terminates, during film sample moved into vacuum tube furnace, argon gas is vacuumized and is passed through, then to film
Sample is thermally dried, and drying terminates rear natural cooling.Because being sintered under the few environment of oxygen content, in sample
Carbon is difficult to burn completely, is susceptible to carbonization, so tried one's best extension soaking time in the low temperature drying stage, by carbon
Content be preferably minimized.
(5), repeat step (3) and (4), until the number of plies coated on substrate reaches the required number of plies.
(6), film sample obtained in upper step is annealed, annealing temperature is 650 DEG C, soaking time is 40 points
Clock, the programming rate in annealing process is 2 DEG C/min, and natural cooling after the completion of annealing is obtained the p-type SnO 2 thin film
Material.
Claims (4)
1. a kind of method that sol-gal process prepares p-type SnO 2 thin film material, it is characterised in that comprise the following steps：(1), will
EGME, stannous chloride dihydrate and monoethanolamine are according to 6.5~7：0.15~0.2:0.8~1 mol ratio is in vessel
It is mixed and stirred for clarification, during solution then moved into vacuum tube furnace, argon gas is vacuumized and be filled with, in 80~100 DEG C of conditions
Under to solution heat 1~2 hour, heating finish after by solution continue in argon gas atmosphere be aged 1~2 day, be obtained colloidal sol；
(2), ultrasonic wave is carried out to substrate with acetone, absolute ethyl alcohol and deionized water successively to clean；
(3), substrate is fixed on sol evenning machine, is rotated with 2000~2500 revs/min of speed, be added dropwise on substrate molten
Glue, carries out revolving Tu whirl coating, and rotational time is 20~30 seconds, and film sample is obtained；
(4) after, whirl coating terminates, during film sample moved into vacuum tube furnace, argon gas is vacuumized and is passed through, then to film sample
It is thermally dried, drying terminates rear natural cooling；
(5), repeat step (3) and (4), until the number of plies coated on substrate 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, the programming rate in annealing process was 1~2 DEG C/min, and natural cooling after the completion of annealing is obtained the p-type oxygen
Change tin thin film material；The square resistance of prepared p-type SnO 2 thin film material is 2.7 × 105~2.8 × 105Ω/, Hall is moved
Shifting rate is 6~12cm2V-1S-1, hole is 2.0 × 1012~3.6 × 1012cm-2。
2. it is according to claim 1 prepare p-type SnO 2 thin film material method, it is characterised in that：Described in step (2)
Substrate for insulation SiO2/ Si substrates, the size of substrate is 10mm × 10mm, SiO on substrate2The thickness 500nm of layer.
3. it is according to claim 1 prepare p-type SnO 2 thin film material method, it is characterised in that：Spin coating in step (3)
The rotating speed of machine is 2000 revs/min, and rotational time is 20 seconds.
4. it is according to claim 1 prepare p-type SnO 2 thin film material method, it is characterised in that：Annealing in step (6)
Temperature is 600 DEG C, and soaking time is 30 minutes, and the programming rate in annealing process is 1 DEG C/min.
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| CN105420696B (en) * | 2015-11-25 | 2016-10-19 | 中国地质大学（武汉） | A kind of preparation method of tin oxide base 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 |
| 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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