CN107393810A - A kind of preparation method of oxide semiconductor thin-film - Google Patents
A kind of preparation method of oxide semiconductor thin-film Download PDFInfo
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- CN107393810A CN107393810A CN201710570025.9A CN201710570025A CN107393810A CN 107393810 A CN107393810 A CN 107393810A CN 201710570025 A CN201710570025 A CN 201710570025A CN 107393810 A CN107393810 A CN 107393810A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02697—Forming conducting materials on a substrate
Abstract
The invention discloses a kind of preparation method of oxide semiconductor thin-film, its preparation method comprises the following steps：(1) semiconductor Colloidal Quantum Dots solution is placed in electrostatic spinning platform, the added electric field between nozzle and substrate, makes solution aerosol dispersion, atomized liquid homogeneous film formation on an insulating substrate；(2) quantum dot film is handled with short chain ligand solution, to displace the long-chain oleic acid on quantum dot film surface；(3) remaining short chain part and its accessory substance are removed；(4) annealing is performed to film formed by atomized liquid in design temperature scope and the time range of setting, obtains oxide semiconductor thin-film.In the above method, can in rigidity or flexible substrate film forming.The preparation method is easy to adjust each component quality proportioning in solution, so as to change thin film composition, oxide semiconductor thin-film is prepared and studied for laboratory and provides new preparation method and thinking, and provides possible approach for large-scale production.
Description
Technical field
The invention belongs to technical field of semiconductor film preparation, more particularly, to one kind with colloidal oxide quantum dot
Solution is the transparent oxide semiconductor thin film preparation method of material.
Background technology
Tin indium oxide (ITO) is used as N-type wide band gap semiconducter oxide, has high visible light transmissivity and high conductivity,
It is widely used in various flat-panel monitors (FEDs), Organic Light Emitting Diode (OLED), touch panel, solar cell, gas
The fields such as body sensor.It is high to microwave attenuation rate, it can also be used to electromagnetic interference.The ratio and heat treatment temperature of tin and indium are to thin
The electric conductivity of film has material impact, industrially using indium oxide and tin oxide mass ratio 9:1 proportioning prepares film.
At present, most widely used ito thin film preparation method is magnetron sputtering.The technique is applied to continuously make on substrate
Standby ito thin film and film forming thickness it is uniform, it is reproducible, suitable for large-scale industrial production.
The Kim in South Korea's Quan Bei national universities thin film technique laboratory etc. is deposited ito thin film using radio-frequency magnetron sputter method
Onto PET base, resistivity has been obtained as 1.9 × 10-3Ω cm, light transmission rate are 80% ito thin film【Kim Y,Park
Y,Ansari S G,et al.Influence of O2admixture and sputtering pressure on the
properties of ITO thin films deposited on PET substrate using RF reactive
magnetron sputtering[J].Surface&Coatings Technology,2003,173(2):299-308.】.It is public
The number of opening is 102324271A, describes one kind in the Chinese patent application of the artificial Nanchang O-film Tech. Co., Ltd. of application with saturating
Bright polymer is crystal type transparent conductive film of base material and preparation method thereof.The upper surface of transparent conductive film on base material
There are one layer or two layers of optical thin film, be prepared for ito thin film with low temperature magnetic sputtering method in optical thin film outermost layer, its visible ray
In the range of average transmittance 88%, it is maximum up to 94%.
However, magnetically controlled DC sputtering is higher to the vacuum level requirements of equipment, therefore also constrain quantity-produced realization.Film
Change of the photoelectric properties to various sputtering parameters it is more sensitive, therefore process adjustments are relatively difficult.Also, target used in sputtering
Utilization rate is relatively low, and only 20% or so.If using radio-frequency magnetron sputter method instead, though process adjustments can be made simpler, ceramic target
Complex manufacturing technology thus be not easy to flexible modulation reactant composition, and equipment complex and expensive, sedimentation rate is low, radio-frequency radiation
There is harmful effect to human body.
In addition, University of Electronic Science and Technology Yuan Hong plums, Lin Zulun et al. are reported using indium nitrate and acetylacetone,2,4-pentanedione (analysis is pure)
For raw material, five hydrous tin chlorides (analysis is pure) prepare the colloidal sol of transparent conductive film for dopant in simple glass substrate
Gel method, realize 10k Ω m resistivity and 82-87% transmissivity【Yuan Hongmei, et al. " sol-gel processes prepare ITO
Research " the electronic devices 33.1 (2010) of film and its photoelectric properties:5-9】.But this method only possesses at the same time suitably mixes
It can just be prepared in the case of Sn ratios, try one's best big concentration of metal ions, appropriate pull rate, temperature as high as possible excellent
Good ito thin film, technology controlling and process are complicated.
Therefore, it is necessary to develop a kind of new method for preparing oxide semiconductor thin-film, it is desirable to its preparation technology is simple,
It can mass produce.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of transparent oxide semiconductor thin film
Preparation method, this method uses electrospinning Printing techniques, can use rigidity or flexible substrate, manufacture craft is simple, is applied to
Laboratory preparation research ito thin film and large-scale production, this method have a good application prospect.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of preparation of oxide semiconductor thin-film
Method, it is characterised in that comprise the following steps：
(1) semiconductor Colloidal Quantum Dots solution is placed in electrostatic spinning platform, electrostatic spinning platform includes nozzle, substrate
And dielectric substrate, apply high direct voltage between nozzle and substrate to form electric field, electric field makes solution aerosol dispersion, and atomized liquid is exhausted
Homogeneous film formation on edge substrate, obtain quantum dot film；
(2) quantum dot film is handled with short chain ligand solution, to displace the long-chain oleic acid of quantum dot surface；
(3) remaining short chain part and its accessory substance are removed；
(4) annealing is performed to film formed by atomized liquid in design temperature scope and the time range of setting, obtained
Oxide semiconductor thin-film, specifically, being annealed at 200 DEG C -500 DEG C 2-8 hours, acquire the oxide with setting thickness
Colloidal Quantum Dots film.
In above inventive method, film is prepared using electrospinning spray printing method, electrospinning spray printing method refers to equipped with semiconductor colloid
Apply high direct voltage between the capillary and ground connection reception device of quantum dot solution, make capillary end droplet surface rupture to form spray
Mist, Colloidal Quantum Dots are deposited on to the method that film is prepared in substrate.
Preferably, the semiconductor Colloidal Quantum Dots solution is In2O3Colloidal Quantum Dots solution, SnO2Colloidal Quantum Dots are molten
The mixed solution of liquid or both.
Preferably, the dielectric substrate is paper, plastics, glass or ceramics.
Preferably, the short chain ligand solution is Cu (CH3COO)2、Cu(NO3)2Or SnCl4Solution.
In general, by the contemplated above technical scheme of the present invention compared with prior art, have below beneficial to effect
Fruit：
The present invention prepares film using electrospinning spray printing method, can prepare transparent oxide semiconductor thin film at room temperature, only exist
Last heat treatment stages need the annealing of certain temperature.Prepare whole low energy consumption, economical environment-protective.It makes under atmospheric pressure
Standby film, is not required to application of vacuum, is easy to industrial circle to realize continuous production.Its preparation process speed is fast, stock utilization is high.
Moreover, transparent oxide semiconductor thin film can not only use conventional heat-resist ceramics, silicon chip or glass
Etc. rigid substrate, the relatively poor flexible substrate of heat resistance, the manufacture crafts such as plastics, paper can also be used simple, shown to be flexible
Show that the production application of panel provides possibility.
The present invention by allocate solution can easily and flexibly adjust indium oxide and tin oxide mass ratio and cost compared with
It is low.Usable this method is met requirement of the different occasions to the transmissivity and sheet resistance of conductive oxide film, then by gained
Mass ratio is applied in the preparation of magnetic control spattering target to adapt to the needs of industrialized production.In view of target used in magnetron sputtering method
The raw material of material and somewhat expensive is prepared, this method has reference significance to preparing target used in magnetron sputtering.
Brief description of the drawings
Fig. 1 is equipment schematic diagram used in present invention method, and the equipment schematic diagram is used to illustrate present invention side
Method preparation process；
Fig. 2 is the enlarged diagram that syringe nozzle goes out to spray Colloidal Quantum Dots solution in Fig. 1；
Fig. 3 is SEM (SEM) photo that sample is made in the inventive method embodiment.
In all of the figs, identical reference represents identical structure or parts from beginning to end, wherein
1- colloidal state quantum dot 2- nozzle 3- DC high-voltage power supplies
4- substrate 5- syringes
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Conflict can is not formed each other to be mutually combined.
It is creative to apply electrospinning spray printing method to transparent oxide semiconductor thin film is prepared in the present invention, it can overcome existing
Some prepares the number of drawbacks of oxide semiconductor thin-film method.
Electrospinning spray printing method is a kind of new method for preparing nano material, there is raw material synthesis to carry out in the solution, equipment
Cost is cheap, the thickness simple and easy to get and more uniform of condition needed for film forming, and the dosage, speed and the thickness that spray film forming can
Control, it is possible to achieve the advantages that large-scale production.Its principle is：In the capillary of the solution equipped with thin film composition and connecing for ground connection
Receiving apparatus is that several kilovolts of high direct voltage is added between substrate, capillary end is ruptured to be formed in hemispherical droplet surface and is penetrated
Stream, deposits to film forming in substrate.At present existing a variety of nanofibers can be prepared with method of electrostatic spinning and apply to laser material,
The field such as sensor and single-molecule detection.
Fig. 1 is equipment schematic diagram used in present invention method, and the equipment schematic diagram is used to illustrate present invention side
Method preparation process, Fig. 2 are the enlarged diagrams that syringe nozzle goes out to spray Colloidal Quantum Dots solution in Fig. 1.As seen from the figure, it is wrapped
Colloidal state quantum dot 1, nozzle 2, DC high-voltage power supply 3, substrate 4 and syringe 5 are included, the device is used to prepare the transparent of the present invention
Oxide semiconductor thin-film, injected specifically, semiconductor Colloidal Quantum Dots 1 (it is solution) are placed in electrostatic spinning platform
Device 5, the added electric field between nozzle 2 and substrate, the electric field are loaded by DC high-voltage power supply 3, make solution aerosol dispersion, and atomized liquid exists
Homogeneous film formation on the substrate 4 of insulation, then by subsequent treatment, transparent conductive oxide film can be obtained.
The preparation method of the transparent oxide semiconductor thin film of the present invention comprises the following steps：
(1) semiconductor Colloidal Quantum Dots solution is made into its homogeneous film formation coated in being printed in the dielectric substrate of electrode.Specifically
Ground, Colloidal Quantum Dots are at room temperature coated in film forming on substrate in a manner of electrospinning spray printing.
(2) quantum dot film is handled with short chain ligand solution, to displace the long-chain oleic acid of quantum dot surface.
(3) remaining short chain part and its accessory substance are removed.
(4) annealed at 200 DEG C -500 DEG C 2-8 hours, complete the preparation of oxide semiconductor thin-film.
The transparent oxide semiconductor thin film of the present invention includes：Dielectric substrate and oxide skin(coating).Oxide skin(coating) is semiconductor
Colloidal Quantum Dots film, specially In2O3Colloidal Quantum Dots film, SnO2Colloidal Quantum Dots film or the two epoxy glue scale of construction
Son point film.Dielectric substrate can be paper, glass, plastics or ceramics or rigid substrate or flexible substrate.
To make those skilled in the art more fully understand the present invention, the colloid amount with reference to specific embodiment to the present invention
The preparation method of son point film oxide semiconductors film is described in detail.
Embodiment 1
(1) In is prepared2O3Colloidal Quantum Dots solution.By the use of indium acetate as indium source, reacted and generated using colloid synthetic method.
Specifically, 0.876g indium acetates are dissolved into 10mL oleic acid (OA) and are heated with stirring to 150 DEG C.It is evacuated to
After bubble-free, nitrogen is led into container, 240 DEG C are warming up in nitrogen atmosphere, reacted 30 minutes at this temperature.Natural cooling
In can be obtained to room temperature2O3Nano particle.Cleaned with ethanol, after with 8000rpm centrifuge 10 minutes, gained nano particle is dissolved in
Hexane.
(2) SnO is prepared2Colloidal Quantum Dots solution.Use SnCl4As zinc source, reacted and generated using colloid synthetic method.
Specifically, by 0.6g SnCl4·5H2It is transparent that O is dissolved into formation in 20mL oleic acid (OA) and 2.5mL oleyl amines (OLA)
Mixed solution prepare Sn presoma.By 1mL H2O and 10mL ethanol adds the mixed liquor under slow stirring.By solution
It is transferred in the stainless steel autoclave of 50mL teflon lineds, is reacted 3 hours at 180 DEG C, rear cold bath is cooled to room
Temperature.Add 80mL ethanol and centrifuge 5 minutes with 6000rpm with separation product.After being dispersed in toluene by sediment and add ethanol
Centrifugation, is repeated twice.
(3) by indium oxide and tin oxide Colloidal Quantum Dots solution according to Solute mass ratio 85:15 mixing, using electrospinning spray printing
Method is coated to glass substrate surface with 1500nL/min fltting speed；By the stannic chloride that membranes submerged to concentration is 10mg/mL
(SnCl4) methanol solution in, infiltrate 60s after with absolute methanol wash away remnants SnCl4Particle and its byproduct of reaction, infiltration
60s；The substrate of coated film is annealed 2 hours at 300 DEG C, room temperature is naturally cooled to, completes oxide semiconductor thin-film
Prepare.
Embodiment 2
In prepared by embodiment 12O3And SnO2Colloidal Quantum Dots solution is according to Solute mass than 90:10 mixing, using electricity
Spin spray printing method and silicon chip substrate surface is coated to 1500nL/min fltting speed；It is 10mg/mL's by membranes submerged to concentration
Cu(NO3)2Methanol solution in, infiltrate 60s after with absolute methanol wash away remnants SnCl4Particle and its byproduct of reaction, infiltration
60s；The substrate of coated film is annealed 8 hours at 500 DEG C, room temperature is naturally cooled to, completes oxide semiconductor thin-film
Prepare.
Embodiment 3
In prepared by embodiment 12O3And SnO2Colloidal Quantum Dots solution is according to Solute mass than 95:5 mixing, using electricity
Spin spray printing method and ceramic substrate surface is coated to 1500nL/min fltting speed；It is 10mg/mL's by membranes submerged to concentration
Stannic chloride (SnCl4) methanol solution in, infiltrate 60s after with absolute methanol wash away remnants SnCl4Particle and its reaction by-product
Thing, infiltrate 60s；The substrate of coated film is annealed 6 hours at 400 DEG C, naturally cools to room temperature, completes oxide semiconductor
The preparation of film.
Embodiment 4
In prepared by embodiment 12O3And SnO2Colloidal Quantum Dots solution is according to Solute mass than 95:5 mixing, using electricity
Spin spray printing method and paper gasket basal surface is coated to 1500nL/min fltting speed；By the Cu that membranes submerged to concentration is 10mg/mL
(CH3COO)2Methanol solution in, infiltrate 60s after with absolute methanol wash away remnants SnCl4Particle and its byproduct of reaction, leaching
Moisten 60s；The substrate for coating ito thin film is annealed 4 hours at 200 DEG C, naturally cools to room temperature, it is thin to complete oxide semiconductor
The preparation of film.
The oxide that oxide semiconductor thin-film prepared by various embodiments of the present invention is prepared with existing magnetron sputtering method half
Conductor thin film is compared, and has substantially met the requirement of transmissivity and sheet resistance.
Fig. 3 is SEM (SEM) photo that sample is made in the inventive method embodiment 3, as seen from the figure, its
The oxide semiconductor thin-film of preparation has loose and porous structure, and gas molecule easily passes in and out, in gas sensor preparation field
There is potential application foreground.
The oxide semiconductor thin-film preparation method of the present invention is not limited to above-described embodiment, specifically, oxide half
Colloidal Quantum Dots film in conductor thin film is not limited to In2O3Colloidal Quantum Dots film or SnO2Colloidal Quantum Dots film, also may be used
To be other semiconductor Colloidal Quantum Dots films.Colloidal Quantum Dots solution in preparation method is not limited to In2O3Colloidal Quantum Dots
Solution or SnO2Colloidal Quantum Dots solution or other semiconductor Colloidal Quantum Dots solution.Dielectric substrate is not limited to
Paper, glass, plastics or ceramics or other dielectric substrates.Short chain ligand solution is not limited to SnCl4Solution, also may be used
To be other short chain inorganic matters or organic matter ligand solution, such as Cu (NO3)2Solution.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (4)
1. a kind of preparation method of oxide semiconductor thin-film, it is characterised in that comprise the following steps：
(1) semiconductor Colloidal Quantum Dots solution being placed in electrostatic spinning platform, electrostatic spinning platform includes nozzle and substrate,
Apply high direct voltage between nozzle and substrate to form electric field, electric field makes solution aerosol dispersion, and atomized liquid is being placed in the insulation of substrate
Homogeneous film formation on substrate, obtain quantum dot film；
(2) quantum dot film is handled with short chain ligand solution, to displace the long-chain oleic acid on quantum dot film surface；
(3) remaining short chain part and its accessory substance are removed；
(4) annealing is performed to film formed by atomized liquid in design temperature scope and the time range of setting, aoxidized
Thing semiconductive thin film, specifically, being annealed at 200 DEG C -500 DEG C 2-8 hours, obtain the oxide colloid amount with setting thickness
Son point film.
2. the preparation method of the oxide semiconductor thin-film described in claim 1, it is characterised in that the oxide colloid quantum
Point solution is indium oxide (In2O3) Colloidal Quantum Dots solution, tin oxide (SnO2) Colloidal Quantum Dots solution or the mixing of the two it is molten
Liquid.
3. the preparation method of the oxide semiconductor thin-film described in claim 1, it is characterised in that the dielectric substrate be paper,
Plastics, ceramics, silicon chip or glass.
4. the preparation method of the oxide semiconductor thin-film described in claim 1, it is characterised in that the short chain ligand solution is
Copper acetate, copper nitrate or tin chloride solution.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108165990A (en) * | 2018-01-22 | 2018-06-15 | 京东方科技集团股份有限公司 | Quantum dot film plating process and system |
| CN110187061A (en) * | 2019-06-03 | 2019-08-30 | 西安奕斯伟硅片技术有限公司 | A kind of processing method of silicon wafer, detection method and processing unit |
| CN110224074A (en) * | 2018-12-29 | 2019-09-10 | 华南理工大学 | A kind of quanta point electroluminescent device and preparation method thereof |
| CN110773341A (en) * | 2019-10-14 | 2020-02-11 | 大族激光科技产业集团股份有限公司 | Atomization cooling device, automatic processing equipment and method |
| CN112111783A (en) * | 2020-10-14 | 2020-12-22 | 天津工业大学 | Electrostatic atomization chemical vapor deposition gallium oxide film system |
| CN108906524B (en) * | 2018-07-14 | 2022-01-18 | 福州大学 | Method for encapsulating quantum dot light guide plate based on electrostatic atomization film forming |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165990A (en) * | 2018-01-22 | 2018-06-15 | 京东方科技集团股份有限公司 | Quantum dot film plating process and system |
| CN108906524B (en) * | 2018-07-14 | 2022-01-18 | 福州大学 | Method for encapsulating quantum dot light guide plate based on electrostatic atomization film forming |
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| CN110187061A (en) * | 2019-06-03 | 2019-08-30 | 西安奕斯伟硅片技术有限公司 | A kind of processing method of silicon wafer, detection method and processing unit |
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| CN112111783A (en) * | 2020-10-14 | 2020-12-22 | 天津工业大学 | Electrostatic atomization chemical vapor deposition gallium oxide film system |
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