CN106086823A - A kind of serigraphy assisting sol gel method is prepared ZnO thin film doped method - Google Patents
A kind of serigraphy assisting sol gel method is prepared ZnO thin film doped method Download PDFInfo
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- CN106086823A CN106086823A CN201610557652.4A CN201610557652A CN106086823A CN 106086823 A CN106086823 A CN 106086823A CN 201610557652 A CN201610557652 A CN 201610557652A CN 106086823 A CN106086823 A CN 106086823A
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
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Abstract
The invention provides a kind of serigraphy assisting sol gel method and prepare ZnO thin film doped method, the method comprises screening and the surface treatment of backing material, the preparation of doping ZnO colloidal sol, the steps such as the ZnO thin film doped and high annealing of serigraphy. preferably, in preparing ZnO thin film doped step, serigraphy assisting sol gel method also comprises the optimization of meshcount in the ZnO thin film doped process of serigraphy, the step of the regulation and control of film thickness and annealing temperature, can obtain the ZnO thin film doped of low-resistivity and high efficiency ultraviolet lasing under room temperature through above-mentioned processing.
Description
Technical field
The present invention relates to a kind of ZnO thin film doped preparation method, relate to particularly a kind of based on the lower resistivity of doping ZnO and good optical characteristics, taking p type single crystal silicon (100) as substrate, serigraphy assisting sol-gel method prepares ZnO thin film doped method.
Background technology
In recent years, the opto-electronic device such as various short-wave long light-emitting diodes, semiconductor laser is because it is in information technology Critical component, be more and more subject in the extensive use in the fields such as optical storage, optical communication, information processing, laser printing, colored demonstration To the concern of researcher. originally scientist is upper semiconductor material with wide forbidden band research emphasis being concentrated on to ZnSe and GaN, but ZnSe is a kind of strong ionic crystal, and when stimulated emission, especially easily Yin Wendu raises and causes rolling up of defect, thereby Cause the laser works life-span shorter; And GaN material is also not easy growth, establishes because lacking proper backing material, film Standby expensive, growth temperature is high, high in cost of production drawbacks limit its application. and ZnO price is low, pollution-free, and have with other half The similar lattice structure of conductor material becomes optimal substitution material, has obtained the extensive concern of researcher.
Broad stopband direct band gap II-VI family semi-conducting material that zinc oxide (ZnO) is wurtzite structure, lattice paprmeter a=0.325nm, c=0.521nm, under room temperature, energy gap is about 3.37eV.ZnO as a kind of new function material, have excellent optics, electricity, mechanical performance and heat endurance, chemical stability. because ZnO has 60meV exciton bind energy and very strong UV Stimulated radiation, therefore at room temperature high efficiency ultraviolet lasing is more easily realized, in exploitation short-wave long light-emitting and inspection survey device as LED, the aspects such as LD have very large potentiality, more the good news is that ZnO can be with various ion dopings to meet the demand of different field. wherein, ZnO (ZAO) film of mixing Al has lower resistivity and good optical characteristics, show ultraviolet cut-on characteristic, within the scope of infrared light district, there is higher reflectivity, there is higher transmissivity at visible region, and its light learning band gap can be changed by the doping content of Al. in addition, Li doped in ZnO, Mg, Mn, Fe, Co, Cu, the metal such as Ga and In from after son, also can change ZnO thin film doped resistivity and the especially optical band gap of optical characteristics in the district of not sharing the same light, this is to change kind laser instrument short wavelength laser output, a kind of effective way of exploitation short-wave long light-emitting and detection means.
At present, the preparation method of ZnO nano material has a lot, electrostatic spinning, hydro-thermal method, Sol-Hydrothermal method, chemical gaseous phase sedimentation, spin-coating method and electrochemical deposition method etc. are all the experimental techniques that is used for synthesizing ZnO nano material of comparative maturity, and ZnO thin film doped preparation method is limited, conventional ZnO thin film doped preparation technology has sol-gel process, direct current (radio frequency) magnetron sputtering, vacuum reaction evaporation, pulsed laser deposition (PLD) etc. present inventor is by mixing various in recent years the assorted preparation method of ZnO film and the comparative studies of photoelectric characteristic, design a kind of based on the lower resistivity of doping ZnO and good good optical characteristics, taking p type single crystal silicon (100) as substrate, serigraphy assisting sol-gel method is prepared ZnO thin film doped method. compared to traditional sol-gel process, serigraphy assisting sol-gel method prepares that ZnO thin film doped to have film thick spend controlled, photoelectric properties are improved significant advantage. and experiment confirmed already, the method is a kind of simple and easy to do ZnO thin film doped Preparation method.
Summary of the invention
The invention provides a kind of serigraphy assisting sol-gel method and prepare ZnO thin film doped method, the method bag Include the screening of backing material and surface processes, the doping preparation of ZnO colloidal sol, silk screen printing are ZnO thin film doped and high annealing etc.Step.Preferably, prepare at silk screen printing assisting sol-gel method ZnO thin film doped step also including, silk screen printing is mixedThe step of the regulation and control of the optimization of meshcount, film thickness and annealing temperature during miscellaneous ZnO film, can obtain through above-mentioned processUnder room temperature, low-resistivity and high efficiency ultraviolet lasing is ZnO thin film doped.
In view of silk screen print method and sol-gel process can perfectly merge setting in ZnO thin film doped preparation technology
Meter thinking, with p type single crystal silicon (100) as substrate, uses silk screen printing assisting sol-gel method to prepare ZnO thin film doped, both gram
The deficiency having taken other preparation method technique being loaded down with trivial details, production cost is high, makes again ZnO thin film doped resistivity and the characteristics of luminescence outstanding
It is that optical band gap significantly improves, the act made the best of both worlds of can yet be regarded as.
Wherein, the screening of backing material is that silk screen printing assisting sol-gel method is prepared ZnO thin film doped firstly the need of solution
A key link certainly.The most substantial amounts of documents and materials show, simple glass, quartz glass, sapphire, monocrystal silicon (100
Or 111) and the 1-D photon crystal prepared by electrochemical corrosion be all to prepare ZnO thin film doped conventional backing material,
But the comparative test that ZnO thin film doped fault of construction and luminescent properties are affected by seminar by above-mentioned backing material finds, p-type
Monocrystal silicon (100) is more beneficial for C axle preferential growth and the improvement of optical characteristics of doping ZnO crystal, is ZnO thin film doped preparation
First-selected backing material.
Doping variety classes and the ZnO thin film doped pattern of content ion pair and photoelectric characteristic impact are notable, are doping ZnO
One key factor of film preparation.Research finds, during undoped p, the Boundary corrosion test of ZnO film is not of uniform size, between crystal block
Boundary line is fuzzyyer；When the content of dopant ion is 2%～4%, the Boundary corrosion test ratio of ZnO film is more uniform, and crystal grain also has
Being grown up, crystal boundary is more visible；When doping is 5%～10%, thin film also becomes apparent from due to crystal grain agglomeration, hole,
And along with the increase of doping, hole gets more and more.Doping Group IIA element (Mg) and Group IIIA element (Al, Ga and In) energy
Improving the conductivity of ZnO film, Li, Co adulterate ZnO optical band gap red shift, and Mg, Al, Mn, Cu adulterate ZnO blue-shift of optical band gap,
Near side (ns) band excitonic luminescence strengthens.
Meshcount is obvious on the impact of ZnO thin film doped pattern, is a key factor of doping ZnO crystal growth.
Experiment shows, along with the increase of meshcount, the ZnO thin film doped gridding pattern presented becomes more and more unintelligible and final
Disappearing, optimization meshcount is 360 mesh.
Film thickness is also one of key factor of impact doping ZnO crystal growth, and film thickness can be dynamic by controlling
Static mode and infiltrating time regulate and control.Research finds, along with the increase of film thickness, in the growth course of doping ZnO crystal grain
In, crystal grain is gradually grown up and tends to complete, and sample forbidden band broadens, and therefore, increasing film thickness within the specific limits can obtain
Perfect crystalline, photoelectric properties be improved significantly thin film.
Annealing temperature is also to affect ZnO thin film doped pattern and the key factor of photoelectric properties.Research finds, along with annealing
Temperature is warming up to 900 DEG C from 400 DEG C every 50 DEG C, the size monotone increasing of doping ZnO crystal grain, and agglomeration occurs, and C axle is selected
Excellent orientational strengthening, stress in thin films reduces, and diminishes with temperature rising energy gap, and the ultraviolet when annealing temperature is 900 DEG C
Luminescence is the strongest.
The method is verified the most repeatedly, and result shows that the method is a kind of simple and easy to do doping ZnO
The preparation method of thin film.
Detailed description of the invention
1 one kinds of silk screen printing assisting sol-gel methods of embodiment prepare ZnO thin film doped method
Silk screen printing assisting sol-gel method prepare ZnO thin film doped method include the screening of backing material and surface process,
The doping preparation of ZnO colloidal sol, silk screen printing be ZnO thin film doped and high annealing several stage.
(1) screening and the surface of backing material processes
Detailed description of the invention 1.5cm p type single crystal silicon (100), first cleans 10min with ultrasonic assistant acetone, then uses ultrasonic assistant washes of absolute alcohol Jie Gouquexian{@} deionized water rinsing; (Yi Yao) ##Bi compare Shi Yan{@} ## In culture dish standby, wherein ultrasonic assistant cleaning parameters is:ultrasonic power 150W, frequency 40KHz.
(2) preparation of doping ZnO colloidal sol
Using Zinc diacetate dihydrate as the mixed liquor of presoma, ethylene glycol monomethyl ether and dehydrated alcohol as solvent, ethanol ammonia conduct
Stabilizer, is dissolved in ethylene glycol monomethyl ether and the 500mL of dehydrated alcohol 1:1 by volume mixing by the Zinc diacetate dihydrate of 0.2mol
In solvent, add the ethanol ammonia of 0.2mol, through being sufficiently stirred for being formed the solution A of clear homogeneous, then by the nine of 0.001mol
Water aluminum nitrate, 0.0023mol tetra-are hydrated cobaltous acetate, 0.0012mol ammonium acetate is dissolved in the dehydrated alcohol of 100mL respectively and making
Bright solution B 1, B2, B3, add 100mL solution B 1, B2, B3 1:1 by volume in solution A the most respectively, stir at 60 DEG C of magnetic force
Mixing 1h and form homogeneous transparent colloidal sol C1, C2, C3, naturally cool to after ambient temperatare puts 12h standby, wherein magnetic agitation rotating speed is
1000r/min。
(3) silk screen printing is ZnO thin film doped
After being dried up by the most each stainless steel cloth nitrogen cleaning 20min of ultrasonic assistant dehydrated alcohol and deionized waterOn the net that stretches tight the most surface treated p type single crystal silicon sheet, then, the p type single crystal silicon sheet of the net that stretches tight is deposited in respectivelyEquipped with in the 500mL shaking flask of doping ZnO colloidal sol C1, C2, C3 of preparation in 200mL step (2), sealing DEG C of constant-temperature table 200r/min of it is placed on 27 with plastic foil dynamically infiltrates 12h, finally, pull out and prepare the use of sample in order to subsequent anneal with antimagnetic type tweezer, Wherein meshcount is 360 mesh.
(4) high annealing
All it is firstly placed on the sample prepared by silk screen printing in step (3) on the electric hot plate of 100 DEG C drying 5min, then puts
Enter in the electric tube furnace of 350 DEG C heat 10min with organics removal, repeat the above steps 3 times, then, back-off takes off each sample
On stainless steel cloth, finally the sample after remove impurity is placed in high-temperature annealing furnace 900 DEG C of annealing 2h, low electricity under room temperature can be obtained
Resistance rate and high efficiency ultraviolet lasing ZnO thin film doped.
By above-mentioned specific embodiment, it is easier to understand the present invention.Above-described embodiment is the description of illustrative, and not
It is appreciated that for limiting the scope of the present invention.
Claims (1)
1. silk screen printing assisting sol-gel method prepares ZnO thin film doped method, it is characterised in that: (1) backing material
Screening and surface process: the comparative test that by backing material, ZnO thin film doped fault of construction and luminescent properties will be affected
1.5cm × 1.5cm p type single crystal silicon (100) of screening, first cleans 10min with ultrasonic assistant acetone, more auxiliary with ultrasound wave
Help washes of absolute alcohol 15min, then with ultrasonic assistant deionized water rinsing 20min, finally dry up with nitrogen and be placed on mouth
In the blank glass culture dish of footpath 9cm standby, wherein ultrasonic assistant cleaning parameters is: ultrasonic power 150W, frequency 40KHz；
(2) preparation of doping ZnO colloidal sol: make using Zinc diacetate dihydrate as the mixed liquor of presoma, ethylene glycol monomethyl ether and dehydrated alcohol
For solvent, the Zinc diacetate dihydrate of 0.2mol, as stabilizer, is dissolved in ethylene glycol monomethyl ether and dehydrated alcohol by body by ethanol ammonia
In the long-pending 500mL solvent than 1:1 mixing, add the ethanol ammonia of 0.2mol, through being sufficiently stirred for being formed the solution A of clear homogeneous,
Then by the nine water aluminum nitrates of 0.001mol, 0.0023mol tetra-is hydrated cobaltous acetate, 0.0012mol ammonium acetate is dissolved in 100mL respectively
Dehydrated alcohol in make clear solution B1、B2、B3, the most respectively by 100mL solution B1、B2、B31:1 adds solution by volume
In A, form homogeneous transparent colloidal sol C 60 DEG C of magnetic agitation 1h1、C2、C3, naturally cool to after ambient temperatare puts 12h standby, its
Middle magnetic agitation rotating speed is 1000r/min；(3) silk screen printing is ZnO thin film doped: will be by ultrasonic assistant dehydrated alcohol and going
Ionized water successively each stainless steel cloth nitrogen cleaning 20min stretches tight after drying up the most surface treated p-type of net
On monocrystalline silicon piece, then, the p type single crystal silicon sheet of the net that stretches tight is deposited in it is respectively provided with in 200mL step (2) the doping ZnO of preparation
Colloidal sol C1、C2、C3500mL shaking flask in, be placed on 27 DEG C of constant-temperature table 200r/min dynamically infiltrate 12h with plastic foil sealing,
After, pull out with antimagnetic type tweezer and prepare sample in case subsequent anneal is used, wherein meshcount is 360 mesh；(4) high annealing:
All it is firstly placed on the sample prepared by silk screen printing in step (3) on the electric hot plate of 100 DEG C drying 5min, places into
In the electric tube furnace of 350 DEG C, heating 10min is with organics removal, and repeat the above steps 3 times, then, back-off takes off in each sample
Stainless steel cloth, finally the sample after remove impurity is placed in high-temperature annealing furnace 900 DEG C of annealing 2h, low resistance under room temperature can be obtained
Rate and high efficiency ultraviolet lasing ZnO thin film doped.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109830586A (en) * | 2019-02-19 | 2019-05-31 | 芜湖德豪润达光电科技有限公司 | The preparation method and light emitting diode of transparency conducting layer |
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| CN103236352A (en) * | 2013-04-23 | 2013-08-07 | 上海大学 | Preparation method of ZnO sol compounded Sn doping ZnO thick films |
| US20130255762A1 (en) * | 2012-03-30 | 2013-10-03 | New E Materials Co., Ltd. | Passivation layer for solar cells and method for manufacturing the same |
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| CN101579673A (en) * | 2009-06-22 | 2009-11-18 | 杭州电子科技大学 | Method for zinc oxide film coating |
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| CN109830586A (en) * | 2019-02-19 | 2019-05-31 | 芜湖德豪润达光电科技有限公司 | The preparation method and light emitting diode of transparency conducting layer |
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Application publication date: 20161109 |