CN106549085A - A kind of preparation method of the light emitting diode based on Zinc oxide quantum dot - Google Patents
A kind of preparation method of the light emitting diode based on Zinc oxide quantum dot Download PDFInfo
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- CN106549085A CN106549085A CN201610901324.1A CN201610901324A CN106549085A CN 106549085 A CN106549085 A CN 106549085A CN 201610901324 A CN201610901324 A CN 201610901324A CN 106549085 A CN106549085 A CN 106549085A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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Abstract
The invention discloses a kind of preparation method of the light emitting diode based on Zinc oxide quantum dot；, used as wide band gap semiconducter, the direct band gap with 3.3eV can be with the exciton number binding energy of 60meV, and this causes which to have extensive practical application in fields such as optics, electricity, catalysis for Zinc Oxide.By the ZnO quantum dot that synthesizes in gentle dehydrated alcohol alkaline solution system and the time to reaction system, temperature, OH‑Content carries out substantial amounts of reference, and carries out surface modification to ZnO quantum dot by normal hexane, so that the good stability of its holding structure and optical property.The present invention uses cheap water as oxidant, can save production cost, is easy to large area production to promote.A kind of light emitting diode based on Zinc oxide quantum dot has the advantages that environmental protection and energy saving, has sustainable development in lighting field application and industry.
Description
Technical field
The invention belongs to light emitting diode (LED, Light Emitting Diode) technical field, and in particular to Yi Zhongji
In the preparation method of the light emitting diode of Zinc oxide quantum dot.
Background technology
Used as a member important in inorganic multifunctional material, ZnO nano material all has important practical valency in many fields
Value and basic scientific research meaning.For example, the four-coordination structure of ZnO can be used to grind the piezoelectricity induced by polarization that makes internal disorder or usurp
Matter, can also carry out research to disclose semiconductor-quantum-point in information processing to the electron spin of ZnO quantum dot（Quantum calculation
Device）The application of aspect.High-quality, large-sized single crystal ZnO are the most preferable substrates of ultraviolet light and blue light emitting device.Meanwhile,
ZnO nano material is in the side such as gas sensor, the electrode of DSSC, fluorescent material and thin film field-effect diode
Mask is widely used.Different-shape, the nano zinc oxide material of shape in luminescent device, biological fluorescent labelling, dyestuff too
There is greatly application in the fields such as positive energy battery, mechanics sensor and nano generator.Exciton Bohr's diameter of ZnO is about 6nm, when receiving
Rice grain shows quantum constraint effect when being smaller in size than 6nm, and the nanocrystal in this size area again can the amount of being called
Sub- point.Due to quantum constraint effect, the valence band and conduction band of ZnO quantum dot show discrete energy level, so as to result in ZnO quantum
Point is with properties such as some the special optics different from body block crystal, electricity.The band gap of ZnO quantum dot is with ZnO quantum dot
The change of granular size and consecutive variations, while the visible luminescent of ZnO quantum dot also continuously can be sent out with the change of its size
Changing.With the prolongation in response time, the particle size of ZnO quantum dot becomes big, ZnO and the change with quantum dot particle size
It is big its uviol lamp under glow color change, color is moved from the blue light of short wavelength to long wave gold-tinted, that is, ZnO
The energy of the visible ray sent by quantum dot weakens as the change of ZnO quantum dot particle size is big.
As updating for Technology, the internal quantum efficiency of LED have had very big improvement, highest can reach
85% or so, the space that can be lifted is less, and the light extraction efficiency of LED is still very low.With regard to Zinc oxide quantum dot
For LED, test result indicate that：When emission wavelength is less than 300nm, light extraction efficiency only has a few percent, therefore lifted
Space is very big.
The content of the invention
In practical study, the defect of ZnO quantum dot is easily caused photoluminescence spectrum and is drastically quenched so as to which performance is easily disliked
Change, and at the initial stage of ZnO quantum dot growth, as Ostwald ripening effect occurs in that double distribution of sizes phenomenons of ZnO quantum dot.
The present invention provides a kind of design of Zinc oxide quantum dot, by the ZnO synthesized in gentle dehydrated alcohol alkaline solution system
Quantum dot the response time to reaction system, temperature, OH- contents some important parameters carry out substantial amounts of reference, by this
The optimization of a little parameters, draws the optimum growth conditionss of ZnO quantum dot, carries out surface to ZnO quantum dot by normal hexane and repair
Decorations, so that the good stability of its holding structure and optical property.
The purpose of the present invention is the deficiency for existing light emitting diode construction and technology of preparing, there is provided a kind of to be based on oxygen
Change the preparation method of the light emitting diode of zinc quantum dot, production cost can be greatly reduced.
The present invention solves the technical scheme that technical problem is adopted, a kind of system of the light emitting diode based on Zinc oxide quantum dot
Preparation Method, including LED chip, quantum dot mixing material, silica gel are used as embedding colloid；Preparation method is comprised the following steps：
（1）Using Aska-Rid., zinc acetate as cadmium presoma and zinc precursor, tributyl phosphorus is dissolved in selenium powder（TBP）Prepare
Tributyl selenizing phosphorus as selenium presoma, the solution of 1- octadecylenes is dissolved in as sulphur source using sulphur powder, with 1- octadecylenes as solvent,
Oleic acid is obtained oil-soluble Cd as reaction partxZn1-xS@ZnSe quantum dots；Ethanol promotes quantum dot to precipitate, and centrifugation is carried
It is pure, chloroform dissolving dispersion；
（2）Cadmium source：Zinc source：Sulphur source：Selenium source is with 1:10:2:4 molar ratio reaction is obtained quantum dot, and now quantum dot contains not anti-
The organic impuritiess answered, add excess ethyl alcohol to promote quantum dot precipitation and centrifugal separation to obtain pressed powder, add chloroform to dissolve again
Plus excess ethyl alcohol precipitation, obtain pure Cd five times repeatedlyxZn1-xS@ZnSe quantum dot powder；
（3）Pure rare earth selenide quantum dots powder is re-dispersed in chloroform；
（4）The preparation of ZnO quantum dot：By the precursor solution of 10ml zinc acetates on digital display intelligent temperature control magnetic stirring apparatuss room temperature
Stirring, the concentration then newly prepared 0.5ml are rapidly injected in reaction solution for the ethanol solution of the NaOH of 0.5M, and
Start timing.A certain amount of reaction solution is taken out after the specific response time and is cooled down with ice-water bath immediately, the reaction of taking-up
Sample solution is stored in 0 DEG C -4 DEG C of refrigerator.
（5）By step（1）、（2）、（3）Obtain CdxZn1-xS@ZnSe quantum dots and step（4）Prepared Zinc Oxide amount
Son point 13:5 mixing.
It is an advantage of the invention that：The present invention uses cheap water as oxidant, can save production cost, be easy to large area
Production is promoted.A kind of light emitting diode based on Zinc oxide quantum dot has the advantages that environmental protection and energy saving, in lighting field application and
Industry has sustainable development.
Specific embodiment
1、CdxZn1-xThe preparation of S@ZnSe quantum dots：（1）Using Aska-Rid., zinc acetate not as cadmium presoma and zinc precursor
Body, is dissolved in tributyl phosphorus with selenium powder（TBP）The tributyl selenizing phosphorus of preparation is dissolved in 1- octadecylene with sulphur powder as selenium presoma
Used as sulphur source, with 1- octadecylenes as solvent, Oleic acid is obtained oil-soluble Cd as reaction part to solutionxZn1-xS@ZnSe quantum dots.
Ethanol promotes quantum dot to precipitate, centrifugation purification, chloroform dissolving dispersion；
（2）Cadmium source：Zinc source：Sulphur source：Selenium source is with 1:10:2:4 molar ratio reaction is obtained quantum dot, and now quantum dot contains not anti-
The organic impuritiess answered, add excess ethyl alcohol to promote quantum dot precipitation and centrifugal separation to obtain pressed powder, add chloroform to dissolve again
Plus excess ethyl alcohol precipitation, obtain pure Cd five times repeatedlyxZn1-xS@ZnSe quantum dot powder；
（3）Pure rare earth selenide quantum dots powder is re-dispersed in chloroform.
2nd, the preparation of ZnO quantum dot：
（1）The preparation of zinc acetate precursor solution, is added to bis- acetate hydrate zinc of 2mmol in 50ml dehydrated alcohol first,
2h is refluxed on 80 DEG C of intelligent temperature control magnetic stirring apparatuss.Then in being down to room temperature and placing it in 0 DEG C -4 DEG C of refrigerator
Preserved.
（2）Prepare the ethanol solution of the NaOH of variable concentrations；
It is 0.25M to prepare molar concentration respectively, and the ethanol solution of the NaOH of 0.4M, 0.6M, 0.7M, 1M, 2M will weighing
Good NaOH is quickly adding in 10ml dehydrated alcohol, ultrasonic disperse 10min.
（3）ZnO quantum dot is prepared under the different response time；
The precursor solution of 10ml zinc acetates is stirred at room temperature on digital display intelligent temperature control magnetic stirring apparatuss with three neck round bottom,
Then concentration 0.5ml newly prepared is rapidly injected in reaction solution for the ethanol solution of the NaOH of 0.5M, and is started
Timing.A certain amount of reaction solution is taken out after the specific response time and is cooled down with ice-water bath immediately, the response sample of taking-up
Solution is stored in 0 DEG C -4 DEG C of refrigerator.
（4）ZnO quantum dot is prepared under different reaction temperatures；
Between 15 DEG C -75 DEG C, the impact of reaction temperature is investigated using 5 DEG C of temperature intervals.With three neck round bottom by 10ml
Zinc acetate precursor solution carries out room temperature thermal agitation on digital display intelligent temperature control magnetic stirring apparatuss, then newly prepares 0.5ml
Concentration is injected in reaction solution for the ethanol solution of the NaOH of 0.5M, reaction solution is cold with ice-water bath immediately after reaction
But and it is stored in 0 DEG C -4 DEG C of refrigerator.
（5）In the OH of different mol ratio-And Zn2+Reaction condition under prepare ZnO quantum dot three neck round bottom will
The precursor solution of 10ml zinc acetates is stirred at room temperature on digital display intelligent temperature control magnetic stirring apparatuss, is then newly prepared 0.5ml
The ethanol solution of the NaOH of variable concentrations is rapidly injected in reaction solution, and starts timing.In the specific response time
After take out a certain amount of reaction solution and cooled down with ice-water bath immediately, the response sample solution of taking-up is stored in 0 DEG C -4 DEG C of ice
In case.
（6）The preparation of the ZnO quantum dot of normal hexane surface modification, with three neck round bottom by the precursor solution of zinc acetate
It is stirred at room temperature on digital display intelligent temperature control magnetic stirring apparatuss, then by certain density NaoH ethanol solutions Glass syringe
Device is rapidly injected in reaction solution by an eck of flask side, and the reaction for after reaction adding excessive just own institute is molten
Centrifugation after in liquid, removes centrifuged supernatant, and with appropriate dehydrated alcohol by resolution of precipitate, such repeatable operation is twice.Finally
Product as white be precipitated and dissolved in dehydrated alcohol.
3rd, the performance characterization of ZnO；
（1）Transmission electron microscope（TEM）And high-resolution-ration transmission electric-lens（HRTEM）Test, the Micro-Structure Analysis of ZnO quantum dot by
HRTEM（High-resolution-ration transmission electric-lens）And SAED（SEAD）Obtain.With ZnO quantum dot of the dehydrated alcohol to preparation gained
Ethanol solution be diluted, the ethanol solution of the ZnO quantum dot after dilution drop one is dripped on the copper mesh containing carbon film, room temperature
Under the conditions of make alcohol solvent volatilize.ZnO quantum dot is observed under the running voltage of 200KV with transmission electron microscope.
（2）X-ray diffraction（XRD）Test, the sign of ZnO quantum dot crystal structure XRD powder diffractometers in 40KV and
Structured testing is carried out to ZnO quantum dot under the working condition of 40mA.Successively silicon chip is entered with acetone, dehydrated alcohol, deionized water
Row is cleaned by ultrasonic, and is then placed at 50 DEG C in air dry oven and dries.The ethanol solution for preparing the ZnO quantum dot of gained is dripped to
On silicon chip after drying, under room temperature condition, alcohol solvent is made to volatilize.
（3）Steady-state fluorescence（PL）, fluorescence spectrum measured by spectrophotometer (FLS920, Edinburgh), herein, xenon lamp
With photomultiplier tube (R955, Hamamatsu) respectively as excitaton source and fluorescent probe.
（4）Ultra-violet absorption spectrum is tested, and ultra-violet absorption spectrum is by ultraviolet-uisible spectrophotometer (Varian Cary
300) test record is obtained.
Can prepare by above-mentioned steps that size is single, constitutionally stable ZnO quantum dot.
4th, Cd will be obtainedxZn1-xS@ZnSe quantum dots and prepared Zinc oxide quantum dot 13:5 mixing.By LED chip extremely
In bottom, CdxZn1-xS@ZnSe quantum dots revolve figure on chip with Zinc oxide quantum dot mixed liquor, then will measure in LED chip
The quantum dot that son point is mixed with silica gel adds embedding colloid finally in 100 DEG C of drying of baking oven.
A kind of light emitting diode based on Zinc oxide quantum dot is successfully prepared by the method, greatly improves light-emitting diodes
The photoelectric transformation efficiency of pipe.
Claims (1)
1. a kind of preparation method of the light emitting diode based on Zinc oxide quantum dot, including LED chip, quantum dot mixing material and
Silica gel, silica gel is used as embedding colloid；Preparation method is comprised the following steps：
（1）Using Aska-Rid., zinc acetate as cadmium presoma and zinc precursor, tributyl phosphorus is dissolved in selenium powder（TBP）Prepare
Tributyl selenizing phosphorus as selenium presoma, the solution of 1- octadecylenes is dissolved in as sulphur source using sulphur powder, with 1- octadecylenes as solvent,
Oleic acid is obtained oil-soluble Cd as reaction partxZn1-xS@ZnSe quantum dots；Ethanol promotes quantum dot to precipitate, and centrifugation is carried
It is pure, chloroform dissolving dispersion；
（2）Cadmium source：Zinc source：Sulphur source：Selenium source is with 1:10:2:4 molar ratio reaction is obtained quantum dot, and now quantum dot contains not anti-
The organic impuritiess answered, add excess ethyl alcohol to promote quantum dot precipitation and centrifugal separation to obtain pressed powder, add chloroform to dissolve again
Plus excess ethyl alcohol precipitation, obtain pure Cd five times repeatedlyxZn1-xS@ZnSe quantum dot powder；
（3）Pure rare earth selenide quantum dots powder is re-dispersed in chloroform；
（4）The preparation of ZnO quantum dot：By the precursor solution of 10ml zinc acetates on digital display intelligent temperature control magnetic stirring apparatuss room temperature
Stirring, the concentration then newly prepared 0.5ml are rapidly injected in reaction solution for the ethanol solution of the NaOH of 0.5M, and
Start timing；A certain amount of reaction solution is taken out after the specific response time and is cooled down with ice-water bath immediately, the reaction of taking-up
Sample solution is stored in 0 DEG C -4 DEG C of refrigerator；
（5）By step（1）、（2）、（3）Obtain CdxZn1-xS@ZnSe quantum dots and step（4）Prepared Zinc oxide quantum dot
13:5 mixing.
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| CN201610901324.1A CN106549085A (en) | 2016-10-17 | 2016-10-17 | A kind of preparation method of the light emitting diode based on Zinc oxide quantum dot |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110061119A (en) * | 2019-04-23 | 2019-07-26 | 山西大同大学 | The method and a kind of LED light and its preparation of reduction LED light source colour temperature and blue ray radiation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090093096A (en) * | 2008-02-28 | 2009-09-02 | 재단법인서울대학교산학협력재단 | ZnO Quantum Dots with Monodisperse and High Quality Photoluminescence and Process for Preparing Same |
| CN105885848A (en) * | 2016-05-16 | 2016-08-24 | 南昌航空大学 | Preparation of Cd[x]Zn[1-x]S@ZnSe quantum dots and application of Cd[x]Zn[1-x]S@ZnSe quantum dots in solar cells |
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- 2016-10-17 CN CN201610901324.1A patent/CN106549085A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090093096A (en) * | 2008-02-28 | 2009-09-02 | 재단법인서울대학교산학협력재단 | ZnO Quantum Dots with Monodisperse and High Quality Photoluminescence and Process for Preparing Same |
| CN105885848A (en) * | 2016-05-16 | 2016-08-24 | 南昌航空大学 | Preparation of Cd[x]Zn[1-x]S@ZnSe quantum dots and application of Cd[x]Zn[1-x]S@ZnSe quantum dots in solar cells |
Non-Patent Citations (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110061119A (en) * | 2019-04-23 | 2019-07-26 | 山西大同大学 | The method and a kind of LED light and its preparation of reduction LED light source colour temperature and blue ray radiation |
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