CN109420772A - Hud typed Cu/SnO2Nano wire, preparation method and application - Google Patents
Hud typed Cu/SnO2Nano wire, preparation method and application Download PDFInfo
- Publication number
- CN109420772A CN109420772A CN201710743075.2A CN201710743075A CN109420772A CN 109420772 A CN109420772 A CN 109420772A CN 201710743075 A CN201710743075 A CN 201710743075A CN 109420772 A CN109420772 A CN 109420772A
- Authority
- CN
- China
- Prior art keywords
- sno
- nano wire
- hud typed
- electrode
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- H01L33/36—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 characterised by the electrodes
- H01L33/40—Materials therefor
Abstract
The present invention provides a kind of hud typed Cu/SnO2Nano wire, the nano wire is core-shell type nano-wire, including Cu nano wire and the SnO for being coated on the Cu nanowire surface2.Hud typed Cu/SnO provided by the invention2Nano wire, using SnO2It is coated on Cu nanowire surface, forms core-shell type nano-wire.The hud typed Cu/SnO2Nano wire not only has excellent electric conductivity, but also it is possible to prevente effectively from Cu is oxidized and corrodes in application process, can be used as the electrode material of LED component.
Description
Technical field
The invention belongs to field of nanometer material technology more particularly to a kind of hud typed Cu/SnO2It nano wire, preparation method and answers
With.
Background technique
Quantum dot (quantum dot) is three dimensions in the nanocrystalline of nanometer scale, since it has hair
In addition printing technology can be used quantum is made in quanta point material by the advantages that light spectrum is adjustable, glow peak is extremely narrow, quantum yield is high
Point luminescent diode (Quantum Dot Light Emitting Diode, abbreviation QLED), recently by the generally pass of people
Note, device performance index also quickly grow, are expected to become the selection of next-generation plate technique.
Although QLED, which generallys use ITO, can get preferable performance as anode using ITO as anode, but due to indium category
It is expensive in rare metal, considerably increase production cost.In addition, QLED is current effect type device, to anode requirement
Height, and the resistance of ITO is larger, so that device uniformity is poor；And since the distance between cathode and anode are relatively close, usual ITO sun
Pole surface or edge out-of-flatness, the out-of-flatness position for easily leading to ito anode surface or edge are directly connected with cathode, generate big
Measure leakage current.Therefore, the existing technology has yet to be improved and developed.
Summary of the invention
The purpose of the present invention is to provide a kind of hud typed Cu/SnO2Nano wire and preparation method thereof, it is intended to solve existing
ITO electrode is at high cost, resistance is big, does not have flexibility, and use Cu easy to oxidize and the problem of corrode as electrode material.
Another object of the present invention is to provide a kind of electrodes and preparation method thereof.
A further object of the present invention is to provide a kind of LED components.
The invention is realized in this way one aspect of the present invention, provides a kind of hud typed Cu/SnO2Nano wire, it is described to receive
Rice noodles are core-shell type nano-wire, including Cu nano wire and the SnO for being coated on the Cu nanowire surface2。
Another aspect of the present invention provides a kind of hud typed Cu/SnO2The preparation method of nano wire, comprising the following steps:
Cu precursor solution and Sn precursor solution are provided；
Reducing agent is added in the Cu precursor solution and obtains mixed solution, under inert atmosphere protection, heating makes Cu
After precursor solution reduction generates copper nano-wire, the Sn precursor solution is added in the mixed solution, heat treatment makes
Sn presoma decomposes, and hud typed Cu/SnO is prepared2Nano wire.
Another aspect of the present invention, provides a kind of electrode, and the electrode contains such as above-mentioned hud typed Cu/SnO2Nanometer
Line.
Another aspect of the present invention provides a kind of preparation method of electrode, comprising the following steps:
Macromolecule polymer solution is provided, such as above-mentioned hud typed Cu/ is added in the macromolecule polymer solution
SnO2Nano wire obtains mixed liquor；
The mixed liquor is deposited in substrate, curing process obtains electrode.
Another aspect of the present invention, provides a kind of LED component, and the LED component includes above-mentioned electrode.
Compared with prior art, hud typed Cu/SnO provided by the invention2Nano wire, using SnO2It is coated on Cu nano wire
Surface forms core-shell type nano-wire.The hud typed Cu/SnO2Nano wire not only has excellent electric conductivity, but also can have
Effect avoids Cu from being oxidized and corrode in application process, can be used as the electrode material of LED component.
Hud typed Cu/SnO provided by the invention2Cu presoma is reduced by the preparation method of nano wire using reducing agent
After Cu nano wire, Sn precursor solution is added, generates SnO after Sn presoma is thermally decomposed2And it is attached to Cu nano wire table
Face obtains hud typed Cu/SnO2Nano wire.This method is not only easy to operate easily-controllable, and can by control reaction temperature and
Time Effective Regulation SnO2Deposition velocity, the hud typed Cu/SnO being evenly coated2Nano wire.
Electrode provided by the invention contains above-mentioned hud typed Cu/SnO2Nano wire, it is not only low in cost but also hud typed
Cu/SnO2Nano wire can be uniformly distributed in electrode film, formed reticular structure, greatly enhanced electric conductivity.Further, since
Conductive bodies ingredient Cu nanowire surface is coated with SnO2, therefore in use can be to avoid being oxidized and corrode.
The preparation method of electrode provided by the invention, using high molecular polymer and hud typed Cu/SnO2Nano wire conduct
Raw material prepares electrode, low raw-material cost, and the electrode film being prepared has good transmitance and electric conductivity.In addition, system
The standby obtained electrode has softness, can be applied to flexible device.
LED component provided by the invention contains hud typed Cu/SnO in electrode material2Nano wire, therefore, obtained LED
Device is not only low in cost, but also due to hud typed Cu/SnO2Nano wire is uniformly distributed in electrode film, forms netted knot
Structure greatly enhances the electric conductivity of electrode.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
On the one hand, the embodiment of the invention provides a kind of hud typed Cu/SnO2Nano wire, the nano wire are hud typed receive
Rice noodles, including Cu nano wire and the SnO for being coated on the Cu nanowire surface2。
Compared with prior art, hud typed Cu/SnO provided in an embodiment of the present invention2Nano wire, using SnO2It is coated on Cu
Nanowire surface forms core-shell type nano-wire.The hud typed Cu/SnO2Nano wire not only has excellent electric conductivity, but also
It is possible to prevente effectively from Cu is oxidized and corrodes in application process, the electrode material of LED component can be used as.
Hud typed Cu/SnO provided in an embodiment of the present invention2Nano wire can be prepared by following methods.
On the other hand, the embodiment of the invention provides a kind of hud typed Cu/SnO2The preparation method of nano wire, including it is following
Step:
S01., Cu precursor solution and Sn precursor solution are provided；
S02. reducing agent is added in the Cu precursor solution and obtains mixed solution, under inert atmosphere protection, heating
Becoming peony to solution, the Sn precursor solution is added in the mixed solution, heat treatment decomposes Sn presoma,
Hud typed Cu/SnO is prepared2Nano wire.
Hud typed Cu/SnO provided in an embodiment of the present invention2The preparation method of nano wire, using reducing agent by Cu presoma
After being reduced into Cu nano wire, Sn precursor solution is added, Sn presoma is thermally decomposed to generate into SnO2And it is attached to Cu nanometers
Line surface obtains hud typed Cu/SnO2Nano wire.This method is not only easy to operate easily-controllable, but also can pass through control reaction temperature
Degree and time Effective Regulation SnO2Deposition velocity, the hud typed Cu/SnO being evenly coated2Nano wire.
Specifically, the Cu precursor solution provides Cu presoma, as hud typed Cu/SnO in above-mentioned steps S012It receives
The source Cu of rice noodles；The Sn precursor solution provides Sn presoma, as hud typed Cu/SnO2The source Sn of nano wire.Specifically,
The Cu forerunner is cupric salt, and the Sn presoma is pink salt, and the Sn presoma can be thermally decomposed in following step
For SnO2, therefore, the Sn presoma is oxygen-containing pink salt.
As a preferred embodiment, the preparation method of the Cu precursor solution is as follows: providing copper source, it is organic to be dissolved in first
In amine solvent, Cu precursor solution is obtained.Wherein, copper source is the mantoquita that can be dissolved in first organic amine solvent,
Including but not limited to CuCl2·2H2O, anhydrous Cu (CH3COO)2、Cu(NO3)2·3H2O.Due to needed in following step S02 by
Sn presoma carries out thermal decomposition process, it is preferred, therefore, that the boiling temperature of first organic amine solvent is higher than pyrolysis
When the temperature that heats, volatilizing to avoid solvent influences reaction effect.Specific preferred, first organic amine solvent is oil
At least one of amine, cetylamine, trioctylamine.In the present embodiment, it is preferred that copper source is in first organic amine solvent
Dissolution, solid copper source substance can be completely dissolved by heat treatment, formed Cu presoma.Specifically, in inert atmosphere
Under, it is heated to 60-90 DEG C, such as 70 DEG C, heat preservation to solid matter is completely dissolved.
As another preferred embodiment, the Sn precursor solution the preparation method is as follows: provide tin source, be dissolved in second
In organic amine solvent, Sn precursor solution is obtained.Wherein, the tin source be can the second organic amine solvent kind dissolve and
It is easy to the oxygen-containing pink salt thermally decomposed, including but not limited to Sn (acac)2、Sn(CH3COO)2.Due to needed in following step S02 by
Sn presoma carries out oxidation processes, it is preferred, therefore, that the boiling temperature of second organic amine solvent adds when being higher than oxidation reaction
The temperature of heat treatment, volatilizing to avoid solvent influences reaction effect.It is specific preferred, second organic amine solvent be oleyl amine,
At least one of cetylamine, trioctylamine.In the present embodiment, it is preferred that the tin source is in second organic amine solvent
Solid tin source substance, can be completely dissolved by dissolution by heat treatment, form Sn presoma.Specifically, in inert atmosphere
Under, it is heated to 120-180 DEG C, such as 150 DEG C, heat preservation to solid matter is completely dissolved.
In above-mentioned steps S02, reducing agent is added in the Cu precursor solution, under inert atmosphere protection, is heating
Under the conditions of, redox reaction occurs for the Cu presoma in the reducing agent and the Cu precursor solution, obtains Cu nano wire.
Specifically, becoming peony when being warming up to solution, redox reaction terminates.
Preferably, the reducing agent is three (trimethylsilyl) silane, glucose, vitamin C, at least one in hydrazine hydrate
Kind, more preferably three (trimethylsilyl) silane.Cu presoma can not only be reduced to copper nano-wire by preferred reducing agent, and
And preferred reducing agent, it will not introduce other miscellaneous side reactions, it especially will not be with the Sn precursor solution of addition in heating condition
Under react, thus the hud typed Cu/SnO that ensure that2The performance of nano wire.
Preferably, the molar ratio of the Cu presoma in the Cu precursor solution and the reducing agent is 1:3-4.If described
The content of reducing agent is very few, then cannot sufficiently restore the Cu presoma, in finally obtained product, before remaining Cu
Body impurity is driven, hud typed Cu/SnO is influenced2The purity of nano wire；If the too high levels of the reducing agent, remaining reducing agent meeting
Cause reaction system viscosity excessively high, the SnO for being unfavorable for the oxidation of subsequent Sn presoma and obtaining2In Cu nanowire surface
Deposition.
Preferably, the step of heating makes the reduction of Cu precursor solution generate copper nano-wire uses temperature programming to realize,
And the method for described program heating is as follows: being heated to 110-130 DEG C, Cu presoma (blue solution) is made to be reduced to monovalence copper
After (solution colour becomes yellow from blue)；It is heated to 160-180 DEG C, so that monovalence copper reduction is generated copper nano-wire, at this time
Solution is in peony.The embodiment of the present invention uses temperature programming, can effectively control reaction rate, high when avoiding directly heating up
Nucleation rate causes Cu presoma side border ring to be accumulated, and directly generates Cu nanoparticle rather than Cu nano wire.
Further, the Sn precursor solution is added in the mixed solution, it is preferred that the Cu precursor solution
In Cu and the Sn precursor solution in Sn molar ratio be 1:0.1-0.5, i.e., the additive amount of the described Sn precursor solution
Meet: in the mixed solution after the Sn precursor solution is added, Cu, Sn molar ratio are 1:0.1-0.5.If the Sn presoma
The additive amount of solution is very few, then the SnO formed2Content is less, cannot coat the surface of Cu nano wire completely, lead to the nucleocapsid
Type Cu/SnO2Nano wire is as electrode material in use, there are still be easily oxidized and corrode.If the Sn presoma
The adding too much of solution is then coated on the SnO of Cu nanowire surface2Thickness spends thickness, influences the electric conductivity of material, is unfavorable for
It is used as electrode material.
The embodiment of the present invention is by heat treatment by Sn oxidation of precursor at SnO2, it is coated on Cu nanowire surface.It is preferred that
, the temperature of the heat treatment is 240-300 DEG C.If temperature is too low, it cannot effectively cause decomposition reaction；If reaction temperature
It is excessively high, on the one hand, to may cause the solvent volatilization in reaction system, influence system material concentration, and then be unfavorable for reaction rate
Adjusting；On the other hand, excessively high temperature may cause side reaction.It is further preferred that being protected under the conditions of above-mentioned temperature
It is 0.5-1 hours warm, guarantee the abundant progress of reaction, and obtain SnO2The suitably hud typed Cu/SnO of thickness degree2Nano wire.
Further, the reaction system after oxidation reaction is cooled to room temperature, is then centrifuged, is centrifugated
Ethyl alcohol can be used with reagent, but not limited to this.It further, can be by isolated hud typed Cu/SnO2Nano wire sample
It is dispersed in spare in n-hexane, toluene or tetrahydrofuran.
On the other hand, the embodiment of the invention provides a kind of electrode, the electrode contains such as above-mentioned hud typed Cu/SnO2
Nano wire.
Electrode provided in an embodiment of the present invention contains above-mentioned hud typed Cu/SnO2Nano wire, it is not only low in cost, but also
Hud typed Cu/SnO2Nano wire can be uniformly distributed in electrode film, formed reticular structure, greatly enhanced electric conductivity.This
Outside, since conductive bodies ingredient Cu nanowire surface is coated with SnO2, therefore can be oxidized in use to avoid copper and
Corrosion.
Preferably, contain high molecular polymer in the electrode.The hud typed Cu/SnO2Nano wire is in the macromolecule
It is evenly dispersed in polymer, reticular structure is formed, electric conductivity is further enhanced.And the electrode being consequently formed, have preferable
Flexibility, can be applied to flexible device.
It is further preferred that the high molecular polymer is transparent high molecular polymer, thus obtained electrode material
Excellent electric conductivity and translucency are had both, the electrode that can be used as LED component uses, to reduce the cost of LED component.It is preferred that
, the high molecular polymer is polyimides, polyurethane, polystyrene, polypropylene, polyaniline, epoxy resin, polyacrylic acid
At least one of ester, but not limited to this.
Further, in the electrode, the hud typed Cu/SnO2The mass ratio of nano wire and high molecular polymer is
5-50:100, so that electrode has both preferably flexible and electric conductivity.If the high molecular polymer content is too low, flexible phase
To variation, but electric conductivity increases；If the high molecular polymer too high levels, the flexibility of product is preferable, but electric conductivity
It is bad.
In the embodiment of the present invention, the electrode is the anode or cathode of LED component, wherein the LED component can be QLED
Device and OLED device.
Electrode provided in an embodiment of the present invention can be prepared by following methods.
On the other hand, the embodiment of the invention provides a kind of preparation methods of electrode, comprising the following steps:
Q01., macromolecule polymer solution is provided, is added in the macromolecule polymer solution as above-mentioned hud typed
Cu/SnO2Nano wire obtains mixed liquor；
Q02. the mixed liquor is deposited in substrate, curing process obtains electrode.
The preparation method of electrode provided in an embodiment of the present invention, using high molecular polymer and hud typed Cu/SnO2Nanometer
Line prepares electrode, low raw-material cost as raw material, and the electrode film being prepared has good transmitance and electric conductivity.This
Outside, the electrode being prepared has softness, can be applied to flexible device.
Specifically, in above-mentioned steps Q01, the hud typed Cu/SnO2Nano wire can be prepared using the above method,
The hud typed Cu/SnO2Nano wire can be added with colloidal solution.High molecular polymerization in the macromolecule polymer solution
The selection of object is as previously mentioned, in order to save length, and details are not described herein again.The macromolecule polymer solution can be the high score
The toluene solution of sub- polymer, but not limited to this.
In above-mentioned steps Q02, the mixed liquor is deposited on substrate, is realized using solution processing method, including but not limited to
Thus spin coating, spraying, inkjet printing etc. obtain flat and smooth fexible film.
In the embodiment of the present invention, the curing process is preferably carried out under the conditions of 60-80 DEG C, to prevent hot conditions from destroying
The property of high molecular polymer, curing time are preferably 40-60min, thus obtain the anode film of homogeneous transparent.
On the other hand, the embodiment of the invention provides a kind of LED component, the LED component includes above-mentioned electrode.
LED component provided in an embodiment of the present invention contains hud typed Cu/SnO in electrode material2Therefore nano wire obtains
LED component it is not only low in cost, but also due to hud typed Cu/SnO2Nano wire is uniformly distributed in electrode film, forms net
Shape structure greatly enhances the electric conductivity of electrode.
Wherein, the LED component can be QLED device or OLED device, and the LED component may include necessary function
Ergosphere, including cathode, anode and luminescent layer, in addition, it can include other auxiliary functional layers, as hole functional layer (including but
It is not limited at least one layer of hole injection layer, hole transmission layer) and electronic work ergosphere (including but not limited to electron injecting layer, electricity
At least one layer of sub- transport layer).And the LED component can (such as LED component successively includes substrate, sun for eurymeric LED component
Pole, hole functional layer, luminescent layer, electronic work ergosphere, cathode), or (such as LED component successively includes sun to transoid LED component
Pole, hole functional layer, luminescent layer, electronic work ergosphere, cathode, substrate).The electrode can be used as the cathode or sun of LED component
Pole.
As a kind of specific preferred situation, the LED component can be QLED device, including anode, the sky successively combined
Cave implanted layer, hole transmission layer, quantum dot light emitting layer, electron transfer layer and cathode, wherein the anode is by hud typed Cu/
SnO2Laminated film made of nano wire and high molecular polymer.
Wherein, the hole injection layer material includes but is not limited to PEDOT:PSS, MoO3、Nb2O5,NiO.This thicknesses of layers
Range is 30-80nm.
The hole transport layer material is organic compound or metal oxide with electron donation, including is organised
Close object and metallic compound.Wherein, with electron donation organic compound include but is not limited to NPB, TPD, TAPC, TFB,
OTPD, QTPD, Poly-TPD, PVK etc.；The metal oxide is molybdenum oxide, in vanadium oxide, nickel oxide, copper oxide, tungsten oxide
One kind.The thicknesses of layers range of the hole transmission layer is 30~100nm.
The quantum dot light emitting layer material is the quanta point material of this field routine, can be three kinds of quantum dots of red, green, blue
Any one quantum dot or in which any two or three of quantum dot combination, or other quantum dots such as yellow light quantum
Point.
The electron transport layer materials can be the preferable metal oxide of electronic transmission performance, such as TiO2, ZnO, but it is unlimited
In this.Preferably, electron transfer layer is the N-shaped zinc oxide with high electronic transmission performance, preferably with a thickness of 30-60nm.
The cathode material chooses one or more of aluminium, magnesium, calcium, barium, titanium, 50~300nm of thicknesses of layers.
The preparation method of QLED device described in the embodiment of the present invention, anode can be prepared in substrate, is then sequentially depositing
Each functional layer and cathode.Wherein, anode or cathode contains hud typed Cu/SnO to be above-mentioned2The electrode of nano wire, preparation method ginseng
According to the preparation method of electrode.Each functional layer can be using the realization of solution processing method, including but not limited to spin coating, spraying and ink-jet
Printing.Without containing Cu/SnO2The electrode of nano wire can be deposited using solwution method or vacuum evaporation.
The substrate does not limit clearly, can be glass substrate, flexible polymer substrate, metal substrate.In order to improve
The adhesion of hearth electrode is surface-treated to described, and method is preferably as follows: substrate is placed in order acetone, washing lotion, go from
It is cleaned by ultrasonic in sub- water and isopropanol, ultrasonic time can be 10-20 minutes, such as 15 minutes.After the completion of being cleaned by ultrasonic,
Substrate is placed in cleaning oven and is dried for standby.
It is illustrated combined with specific embodiments below.
Embodiment 1
A kind of hud typed Cu/SnO2The preparation method of nano wire colloid, comprising the following steps:
The preparation of S11.Cu precursor solution: in the three-necked flask of 50mL, 85-170mg CuCl is added2·2H2O(0.5-
1mmol), 10-20mL oleyl amine is added, is heated to 70 DEG C under protection of argon gas；Heat preservation is completely dissolved up to solid matter, is formed
Cu precursor solution；
The preparation of S12.Sn precursor solution: in the three-necked flask of 50mL, 31.6-63.4mg acetylacetone,2,4-pentanedione tin is added
(0.1-0.2mmol), adds 10mL trioctylamine, is heated to 150 DEG C under inert gas protection；Until solid matter is completely molten
Solution forms Sn presoma；
S13. three (trimethylsilyl) silane 2-4mmol are added in Cu precursor solution in step s 11；In indifferent gas
After body protects lower solution blue, temperature is slowly risen to 120 DEG C, after solution gradually becomes yellow by blue, then slowly will
Temperature rises to 160-180 DEG C of stirring 5-20h；Sn presoma after solution colour becomes peony, in disposable injection step S12
The mole of solution 4-8mL, injected Sn are 0.1-0.5 times of Cu mole；It is to slowly warm up to 240-300 DEG C and keeps the temperature 1h；
It is cooled to room temperature, ethyl alcohol is added, it is after centrifuge separation, sample dispersion is spare in n-hexane.
Embodiment 2
It is a kind of to utilize hud typed Cu/SnO2Preparation method of the nano wire colloid as the QLED device of anode, including it is following
Step:
Anode is made in substrate；The anode specifically the production method is as follows:
Macromolecule polymer solution is provided, one of described high molecular polymer is dissolved in toluene and is formed after solution again
The hud typed Cu/SnO provided with above-described embodiment 12The mixing of nano wire colloidal solution, the mixed liquor is deposited in substrate
On, solidify 40-60min under the conditions of 60-80 DEG C, obtains homogeneous transparent anode film.The anode film with a thickness of 30-
100nm。
Deposition of hole transport layer, quantum dot light emitting layer, electron transfer layer on the anode, last evaporation cathode, obtain
QLED device.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (16)
1. a kind of hud typed Cu/SnO2Nano wire, which is characterized in that the nano wire is core-shell type nano-wire, including Cu nano wire
With the SnO for being coated on the Cu nanowire surface2。
2. a kind of hud typed Cu/SnO2The preparation method of nano wire, which comprises the following steps:
Cu precursor solution and Sn precursor solution are provided；
Reducing agent is added in the Cu precursor solution and obtains mixed solution, under inert atmosphere protection, heating makes Cu forerunner
After liquid solution reduction generates copper nano-wire, the Sn precursor solution is added in the mixed solution, before heat treatment makes Sn
It drives body to decompose, hud typed Cu/SnO is prepared2Nano wire.
3. hud typed Cu/SnO as claimed in claim 22The preparation method of nano wire, which is characterized in that before the heating makes Cu
It drives the step of liquid solution reduction generates copper nano-wire to realize using temperature programming, and the method for described program heating is as follows: heating
It is warming up to 110-130 DEG C, after so that Cu presoma is reduced to monovalence copper；It is heated to 160-180 DEG C, generates monovalence copper reduction
Copper nano-wire.
4. hud typed Cu/SnO as claimed in claim 22The preparation method of nano wire, which is characterized in that the heat treatment
Temperature is 240-300 DEG C.
5. such as the described in any item hud typed Cu/SnO of claim 2-42The preparation method of nano wire, which is characterized in that described to go back
Former agent is at least one of three (trimethylsilyl) silane, glucose, vitamin C, hydrazine hydrate.
6. such as the described in any item hud typed Cu/SnO of claim 2-42The preparation method of nano wire, which is characterized in that the Cu
The molar ratio of Cu presoma and the reducing agent in precursor solution is 1:3-4；And/or
The molar ratio of the Sn in Cu and the Sn precursor solution in the Cu precursor solution is 1:0.1-0.5.
7. such as the described in any item hud typed Cu/SnO of claim 2-42The preparation method of nano wire, which is characterized in that the Cu
Precursor solution the preparation method is as follows: provide copper source, be dissolved in the first organic amine solvent, obtain Cu precursor solution；And/or
The Sn precursor solution the preparation method is as follows: provide tin source, be dissolved in the second organic amine solvent, obtain Sn presoma
Solution.
8. hud typed Cu/SnO as claimed in claim 72The preparation method of nano wire, which is characterized in that first organic amine
Solvent, second organic amine solvent boiling temperature be higher than the heat treatment temperature.
9. a kind of electrode, which is characterized in that the electrode contains such as the described in any item hud typed Cu/SnO of claim 2-82It receives
Rice noodles.
10. electrode as claimed in claim 9, which is characterized in that contain high molecular polymer in the electrode.
11. electrode as claimed in claim 10, which is characterized in that the high molecular polymer is transparent high molecular polymerization
Object.
12. electrode as claimed in claim 10, which is characterized in that in the electrode, the high molecular polymer is that polyamides is sub-
At least one of amine, polyurethane, polystyrene, polypropylene, polyaniline, epoxy resin, polyacrylate.
13. electrode as claimed in claim 10, which is characterized in that in the electrode, the hud typed Cu/SnO2Nano wire with
The mass ratio of high molecular polymer is 5-50:100.
14. such as the described in any item electrodes of claim 9-13, which is characterized in that the electrode is the anode or yin of LED component
Pole.
15. a kind of preparation method of electrode, which comprises the following steps:
Macromolecule polymer solution is provided, is added as described in claim any one of 2-8 in the macromolecule polymer solution
Hud typed Cu/SnO2Nano wire obtains mixed liquor；
The mixed liquor is deposited in substrate, curing process obtains electrode.
16. a kind of LED component, which is characterized in that the LED component includes such as the described in any item electrodes of claim 9-14.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710743075.2A CN109420772A (en) | 2017-08-25 | 2017-08-25 | Hud typed Cu/SnO2Nano wire, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710743075.2A CN109420772A (en) | 2017-08-25 | 2017-08-25 | Hud typed Cu/SnO2Nano wire, preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109420772A true CN109420772A (en) | 2019-03-05 |
Family
ID=65501647
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710743075.2A Pending CN109420772A (en) | 2017-08-25 | 2017-08-25 | Hud typed Cu/SnO2Nano wire, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109420772A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112863875A (en) * | 2020-11-26 | 2021-05-28 | 南昌航空大学 | Preparation method of core-shell structure tin oxide photo-anode dye-sensitized solar cell |
| CN114591715A (en) * | 2020-12-04 | 2022-06-07 | 哈尔滨工业大学 | Preparation method of C-band composite electromagnetic wave-absorbing material |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1727523A (en) * | 2004-07-26 | 2006-02-01 | 中国科学院物理研究所 | The method of liquid phase synthesizing one-dimensional super long Nano line of metal copper |
| US20070212562A1 (en) * | 2006-02-24 | 2007-09-13 | Samsung Electro-Mecanics Co., Ltd. | Core-shell structure metal nanoparticles and its manufacturing method |
| CN101319357A (en) * | 2008-06-20 | 2008-12-10 | 江苏大学 | Preparation of copper nano-wire with microwave auxiliary liquid phase reduction |
| CN102251278A (en) * | 2011-05-31 | 2011-11-23 | 常州大学 | Controllable preparation method of monocrystal copper nanowires |
| CN102554219A (en) * | 2012-01-31 | 2012-07-11 | 云南云天化股份有限公司 | Nanoparticle of copper-tin nuclear shell structure and preparation method for nanoparticle |
| CN103084581A (en) * | 2013-01-08 | 2013-05-08 | 河南大学 | Preparation method for copper nanowire |
| CN104959626A (en) * | 2015-06-30 | 2015-10-07 | 厦门大学 | Method for preparing multifunctional core-shell nano-material by using alloy to wrap copper nanowires |
| CN105304829A (en) * | 2015-11-18 | 2016-02-03 | Tcl集团股份有限公司 | Double-sided emission quantum dot light emitting diode and manufacturing method thereof |
| CN105576145A (en) * | 2016-02-29 | 2016-05-11 | Tcl集团股份有限公司 | Quantum dot light emitting diode (QLED), display and preparation method |
| CN105618785A (en) * | 2016-01-15 | 2016-06-01 | 浙江大学 | Preparation method for copper/silver nanowires of core-shell structures |
| CN106670496A (en) * | 2015-11-10 | 2017-05-17 | 南京理工大学 | Preparation method of copper nanowires or copper nanoparticles |
-
2017
- 2017-08-25 CN CN201710743075.2A patent/CN109420772A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1727523A (en) * | 2004-07-26 | 2006-02-01 | 中国科学院物理研究所 | The method of liquid phase synthesizing one-dimensional super long Nano line of metal copper |
| US20070212562A1 (en) * | 2006-02-24 | 2007-09-13 | Samsung Electro-Mecanics Co., Ltd. | Core-shell structure metal nanoparticles and its manufacturing method |
| CN101319357A (en) * | 2008-06-20 | 2008-12-10 | 江苏大学 | Preparation of copper nano-wire with microwave auxiliary liquid phase reduction |
| CN102251278A (en) * | 2011-05-31 | 2011-11-23 | 常州大学 | Controllable preparation method of monocrystal copper nanowires |
| CN102554219A (en) * | 2012-01-31 | 2012-07-11 | 云南云天化股份有限公司 | Nanoparticle of copper-tin nuclear shell structure and preparation method for nanoparticle |
| CN103084581A (en) * | 2013-01-08 | 2013-05-08 | 河南大学 | Preparation method for copper nanowire |
| CN104959626A (en) * | 2015-06-30 | 2015-10-07 | 厦门大学 | Method for preparing multifunctional core-shell nano-material by using alloy to wrap copper nanowires |
| CN106670496A (en) * | 2015-11-10 | 2017-05-17 | 南京理工大学 | Preparation method of copper nanowires or copper nanoparticles |
| CN105304829A (en) * | 2015-11-18 | 2016-02-03 | Tcl集团股份有限公司 | Double-sided emission quantum dot light emitting diode and manufacturing method thereof |
| CN105618785A (en) * | 2016-01-15 | 2016-06-01 | 浙江大学 | Preparation method for copper/silver nanowires of core-shell structures |
| CN105576145A (en) * | 2016-02-29 | 2016-05-11 | Tcl集团股份有限公司 | Quantum dot light emitting diode (QLED), display and preparation method |
Non-Patent Citations (3)
| Title |
|---|
| HUI LIUN等: "Preparation andenhancedphotocatalyticactivityofAg-nanowires@SnO2 core–shell heterogeneousstructures", 《CERAMICS INTERNATIONAL》 * |
| 牟国俊: "纳米核壳式铜-锡双金属粉的制备及性能研究", 《无机化学学报》 * |
| 胡天麒: "Cu@Sn核壳粉体制备及其高熔点焊缝的性能与组织演变", 《博士论文》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112863875A (en) * | 2020-11-26 | 2021-05-28 | 南昌航空大学 | Preparation method of core-shell structure tin oxide photo-anode dye-sensitized solar cell |
| CN114591715A (en) * | 2020-12-04 | 2022-06-07 | 哈尔滨工业大学 | Preparation method of C-band composite electromagnetic wave-absorbing material |
| CN114591715B (en) * | 2020-12-04 | 2023-09-12 | 哈尔滨工业大学 | Preparation method of C-band composite electromagnetic wave-absorbing material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104064690B (en) | There is Organic Light Emitting Diode of double-decker electron transfer layer and preparation method thereof | |
| JP4983021B2 (en) | Transparent conductive laminate, organic EL element using the same, and method for producing the same | |
| CN106654016B (en) | A kind of organic electro-optic device and preparation method thereof and the composition with hole transport performance | |
| CN106784348A (en) | QLED containing noble metal nanometer material and preparation method thereof | |
| KR20170041735A (en) | Electroluminescent crosslinked nanocrystal films | |
| CN105470400B (en) | A kind of preparation method and application of perovskite film | |
| CN108735906A (en) | Metal oxide, QLED and the preparation method of acrylate copolymer modification | |
| CN110273170B (en) | Graphene-coated metal nanowire network and preparation method thereof | |
| CN109980097A (en) | A kind of preparation method of film and QLED device | |
| US6949403B2 (en) | Non-vacuum methods for the fabrication of organic semiconductor devices | |
| CN109420772A (en) | Hud typed Cu/SnO2Nano wire, preparation method and application | |
| JPH0541285A (en) | Electroluminescence element | |
| Jeong et al. | Characteristics of inkjet-printed nano indium tin oxide particles for transparent conducting electrodes | |
| CN105047827A (en) | Top-emitting organic electroluminescent device | |
| CN106450042A (en) | Metal oxide, QLED and preparation method | |
| CN101835709B (en) | Wet-processible metal oxide solution, preparation method of the same, and organic photovoltaic cell of using the same | |
| CN104540777B (en) | For forming the core-shell nanoparticles of nesa coating and using its manufacture method of nesa coating | |
| US11823849B2 (en) | Efficient and stable inorganic lead-free perovskite solar cell and method for preparing the same | |
| Wu et al. | Room-temperature preparation of crystalline TiO2 thin films and their applications in polymer/TiO2 hybrid optoelectronic devices | |
| CN114260450A (en) | Silver-plated micron-sized particles and preparation method and application thereof | |
| CN109817838A (en) | The preparation method and QLED device of sull | |
| CN113773695A (en) | Metal oxide ink based on chemical modification and preparation method and application thereof | |
| CN106395894A (en) | Process for preparing film material by covering film hydrolysis | |
| CN109962133B (en) | QLED device and preparation method thereof | |
| CN110473986A (en) | Flexible organic electroluminescent device and preparation method based on silver nanowires film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190305 |
|
| RJ01 | Rejection of invention patent application after publication |