CN108232038A - A kind of light emitting diode based on calcium nutrition film and preparation method thereof - Google Patents
A kind of light emitting diode based on calcium nutrition film and preparation method thereof Download PDFInfo
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- CN108232038A CN108232038A CN201810014483.9A CN201810014483A CN108232038A CN 108232038 A CN108232038 A CN 108232038A CN 201810014483 A CN201810014483 A CN 201810014483A CN 108232038 A CN108232038 A CN 108232038A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
- H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
Abstract
The invention discloses a kind of light emitting diodes based on calcium nutrition film and preparation method thereof, the light emitting diode sequentially consists of substrate, anode layer, hole transmission layer, luminescent layer, electron transfer layer and cathode layer, and the luminescent layer is using organic and inorganic hybridization ABX3Type cubic crystal structure luminescent material is made, wherein A is organic amine group, B is the 4th main group metal, X is the combination of unitary halogen or polynary halogen, steaming perovskite precursor material is mixed using double source perovskite thin film is formed on substrate in the preparation process of the luminescent layer, the substrate contact refrigeration backboard, substrate is kept during vapor deposition in low-temperature condition, precursor material molecule can crystallize rapidly in low temperature substrates, crystal grain roughness is low in the perovskite thin film of formation, good crystallinity, crystal grain are small.The method improves brightness and the quantum efficiency of light emitting diode, solves the problems, such as that perovskite light emitting diode aberrations in property is big, brightness is weak.
Description
Technical field
The present invention relates to electroluminescent device technical field more particularly to a kind of light emitting diodes based on calcium nutrition film
And preparation method thereof.
Background technology
MAPbX3(metal halide perovskite material), wherein X are Br, I and Cl, and such material has excellent photoelectricity spy
Property, it can be widely applied in the photoelectric devices such as solar cell, optical detector and light emitting diode, wherein, based on perovskite
Light emitting diode has the characteristics that luminance purity is high, emission effciency is high low with excitation energy, therefore will become and substitute inorganic quantum
The advanced luminescent material of point and conventional organic luminescence material.
It compares patent " 201610635175.9 " a kind of Double Perovskite light emitting diode and preparation method thereof and comparison is special
Sharp " 201610083290.X " a kind of light emitting diode based on perovskite material and preparation method thereof, perovskite luminescent layer is all
It is prepared using spin coating proceeding, preparation process controllability and poor repeatability, at the same time, is prepared using pressure decatizing depositing process
The problem of perovskite light emitting diode performance is relatively low, and especially brightness is very weak is urgently to be resolved hurrily.
Invention content
It is an object of the invention to：A kind of light emitting diode based on calcium nutrition film and preparation method thereof is provided, is solved
The problem of perovskite light emitting diode aberrations in property is big, brightness is weak.
The technical solution adopted by the present invention is as follows：
A kind of light emitting diode based on calcium nutrition film, it is characterised in that：The light emitting diode is from bottom to up successively
For substrate, anode layer, hole transmission layer, luminescent layer, electron transfer layer and cathode layer.
Further, the luminescent layer is using organic and inorganic hybridization ABX3 type cubic crystal structure perovskite luminescent materials
It is made.
Further, the thickness of the anode layer be 10~200nm, thickness of hole transport layer be 20~80nm, luminescent layer
Thickness is 20~80nm, and electronics layer thickness is 20~80nm, and cathode electrode layer thickness is 100~200nm.
A kind of light-emitting diodes tube preparation method based on calcium nutrition film, includes the following steps：
Step 1：It is dried after being cleaned to substrate；
Step 2：Dried substrate is pre-processed with UV；
Step 3：Pretreated substrate is passed to the preparation of vacuum chamber progress anode layer；
Step 4：The substrate for being prepared for anode layer is passed to and is evaporated in vacuo room, and according to diode device structure successively to sky
Cave transport layer, luminescent layer, electron transfer layer and cathode layer carry out vapor deposition treatment；
Step 5：Diode component after vapor deposition treatment is packaged.
Further, it is clear to carry out ultrasound using ethanol solution, acetone soln and deionized water to substrate successively for the step 1
It washes.
Preferably, the step 4 carries out cooling processing using refrigeration backboard during luminescent layer is deposited to substrate.
Further, the temperature of the refrigeration backboard is controlled at -10 DEG C~5 DEG C.
Further, the packaging environment of diode component is in the glove box of atmosphere of inert gases in the step 5.
Preferably, the precursor material that the step 4 luminescent layer vapor deposition uses is CH3NH3Br3And PbBr2。
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1st, in the present invention, by changing the preparation process of diode component luminescent layer, steaming perovskite is mixed using double source
CH3NH3Br3And PbBr2As vapor deposition precursor material, perovskite thin film is formed on substrate, is subject to low temperature to substrate, using this
Perovskite thin film roughness prepared by technique is low, and good crystallinity, crystal grain is small, while controls diode by controlling temperature
Light emission luminance enhances the controllability of preparation process.
2nd, by the present invention in that using ABX3Luminescent layer of the perovskite of structure as diode component realizes high brightness, height
The perovskite light emitting diode of efficiency.
Description of the drawings
Fig. 1 is the structure diagram of light emitting diode of the present invention；
Fig. 2 is 2 light emitting diode electroluminescent spectrum of the embodiment of the present invention；
It is marked in figure：1- transparent substrates, 2- anode layers, 3- hole transmission layers, 4- luminescent layers, 5- electron transfer layers, 6- are cloudy
Pole layer, 7- additional power sources.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.
As shown in Figure 1, a kind of light emitting diode based on calcium nutrition film, the light emitting diode sequentially consist of
Substrate 1, anode layer 2, hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6.Wherein anode layer 2 is located at 1 table of substrate
Face, diode component shine under the driving of additional power source 7.
The anode layer 2, which includes, has sufficiently conductive property to convey hole to the electrode of hole transport 3, preferably work function compared with
High material, generally use inorganic, metal oxide (such as tin indium oxide ITO), organic conductive polymer (such as PEDOT：PSS、
PANI etc.), high-work-function metal material (such as gold, copper, silver, platinum), the anode layer 2 further includes buffer layer, which can
To be inorganic compound or there is the organic compound of low HOMO, such as phthalein cyanogen copper, molybdenum oxide, vanadium oxide, copper oxide, oxidation
Nickel, silica etc., the preferred tin indium oxide of 2 material of anode layer of the present invention (ITO).
The material of the hole transmission layer 3 is aromatic diamines compound, aromatic triamine class compound, carbazoles
It closes one or more in object, star triphenylamine compound, furfuran compound, spiral shell shape structural compounds or polymer material
Combination, 3 material of hole transmission layer preferably 4,4'- cyclohexyl two [N, N- bis- (4- aminomethyl phenyls) aniline] (TAPC).
For the luminescent layer 4 using the luminescent material with perovskite structure, the perovskite material is hybrid
ABX3Type cubic crystal structure, A are organic amine group；B is the 4th main group metal；X is unitary halogen or polynary halogen family member
The combination of element.
The material of the electron transfer layer 5 is 2- (4- diphenyl) -5- (4- 2-methyl-2-phenylpropanes base) -1,3,4- oxadiazole, Evil bis-
Azole electron transport material 2- (4- diphenyl) -5- (4- 2-methyl-2-phenylpropanes base) -1,3,4- oxadiazoles, imidazoles electron transport material 1,
Any one or a variety of combinations, electron transfer layer of the present invention in 3,5- tri- (N- phenyl -2- benzimidazolyl-2 radicals) benzene is preferred
1,3,5- tri- (1- phenyl -1H- benzimidazolyl-2 radicals-yl) benzene (TPBi).
The cathode layer 6 includes, and there is sufficiently conductive property to convey electronics to the electrode of electron transfer layer 5, preferably work content
The relatively low material of number, generally use metal-oxide film (such as tin indium oxide ITO, zinc oxide, zinc tin oxide) or metal foil
Film (alloys of the metals such as lithium, magnesium, calcium, strontium, aluminium, indium or copper, gold, silver), the cathode layer 6 include buffer layer, the buffer layer
Can be inorganic compound or the organic compound with high LUMO, such as ZnO, LiF or CsF, 6 material of cathode layer of the present invention is excellent
Select Mg:Ag.
Further, the thickness of the anode layer 2 is 10~200nm, and 3 thickness of hole transmission layer is 20~80nm, is shone
4 thickness of layer are 20~80nm, and 5 thickness of electron transfer layer is 20~80nm, and 6 thickness of cathode layer is 100~200nm.
The present invention proposes a kind of above-mentioned light-emitting diodes tube preparation method based on calcium nutrition film, includes the following steps：
Step 1：It is dried after being cleaned to substrate 1；
Step 2：Dried substrate 1 is pre-processed with UV；
Step 3：Pretreated substrate 1 is passed to the preparation of vacuum chamber progress anode layer 2；
Step 4：The incoming vacuum evaporation room of substrate 1 that will be prepared for anode layer 2, and it is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment；
Step 5：Diode component after vapor deposition treatment is packaged.
Further, the step 1 carries out ultrasound using ethanol solution, acetone soln and deionized water to substrate 1 successively
Cleaning.
Preferably, the step 4 carries out cooling processing using refrigeration backboard during luminescent layer 4 is deposited to substrate.
Further, the temperature of the refrigeration backboard is controlled at -10 DEG C~5 DEG C.
Further, the packaging environment of diode component is in the glove box of atmosphere of inert gases in the step 5.
Preferably, the precursor material that the step 4 luminescent layer vapor deposition uses is CH3NH3Br3And PbBr2。
Embodiment 1 (control group)
Diode device structure sequentially consists of：
ITO/TAPC(40nm)/CH3NH3PbBr3(50nm)/TPBi(40nm)/Ag(100nm)
Preparation method step is as follows：
Step 1：It is dried after being cleaned by ultrasonic with ethanol solution, acetone soln and deionized water to substrate 1；
Step 2：Dried substrate 1 is pre-processed with UV；
Step 3：Pretreated substrate is passed to the preparation of vacuum chamber progress anode layer；
Step 4：The incoming vacuum evaporation room of substrate 1 that will be prepared for anode layer 2, and it is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment；
Step 5：Diode component after vapor deposition treatment is packaged in glove box, the glove box is inert gas
Atmosphere；
Step 6：The current-voltage-brightness characteristic curve of device is tested, and the luminescent spectrum of test diode device is special
Property.
Device opens bright voltage as 4.3V, maximum brightness 652cd/m2。
Embodiment 2
Diode device structure sequentially consists of：
TO/TAPC(40nm)/CH3NH3PbBr3(50nm)/TPBi(40nm)/Ag(100nm)
Preparation method step is as follows：
Step 1：It is dried after being cleaned by ultrasonic with ethanol solution, acetone soln and deionized water to substrate 1；
Step 2：Dried substrate 1 is pre-processed with UV；
Step 3：Pretreated substrate 1 is passed to the preparation of vacuum chamber progress anode layer 2；
Step 4：The incoming vacuum evaporation room of substrate 1 that will be prepared for anode layer 2, and it is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment, wherein, in the process of vapor deposition luminescent layer 4
In, cooling processing is carried out to substrate using refrigeration backboard, the temperature control for the backboard that freezes makes to be restored to after -5 DEG C, vapor deposition
Room temperature closes backboard refrigeration system, continues that electron transfer layer is deposited；
Step 5：Diode component after vapor deposition treatment is packaged in glove box, the glove box is inert gas
Atmosphere；
Step 6：The current-voltage-brightness characteristic curve of device is tested, and tests the luminosity spectral characteristic of device.
Device opens bright voltage as 3.5V, maximum brightness 5634cd/m2, the electroluminescent hair of the perovskite light emitting diode of preparation
Light spectrum is as shown in Figure 2.
Embodiment 3
Diode device structure sequentially consists of：
ITO/TAPC(30nm)/CH3NH3PbBr3(200nm)/TPBi(40nm)/Ag(100nm)
Preparation method step is as follows：
Step 1：It is dried after being cleaned by ultrasonic with ethanol solution, acetone soln and deionized water to substrate 1；
Step 2：Substrate after dry 1 is pre-processed with UV；
Step 3：Pretreated substrate is passed to the preparation of vacuum chamber progress anode layer 2；
Step 4：The substrate for being prepared for anode layer 2 is passed to and is evaporated in vacuo room, and is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment, wherein, in the process of vapor deposition luminescent layer 4
In, cooling processing is carried out to substrate using refrigeration backboard, the temperature for the backboard that freezes is controlled after -10 DEG C, vapor deposition after continuation of insurance
It holds the temperature 10 minutes, closes backboard refrigeration system, continue that electron transfer layer is deposited；
Step 5：Diode component after vapor deposition treatment is packaged in glove box, the glove box is inert gas
Atmosphere；
Step 6：The current-voltage-brightness characteristic curve of device is tested, and tests the luminosity spectral characteristic of device.
Device opens bright voltage as 3.1V, maximum brightness 3873cd/m2。
Embodiment 4
Diode device structure sequentially consists of：
ITO/TAPC(40nm)/CH3NH3PbBr3(70nm)/TPBi(40nm)/Ag(100nm)
Preparation method step is as follows：
Step 1：It is dried after being cleaned by ultrasonic with ethanol solution, acetone soln and deionized water to substrate 1；
Step 2：Dried substrate 1 is pre-processed with UV；
Step 3：Pretreated substrate 1 is passed to the preparation of vacuum chamber progress anode layer 2；
Step 4：The substrate for being prepared for anode layer 2 is passed to and is evaporated in vacuo room, and is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment.Wherein, in the process of vapor deposition luminescent layer 4
In, cooling processing is carried out to substrate using refrigeration backboard, the temperature for the backboard that freezes is controlled at 0 DEG C, makes to be restored to after vapor deposition
Room temperature closes backboard refrigeration system, continues that electron transfer layer is deposited；
Step 5：Diode component after vapor deposition treatment is packaged in glove box, the glove box is inert gas
Atmosphere；
Step 6：The current-voltage-brightness characteristic curve of device is tested, and tests the luminosity spectral characteristic of device.
Device opens bright voltage as 2.7V, maximum brightness 25427cd/m2。
Embodiment 5
Diode device structure sequentially consists of：
ITO/TAPC(40nm)/CH3NH3PbBr3(100nm)/TPBi(40nm)/Ag(100nm)
Preparation method step is as follows：
Step 1：It is dried after being cleaned by ultrasonic with ethanol solution, acetone soln and deionized water to substrate 1；
Step 2：Dried substrate 1 is pre-processed with UV；
Step 3：Pretreated substrate 1 is passed to the preparation of vacuum chamber progress anode layer 2；
Step 4：The incoming vacuum evaporation room of substrate 1 that will be prepared for anode layer 2, and it is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment.Wherein, in the process of vapor deposition luminescent layer 4
In, cooling processing is carried out to substrate using refrigeration backboard, the temperature for the backboard that freezes is controlled at 5 DEG C, makes to be restored to after vapor deposition
Room temperature closes backboard refrigeration system, continues that electron transfer layer is deposited；
Step 5：Diode component after vapor deposition treatment is packaged in glove box, the glove box is inert gas
Atmosphere；
Step 6：The current-voltage-brightness characteristic curve of device is tested, and tests the luminosity spectral characteristic of device.
Device opens bright voltage as 3.5V, maximum brightness 6276cd/m2。
Embodiment 6
Diode device structure sequentially consists of：
ITO/TAPC(40nm)/CH3NH3PbBr3(100nm)/TPBi(40nm)/Ag(100nm)
Preparation method step is as follows：
Step 1：It is dried after being cleaned by ultrasonic with ethanol solution, acetone soln and deionized water to substrate 1；
Step 2：Dried substrate 1 is pre-processed with UV；
Step 3：Pretreated substrate 1 is passed to the preparation of vacuum chamber progress anode layer 2；
Step 4：The incoming vacuum evaporation room of substrate 1 that will be prepared for anode layer 2, and it is right successively according to diode device structure
Hole transmission layer 3, luminescent layer 4, electron transfer layer 5 and cathode layer 6 carry out vapor deposition treatment.Wherein, in the process of vapor deposition luminescent layer 4
In, cooling processing is carried out to substrate using refrigeration backboard, the temperature control for the backboard that freezes makes recovery after -10 DEG C, vapor deposition
To room temperature, backboard refrigeration system is closed, continues that electron transfer layer is deposited；
Step 5：Diode component after vapor deposition treatment is packaged in glove box, the glove box is inert gas
Atmosphere；
Step 6：The current-voltage-brightness characteristic curve of device is tested, and tests the luminosity spectral characteristic of device.
Device opens bright voltage as 3.1V, maximum brightness 4576cd/m2。
The present invention is mixed using double source by changing the preparation process of luminescent layer 4 and steams perovskite precursor material CH3NH3Br3With
PbBr2Perovskite thin film is formed on substrate, substrate contact refrigeration backboard keeps substrate in low temperature shape during vapor deposition
State.The perovskite thin film roughness prepared using this technique is low, and good crystallinity, crystal grain is small, applies in perovskite light emitting diode
In can improve brightness and the quantum efficiency of light emitting diode.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of light emitting diode based on calcium nutrition film, it is characterised in that：The light emitting diode sequentially consists of
Substrate (1), anode layer (2), hole transmission layer (3), luminescent layer (4), electron transfer layer (5) and cathode layer (6).
2. a kind of perovskite light emitting diode according to claim 1, it is characterised in that：The luminescent layer (4) is using organic
It is made with inorganic hybridization ABX3 type cubic crystal structure perovskite luminescent materials.
3. a kind of light emitting diode based on calcium nutrition film according to claim 1, it is characterised in that：The anode layer
(2) thickness be 10~200nm, hole transmission layer (3) thickness be 20~80nm, luminescent layer (4) thickness be 20~80nm, electronics
Transport layer (5) thickness is 20~80nm, and cathode layer (6) thickness is 100~200nm.
4. a kind of light-emitting diodes tube preparation method based on calcium nutrition film, which is characterized in that include the following steps：
Step 1：It is dried after being cleaned to substrate (1)；
Step 2：Dried substrate is pre-processed with UV；
Step 3：Pretreated substrate is passed to the preparation of vacuum chamber progress anode layer (2)；
Step 4：The incoming vacuum evaporation room of substrate (1) of anode layer (2) will be prepared for, and right successively according to diode device structure
Hole transmission layer (3), luminescent layer (4), electron transfer layer (5) and cathode layer (6) carry out vapor deposition treatment；
Step 5：Diode component after vapor deposition treatment is packaged.
5. a kind of light-emitting diodes tube preparation method based on calcium nutrition film according to claim 4, it is characterised in that：It is described
Step 1 is successively cleaned by ultrasonic substrate (1) using ethanol solution, acetone soln and deionized water.
6. a kind of light-emitting diodes tube preparation method based on calcium nutrition film according to claim 4, it is characterised in that：It is described
Step 4 carries out cooling processing during vapor deposition luminescent layer (4), using refrigeration backboard to substrate.
7. a kind of light-emitting diodes tube preparation method based on calcium nutrition film according to claim 4, it is characterised in that：It is described
The temperature of refrigeration backboard is controlled at -10 DEG C~5 DEG C.
8. a kind of light-emitting diodes tube preparation method based on calcium nutrition film according to claim 4, it is characterised in that：It is described
The packaging environment of diode component is in the glove box of atmosphere of inert gases in step 5.
9. a kind of light-emitting diodes tube preparation method based on calcium nutrition film according to claim 4, it is characterised in that：It is described
The precursor material that step 4 luminescent layer (4) vapor deposition uses is CH3NH3Br3And PbBr2。
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| CN110350096A (en) * | 2019-06-27 | 2019-10-18 | 深圳市华星光电半导体显示技术有限公司 | A kind of Ca-Ti ore type electroluminescent device and preparation method thereof |
| CN111244279A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Reel-to-reel vacuum deposition system and preparation method for flexible perovskite solar cell |
| CN111916572A (en) * | 2020-06-24 | 2020-11-10 | 华南理工大学 | Perovskite light-emitting diode with mixed cations and mixed anions and preparation method thereof |
| CN112002815A (en) * | 2020-07-30 | 2020-11-27 | 隆基绿能科技股份有限公司 | Production method of perovskite thin film and preparation method of perovskite solar cell |
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