CN107104158B - A kind of preparation method for adulterating CdTe nano photovoltaic material - Google Patents
A kind of preparation method for adulterating CdTe nano photovoltaic material Download PDFInfo
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- CN107104158B CN107104158B CN201710452467.3A CN201710452467A CN107104158B CN 107104158 B CN107104158 B CN 107104158B CN 201710452467 A CN201710452467 A CN 201710452467A CN 107104158 B CN107104158 B CN 107104158B
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- 239000000463 material Substances 0.000 title claims abstract description 48
- 229910004613 CdTe Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 92
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 49
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000005273 aeration Methods 0.000 claims abstract description 45
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000137 annealing Methods 0.000 claims abstract description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000000460 chlorine Substances 0.000 claims description 22
- 229910052801 chlorine Inorganic materials 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 22
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 21
- 238000013019 agitation Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims description 7
- 125000004122 cyclic group Chemical group 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000002459 sustained effect Effects 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 11
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 abstract description 8
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 4
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 description 12
- 230000009466 transformation Effects 0.000 description 10
- 230000031700 light absorption Effects 0.000 description 8
- 238000007650 screen-printing Methods 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 5
- 230000005693 optoelectronics Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 239000011267 electrode slurry Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- -1 tellurium ion Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
- H01L31/02963—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe characterised by the doping material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1828—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/543—Solar cells from Group II-VI materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention discloses a kind of preparation method for adulterating CdTe nano photovoltaic material, suspended alcohol liquid is prepared using tellurium powder as raw material, and is mixed with the dropwise addition of the aqueous solution of caddy, and suspended aqueous solution is formed after vacuum distillation；Then ammonia aeration reaction is carried out to suspended aqueous solution, cadmium telluride precipitating is obtained under the conditions of constant pressure back flow reaction, finally cadmium telluride is dispersed in caddy methanol solution, be sprayed on substrate after carrying out annealing reaction and obtain doping CdTe nano photovoltaic material.Doping CdTe nano photovoltaic material prepared by the present invention is stable by the way of solute doping to be doped into chloride ion and cadmium ion in film, adulterates uniform in effect, performance is stablized.
Description
Technical field
The invention belongs to photovoltaic material technical fields, and in particular to a kind of preparation side for adulterating CdTe nano photovoltaic material
Method.
Background technique
Photovoltaic material is also known as solar cell material, refers to the material that solar energy can be directly changed into electric energy.Only partly lead
Body material has this function.Can do solar cell material material have monocrystalline silicon, polysilicon, amorphous silicon, GaAs, GaAlAs,
InP, CdS, CdTe etc..There are monocrystalline silicon, GaAs, InP for space.There are monocrystalline silicon, polycrystalline for what ground had been produced in batches
Silicon, amorphous silicon.Other are still in the development phase.It is dedicated to reducing material cost at present and improves transfer efficiency, makes solar cell
Power price and thermal power generation power price compete, thus for more extensively more large-scale application create conditions.However, such
There is still a need for improve incident photon-to-electron conversion efficiency for material, wherein doping is the emphasis direction studied at present.
Summary of the invention
The object of the present invention is to provide a kind of preparation method for adulterating CdTe nano photovoltaic material, doping prepared by the present invention
CdTe nano photovoltaic material is stable by the way of solute doping to be doped into chloride ion and cadmium ion in film, adulterates effect
Uniformly, performance is stablized.
Technical purpose of the invention has the technical scheme that a kind of doping CdTe nano photovoltaic material
Preparation method, its step are as follows:
Step 1, tellurium powder is put into dehydrated alcohol, polyvinylpyrrolidone is added, ultrasonic agitation forms finely dispersed
Suspended alcohol liquid；
Step 2, caddy is added to the water, suspended alcohol liquid is slowly added dropwise after stirring and dissolving, until stirring evenly completely, subtracted
Pressure distillation excludes completely to ethyl alcohol, obtains suspended aqueous solution；
Step 3, suspended aqueous solution is put into reaction kettle, then passes to ammonia and carries out cyclic aeration reaction 2-5h, it is natural
It is cooling, obtain coordination suspension；
Step 4, coordination suspension is subjected to chlorine aeration reaction 3-5h, then constant pressure back flow reaction 5-8h, cold filtration
After obtain sediment；
Step 5, sediment is put into caddy methanol solution, is sprayed to substrate surface after mixing evenly, is then moved back
Fire processing 3h, obtains doping CdTe nano photovoltaic material after cooling.
Tellurium powder concentration in the step 1 is 20-30mg/L, and the additional amount of the polyvinylpyrrolidone is tellurium powder mole
The 5-8% of amount, the frequency of the ultrasonic agitation are 5-10kHz, and the ultrasonic agitation time is 10-30min；The step is by tellurium powder
It is dissolved in dehydrated alcohol, and is aided with polyvinylpyrrolidone as dispersing agent, tellurium powder is evenly distributed in solution, formed steady
Fixed suspended alcohol liquid.
Caddy additional amount in the step 2 is 1.1-1.2 times of tellurium powder mole, and the additional amount of the water is anhydrous
The 0.3-0.5 of ethyl alcohol, the speed being slowly added dropwise is 4-8mL/min；The step is by the way of being slowly added dropwise by tellurium powder alcohol
Liquid is added into dehydrated alcohol, using the intersolubility of ethyl alcohol and water, guarantees that the tellurium powder of polyvinylpyrrolidone package is dispersed to water
In, form stable water phase suspension solution.
The temperature of vacuum distillation in the step 2 is 80-90 DEG C, and the pressure of the vacuum distillation is the 50- of atmospheric pressure
60%, the vacuum distillation time is 2-3h, and the volume of the vacuum distillation is the 40-50% of original volume, which is depressurizing
Under conditions of distillation, by dehydrated alcohol evaporating completely, it is converted into aqueous solution, while ensure that the dispersion effect of tellurium powder.
Ammonia additional amount in the step 3 is 1.5-1.7 times of tellurium powder mole, and the aeration flow velocity is 10-15mL/
Min, the aeration reaction temperature are 60-70 DEG C；Cadmium ion and ammonium ion are formed complexation reaction by the step, play fixed cadmium from
The effect of son.
The intake of chlorine in the step 4 is 1.8-2.2 times of tellurium powder, and the temperature of the chlorine aeration reaction is
60-100 DEG C, the aeration flow velocity is 5-8mL/min, and the pressure of the constant pressure back flow reaction is atmospheric pressure, and the temperature is
100-110 DEG C, the reflux, which is adopted, to be water-cooled；The step reacts tellurium powder in such a way that chlorine cyclic aeration reacts, and is formed
Stable ionic condition, and react to form cadmium telluride in the cadmium ion of coordination, and form precipitating in water, using perseverance in the step
The mode for pushing back stream can remove the volatile impurity such as hydrogen chloride, obtain relatively stable cadmium telluride, and in polyvinyl pyrrole
The effect of alkanone forms good dispersion effect；Using more chlorine as reducing agent in the step, and using aeration as instead
Mode is answered, the reaction speed and reaction depth of tellurium powder are substantially increased, it is ensured that the complete reaction of tellurium powder.
The chlorine aeration reaction is reacted using gradient, i.e. 60-65 DEG C of sustained response 0.5-1h, 80-90 DEG C of reaction 0.5h,
100 DEG C of reactions can be carried out tellurium powder reaction process by the way of gradient reaction detailed-oriented to terminating, and pass through 60-65 DEG C of item
Tellurium powder is converted tellurium ion by aeration reaction under part, and under the conditions of 80-90 DEG C, aeration reaction promotes the mixing effect of internal solution
Fruit, the reaction for substantially increasing cadmium telluride generate, and form aeration dispersion to cadmium telluride product under the conditions of last 100 DEG C, play
Good dispersion effect, while the dispersion effect of polyvinylpyrrolidone being promoted effectively to act on to particle surface.
The concentration of caddy methanol solution is 10-15mg/L in the step 5, and the mixing speed is 1500-2000r/
Min, the step are formed using caddy formalin as doped solution and are effectively dispersed to precipitation surface, formed relatively stable
Suspended state.
Fountain height in the step 5 is 2-4mg/cm2, the annealing temperature is 400-450 DEG C, and the annealing reaction is adopted
With nitrogen protection annealing reaction, the annealing reaction uses Gradient annealing method, i.e., reacts 1-2h under the conditions of 200-250 DEG C, so
Continue to react at 350 DEG C afterwards, until reaction reacts 0.5h under the conditions of 400-450 DEG C before terminating.The step is to spray as painting
The mode of covering can effectively in solution metal ion and Doped ions stay in substrate surface, under the conditions of Gradient annealing, first
By the impurity complete oxidation such as polyvinylpyrrolidone, then under high annealing under a nitrogen atmosphere, by chloride ion and cadmium ion
It is doped into cadmium telluride, forms stable doping effect, effectively raise its incident photon-to-electron conversion efficiency.
The present invention prepares suspended alcohol liquid using tellurium powder as raw material, and mixes with the dropwise addition of the aqueous solution of caddy, is evaporated under reduced pressure
After form suspended aqueous solution；Then ammonia aeration reaction is carried out to suspended aqueous solution, obtains tellurium under the conditions of constant pressure back flow reaction
Cadmium telluride, is finally dispersed in caddy methanol solution by cadmium precipitating, is sprayed at after carrying out annealing reaction on substrate and is adulterated
CdTe nano photovoltaic material.
In conclusion the invention has the following beneficial effects:
Preparation method simple possible of the present invention, practicality and versatile.Doping CdTe nano photovoltaic prepared by the present invention
Material is stable by the way of solute doping to be doped into chloride ion and cadmium ion in film, adulterates uniform in effect, performance is steady
It is fixed.Photovoltaic material prepared by the present invention effectively raises photoelectricity conduction efficiency, effectively raises internal conduction velocity.This
It is simple and quick to invent the preparation method provided, while its optoelectronic transformation efficiency can reach commercialization standard.
Specific embodiment
Embodiment 1
A kind of preparation method for adulterating CdTe nano photovoltaic material, its step are as follows:
Step 1, tellurium powder is put into dehydrated alcohol, polyvinylpyrrolidone is added, ultrasonic agitation forms finely dispersed
Suspended alcohol liquid；
Step 2, caddy is added to the water, suspended alcohol liquid is slowly added dropwise after stirring and dissolving, until stirring evenly completely, subtracted
Pressure distillation excludes completely to ethyl alcohol, obtains suspended aqueous solution；
Step 3, suspended aqueous solution is put into reaction kettle, then passes to ammonia and carries out cyclic aeration reaction 2h, it is naturally cold
But, coordination suspension is obtained；
Step 4, coordination suspension is subjected to chlorine aeration reaction 3h, then constant pressure back flow reaction 5h, after cold filtration
To sediment；
Step 5, sediment is put into caddy methanol solution, is sprayed to substrate surface after mixing evenly, is then moved back
Fire processing 3h, obtains doping CdTe nano photovoltaic material after cooling.
Tellurium powder concentration in the step 1 is 20mg/L, and the additional amount of the polyvinylpyrrolidone is tellurium powder mole
5%, the frequency of the ultrasonic agitation is 5kHz, and the ultrasonic agitation time is 10min.
Caddy additional amount in the step 2 is 1.1 times of tellurium powder mole, and the additional amount of the water is dehydrated alcohol
0.3, the speed being slowly added dropwise is 4mL/min.
The temperature of vacuum distillation in the step 2 is 80 DEG C, and the pressure of the vacuum distillation is the 50% of atmospheric pressure, institute
Stating the vacuum distillation time is 2h, and the volume of the vacuum distillation is the 40% of original volume.
Ammonia additional amount in the step 3 is 1.5 times of tellurium powder mole, and the aeration flow velocity is 10mL/min, described
Aeration reaction temperature is 60 DEG C.
The intake of chlorine in the step 4 is 1.8 times of tellurium powder, and the temperature of the chlorine aeration reaction is 60 DEG C,
The aeration flow velocity is 5mL/min, and the pressure of the constant pressure back flow reaction is atmospheric pressure, and the temperature is 100 DEG C, the reflux
It adopts and is water-cooled.
The concentration of caddy methanol solution is 10mg/L in the step 5, and the mixing speed is 1500r/min.
Fountain height in the step 5 is 2mg/cm2, the annealing temperature is 400 DEG C, and the annealing reaction uses nitrogen
Annealing reaction is protected, the annealing reaction uses Gradient annealing method, i.e., reacts 1h under the conditions of 200 DEG C, then continues at 350 DEG C
Reaction, until reaction reacts 0.5h under the conditions of 400 DEG C before terminating.
One block of FTO glass is selected, is cleaned up and is further dried, uses screen printing on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass after heating 25min at 500 DEG C, the densification
The photovoltaic material being made by embodiment 1 dissolution is spun on compacted zone thereafter by layer with a thickness of 50nm, and heats 10 at 80 DEG C
The coating that minute makes the photovoltaic material form 30nm is affixed on compacted zone and forms light-absorption layer, then will pass through screen printing to electrode slurry
Brush method is printed on the light-absorption layer, and levelling is placed in 80 DEG C of baking ovens dry 10min and obtains solar battery,
Battery performance test is carried out, is used in experimentation in 100mW/cm2Solar simulator (Newport) AM1.5G
It is carried out under illumination, measuring optoelectronic transformation efficiency is 20.11%.It is kept for 20 days in 20 degrees Celsius of temperature, the environment that humidity is 45%
Afterwards, testing its transformation efficiency is 18.8%.
Embodiment 2
A kind of preparation method for adulterating CdTe nano photovoltaic material, its step are as follows:
Step 1, tellurium powder is put into dehydrated alcohol, polyvinylpyrrolidone is added, ultrasonic agitation forms finely dispersed
Suspended alcohol liquid；
Step 2, caddy is added to the water, suspended alcohol liquid is slowly added dropwise after stirring and dissolving, until stirring evenly completely, subtracted
Pressure distillation excludes completely to ethyl alcohol, obtains suspended aqueous solution；
Step 3, suspended aqueous solution is put into reaction kettle, then passes to ammonia and carries out cyclic aeration reaction 5h, it is naturally cold
But, coordination suspension is obtained；
Step 4, coordination suspension is subjected to chlorine aeration reaction 5h, then constant pressure back flow reaction 8h, after cold filtration
To sediment；
Step 5, sediment is put into caddy methanol solution, is sprayed to substrate surface after mixing evenly, is then moved back
Fire processing 3h, obtains doping CdTe nano photovoltaic material after cooling.
Tellurium powder concentration in the step 1 is 30mg/L, and the additional amount of the polyvinylpyrrolidone is tellurium powder mole
8%, the frequency of the ultrasonic agitation is 10kHz, and the ultrasonic agitation time is 30min.
Caddy additional amount in the step 2 is 1.2 times of tellurium powder mole, and the additional amount of the water is dehydrated alcohol
0.5, the speed being slowly added dropwise is 8mL/min.
The temperature of vacuum distillation in the step 2 is 90 DEG C, and the pressure of the vacuum distillation is the 60% of atmospheric pressure, institute
Stating the vacuum distillation time is 3h, and the volume of the vacuum distillation is the 50% of original volume.
Ammonia additional amount in the step 3 is 1.7 times of tellurium powder mole, and the aeration flow velocity is 15mL/min, described
Aeration reaction temperature is 70 DEG C.
The intake of chlorine in the step 4 is 2.2 times of tellurium powder, and the temperature of the chlorine aeration reaction is 100 DEG C,
The aeration flow velocity is 8mL/min, and the pressure of the constant pressure back flow reaction is atmospheric pressure, and the temperature is 110 DEG C, the reflux
It adopts and is water-cooled.
The concentration of caddy methanol solution is 15mg/L in the step 5, and the mixing speed is 2000r/min.
Fountain height in the step 5 is 4mg/cm2, the annealing temperature is 450 DEG C, and the annealing reaction uses nitrogen
Annealing reaction is protected, the annealing reaction uses Gradient annealing method, i.e., reacts 2h under the conditions of 250 DEG C, then continues at 350 DEG C
Reaction, until reaction reacts 0.5h under the conditions of 450 DEG C before terminating.
One block of FTO glass is selected, is cleaned up and is further dried, uses screen printing on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass after heating 25min at 500 DEG C, the densification
The photovoltaic material as made from embodiment 2 is spun on compacted zone thereafter, and heat 10 minutes at 80 DEG C by layer with a thickness of 50nm
It is affixed on the coating of photovoltaic material formation 30nm on compacted zone and forms light-absorption layer, then silk screen print method will be passed through to electrode slurry
It being printed on the light-absorption layer, levelling is placed in 80 DEG C of baking ovens dry 10min and obtains solar battery,
Battery performance test is carried out, is used in experimentation in 100mW/cm2Solar simulator (Newport) AM1.5G
It is carried out under illumination, measuring optoelectronic transformation efficiency is 19.72%.It is kept for 20 days in 20 degrees Celsius of temperature, the environment that humidity is 45%
Afterwards, testing its transformation efficiency is 17.32%.
Embodiment 3
A kind of preparation method for adulterating CdTe nano photovoltaic material, its step are as follows:
Step 1, tellurium powder is put into dehydrated alcohol, polyvinylpyrrolidone is added, ultrasonic agitation forms finely dispersed
Suspended alcohol liquid；
Step 2, caddy is added to the water, suspended alcohol liquid is slowly added dropwise after stirring and dissolving, until stirring evenly completely, subtracted
Pressure distillation excludes completely to ethyl alcohol, obtains suspended aqueous solution；
Step 3, suspended aqueous solution is put into reaction kettle, then passes to ammonia and carries out cyclic aeration reaction 3h, it is naturally cold
But, coordination suspension is obtained；
Step 4, coordination suspension is subjected to chlorine aeration reaction 4h, then constant pressure back flow reaction 6h, after cold filtration
To sediment；
Step 5, sediment is put into caddy methanol solution, is sprayed to substrate surface after mixing evenly, is then moved back
Fire processing 3h, obtains doping CdTe nano photovoltaic material after cooling.
Tellurium powder concentration in the step 1 is 25mg/L, and the additional amount of the polyvinylpyrrolidone is tellurium powder mole
6%, the frequency of the ultrasonic agitation is 7kHz, and the ultrasonic agitation time is 20min.
Caddy additional amount in the step 2 is 1.1 times of tellurium powder mole, and the additional amount of the water is dehydrated alcohol
0.4, the speed being slowly added dropwise is 6mL/min.
The temperature of vacuum distillation in the step 2 is 85 DEG C, and the pressure of the vacuum distillation is the 55% of atmospheric pressure, institute
Stating the vacuum distillation time is 2h, and the volume of the vacuum distillation is the 45% of original volume.
Ammonia additional amount in the step 3 is 1.6 times of tellurium powder mole, and the aeration flow velocity is 12mL/min, described
Aeration reaction temperature is 65 DEG C.
The intake of chlorine in the step 4 is 2.0 times of tellurium powder, and the temperature of the chlorine aeration reaction is 80 DEG C,
The aeration flow velocity is 6mL/min, and the pressure of the constant pressure back flow reaction is atmospheric pressure, and the temperature is 105 DEG C, the reflux
It adopts and is water-cooled.
The concentration of caddy methanol solution is 13mg/L in the step 5, and the mixing speed is 1800r/min.
Fountain height in the step 5 is 3mg/cm2, the annealing temperature is 430 DEG C, and the annealing reaction uses nitrogen
Annealing reaction is protected, the annealing reaction uses Gradient annealing method, i.e., reacts 2h under the conditions of 230 DEG C, then continues at 350 DEG C
Reaction, until reaction reacts 0.5h under the conditions of 430 DEG C before terminating.
One block of FTO glass is selected, is cleaned up and is further dried, uses screen printing on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass after heating 25min at 500 DEG C, the densification
The dissolution of the photovoltaic material as made from embodiment 3 is spun on compacted zone thereafter by layer with a thickness of 50nm, and heats 10 at 80 DEG C
The coating that minute makes the photovoltaic material form 30nm is affixed on compacted zone and forms light-absorption layer, then will pass through screen printing to electrode slurry
Brush method is printed on the light-absorption layer, and levelling is placed in 80 DEG C of baking ovens dry 10min and obtains solar battery,
Battery performance test is carried out, is used in experimentation in 100mW/cm2Solar simulator (Newport) AM1.5G
It is carried out under illumination, measuring optoelectronic transformation efficiency is 20.41%.It is kept for 20 days in 20 degrees Celsius of temperature, the environment that humidity is 45%
Afterwards, testing its transformation efficiency is 19.12%.
Embodiment 4
A kind of preparation method for adulterating CdTe nano photovoltaic material, its step are as follows:
Step 1, tellurium powder is put into dehydrated alcohol, polyvinylpyrrolidone is added, ultrasonic agitation forms finely dispersed
Suspended alcohol liquid；
Step 2, caddy is added to the water, suspended alcohol liquid is slowly added dropwise after stirring and dissolving, until stirring evenly completely, subtracted
Pressure distillation excludes completely to ethyl alcohol, obtains suspended aqueous solution；
Step 3, suspended aqueous solution is put into reaction kettle, then passes to ammonia and carries out cyclic aeration reaction 4h, it is naturally cold
But, coordination suspension is obtained；
Step 4, coordination suspension is subjected to chlorine aeration reaction 4h, then constant pressure back flow reaction 7h, after cold filtration
To sediment；
Step 5, sediment is put into caddy methanol solution, is sprayed to substrate surface after mixing evenly, is then moved back
Fire processing 3h, obtains doping CdTe nano photovoltaic material after cooling.
Tellurium powder concentration in the step 1 is 28mg/L, and the additional amount of the polyvinylpyrrolidone is tellurium powder mole
7%, the frequency of the ultrasonic agitation is 8kHz, and the ultrasonic agitation time is 25min.
Caddy additional amount in the step 2 is 1.2 times of tellurium powder mole, and the additional amount of the water is dehydrated alcohol
0.4, the speed being slowly added dropwise is 7mL/min.
The temperature of vacuum distillation in the step 2 is 86 DEG C, and the pressure of the vacuum distillation is the 57% of atmospheric pressure, institute
Stating the vacuum distillation time is 3h, and the volume of the vacuum distillation is the 45% of original volume.
Ammonia additional amount in the step 3 is 1.6 times of tellurium powder mole, and the aeration flow velocity is 14mL/min, described
Aeration reaction temperature is 65 DEG C.
The intake of chlorine in the step 4 is 2.1 times of tellurium powder, and the aeration flow velocity is 7mL/min, the constant pressure
The pressure of back flow reaction is atmospheric pressure, and the temperature is 108 DEG C, and the reflux, which is adopted, to be water-cooled.
The chlorine aeration reaction is reacted using gradient, i.e. 63 DEG C of sustained response 0.7h, and 85 DEG C of reaction 0.5h, 100 DEG C anti-
It should be to terminating.
The concentration of caddy methanol solution is 14mg/L in the step 5, and the mixing speed is 1700r/min.
Fountain height in the step 5 is 3mg/cm2, the annealing temperature is 440 DEG C, and the annealing reaction uses nitrogen
Annealing reaction is protected, the annealing reaction uses Gradient annealing method, i.e., reacts 2h under the conditions of 220 DEG C, then continues at 350 DEG C
Reaction, until reaction reacts 0.5h under the conditions of 440 DEG C before terminating.
One block of FTO glass is selected, is cleaned up and is further dried, uses screen printing on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass after heating 25min at 500 DEG C, the densification
The dissolution of the photovoltaic material as made from embodiment 4 is spun on compacted zone thereafter by layer with a thickness of 50nm, and heats 10 at 80 DEG C
The coating that minute makes the photovoltaic material form 30nm is affixed on compacted zone and forms light-absorption layer, then will pass through screen printing to electrode slurry
Brush method is printed on the light-absorption layer, and levelling is placed in 80 DEG C of baking ovens dry 10min and obtains solar battery,
Battery performance test is carried out, is used in experimentation in 100mW/cm2Solar simulator (Newport) AM1.5G
It is carried out under illumination, measuring optoelectronic transformation efficiency is 22.37%.It is kept for 20 days in 20 degrees Celsius of temperature, the environment that humidity is 45%
Afterwards, testing its transformation efficiency is 20.07%.
The foregoing is merely one embodiment of the invention, are not intended to limit the present invention, all to use equivalent substitution or equivalent transformation
Mode technical solution obtained, fall within the scope of protection of the present invention.
Claims (9)
1. a kind of preparation method for adulterating CdTe nano photovoltaic material, it is characterised in that: its step are as follows:
Step 1, tellurium powder is put into dehydrated alcohol, polyvinylpyrrolidone is added, ultrasonic agitation forms finely dispersed suspended
Alcohol liquid；
Step 2, caddy is added to the water, suspended alcohol liquid is slowly added dropwise after stirring and dissolving, until stirring evenly completely, decompression is steamed
It evaporates to ethyl alcohol and excludes completely, obtain suspended aqueous solution；
Step 3, suspended aqueous solution is put into reaction kettle, then pass to ammonia carry out cyclic aeration reaction 2-5h, natural cooling,
Obtain coordination suspension；
Step 4, coordination suspension is subjected to chlorine aeration reaction 3-5h, then constant pressure back flow reaction 5-8h, after cold filtration
To sediment；
Step 5, sediment is put into caddy methanol solution, is sprayed to substrate surface after mixing evenly, then carried out at annealing
3h is managed, doping CdTe nano photovoltaic material is obtained after cooling.
2. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
Tellurium powder concentration in step 1 is 20-30mg/L, and the additional amount of the polyvinylpyrrolidone is the 5-8% of tellurium powder mole, institute
The frequency for stating ultrasonic agitation is 5-10kHz, and the ultrasonic agitation time is 10-30min.
3. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
Caddy additional amount in step 2 is 1.1-1.2 times of tellurium powder mole, and the additional amount of the water is the 0.3- of dehydrated alcohol
0.5, the speed being slowly added dropwise is 4-8mL/min.
4. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
The temperature of vacuum distillation in step 2 is 80-90 DEG C, and the pressure of the vacuum distillation is the 50-60% of atmospheric pressure, the decompression
Distillation time is 2-3h, and the volume of the vacuum distillation is the 40-50% of original volume.
5. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
Ammonia additional amount in step 3 is 1.5-1.7 times of tellurium powder mole, and the aeration flow velocity is 10-15mL/min, and the aeration is anti-
Answering temperature is 60-70 DEG C.
6. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
The intake of chlorine in step 4 is 1.8-2.2 times of tellurium powder, and the temperature of the chlorine aeration reaction is 60-100 DEG C, described
Aeration flow velocity is 5-8mL/min, and the pressure of the constant pressure back flow reaction is atmospheric pressure, and the temperature is 100-110 DEG C, described time
Stream, which is adopted, to be water-cooled.
7. a kind of preparation method of doping CdTe nano photovoltaic material according to claim 6, it is characterised in that: described
Chlorine aeration reaction is reacted using gradient, i.e. 60-65 DEG C of sustained response 0.5-1h, and 80-90 DEG C of reaction 0.5h, 100 DEG C of reactions are extremely
Terminate.
8. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
The concentration of caddy methanol solution is 10-15mg/L in step 5, and the mixing speed is 1500-2000r/min.
9. the preparation method of a kind of doping CdTe nano photovoltaic material according to claim 1, it is characterised in that: described
Fountain height in step 5 is 2-4mg/cm2, the annealing temperature is 400-450 DEG C, and the annealing reaction is moved back using nitrogen protection
Fire reaction, the annealing reaction use Gradient annealing method, i.e., react 1-2h under the conditions of 200-250 DEG C, then continue at 350 DEG C
Reaction, until reaction reacts 0.5h under the conditions of 400-450 DEG C before terminating.
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