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CN107104158A - A kind of preparation method of doping CdTe nano photovoltaic materials - Google Patents

A kind of preparation method of doping CdTe nano photovoltaic materials Download PDF

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Publication number
CN107104158A
CN107104158A CN201710452467.3A CN201710452467A CN107104158A CN 107104158 A CN107104158 A CN 107104158A CN 201710452467 A CN201710452467 A CN 201710452467A CN 107104158 A CN107104158 A CN 107104158A
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reaction
preparation
cdte nano
photovoltaic material
tellurium powder
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CN107104158B (en
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李志彬
魏雷杰
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University of Shaoxing
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University of Shaoxing
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10FINORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00Constructional details of devices covered by this subclass
    • H10F77/10Semiconductor bodies
    • H10F77/12Active materials
    • H10F77/123Active materials comprising only Group II-VI materials, e.g. CdS, ZnS or HgCdTe
    • H10F77/1233Active materials comprising only Group II-VI materials, e.g. CdS, ZnS or HgCdTe characterised by the dopants
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10FINORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00Manufacture or treatment of devices covered by this subclass
    • H10F71/125The active layers comprising only Group II-VI materials, e.g. CdS, ZnS or CdTe
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/543Solar cells from Group II-VI materials
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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Abstract

The invention discloses a kind of preparation method of doping CdTe nano photovoltaic materials, suspended alcohol liquid is prepared using tellurium powder as raw material, and is mixed with the aqueous solution dropwise addition of caddy, the suspended aqueous solution is formed after vacuum distillation;Then ammonia is carried out to the suspended aqueous solution and takes reaction and aerated reaction in one's arms, cadmium telluride precipitation is obtained under the conditions of constant pressure back flow reaction, finally cadmium telluride is dispersed in caddy methanol solution, is sprayed on base material and carries out obtaining the CdTe nano photovoltaic materials that adulterate after annealing reaction.Doping CdTe nano photovoltaics material prepared by the present invention is stable by the way of solute doping to be doped into chlorion and cadmium ion in film, and uniform in effect of adulterating, performance is stable.

Description

A kind of preparation method of doping CdTe nano photovoltaic materials
Technical field
The invention belongs to photovoltaic material technical field, and in particular to a kind of preparation side of doping CdTe nano photovoltaic materials Method.
Background technology
Photovoltaic material is also known as solar cell material, refers to solar energy can be directly changed into the material of electric energy.Only partly lead Body material has this function.Can do the material of solar cell material have monocrystalline silicon, polysilicon, non-crystalline 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, non-crystalline silicon.Other are still in the development phase.Reduction material cost is directed at present and conversion efficiency is improved, and makes solar cell Power price and thermal power generation power price compete so that for more extensively more large-scale application create conditions.However, such Material still needs raising electricity conversion, wherein, doping is the emphasis direction studied at present.
The content of the invention
It is an object of the invention to provide doping prepared by a kind of preparation method of doping CdTe nano photovoltaic materials, the present invention CdTe nano photovoltaics material is stable by the way of solute doping to be doped into chlorion and cadmium ion in film, effect of adulterating Uniformly, performance is stable.
The present invention technical purpose technical scheme is that:One kind doping CdTe nano photovoltaic materials Preparation method, its step is as follows:
Step 1, tellurium powder is put into absolute ethyl alcohol, adds polyvinylpyrrolidone, 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 completely, decompression is steamed Evaporate to ethanol and exclude completely, obtain the suspended aqueous solution;
Step 3, the suspended aqueous solution is put into reactor, then pass to ammonia carry out cyclic aeration reaction 2-5h, natural cooling, Obtain being coordinated suspension;
Step 4, coordination suspension is subjected to chlorine aerated 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, substrate surface is sprayed to after stirring, then carried out at annealing 3h is managed, the CdTe nano photovoltaic materials that adulterate are obtained after cooling.
Tellurium powder concentration in the step 1 is 20-30mg/L, and the addition of the polyvinylpyrrolidone is tellurium powder mole The 5-8% of amount, the frequency of the ultrasonic agitation is 5-10kHz, and the ultrasonic agitation time is 10-30min;The step is by tellurium powder It is dissolved in absolute ethyl alcohol, and is aided with polyvinylpyrrolidone as dispersant, tellurium powder is evenly distributed in solution, forms steady Fixed suspended alcohol liquid.
Caddy addition in the step 2 is 1.1-1.2 times of tellurium powder mole, and the addition of the water is anhydrous The 0.3-0.5 of ethanol, 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 absolute ethyl alcohol, utilizes the intersolubility of ethanol and water, it is ensured that the tellurium powder of polyvinylpyrrolidone parcel is dispersed to water In, form stable aqueous 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, and the step is steamed in decompression Under conditions of evaporating, by absolute ethyl alcohol evaporating completely, the aqueous solution is converted into, while ensure that the dispersion effect of tellurium powder.
Ammonia addition in the step 3 is 1.5-1.7 times of tellurium powder mole, and the aeration flow velocity is 10-15mL/ Min, the aerated reaction temperature is 60-70 DEG C;The step by cadmium ion and ammonium ion formation complexation reaction, 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 aerated 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 backflow uses water cooling;The step reacts tellurium powder by way of chlorine cyclic aeration reacts, and is formed Stable ionic condition, and react to form cadmium telluride in the cadmium ion of coordination, and formed in water in precipitation, the step using perseverance The volatile impurity such as hydrogen chloride can be removed by pushing back the mode of stream, 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 to be aerated as anti- Mode is answered, the reaction speed and reaction depth of tellurium powder is substantially increased, it is ensured that the complete reaction of tellurium powder.
The chlorine aerated reaction is reacted using gradient, i.e., 60-65 DEG C sustained response 0.5-1h, 80-90 DEG C of reaction 0.5h, 100 DEG C of reactions can carry out tellurium powder course of reaction by the way of gradient is reacted detailed-oriented to terminating, and pass through 60-65 DEG C of bar Tellurium powder is converted into tellurium ion by the aerated reaction under part, under the conditions of 80-90 DEG C, and aerated reaction promotes the mixing effect of internal solution Really, the reaction for substantially increasing cadmium telluride is produced, scattered to cadmium telluride product formation aeration under the conditions of last 100 DEG C, is played Good dispersion effect, while promoting the dispersion effect of polyvinylpyrrolidone 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 is formed using caddy formalin as doped solution and is effectively dispersed to precipitation surface, is 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 Annealing reaction is protected with nitrogen, the annealing reaction uses Gradient annealing method, i.e., 1-2h reacted under the conditions of 200-250 DEG C, so Continue afterwards in 350 DEG C of reactions, until reaction reacts 0.5h before terminating under the conditions of 400-450 DEG C.The step is used as painting to spray Metal ion and Doped ions in solution effectively can be stayed in substrate surface by the mode of covering, under the conditions of Gradient annealing, first By the impurity complete oxidation such as polyvinylpyrrolidone, then under high annealing under a nitrogen atmosphere, by chlorion and cadmium ion It is doped into cadmium telluride, forms stable doping effect, effectively raise its electricity conversion.
The present invention prepares suspended alcohol liquid using tellurium powder as raw material, and is mixed with the aqueous solution dropwise addition of caddy, vacuum distillation After form the suspended aqueous solution;Then ammonia is carried out to the suspended aqueous solution and takes reaction and aerated reaction in one's arms, in constant pressure back flow reaction bar Cadmium telluride precipitation is obtained under part, finally cadmium telluride is dispersed in caddy methanol solution, is sprayed on base material and carries out annealing reaction After obtain adulterate CdTe nano photovoltaic materials.
In summary, the present invention has the advantages that:
Preparation method simple possible of the present invention, practicality and highly versatile.Doping CdTe nano photovoltaic materials prepared by the present invention Stable by the way of solute doping that chlorion and cadmium ion are doped into film, uniform in effect of adulterating, performance is stable.This Photovoltaic material prepared by invention effectively raises photoelectricity conduction efficiency, effectively raises the conduction velocity of inside.The present invention The preparation method of offer is simple and quick, while its optoelectronic transformation efficiency can reach commercialization standard.
Embodiment
Embodiment 1
A kind of preparation method of doping CdTe nano photovoltaic materials, its step is as follows:
Step 1, tellurium powder is put into absolute ethyl alcohol, adds polyvinylpyrrolidone, 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 completely, decompression is steamed Evaporate to ethanol and exclude completely, obtain the suspended aqueous solution;
Step 3, the suspended aqueous solution is put into reactor, then passes to ammonia and carry out cyclic aeration reaction 2h, natural cooling is obtained To coordination suspension;
Step 4, coordination suspension is subjected to chlorine aerated reaction 3h, then constant pressure back flow reaction 5h, sunk after cold filtration Starch;
Step 5, sediment is put into caddy methanol solution, substrate surface is sprayed to after stirring, then carried out at annealing 3h is managed, the CdTe nano photovoltaic materials that adulterate are obtained after cooling.
Tellurium powder concentration in the step 1 is 20mg/L, and the addition of the polyvinylpyrrolidone is tellurium powder mole 5%, the frequency of the ultrasonic agitation is 5kHz, and the ultrasonic agitation time is 10min.
Caddy addition in the step 2 is 1.1 times of tellurium powder mole, and the addition of the water is absolute ethyl 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 The vacuum distillation time is stated for 2h, the volume of the vacuum distillation is the 40% of original volume.
Ammonia addition in the step 3 is 1.5 times of tellurium powder mole, and the aeration flow velocity is 10mL/min, described Aerated 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 aerated 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 backflow Using water cooling.
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., 1h is reacted under the conditions of 200 DEG C, then continues at 350 DEG C Reaction, until reaction reacts 0.5h before terminating under the conditions of 400 DEG C.
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on its backward FTO glass Brush method prints one layer of TiO2Film layer, in the compacted zone for obtaining being carried on FTO glass after heating 25min at 500 DEG C, the densification Thickness degree is 50nm, photovoltaic material dissolving will be spun on as made from embodiment 1 on compacted zone thereafter, and in heating 10 at 80 DEG C The coating that minute makes the photovoltaic material form 30nm, which is affixed on compacted zone, forms light-absorption layer, then will pass through silk screen to electrode slurry Print process is printed on the light-absorption layer, and dry 10min is placed in 80 DEG C of baking ovens after levelling and obtains solar cell,
Used in battery performance test, experimentation in 100mW/cm2 Solar simulator (Newport) AM1.5G Carried out under illumination, it is 20.11% to measure optoelectronic transformation efficiency.After being kept for 20 days during 20 degrees Celsius of temperature, humidity is 45% environment, It is 18.8% to test its transformation efficiency.
Embodiment 2
A kind of preparation method of doping CdTe nano photovoltaic materials, its step is as follows:
Step 1, tellurium powder is put into absolute ethyl alcohol, adds polyvinylpyrrolidone, 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 completely, decompression is steamed Evaporate to ethanol and exclude completely, obtain the suspended aqueous solution;
Step 3, the suspended aqueous solution is put into reactor, then passes to ammonia and carry out cyclic aeration reaction 5h, natural cooling is obtained To coordination suspension;
Step 4, coordination suspension is subjected to chlorine aerated reaction 5h, then constant pressure back flow reaction 8h, sunk after cold filtration Starch;
Step 5, sediment is put into caddy methanol solution, substrate surface is sprayed to after stirring, then carried out at annealing 3h is managed, the CdTe nano photovoltaic materials that adulterate are obtained after cooling.
Tellurium powder concentration in the step 1 is 30mg/L, and the addition of the polyvinylpyrrolidone is tellurium powder mole 8%, the frequency of the ultrasonic agitation is 10kHz, and the ultrasonic agitation time is 30min.
Caddy addition in the step 2 is 1.2 times of tellurium powder mole, and the addition of the water is absolute ethyl 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 The vacuum distillation time is stated for 3h, the volume of the vacuum distillation is the 50% of original volume.
Ammonia addition in the step 3 is 1.7 times of tellurium powder mole, and the aeration flow velocity is 15mL/min, described Aerated 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 aerated 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 backflow Using water cooling.
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., 2h is reacted under the conditions of 250 DEG C, then continues at 350 DEG C Reaction, until reaction reacts 0.5h before terminating under the conditions of 450 DEG C.
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on its backward FTO glass Brush method prints one layer of TiO2Film layer, in the compacted zone for obtaining being carried on FTO glass after heating 25min at 500 DEG C, the densification Thickness degree is 50nm, and the photovoltaic material as made from embodiment 2 is spun on compacted zone thereafter, and in heating 10 minutes at 80 DEG C Photovoltaic material formation 30nm coating is affixed on compacted zone and form light-absorption layer, then silk-screen printing will be passed through to electrode slurry Method is printed on the light-absorption layer, and dry 10min is placed in 80 DEG C of baking ovens after levelling and obtains solar cell,
Used in battery performance test, experimentation in 100mW/cm2 Solar simulator (Newport) AM1.5G Carried out under illumination, it is 19.72% to measure optoelectronic transformation efficiency.After being kept for 20 days during 20 degrees Celsius of temperature, humidity is 45% environment, It is 17.32% to test its transformation efficiency.
Embodiment 3
A kind of preparation method of doping CdTe nano photovoltaic materials, its step is as follows:
Step 1, tellurium powder is put into absolute ethyl alcohol, adds polyvinylpyrrolidone, 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 completely, decompression is steamed Evaporate to ethanol and exclude completely, obtain the suspended aqueous solution;
Step 3, the suspended aqueous solution is put into reactor, then passes to ammonia and carry out cyclic aeration reaction 3h, natural cooling is obtained To coordination suspension;
Step 4, coordination suspension is subjected to chlorine aerated reaction 4h, then constant pressure back flow reaction 6h, sunk after cold filtration Starch;
Step 5, sediment is put into caddy methanol solution, substrate surface is sprayed to after stirring, then carried out at annealing 3h is managed, the CdTe nano photovoltaic materials that adulterate are obtained after cooling.
Tellurium powder concentration in the step 1 is 25mg/L, and the addition of the polyvinylpyrrolidone is tellurium powder mole 6%, the frequency of the ultrasonic agitation is 7kHz, and the ultrasonic agitation time is 20min.
Caddy addition in the step 2 is 1.1 times of tellurium powder mole, and the addition of the water is absolute ethyl 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 The vacuum distillation time is stated for 2h, the volume of the vacuum distillation is the 45% of original volume.
Ammonia addition in the step 3 is 1.6 times of tellurium powder mole, and the aeration flow velocity is 12mL/min, described Aerated 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 aerated 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 backflow Using water cooling.
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., 2h is reacted under the conditions of 230 DEG C, then continues at 350 DEG C Reaction, until reaction reacts 0.5h before terminating under the conditions of 430 DEG C.
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on its backward FTO glass Brush method prints one layer of TiO2Film layer, in the compacted zone for obtaining being carried on FTO glass after heating 25min at 500 DEG C, the densification Thickness degree is 50nm, photovoltaic material dissolving will be spun on as made from embodiment 3 on compacted zone thereafter, and in heating 10 at 80 DEG C The coating that minute makes the photovoltaic material form 30nm, which is affixed on compacted zone, forms light-absorption layer, then will pass through screen printing to electrode slurry Brush method is printed on the light-absorption layer, and dry 10min is placed in 80 DEG C of baking ovens after levelling and obtains solar cell,
Used in battery performance test, experimentation in 100mW/cm2 Solar simulator (Newport) AM1.5G Carried out under illumination, it is 20.41% to measure optoelectronic transformation efficiency.After being kept for 20 days during 20 degrees Celsius of temperature, humidity is 45% environment, It is 19.12% to test its transformation efficiency.
Embodiment 4
A kind of preparation method of doping CdTe nano photovoltaic materials, its step is as follows:
Step 1, tellurium powder is put into absolute ethyl alcohol, adds polyvinylpyrrolidone, 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 completely, decompression is steamed Evaporate to ethanol and exclude completely, obtain the suspended aqueous solution;
Step 3, the suspended aqueous solution is put into reactor, then passes to ammonia and carry out cyclic aeration reaction 4h, natural cooling is obtained To coordination suspension;
Step 4, coordination suspension is subjected to chlorine aerated reaction 4h, then constant pressure back flow reaction 7h, sunk after cold filtration Starch;
Step 5, sediment is put into caddy methanol solution, substrate surface is sprayed to after stirring, then carried out at annealing 3h is managed, the CdTe nano photovoltaic materials that adulterate are obtained after cooling.
Tellurium powder concentration in the step 1 is 28mg/L, and the addition of the polyvinylpyrrolidone is tellurium powder mole 7%, the frequency of the ultrasonic agitation is 8kHz, and the ultrasonic agitation time is 25min.
Caddy addition in the step 2 is 1.2 times of tellurium powder mole, and the addition of the water is absolute ethyl 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 The vacuum distillation time is stated for 3h, the volume of the vacuum distillation is the 45% of original volume.
Ammonia addition in the step 3 is 1.6 times of tellurium powder mole, and the aeration flow velocity is 14mL/min, described Aerated 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 backflow uses water cooling.
The chlorine aerated reaction is reacted using gradient, i.e., 63 DEG C sustained responses 0.7h, 85 DEG C of reaction 0.5h, and 100 DEG C anti- 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., 2h is reacted under the conditions of 220 DEG C, then continues at 350 DEG C Reaction, until reaction reacts 0.5h before terminating under the conditions of 440 DEG C.
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on its backward FTO glass Brush method prints one layer of TiO2Film layer, in the compacted zone for obtaining being carried on FTO glass after heating 25min at 500 DEG C, the densification Thickness degree is 50nm, photovoltaic material dissolving will be spun on as made from embodiment 4 on compacted zone thereafter, and in heating 10 at 80 DEG C The coating that minute makes the photovoltaic material form 30nm, which is affixed on compacted zone, forms light-absorption layer, then will pass through screen printing to electrode slurry Brush method is printed on the light-absorption layer, and dry 10min is placed in 80 DEG C of baking ovens after levelling and obtains solar cell,
Used in battery performance test, experimentation in 100mW/cm2 Solar simulator (Newport) AM1.5G Carried out under illumination, it is 22.37% to measure optoelectronic transformation efficiency.After being kept for 20 days during 20 degrees Celsius of temperature, humidity is 45% environment, It is 20.07% to test its transformation efficiency.
One embodiment of the invention is the foregoing is only, the present invention, all use equivalent substitutions or equivalent transformation is not intended to limit The technical scheme that is obtained of mode, all fall within protection scope of the present invention.

Claims (9)

1.一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:其步骤如下:1. A preparation method of doped CdTe nano-photovoltaic material, characterized in that: its steps are as follows: 步骤1,将碲粉放入无水乙醇中,加入聚乙烯吡咯烷酮,超声搅拌形成分散均匀的悬浊醇液;Step 1, put tellurium powder into absolute ethanol, add polyvinylpyrrolidone, and ultrasonically stir to form a uniformly dispersed alcohol suspension; 步骤2,将氯化镉加入水中,搅拌溶解后缓慢滴加悬浊醇液,直至完全搅拌均匀,减压蒸馏至乙醇完全排除,得到悬浊水溶液;Step 2, adding cadmium chloride into water, stirring and dissolving, slowly adding the suspended alcohol solution dropwise until it is completely stirred evenly, and distilling under reduced pressure until the ethanol is completely removed to obtain a suspended aqueous solution; 步骤3,将悬浊水溶液放入反应釜中,然后通入氨气进行循环曝气反应2-5h,自然冷却,得到配位悬浊液;Step 3, put the suspended aqueous solution into the reaction kettle, then pass through ammonia gas to carry out the circular aeration reaction for 2-5 hours, and cool naturally to obtain the coordination suspension; 步骤4,将配位悬浊液进行氯气曝气反应3-5h,然后恒压回流反应5-8h,冷却过滤后得到沉淀物;Step 4, subjecting the coordination suspension to chlorine gas aeration reaction for 3-5 hours, then reflux reaction at constant pressure for 5-8 hours, cooling and filtering to obtain a precipitate; 步骤5,将沉淀物放入氯化镉甲醇液中,搅拌均匀后喷洒至基材表面,然后进行退火处理3h,冷却后得到掺杂CdTe纳米光伏材料。Step 5, putting the precipitate into the cadmium chloride methanol solution, stirring evenly, spraying it on the surface of the substrate, and then performing annealing treatment for 3 hours, and obtaining the doped CdTe nano-photovoltaic material after cooling. 2.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤1中的碲粉浓度为20-30mg/L,所述聚乙烯吡咯烷酮的加入量是碲粉摩尔量的5-8%,所述超声搅拌的频率为5-10kHz,所述超声搅拌时间为10-30min。2. the preparation method of a kind of doped CdTe nano photovoltaic material according to claim 1, is characterized in that: the tellurium powder concentration in the described step 1 is 20-30mg/L, and the add-on of described polyvinylpyrrolidone is The molar weight of tellurium powder is 5-8%, the frequency of the ultrasonic stirring is 5-10kHz, and the ultrasonic stirring time is 10-30min. 3.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤2中的氯化镉加入量是碲粉摩尔量的1.1-1.2倍,所述水的加入量是无水乙醇的0.3-0.5,所述缓慢滴加的速度是4-8mL/min。3. The preparation method of a kind of doped CdTe nano-photovoltaic material according to claim 1, characterized in that: the amount of cadmium chloride added in the step 2 is 1.1-1.2 times of the molar weight of tellurium powder, and the water The addition amount is 0.3-0.5 of dehydrated alcohol, and the speed of described slow drop is 4-8mL/min. 4.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤2中的减压蒸馏的温度为80-90℃,所述减压蒸馏的压力为大气压的50-60%,所述减压蒸馏时间为2-3h,所述减压蒸馏的体积是原体积的40-50%。4. A kind of preparation method of doped CdTe nano-photovoltaic material according to claim 1, it is characterized in that: the temperature of the vacuum distillation in described step 2 is 80-90 ℃, and the pressure of described vacuum distillation is 50-60% of the atmospheric pressure, the vacuum distillation time is 2-3h, and the volume of the vacuum distillation is 40-50% of the original volume. 5.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤3中的氨气加入量是碲粉摩尔的1.5-1.7倍,所述曝气流速为10-15mL/min,所述曝气反应温度为60-70℃。5. The preparation method of a kind of doped CdTe nano-photovoltaic material according to claim 1, characterized in that: the amount of ammonia added in the step 3 is 1.5-1.7 times of the mole of tellurium powder, and the aeration flow rate is 10-15mL/min, and the aeration reaction temperature is 60-70°C. 6.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤4中的氯气的通入量是碲粉的1.8-2.2倍,所述氯气曝气反应的温度为60-100℃,所述曝气流速为5-8mL/min,所述恒压回流反应的压力为大气压,所述温度为100-110℃,所述回流采用水冷却。6. The preparation method of a kind of doped CdTe nano-photovoltaic material according to claim 1, characterized in that: the intake of chlorine in the step 4 is 1.8-2.2 times that of tellurium powder, and the chlorine aeration The reaction temperature is 60-100°C, the aeration flow rate is 5-8mL/min, the pressure of the constant-pressure reflux reaction is atmospheric pressure, the temperature is 100-110°C, and the reflux is cooled by water. 7.根据权利要求 6 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述氯气曝气反应采用梯度反应,即60-65℃持续反应0.5-1h,80-90℃反应0.5h,100℃反应至结束。7. The preparation method of a doped CdTe nano-photovoltaic material according to claim 6, characterized in that: the chlorine gas aeration reaction adopts a gradient reaction, that is, the reaction is continued at 60-65°C for 0.5-1h, and at 80-90°C The reaction was carried out for 0.5h, and the reaction was completed at 100°C. 8.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤5中氯化镉甲醇溶液的浓度为10-15mg/L,所述搅拌速度为1500-2000r/min。8. The preparation method of a kind of doped CdTe nano-photovoltaic material according to claim 1, characterized in that: the concentration of cadmium chloride methanol solution in the step 5 is 10-15mg/L, and the stirring speed is 1500 -2000r/min. 9.根据权利要求 1 所述的一种掺杂CdTe纳米光伏材料的制备方法,其特征在于:所述步骤5中的喷洒量为2-4mg/cm2,所述退火温度为400-450℃,所述退火反应采用氮气保护退火反应,所述退火反应采用梯度退火法,即在200-250℃条件下反应1-2h,然后持续在350℃反应,直至反应结束前在400-450℃条件下反应0.5h。9. The preparation method of a doped CdTe nano-photovoltaic material according to claim 1, characterized in that: the spraying amount in the step 5 is 2-4mg/cm 2 , and the annealing temperature is 400-450°C , the annealing reaction adopts nitrogen protection annealing reaction, and the annealing reaction adopts gradient annealing method, that is, reacting at 200-250°C for 1-2h, and then continuing to react at 350°C until the end of the reaction at 400-450°C Under reaction 0.5h.
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