CN107275491A - A kind of graphene superconduction type perovskite photovoltaic light absorbent - Google Patents

A kind of graphene superconduction type perovskite photovoltaic light absorbent Download PDF

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CN107275491A
CN107275491A CN201710452468.8A CN201710452468A CN107275491A CN 107275491 A CN107275491 A CN 107275491A CN 201710452468 A CN201710452468 A CN 201710452468A CN 107275491 A CN107275491 A CN 107275491A
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graphene
perovskite photovoltaic
solution
reaction
light absorbent
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CN107275491B (en
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徐海涛
徐闰
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Li Miao
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University of Shaoxing
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    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract

The invention discloses a kind of graphene superconduction type perovskite photovoltaic light absorbent, finely dispersed stablizing solution is respectively configured in graphene and lead iodide, and FTO surfaces are sprayed at respectively, carry out sealing reaction, obtain the FTO glass of graphene film and lead iodide films, then it is immersed in methylamine solution, hydroiodic acid is added dropwise, sealing aerated reaction obtains thin-film material with cooling after distillation reaction；Thin-film material sealing reaction is finally obtained into graphene perovskite photovoltaic absorbing material.The membrane structure compactness of graphene perovskite photovoltaic absorbing material prepared by the present invention is good, has good assimilation effect under visible light conditions.Preparation method reaction condition that the present invention is provided is gentle, and temperature-controllable is strong, and the condition such as unprotect gas, and reactive mode is simple, can industrialized production.

Description

A kind of graphene superconduction type perovskite photovoltaic light absorbent
Technical field
The invention belongs to photovoltaic material technical field, and in particular to a kind of graphene superconduction type perovskite photovoltaic extinction material Material.
Background technology
Solar cell material passes through the development of more than 60 years, has there is many different types.Mainly include monocrystalline/polycrystalline Silicon, GaAs, cadmium telluride, CIGS, dye sensitization etc..Only monocrystalline/polycrystalline silicon solar cell has obtained extensively should at present With, other kinds of solar cell because the shortcomings of raw material are rare, poisonous, efficiency is low, stability is poor in actual applications by To limitation.But monocrystalline/polycrystalline silicon solar cell production cost is high, it is still the heat studied at present to find new solar cell Point.
Ca-Ti ore type organic metal haloid material has excellent photoelectric properties and is readily synthesized, in solar-electricity Widely used in the research of pond, the solar cell highest energy conversion efficiency for being currently based on this material has reached 19%, it is managed 50% can be reached by transformation efficiency, with very big exploitation potential.
Perovskite solar cell is typically to be transmitted by transparent conducting glass, compacted zone, perovskite absorbed layer, organic hole Layer, the part of metal back electrode five composition.When perovskite solar cell works, perovskite compound absorbs photon under light illumination, its Valence-band electrons transit to conduction band, and conduction band electron is then injected into TiO2 conduction band, then are transferred to FTO, meanwhile, hole transport is extremely Organic cavity transmission layer, so that electron-hole pair is separated, when connecting external circuit, the movement in electronics and hole will be produced Raw electric current.
Wherein, the main function of perovskite absorbed layer is to absorb the electron-hole pair that sunshine is produced, and can high efficiency of transmission Electron-hole pair, electronics, hole to corresponding compacted zone and organic cavity transmission layer.Perovskite absorbed layer is typically using mesoporous Nanostructured loads perovskite light absorbent as support, because meso-porous nano structure specific surface area is big, adsorbable more suction Stimulative substance, so as to obtain larger cell power conversion efficiency, composition, micro-structural and the property of meso-porous nano material are to perovskite The energy conversion efficiency of battery is extremely important.But perovskite absorbed layer is not high to absorbing amount, the solar cell light of assembling Electric conversion ratio is not high.
The content of the invention
It is an object of the invention to provide a kind of graphene superconduction type perovskite photovoltaic light absorbent, the graphene calcium titanium of preparation The membrane structure compactness of ore deposit photovoltaic absorbing material is good, has good assimilation effect under visible light conditions.
The present invention technical purpose technical scheme is that：A kind of graphene superconduction type perovskite light Light absorbent is lied prostrate, its step is as follows：
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., faint yellow Transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, adds dispersant, graphene dispersing solution is formed after ultrasound is uniform；
Step 3, graphene dispersing solution is sprayed on FTO glass surfaces, then carries out high pressure sealing reaction 2-3h, formed after cooling Uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide on constant temperature drying formation surface is thin Film；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound stirring After uniform, natural cooling after aerated reaction 3-6h, vacuum distillation 1-3h is sealed, thin-film material drying is taken out；
Step 6, thin-film material is put into sealing reactor, carries out sealing reaction, graphene perovskite photovoltaic is obtained after cooling Absorbing material.
Iodate lead concentration is 0.3-0.6g/L in the step 1, and the temperature of the constant temperature stirring is 70-80 DEG C, described to stir Speed is mixed for 1000-1500r/min, lead iodide, which is dissolved in DMF, can form stable iodate lead solution, be easy to lead iodide thin The preparation of film, while DMF can prevent it from volatilizing under whipping temp in stable liquid.
The mole of nano-graphene in the step 2 is 1.5-1.8 times of lead iodide, the nano-graphene it is dense Spend for 1.1-1.5g/L, the dispersant uses organosilicone spreading agent, and the addition of the dispersant is nano-graphene mole The 3-5% of amount, the frequency of the ultrasonic agitation is 1.5-2.5kHz, and the ultrasonic time is 30-45min；The step is using organic Silicon dispersant, it contains element silicon material, and effectively graphene can be fixed on FTO glass in subsequent reactions, increase Cementation fastness；Nano-graphene dissolving is dispersed in water by the step, forms stable graphene dispersing solution, and use The mode of ultrasound carries out rapid dispersion, and the effect using its clutch energy is dispersed by nano-graphene, it is ensured that dispersant is acted on To each particle, the reunion of graphene is reduced.
The quantity for spray of graphene dispersing solution is 10-15mg/cm in the step 32, the pressure of high pressure sealing reaction is 10-15MPa, the temperature is 150-200 DEG C；Graphene dispersing solution is evenly distributed on FTO by the step by the way of spraying Glass surface, under high pressure sealing reaction condition, the organosilicone spreading agent in graphene connects with glass, and graphene is firm viscous Glass surface is attached to, steadiness thin-film material is formed.
The fountain height of iodate lead solution is 20-25mg/cm in step 42, the temperature of the constant temperature drying is 60-80 DEG C；Should Step forms stable lead iodide films by way of sprinkling in graphenic surface, and during constant temperature drying, by iodine Change lead to infiltrate into the defect gap of graphene film, form the lead iodide films of the covering property on surface.
The mol ratio of methylamine and hydroiodic acid in step 5 is 1:1.01-1.05, the mole of the hydroiodic acid is lead iodide 1.01-1.15 times, the rate of addition of the hydroiodic acid is 5-10mL/min, and the low frequency ultrasound is 0.8-1.2kHz, institute Ultrasonic time is stated for 10-15min, the gas of the sealing aerated reaction is nitrogen, and aeration flow velocity is 10-15mL/min, described It is 100-110 DEG C to seal reaction temperature, and pressure is 2-4MPa, and the pressure of the vacuum distillation is the 60-70% of atmospheric pressure, described Volume after vacuum distillation is the 40-50% before reaction；Thin-film material is put into methylamine solution by the step, it is ensured that methylamine is complete Film surface is dispersed to entirely, especially into graphene film gap；By the side that hydroiodic acid and ultrasonic agitation is added dropwise Formula can form the dispersion effect of stable and uniform, and with the methylamine joint of film surface；During sealing aerated reaction Hydroiodic acid and methylamine reaction precipitation form crystal grain in graphenic surface, and ensure in aerated reaction its stable and uniform Dispersion effect, play stable reactive film material；The reactive film material reacts to form perovskite structure with lead iodide CH3NH3PbI3 Perovskite thin film, the mode through vacuum distillation carries out concentration enrichment, so as to add film thickness；The step Middle methylamine solution repairs graphene film gap during aerated reaction, solves graphene defect problem, improves stone Black alkene conduction efficiency.
Sealing reaction temperature in the step 6 is 90-100 DEG C, and pressure is 5-10MPa, by the condition for sealing reaction Under, by graphene and CH3NH3PbI3 Perovskite thin film carry out consolidation sealing pressing reaction, obtained thin-film material compactness More preferably, conduction efficiency is higher.
Finely dispersed stablizing solution is respectively configured in graphene and lead iodide by the present invention, and is sprayed at FTO surfaces respectively, Sealing reaction is carried out, the FTO glass of graphene film and lead iodide films is obtained, is then immersed in methylamine solution, hydrogen is added dropwise Acid iodide, sealing aerated reaction obtains thin-film material with cooling after distillation reaction；Thin-film material sealing reaction is finally obtained into graphite Alkene perovskite photovoltaic absorbing material.
In summary, the present invention has the advantages that：
Preparation method simple possible of the present invention, practicality and highly versatile.Graphene perovskite photovoltaic prepared by the present invention absorbs The membrane structure compactness of material is good, has good assimilation effect under visible light conditions.The preparation side that the present invention is provided Method reaction condition is gentle, and temperature-controllable is strong, and the condition such as unprotect gas, and reactive mode is simple, can industrialized production.
Embodiment
Embodiment 1
A kind of graphene superconduction type perovskite photovoltaic light absorbent, its step is as follows：
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., faint yellow Transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, adds dispersant, graphene dispersing solution is formed after ultrasound is uniform；
Step 3, graphene dispersing solution is sprayed on FTO glass surfaces, then carries out high pressure sealing reaction 2h, formed after cooling equal Even graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide on constant temperature drying formation surface is thin Film；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound stirring After uniform, natural cooling after aerated reaction 3h, vacuum distillation 1h is sealed, thin-film material drying is taken out；
Step 6, thin-film material is put into sealing reactor, carries out sealing reaction, graphene perovskite photovoltaic is obtained after cooling Absorbing material.
Iodate lead concentration is 0.3g/L in the step 1, and the temperature of the constant temperature stirring is 70 DEG C, and the mixing speed is 1000r/min。
The mole of nano-graphene in the step 2 is 1.5 times of lead iodide, and the concentration of the nano-graphene is 1.1g/L, the dispersant uses organosilicone spreading agent, and the addition of the dispersant is the 3% of nano-graphene mole, institute The frequency for stating ultrasonic agitation is 1.5kHz, and the ultrasonic time is 30min.
The quantity for spray of graphene dispersing solution is 10mg/cm in the step 32, the pressure of high pressure sealing reaction is 10MPa, the temperature is 150 DEG C.
The fountain height of iodate lead solution is 20mg/cm in step 42, the temperature of the constant temperature drying is 60 DEG C.
The mol ratio of methylamine and hydroiodic acid in step 5 is 1:1.01, the mole of the hydroiodic acid is lead iodide 1.01 times, the rate of addition of the hydroiodic acid is 5mL/min, and the low frequency ultrasound is 0.8kHz, and the ultrasonic time is 10min, the gas of the sealing aerated reaction is nitrogen, and aeration flow velocity is 10mL/min, and the sealing reaction temperature is 100 DEG C, pressure is 2MPa, and the pressure of the vacuum distillation is the 60% of atmospheric pressure, and the volume after the vacuum distillation is before reacting 40%。
Sealing reaction temperature in the step 6 is 90 DEG C, and pressure is 5MPa.
Solar cell is assembled using graphene superconduction type perovskite photovoltaic light absorbent manufactured in the present embodiment, battery Optoelectronic transformation efficiency is 13.1%.
Embodiment 2
A kind of graphene superconduction type perovskite photovoltaic light absorbent, its step is as follows：
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., faint yellow Transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, adds dispersant, graphene dispersing solution is formed after ultrasound is uniform；
Step 3, graphene dispersing solution is sprayed on FTO glass surfaces, then carries out high pressure sealing reaction 3h, formed after cooling equal Even graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide on constant temperature drying formation surface is thin Film；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound stirring After uniform, natural cooling after aerated reaction 6h, vacuum distillation 3h is sealed, thin-film material drying is taken out；
Step 6, thin-film material is put into sealing reactor, carries out sealing reaction, graphene perovskite photovoltaic is obtained after cooling Absorbing material.
Iodate lead concentration is 0.6g/L in the step 1, and the temperature of the constant temperature stirring is 80 DEG C, and the mixing speed is 1500r/min。
The mole of nano-graphene in the step 2 is 1.8 times of lead iodide, and the concentration of the nano-graphene is 1.5g/L, the dispersant uses organosilicone spreading agent, and the addition of the dispersant is the 5% of nano-graphene mole, institute The frequency for stating ultrasonic agitation is 2.5kHz, and the ultrasonic time is 45min.
The quantity for spray of graphene dispersing solution is 15mg/cm in the step 32, the pressure of high pressure sealing reaction is 15MPa, the temperature is 200 DEG C.
The fountain height of iodate lead solution is 25mg/cm in step 42, the temperature of the constant temperature drying is 80 DEG C.
The mol ratio of methylamine and hydroiodic acid in step 5 is 1:1.05, the mole of the hydroiodic acid is lead iodide 1.15 times, the rate of addition of the hydroiodic acid is 10mL/min, and the low frequency ultrasound is 1.2kHz, and the ultrasonic time is 15min, the gas of the sealing aerated reaction is nitrogen, and aeration flow velocity is 15mL/min, and the sealing reaction temperature is 110 DEG C, pressure is 4MPa, and the pressure of the vacuum distillation is the 70% of atmospheric pressure, and the volume after the vacuum distillation is before reacting 50%。
Sealing reaction temperature in the step 6 is 100 DEG C, and pressure is 10MPa.
Solar cell is assembled using graphene superconduction type perovskite photovoltaic light absorbent manufactured in the present embodiment, battery Optoelectronic transformation efficiency is 12.8%.
Embodiment 3
A kind of graphene superconduction type perovskite photovoltaic light absorbent, its step is as follows：
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., faint yellow Transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, adds dispersant, graphene dispersing solution is formed after ultrasound is uniform；
Step 3, graphene dispersing solution is sprayed on FTO glass surfaces, then carries out high pressure sealing reaction 2h, formed after cooling equal Even graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide on constant temperature drying formation surface is thin Film；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound stirring After uniform, natural cooling after aerated reaction 4h, vacuum distillation 2h is sealed, thin-film material drying is taken out；
Step 6, thin-film material is put into sealing reactor, carries out sealing reaction, graphene perovskite photovoltaic is obtained after cooling Absorbing material.
Iodate lead concentration is 0.4g/L in the step 1, and the temperature of the constant temperature stirring is 75 DEG C, and the mixing speed is 1200r/min。
The mole of nano-graphene in the step 2 is 1.6 times of lead iodide, and the concentration of the nano-graphene is 1.2g/L, the dispersant uses organosilicone spreading agent, and the addition of the dispersant is the 4% of nano-graphene mole, institute The frequency for stating ultrasonic agitation is 1.8kHz, and the ultrasonic time is 35min.
The quantity for spray of graphene dispersing solution is 12mg/cm in the step 32, the pressure of high pressure sealing reaction is 12MPa, the temperature is 170 DEG C.
The fountain height of iodate lead solution is 23mg/cm in step 42, the temperature of the constant temperature drying is 70 DEG C.
The mol ratio of methylamine and hydroiodic acid in step 5 is 1:1.04, the mole of the hydroiodic acid is lead iodide 1.08 times, the rate of addition of the hydroiodic acid is 7mL/min, and the low frequency ultrasound is 1.0kHz, and the ultrasonic time is 12min, the gas of the sealing aerated reaction is nitrogen, and aeration flow velocity is 12mL/min, and the sealing reaction temperature is 104 DEG C, pressure is 3MPa, and the pressure of the vacuum distillation is the 65% of atmospheric pressure, and the volume after the vacuum distillation is before reacting 45%。
Sealing reaction temperature in the step 6 is 95 DEG C, and pressure is 7MPa.
Solar cell is assembled using graphene superconduction type perovskite photovoltaic light absorbent manufactured in the present embodiment, battery Optoelectronic transformation efficiency is 13.5%.
Embodiment 4
A kind of graphene superconduction type perovskite photovoltaic light absorbent, its step is as follows：
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., faint yellow Transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, adds dispersant, graphene dispersing solution is formed after ultrasound is uniform；
Step 3, graphene dispersing solution is sprayed on FTO glass surfaces, then carries out high pressure sealing reaction 3h, formed after cooling equal Even graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide on constant temperature drying formation surface is thin Film；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound stirring After uniform, natural cooling after aerated reaction 5h, vacuum distillation 2h is sealed, thin-film material drying is taken out；
Step 6, thin-film material is put into sealing reactor, carries out sealing reaction, graphene perovskite photovoltaic is obtained after cooling Absorbing material.
Iodate lead concentration is 0.5g/L in the step 1, and the temperature of the constant temperature stirring is 78 DEG C, and the mixing speed is 1300r/min。
The mole of nano-graphene in the step 2 is 1.7 times of lead iodide, and the concentration of the nano-graphene is 1.4g/L, the dispersant uses organosilicone spreading agent, and the addition of the dispersant is the 4% of nano-graphene mole, institute The frequency for stating ultrasonic agitation is 2.2kHz, and the ultrasonic time is 40min.
The quantity for spray of graphene dispersing solution is 14mg/cm in the step 32, the pressure of high pressure sealing reaction is 14MPa, the temperature is 180 DEG C.
The fountain height of iodate lead solution is 24mg/cm in step 42, the temperature of the constant temperature drying is 75 DEG C.
The mol ratio of methylamine and hydroiodic acid in step 5 is 1:1.04, the mole of the hydroiodic acid is lead iodide 1.12 times, the rate of addition of the hydroiodic acid is 8mL/min, and the low frequency ultrasound is 1.1kHz, and the ultrasonic time is 14min, the gas of the sealing aerated reaction is nitrogen, and aeration flow velocity is 14mL/min, and the sealing reaction temperature is 108 DEG C, pressure is 3MPa, and the pressure of the vacuum distillation is the 68% of atmospheric pressure, and the volume after the vacuum distillation is before reacting 47%。
Sealing reaction temperature in the step 6 is 98 DEG C, and pressure is 8MPa.
Solar cell is assembled using graphene superconduction type perovskite photovoltaic light absorbent manufactured in the present embodiment, battery Optoelectronic transformation efficiency is 13.9%.
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. a kind of graphene superconduction type perovskite photovoltaic light absorbent, it is characterised in that its preparation process is as follows：
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., faint yellow Transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, adds dispersant, graphene dispersing solution is formed after ultrasound is uniform；
Step 3, graphene dispersing solution is sprayed on FTO glass surfaces, then carries out high pressure sealing reaction 2-3h, formed after cooling Uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide on constant temperature drying formation surface is thin Film；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound stirring After uniform, natural cooling after aerated reaction 3-6h, vacuum distillation 1-3h is sealed, thin-film material drying is taken out；
Step 6, thin-film material is put into sealing reactor, carries out sealing reaction, graphene perovskite photovoltaic is obtained after cooling Absorbing material.
2. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：It is described Iodate lead concentration is 0.3-0.6g/L in step 1, and the temperature of the constant temperature stirring is 70-80 DEG C, and the mixing speed is 1000- 1500r/min。
3. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：It is described The mole of nano-graphene in step 2 is 1.5-1.8 times of lead iodide, and the concentration of the nano-graphene is 1.1- 1.5g/L, the dispersant uses organosilicone spreading agent, and the addition of the dispersant is the 3-5% of nano-graphene mole.
4. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：It is described The frequency of ultrasonic agitation is 1.5-2.5kHz, and the ultrasonic time is 30-45min.
5. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：It is described The quantity for spray of graphene dispersing solution is 10-15mg/cm in step 32, the pressure of the high pressure sealing reaction is 10-15MPa, institute Temperature is stated for 150-200 DEG C.
6. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：Step The fountain height of iodate lead solution is 20-25mg/cm in 42, the temperature of the constant temperature drying is 60-80 DEG C.
7. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：Step The mol ratio of methylamine and hydroiodic acid in 5 is 1:1.01-1.05, the mole of the hydroiodic acid is the 1.01-1.15 of lead iodide Times.
8. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：It is described The rate of addition of hydroiodic acid is 5-10mL/min, and the low frequency ultrasound is 0.8-1.2kHz, and the ultrasonic time is 10- 15min, the gas of the sealing aerated reaction is nitrogen, and aeration flow velocity is 10-15mL/min, and the sealing reaction temperature is 100-110 DEG C, pressure is 2-4MPa, and the pressure of the vacuum distillation is the 60-70% of atmospheric pressure, the body after the vacuum distillation Product is the 40-50% before reaction.
9. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that：It is described Sealing reaction temperature in step 6 is 90-100 DEG C, and pressure is 5-10MPa.
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Cited By (1)

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CN108922782A (en) * 2018-07-12 2018-11-30 山东佳星环保科技有限公司 A kind of preparation method of graphene superconduction type perovskite photovoltaic light absorbent

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