CN107275491B - A kind of graphene superconduction type perovskite photovoltaic light absorbent - Google Patents
A kind of graphene superconduction type perovskite photovoltaic light absorbent Download PDFInfo
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- CN107275491B CN107275491B CN201710452468.8A CN201710452468A CN107275491B CN 107275491 B CN107275491 B CN 107275491B CN 201710452468 A CN201710452468 A CN 201710452468A CN 107275491 B CN107275491 B CN 107275491B
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Abstract
The invention discloses a kind of graphene superconduction type perovskite photovoltaic light absorbents, finely dispersed stablizing solution is respectively configured in graphene and lead iodide, and it is sprayed at the surface FTO respectively, it is sealed reaction, obtain the FTO glass of graphene film and lead iodide films, then it is immersed in methylamine solution, hydroiodic acid is added dropwise, cooling obtains thin-film material after sealing aeration reaction and 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 provided by the invention is mild, and temperature-controllable is strong, and the conditions such as unprotect gas, and reactive mode is simple, can industrialized production.
Description
Technical field
The invention belongs to photovoltaic material technical fields, and in particular to a kind of graphene superconduction type perovskite photovoltaic extinction material
Material.
Background technique
Solar cell material passes through development in more than 60 years, has there is many different types.It mainly include monocrystalline/polycrystalline
Silicon, GaAs, cadmium telluride, copper indium gallium selenide, dye sensitization etc..Only monocrystalline/polycrystalline silicon solar cell has obtained answering extensively at present
With, other kinds of solar battery because the disadvantages of raw material are rare, toxic, low efficiency, poor stability in practical applications by
To limitation.But monocrystalline/polycrystalline silicon solar cell high production cost, finding novel solar battery is still the heat studied at present
Point.
Ca-Ti ore type organic metal haloid material has excellent photoelectric properties and is readily synthesized, in solar-electricity
It is widely used in the research of pond, has reached 19% currently based on the solar battery highest energy transfer efficiency of this material, reason
It can achieve 50% by transformation efficiency, there is very big exploitation potential.
Perovskite solar cell is usually to be transmitted by transparent conducting glass, compacted zone, perovskite absorbed layer, organic hole
Layer, five part of metal back electrode composition.When perovskite solar cell works, perovskite compound absorbs photon under light illumination,
Valence-band electrons transit to conduction band, and conduction band electron is then injected into the conduction band of TiO2, then are transferred to FTO, meanwhile, hole transport is extremely
Organic cavity transmission layer, so that electron-hole pair separates, 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 the electron-hole pair for absorbing sunlight and generating, and can high efficiency of transmission
Electron-hole pair, electronics, hole to corresponding compacted zone and organic cavity transmission layer.Perovskite absorbed layer generally uses mesoporous
Nanostructure loads perovskite light absorbent, because of meso-porous nano structure large specific surface area, adsorbable more suction as bracket
Stimulative substance, to obtain biggish cell power conversion efficiency, composition, micro-structure 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 battery light of assembling
Electrotransformation rate is not high.
Summary of the invention
The object of the present invention is to provide a kind of graphene superconduction type perovskite photovoltaic light absorbent, the graphene calcium titaniums of preparation
The membrane structure compactness of mine photovoltaic absorbing material is good, has good assimilation effect under visible light conditions.
Technical purpose of the invention has the technical scheme that a kind of graphene superconduction type perovskite light
Light absorbent is lied prostrate, its step are as follows:
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., light
Yellow transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, dispersing agent is added, ultrasound is uniformly rear to form graphene dispersing solution；
Step 3, graphene dispersing solution is sprayed on FTO glass surface, then carries out high pressure sealing and react 2-3h, after cooling
Form uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, constant temperature drying forms the iodate on surface
Thin film lead；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound
After mixing evenly, aeration reaction 3-6h is sealed, natural cooling after 1-3h is evaporated under reduced pressure, takes out thin-film material drying；
Step 6, thin-film material is put into sealing reaction kettle, is sealed reaction, obtains graphene perovskite after cooling
Photovoltaic 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
Mixing speed is 1000-1500r/min, and lead iodide is dissolved in DMF and is capable of forming stable iodate lead solution, thin convenient for lead iodide
The preparation of film, while DMF can be in stable liquid under whipping temp, prevent its volatilization.
The mole of nano-graphene in the step 2 is 1.5-1.8 times of lead iodide, the nano-graphene it is dense
Degree is 1.1-1.5g/L, and the dispersing agent uses organosilicone spreading agent, and the additional amount of the dispersing agent is nano-graphene mole
The 3-5% of amount, the frequency of the ultrasonic agitation are 1.5-2.5kHz, and the ultrasonic time is 30-45min；The step is using organic
Graphene can be effectively fixed on FTO glass in subsequent reactions by silicon dispersing agent containing element silicon material, be increased
Cementation fastness；Nano-graphene dissolution is dispersed in water by the step, forms the graphene dispersing solution stablized, and use
The mode of ultrasound carries out rapid dispersion, and the effect using its clutch energy is evenly dispersed by nano-graphene, guarantees dispersing agent effect
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 are 150-200 DEG C；Graphene dispersing solution is evenly distributed on FTO by the way of spraying by the step
Glass surface, under high pressure sealing reaction condition, the organosilicone spreading agent in graphene connects with glass, and graphene is firm viscous
It is attached to glass surface, forms stability thin-film material.
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；It should
Step forms stable lead iodide films on the surface of graphene by way of sprinkling, and during constant temperature drying, by iodine
Change lead to infiltrate into the defect gap of graphene film, forms the lead iodide films of the covering property on surface.
The molar ratio of methylamine and hydroiodic acid in step 5 is 1:1.01-1.05, and 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
Stating ultrasonic time is 10-15min, and the gas of the sealing aeration reaction is nitrogen, and aeration flow velocity is 10-15mL/min, described
Sealing reaction temperature is 100-110 DEG C, pressure 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, is guaranteed methylamine is complete
It is dispersed to film surface entirely, especially into graphene film gap；By the side that hydroiodic acid and ultrasonic agitation is added dropwise
Formula is capable of forming the dispersion effect of stable and uniform, and the methylamine joint with film surface；During sealing aeration reaction
Hydroiodic acid reacts precipitating with methylamine on the surface of graphene, forms crystal grain, and guarantee its stable and uniform in aeration reaction
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 being evaporated under reduced pressure carries out concentration enrichment, to increase film thickness；The step
Middle methylamine solution repairs graphene film gap during aeration reaction, solves graphene defect problem, improves stone
Black alkene conduction efficiency.
Sealing reaction temperature in the step 6 is 90-100 DEG C, pressure 5-10MPa, passes through the condition of sealing reaction
Under, by graphene and CH3NH3PbI3 Perovskite thin film carry out the reaction of consolidation sealing pressing, 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 the surface FTO respectively,
It is sealed reaction, 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 aeration reaction obtain thin-film material with cooling after distillation reaction；Thin-film material sealing reaction is finally obtained into graphite
Alkene perovskite photovoltaic absorbing material.
In conclusion the invention has the following beneficial effects:
Preparation method simple possible of the present invention, practicality and versatile.Graphene perovskite photovoltaic prepared by the present invention
The membrane structure compactness of absorbing material is good, has good assimilation effect under visible light conditions.System provided by the invention
Preparation Method reaction condition is mild, and temperature-controllable is strong, and the conditions such as unprotect gas, and reactive mode is simple, can industrialized production.
Specific embodiment
Embodiment 1
A kind of graphene superconduction type perovskite photovoltaic light absorbent, its step are as follows:
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., light
Yellow transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, dispersing agent is added, ultrasound is uniformly rear to form graphene dispersing solution；
Step 3, graphene dispersing solution is sprayed on FTO glass surface, then carries out high pressure sealing and reacts 2h, shape after cooling
At uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, constant temperature drying forms the iodate on surface
Thin film lead；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound
After mixing evenly, aeration reaction 3h is sealed, natural cooling after 1h is evaporated under reduced pressure, takes out thin-film material drying；
Step 6, thin-film material is put into sealing reaction kettle, is sealed reaction, obtains graphene perovskite after cooling
Photovoltaic 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 dispersing agent use organosilicone spreading agent, and the additional amount of the dispersing agent 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 are 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 molar ratio of methylamine and hydroiodic acid in step 5 is 1:1.01, and 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 aeration reaction are nitrogen, and aeration flow velocity is 10mL/min, and the sealing reaction temperature is 100
DEG C, pressure 2MPa, 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, pressure 5MPa.
Solar battery 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 are as follows:
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., light
Yellow transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, dispersing agent is added, ultrasound is uniformly rear to form graphene dispersing solution；
Step 3, graphene dispersing solution is sprayed on FTO glass surface, then carries out high pressure sealing and reacts 3h, shape after cooling
At uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, constant temperature drying forms the iodate on surface
Thin film lead；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound
After mixing evenly, aeration reaction 6h is sealed, natural cooling after 3h is evaporated under reduced pressure, takes out thin-film material drying；
Step 6, thin-film material is put into sealing reaction kettle, is sealed reaction, obtains graphene perovskite after cooling
Photovoltaic 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 dispersing agent use organosilicone spreading agent, and the additional amount of the dispersing agent 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 are 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 molar ratio of methylamine and hydroiodic acid in step 5 is 1:1.05, and 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 aeration reaction are nitrogen, and aeration flow velocity is 15mL/min, and the sealing reaction temperature is 110
DEG C, pressure 4MPa, 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, pressure 10MPa.
Solar battery 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 are as follows:
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., light
Yellow transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, dispersing agent is added, ultrasound is uniformly rear to form graphene dispersing solution；
Step 3, graphene dispersing solution is sprayed on FTO glass surface, then carries out high pressure sealing and reacts 2h, shape after cooling
At uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, constant temperature drying forms the iodate on surface
Thin film lead；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound
After mixing evenly, aeration reaction 4h is sealed, natural cooling after 2h is evaporated under reduced pressure, takes out thin-film material drying；
Step 6, thin-film material is put into sealing reaction kettle, is sealed reaction, obtains graphene perovskite after cooling
Photovoltaic 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 dispersing agent use organosilicone spreading agent, and the additional amount of the dispersing agent 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 are 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 molar ratio of methylamine and hydroiodic acid in step 5 is 1:1.04, and 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 aeration reaction are nitrogen, and aeration flow velocity is 12mL/min, and the sealing reaction temperature is 104
DEG C, pressure 3MPa, 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, pressure 7MPa.
Solar battery 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 are as follows:
Step 1, lead iodide is dissolved in DMF solution, then constant temperature stirs to form stable homogeneous transparent solution, i.e., light
Yellow transparent iodate lead solution；
Step 2, nano-graphene powder is added to the water, dispersing agent is added, ultrasound is uniformly rear to form graphene dispersing solution；
Step 3, graphene dispersing solution is sprayed on FTO glass surface, then carries out high pressure sealing and reacts 3h, shape after cooling
At uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, constant temperature drying forms the iodate on surface
Thin film lead；
Step 5, the thin-film material of step 4 is put into methylamine solution, hydroiodic acid is slowly added dropwise, until low frequency ultrasound
After mixing evenly, aeration reaction 5h is sealed, natural cooling after 2h is evaporated under reduced pressure, takes out thin-film material drying；
Step 6, thin-film material is put into sealing reaction kettle, is sealed reaction, obtains graphene perovskite after cooling
Photovoltaic 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 dispersing agent use organosilicone spreading agent, and the additional amount of the dispersing agent 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 are 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 molar ratio of methylamine and hydroiodic acid in step 5 is 1:1.04, and 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 aeration reaction are nitrogen, and aeration flow velocity is 14mL/min, and the sealing reaction temperature is 108
DEG C, pressure 3MPa, 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, pressure 8MPa.
Solar battery is assembled using graphene superconduction type perovskite photovoltaic light absorbent manufactured in the present embodiment, battery
Optoelectronic transformation efficiency is 13.9%.
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 graphene superconduction type perovskite photovoltaic light absorbent, which is characterized in that its preparation 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, dispersing agent is added, ultrasound is uniformly rear to form graphene dispersing solution；
Step 3, graphene dispersing solution is sprayed on FTO glass surface, then carries out high pressure sealing and react 2-3h, is formed after cooling
Uniform graphene molecules film；
Step 4, iodate lead solution is uniformly sprayed at graphene molecules film surface, the lead iodide that constant temperature drying forms 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 stirs
After uniformly, aeration reaction 3-6h is sealed, is evaporated under reduced pressure natural cooling after 1-3h, takes out thin-film material drying；
Step 6, thin-film material is put into sealing reaction kettle, is sealed reaction, obtains graphene perovskite photovoltaic after cooling
Absorbing material.
2. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that: the step
Iodate lead concentration is 0.3-0.6g/L in rapid 1, and the temperature of constant temperature stirring is 70-80 DEG C, mixing speed 1000-1500r/min.
3. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that: the step
The mole of nano-graphene in rapid 2 is 1.5-1.8 times of lead iodide, and the concentration of the nano-graphene is 1.1-1.5g/
L, dispersing agent use organosilicone spreading agent, and the additional amount of dispersing agent 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: the step
The frequency of ultrasonic agitation in rapid 2 is 1.5-2.5kHz, ultrasonic time 30-45min.
5. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that: the step
The quantity for spray of graphene dispersing solution is 10-15mg/cm in rapid 32, the pressure of high pressure sealing reaction is 10-15MPa, and temperature is
150-200℃。
6. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that: the step
The fountain height of iodate lead solution is 20-25mg/cm in rapid 42, the temperature of 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 5
In methylamine and hydroiodic acid molar ratio be 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: the step
The rate of addition of hydroiodic acid in rapid 5 is 5-10mL/min, low frequency ultrasound 0.8-1.2kHz, ultrasonic time 10-
15min, the gas for sealing aeration reaction is nitrogen, and aeration flow velocity is 10-15mL/min, and sealing reaction temperature is 100-110 DEG C,
Pressure is 2-4MPa, and the pressure of vacuum distillation is the 60-70% of atmospheric pressure, and the volume after vacuum distillation is the 40- before reaction
50%.
9. a kind of graphene superconduction type perovskite photovoltaic light absorbent according to claim 1, it is characterised in that: the step
Sealing reaction temperature in rapid 6 is 90-100 DEG C, pressure 5-10MPa.
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