CN107994122A - Zinc doping nickel oxide nanoparticle hole transmission layer is just putting perovskite solar cell and preparation method - Google Patents
Zinc doping nickel oxide nanoparticle hole transmission layer is just putting perovskite solar cell and preparation method Download PDFInfo
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- CN107994122A CN107994122A CN201711204673.9A CN201711204673A CN107994122A CN 107994122 A CN107994122 A CN 107994122A CN 201711204673 A CN201711204673 A CN 201711204673A CN 107994122 A CN107994122 A CN 107994122A
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/60—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation in which radiation controls flow of current through the devices, e.g. photoresistors
- H10K30/65—Light-sensitive field-effect devices, e.g. phototransistors
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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Abstract
The present invention relates to the preparation method that a kind of zinc doping nickel oxide nanoparticle hole transmission layer is just putting perovskite solar cell.The present invention uses brand-new inorganic hole-transporting layer, obtains high transparency, high conductivity by adulterating zinc optimization nickel oxide nanoparticle, high work content matches good hole extract layer with perovskite, and efficient perovskite solar cell is obtained by assembling.Zinc nitrate and nickel nitrate hexahydrate are mixed in alkaline aqueous solution in proportion first, zinc doping nickel oxide nanoparticle is obtained by centrifugation, drying and calcination, then it is spun on fluorine-doped tin oxide glass, high-performance zinc doping nickel oxide film is obtained by heat drying, improve film light transmittance and hole extraction efficiency, cell series resistance is thereby reduced, optimizes cell photoelectric transfer efficiency.
Description
Technical field
The invention belongs to technical field prepared by perovskite solar cell, more particularly to a kind of zinc doping nickel oxide nano
Particle hole transmission layer is just putting perovskite solar cell and preparation method.
Background technology
Perovskite solar cell is since 2009 report for the first time, and energy conversion efficiency is maked rapid progress, by initial
3.8% is lifted to 22.1%.Being announced to the world splendidly for perovskite solar cell brings new hope for the development of solar cell.Calcium
Titanium ore light-absorption layer both sides are electron transfer layer and hole transmission layer respectively, and the ability in its hole-transporting layer extraction hole is directly determined
Determine the photoelectric conversion efficiency of solar cell, it is seen that the importance of hole transmission layer is self-evident.
Hole transmission layer used in the solar cell of current most of high-photoelectric transformation efficiencies transmits for organic hole
Layer（Such as PEDOT：PSS, PTAA, spiro-OMeTAD etc.）, but organic hole transport material preparation process is complicated, price is held high
It is expensive, and it is unsatisfactory for the requirement of large-scale production.Therefore, the inorganic material for finding replacement organic cavity transmission layer is most important.
Nickel oxide is a kind of p-type simconductor material, and energy gap is 3.6 eV, and perovskite level-density parameter, and
And there is high-transmittance in visible-range, it is suitable in the opto-electronic devices such as perovskite solar cell, but its is relatively low
Electrical conductivity be always the hole transmission layer inferior position where, and adulterate can change this present situation to greatest extent.
The content of the invention
It is an object of the invention to overcome above-mentioned existing technical deficiency, there is provided one kind utilizes cheap new material（Oxidation
Nickel）The zinc doping nickel oxide nanoparticle hole transmission layer of preparation is just putting perovskite solar cell, improves battery series electrical
Resistance, by improving hole extraction efficiency so as to optimize battery performance, provides to develop the perovskite solar cell of Cheap highly effective
A kind of new approaches.
Present invention also offers the preparation method of above-mentioned solar cell.
In order to overcome existing technical deficiency, the technical scheme is that：
The present invention has separated a kind of zinc doping nickel oxide nanoparticle hole transmission layer and has just put perovskite solar cell, its feature
It is to be made of following preparation method：（1）, using FTO glass as Window layer carry out partial etching；（2）, prepare electric transmission
Layer；（3）, prepare perovskite bulk heterojunction film；（4）, prepare on calcium titanium ore bed zinc doping nickel oxide nanoparticle hole biography
Defeated layer；（5）, electrode modification layer is prepared on hole transmission layer；（6）, on electrode modification layer prepare metal electrode, so as to obtain
Solar cell；
The zinc doping nickel oxide nanoparticle hole transmission layer is made of using following methods：By six water of zinc nitrate and nickel nitrate
Compound is mixed in alkaline aqueous solution in proportion（PH=10）In, 8h and 275 DEG C of 3 times, 80 DEG C of dryings calcining 2h are centrifuged by isopropanol
Obtain zinc doping nickel oxide nanoparticle, then by black powder be dissolved in aqueous isopropanol zinc doping nickel oxide be made before
Liquid is driven, then 2500rmp spin coatings precursor liquid 1min is in fluorine-doped tin oxide glass（FTO glass）Substrate, last need to be gained
Substrate is placed on to be spontaneously dried at room temperature, that is, obtains zinc doping nickel oxide nanoparticle hole transmission layer.
The invention described above just puts perovskite solar cell, preferably：The molar ratio of the zinc nitrate and nickel nitrate is
3-7:97-93, zinc nitrate are 1M in the concentration of in the mixed solvent with nickel nitrate.
The invention described above just puts perovskite solar cell, preferably：The thickness of the FTO glass is 300nm；Zinc is mixed
The thickness of miscellaneous nickel oxide hole transmission layer is 30nm；The thickness of perovskite bulk heterojunction film is 300nm；The thickness of electron transfer layer
Spend for 30nm；The thickness of electrode modification layer is 10nm；The thickness of metal electrode is 60nm.
The invention described above just puts perovskite solar cell, preferably：The grain of the zinc doping nickel oxide nanoparticle
Footpath is 30-50nm.
The invention also discloses a kind of above-mentioned zinc doping nickel oxide nanoparticle hole transmission layer just to put perovskite solar energy
The preparation method of battery, it is characterised in that using following steps：
（1）FTO transparent conducting glass is cut into the strip of 1.6cm, then sticks the adhesive tape of 1cm wide, then with zinc powder and dense salt
Acid is 1 with water volume ratio:5 dilute hydrochloric acid etches 15 minutes, and the zinc powder of remnants is cleaned with dilute hydrochloric acid, the glass etched is cut into
1.6 × 1.7cm rectangles, with lye be cleaned by ultrasonic 30-60 min, then with alcohol be cleaned by ultrasonic 30-60 min, finally spend from
Sub- water is cleaned by ultrasonic 10-30 min, is put into drying baker drying with spare；
（2）Spin coating concentration is the chlorobenzene solution of the PCBM of 15-20mg/ml in fluorine-doped tin oxide glass in glove box（FTO glass
Glass）Substrate obtains electron transfer layer；
（3）Lead acetate and iodine methylamine are dissolved in n,N-Dimethylformamide solvent, is subsequently placed on magnetic stirring apparatus and stirs 30
Min obtains perovskite precursor solution, is then spin coated onto precursor liquid on electron transfer layer and 100 DEG C of annealing obtain calcium titanium in 10 minutes
Ore deposit light-absorption layer；
（4）Zinc nitrate and nickel nitrate hexahydrate are mixed in alkaline aqueous solution in proportion（PH=10）In, centrifuged by isopropanol
3 times, 8h and 275 DEG C of calcining 2h of 80 DEG C of dryings obtain zinc doping nickel oxide nanoparticle, then by black powder be dissolved in it is different
Zinc doping nickel oxide precursor liquid is made in propanol solution, 2500rmp spin coatings precursor liquid 1min is in perovskite extinction in glove box
On layer, last gained substrate need to be only placed on spontaneously dries at room temperature, that is, obtains zinc doping nickel oxide nanoparticle hole transport
Layer；
（5）Finally the sample prepared is taken out, with vacuum thermal evaporation plated film instrument successively electrode evaporation decorative layer and metal electrode.
The invention described above, the reaction principle of zinc nitrate and nickel nitrate is in the preparation process of zinc doping nickel oxide nanoparticle
It is such：Zinc nitrate and nickel nitrate hexahydrate basic salt corresponding with alkaline aqueous solution reaction generation precipitate, then through excessive
Temperature calcining obtains nickel oxide nanoparticle.Can be with oxidation under oxygen atmosphere as the zinc oxide of zinc hydroxide calcination reaction generation
Nickel reacts, and the lattice position for having entered nickel is adulterated in Zn-ef ficiency displacement, but since both radiuses are not much different, it is not occurred
Obvious distortion of lattice, finally obtains zinc doping nickel oxide nanoparticle.
Manufactured zinc doping nickel oxide nanoparticle belongs to closs packing face-centered cubic sodium chloride structure, its lattice in the present invention
Constant is a=0.418nm, is formed by the octahedra height aligned transfer accumulation on common side.Macroscopically particle diameter is 30-50nm, and shape is in
Global shape.Compared to the nickel oxide nanoparticle undoped with zinc, its electrical conductivity with higher, thus it is as hole transmission layer
Carrier concentration higher, hole extractability is more preferable, thus battery performance is more preferable.
The zinc doping nickel oxide nanoparticle hole transmission layer of the present invention is just putting perovskite solar cell, including electronics passes
Defeated layer, light absorbing layer, hole transmission layer, electrode modification layer, metal electrode.Zinc nitrate is mixed system with nickel nitrate by the present invention first
Into zinc doping nickel oxide nanoparticle as hole transmission layer, and it is prepared for battery.Cell series resistance is improved, and is obtained
17.7% photoelectric conversion efficiency.Photoactive layer is prepared by spin-coating method, and its thickness is between 250-300nm.Commonly use without electromechanics
Sub- transmission material has TiO2、ZnO、SnO2Deng, Organic Electron Transport Material has PCBM etc., pass through spin-coating method prepare PCBM electronics
Transmission layer thickness is 30nm, the MoO prepared by vacuum vapour deposition3Electrode modification layer thickness is 10nm, passes through vacuum vapour deposition
The Ag thickness of electrode of preparation is 60nm.
Zinc doping nickel oxide nanoparticle hole transmission layer of the present invention is just putting perovskite solar cell, and the present invention uses brand-new
Inorganic hole-transporting layer, high transparency, high conductivity, high work content and calcium titanium are obtained by adulterating zinc optimization nickel oxide nanoparticle
Ore deposit matches good hole extract layer, and efficient perovskite solar cell is obtained by assembling.First by zinc nitrate and nitre
Sour nickel hexahydrate is mixed in alkaline aqueous solution in proportion, and zinc doping nickel oxide nano is obtained by centrifugation, drying and calcination
Particle, is then spun to fluorine-doped tin oxide glass（FTO glass）On, high-performance zinc doping oxygen is obtained by heat drying
Change nickel film, improve film light transmittance and hole extraction efficiency, thereby reduce cell series resistance, optimize cell photoelectric
Transfer efficiency.For the inorganic hole-transporting layer that the present invention obtains compared with traditional hole mobile material, semiconductive thin film has height
Electrical conductivity, high work content, device has the advantages that high efficiency, stiff stability.Its performance optimized and the structure stablized are calcium
The commercial applications of titanium ore solar cell provide new thinking.
The preparation method of the present invention is simple with method, easily operated, is suitable for industrialized production, obtained hole transport
Layer has the advantages that high conductivity, high work content, high efficiency, stiff stability compared with traditional hole mobile material.
Brief description of the drawings
Fig. 1 is the solar battery structure schematic diagram of the present invention,
Fig. 2 is the nickel oxide perovskite solar cell IPCE figures do not mixed zinc and mix zinc,
Fig. 3 is the I-V curve for the nickel oxide hole transmission layer/perovskite solar cell do not mixed zinc and mix zinc.
Wherein 1. FTO, 2. electron transfer layers, 3. light absorbing layers, 4. hole transmission layers, 5. electrode modification layers, 6.Ag electricity
Pole.
Embodiment
Embodiment 1
（1）Prepare the positive horizontalization face heterojunction solar battery structure diagram such as Fig. 1 of tradition.FTO transparent conducting glass is cut into
The strip of 1.6cm, then sticks one centimetre of wide adhesive tape, is then 1 with zinc powder and concentrated hydrochloric acid and water volume ratio:5 dilute hydrochloric acid
Etching 15 minutes, the zinc powder of remnants is cleaned with dilute hydrochloric acid, the glass etched is cut into 1.6 × 1.7cm rectangles, is surpassed with lye
Sound cleans 30-60 min, then is cleaned by ultrasonic 30-60 min with alcohol, is finally cleaned by ultrasonic 10-30 min with deionized water, so
After be put into drying baker drying with spare；
（2）Spin coating concentration is the chlorobenzene solution of the PCBM of 15-20mg/ml in fluorine-doped tin oxide glass in glove box（FTO glass
Glass）Substrate obtains electron transfer layer.
（3）Lead acetate and iodine methylamine are dissolved in n,N-Dimethylformamide solvent, is subsequently placed on magnetic stirring apparatus and stirs
Mix 30 min and obtain perovskite precursor solution.It is then spin coated onto precursor liquid and 100 DEG C of annealing obtains perovskite light-absorption layer in 10 minutes.
A series of processes operate in glove box before this.
（4）Nickelous nitrate hexahydrate is dissolved in alkaline aqueous solution（PH=10）In, 3 times, 80 DEG C of dry 8h are centrifuged by isopropanol
And 275 DEG C of calcining 2h obtain nickel oxide nanoparticle, then by black powder be dissolved in aqueous isopropanol nickel oxide be made
Precursor liquid, on perovskite light-absorption layer, last need to be placed on gained substrate 2500rmp spin coatings precursor liquid 1min in glove box
Spontaneously dry at room temperature, that is, obtain nickel oxide nanoparticle film.MoO is finally deposited successively with vacuum thermal evaporation plated film instrument3Electricity
Pole decorative layer 10nm and Ag electrode 60nm, evaporation rate is 0.5/s.Surveyed photoelectric conversion efficiency such as Fig. 3.
Embodiment 2
The present embodiment is same as Example 1, and difference is that step 2 mixes the hexahydrate of nickel nitrate and zinc nitrate in proportion
Together in alkaline aqueous solution（PH=10）In, wherein zinc nitrate molar ratio is 3%,（The molar ratio of the zinc nitrate and nickel nitrate is 3:
97, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.）Then the 2500rmp spin coatings precursor liquid 1min in glove box
In on perovskite light-absorption layer, last gained substrate need to be only placed on spontaneously dries at room temperature, that is, obtains zinc doping nickel oxide nano
Particle film.
Embodiment 3
The present embodiment is same as Example 2, and difference is that step 2 mixes the hexahydrate of nickel nitrate and zinc nitrate in proportion
Together in alkaline aqueous solution（PH=10）In, wherein zinc nitrate molar ratio is 5%,（The molar ratio of the zinc nitrate and nickel nitrate is 5:
95, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.）Then the 2500rmp spin coatings precursor liquid 1min in glove box
In on perovskite light-absorption layer, last gained substrate need to be only placed on spontaneously dries at room temperature, that is, obtains zinc doping nickel oxide nano
Particle film.
Embodiment 4
The present embodiment is same as Example 3, and difference is that step 2 mixes the hexahydrate of nickel nitrate and zinc nitrate in proportion
Together in alkaline aqueous solution（PH=10）In, wherein zinc nitrate molar ratio is 7%,（The molar ratio of the zinc nitrate and nickel nitrate is 7:
93, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.）Then the 2500rmp spin coatings precursor liquid 1min in glove box
In on perovskite light-absorption layer, last gained substrate need to be only placed on spontaneously dries at room temperature, that is, obtains zinc doping nickel oxide nano
Particle film.
Solar battery structure is made as shown in Figure 1, wherein, wherein 1. FTO, 2. electron transfer layers, 3. light absorbing layers, 4.
Hole transmission layer, 5. electrode modification layers, 6.Ag electrodes.Each layer thickness is respectively 300nm, 30nm, 300nm, 30nm, 10nm,
60nm。
The test result of above-described embodiment 1 and embodiment 2-4 are as follows.
Fig. 2 is the nickel oxide perovskite solar cell IPCE figures do not mixed zinc and mix zinc.
Abscissa is wavelength, and ordinate is external quantum efficiency（It is left）And current density（It is right）.Top curve is to mix the oxygen of zinc
Change the IPCE curves of nickel hole transmission layer/perovskite solar cell, lower curve be do not mix the nickel oxide hole transmission layer of zinc/
The IPCE curves of perovskite solar cell.
Fig. 3 is not mix zinc and mix nickel oxide hole transmission layer/perovskite solar cell of zinc（Embodiment 3）I-V it is bent
Line.
Abscissa is voltage, and ordinate is electric current.Top curve is to mix nickel oxide hole transmission layer/perovskite sun of zinc
The I-V curve of energy battery, lower curve are the I-V curve for the nickel oxide hole transmission layer/perovskite solar cell for not mixing zinc.
Table one summarizes the solar cell items photoelectric parameter that four kinds of embodiments obtain.The battery that wherein embodiment 3 obtains
Best performance, peak efficiency is up to 17.7%.
Finally illustrate personal view, above example is only the preferred embodiments of the present invention, is not intended to limit the invention, in every case
All any modification, equivalent and improvement done within the spirit and principles in the present invention etc., should be included in the guarantor of the present invention
Within the scope of shield.
Table 1
Claims (5)
1. a kind of zinc doping nickel oxide nanoparticle hole transmission layer is just putting perovskite solar cell, it is characterised in that use with
Lower preparation method is made：（1）, using FTO glass as Window layer carry out partial etching；（2）, prepare electron transfer layer；（3）, system
Standby perovskite bulk heterojunction film；（4）, zinc doping nickel oxide nanoparticle hole transmission layer is prepared on calcium titanium ore bed；（5）、
Electrode modification layer is prepared on hole transmission layer；（6）, on electrode modification layer prepare metal electrode, so as to obtain solar-electricity
Pond；
The zinc doping nickel oxide nanoparticle hole transmission layer is made of using following methods：By six water of zinc nitrate and nickel nitrate
Compound is mixed in alkaline aqueous solution in proportion（PH=10）In, 8h and 275 DEG C of 3 times, 80 DEG C of dryings calcining 2h are centrifuged by isopropanol
Obtain zinc doping nickel oxide nanoparticle, then by black powder be dissolved in aqueous isopropanol zinc doping nickel oxide be made before
Liquid is driven, then 2500rmp spin coatings precursor liquid 1min is in fluorine-doped tin oxide glass（FTO glass）Substrate, last need to be gained
Substrate is placed on to be spontaneously dried at room temperature, that is, obtains zinc doping nickel oxide nanoparticle hole transmission layer.
2. perovskite solar cell according to claim 1, it is characterised in that：Mole of the zinc nitrate and nickel nitrate
Than for 3-7:97-93, zinc nitrate are 1M in the concentration of in the mixed solvent with nickel nitrate.
3. perovskite solar cell according to claim 1, it is characterised in that：The thickness of the FTO glass is
300nm；The thickness of zinc doping nickel oxide hole transmission layer is 30nm；The thickness of perovskite bulk heterojunction film is 300nm；Electronics
The thickness of transport layer is 30nm；The thickness of electrode modification layer is 10nm；The thickness of metal electrode is 60nm.
4. according to claim 1 just putting perovskite solar cell, it is characterised in that：The zinc doping nickel oxide nano
The particle diameter of particle is 30-50nm.
5. the zinc doping nickel oxide nanoparticle hole transmission layer described in a kind of claim 1 is just putting perovskite solar cell
Preparation method, it is characterised in that using following steps：
（1）FTO transparent conducting glass is cut into the strip of 1.6cm, then sticks the adhesive tape of 1cm wide, then with zinc powder and dense salt
Acid is 1 with water volume ratio:5 dilute hydrochloric acid etches 15 minutes, and the zinc powder of remnants is cleaned with dilute hydrochloric acid, the glass etched is cut into
1.6 × 1.7cm rectangles, with lye be cleaned by ultrasonic 30-60 min, then with alcohol be cleaned by ultrasonic 30-60 min, finally spend from
Sub- water is cleaned by ultrasonic 10-30 min, is put into drying baker drying with spare；
（2）Spin coating concentration is the chlorobenzene solution of the PCBM of 15-20mg/ml in fluorine-doped tin oxide glass in glove box（FTO glass
Glass）Substrate obtains electron transfer layer；
（3）Lead acetate and iodine methylamine are dissolved in n,N-Dimethylformamide solvent, is subsequently placed on magnetic stirring apparatus and stirs 30
Min obtains perovskite precursor solution, is then spin coated onto precursor liquid on electron transfer layer and 100 DEG C of annealing obtain calcium titanium in 10 minutes
Ore deposit light-absorption layer；
（4）Zinc nitrate and nickel nitrate hexahydrate are mixed in alkaline aqueous solution in proportion（PH=10）In, centrifuged by isopropanol
3 times, 8h and 275 DEG C of calcining 2h of 80 DEG C of dryings obtain zinc doping nickel oxide nanoparticle, then by black powder be dissolved in it is different
Zinc doping nickel oxide precursor liquid is made in propanol solution, 2500rmp spin coatings precursor liquid 1min is in perovskite extinction in glove box
On layer, last gained substrate need to be only placed on spontaneously dries at room temperature, that is, obtains zinc doping nickel oxide nanoparticle hole transport
Layer；
（5）Finally the sample prepared is taken out, with vacuum thermal evaporation plated film instrument successively electrode evaporation decorative layer and metal electrode.
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| CN201711204673.9A CN107994122A (en) | 2017-11-27 | 2017-11-27 | Zinc doping nickel oxide nanoparticle hole transmission layer is just putting perovskite solar cell and preparation method |
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| CN108574046A (en) * | 2018-05-24 | 2018-09-25 | 中节能万润股份有限公司 | A kind of perovskite solar cell and preparation method thereof |
| CN109950399A (en) * | 2019-03-11 | 2019-06-28 | 湖北大学 | A kind of preparation method of hole transmission layer and trans- perovskite solar battery |
| CN111864082A (en) * | 2020-06-09 | 2020-10-30 | 北京化工大学 | Positive structure perovskite solar cell adopting doped nickel oxide as hole transport layer and preparation method thereof |
| CN112151679A (en) * | 2020-09-29 | 2020-12-29 | 西北工业大学 | Nano-crystal composite perovskite solar cell and preparation method thereof |
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| CN108574046A (en) * | 2018-05-24 | 2018-09-25 | 中节能万润股份有限公司 | A kind of perovskite solar cell and preparation method thereof |
| CN109950399A (en) * | 2019-03-11 | 2019-06-28 | 湖北大学 | A kind of preparation method of hole transmission layer and trans- perovskite solar battery |
| CN111864082A (en) * | 2020-06-09 | 2020-10-30 | 北京化工大学 | Positive structure perovskite solar cell adopting doped nickel oxide as hole transport layer and preparation method thereof |
| CN112151679A (en) * | 2020-09-29 | 2020-12-29 | 西北工业大学 | Nano-crystal composite perovskite solar cell and preparation method thereof |
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