CN107634143A - The composite absorbed layer and its preparation method of a kind of perovskite battery - Google Patents

The composite absorbed layer and its preparation method of a kind of perovskite battery Download PDF

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Publication number
CN107634143A
CN107634143A CN201710872143.5A CN201710872143A CN107634143A CN 107634143 A CN107634143 A CN 107634143A CN 201710872143 A CN201710872143 A CN 201710872143A CN 107634143 A CN107634143 A CN 107634143A
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absorbed layer
composite
nanogold
lead
pbx
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CN107634143B (en
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赵晓冲
杨盼
杨丽军
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Institute of Materials of CAEP
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Abstract

The invention discloses a kind of composite absorbed layer of perovskite battery, solves and uses absorbed layer of the metal organic halide materials as perovskite battery in the prior art, not high to the absorption intensity of sunshine, the problem of absorption spectrum narrower width.The composite absorbed layer of the present invention is the film in core shell structure being coated in substrate；Including nanogold particle and the CH being wrapped in outside the nanogold particle3NH3PbX3Material, wherein the mol ratio of gold and lead is 1:5‑1:100, the X are halogen.Preparation method of the present invention comprises the following steps：Nano-Au solution is prepared, then adds lead halide and methylamine thereto, obtains nanogold/CH3NH3PbX3The precursor solution of composite, is coated in substrate, dries, produces.The Au/CH of the present invention3NH3PbX3The uniformity of composite absorbed layer electrode is good, absorbance is strong, and electricity conversion is high.

Description

The composite absorbed layer and its preparation method of a kind of perovskite battery
Technical field
The present invention relates to cell art, and in particular to the composite absorbed layer and its system of a kind of perovskite battery Method.
Background technology
By its high carrier mobility, low preparation cost, high solid-state stability, overlength electron-hole diffusion length etc. Advantage, perovskite battery metal organohalogen compounds (CH3NH3PbX3) material can effectively improve the transformation efficiency of battery, thus into For the focus of research.
But absorbed layer of the metal organic halide materials as perovskite battery is used, the absorption existed to sunshine is strong Degree is not high, the problem of absorption spectrum narrower width, so as to influence the optoelectronic transformation efficiency of battery.Therefore it provides a kind of be used for calcium titanium The material of ore deposit battery obsorbing layer, the absorption intensity to sunshine can be improved, absorption spectrum width be extended, to improve the photoelectricity of battery Conversion ratio, become those skilled in the art's urgent problem to be solved.
The content of the invention
An object of the present invention is to provide a kind of composite absorbed layer of perovskite battery, to solve prior art It is middle using absorbed layer of the metal organic halide materials as perovskite battery, it is not high to the absorption intensity of sunshine, absorb ripple The problem of spectral width is narrower.
The second object of the present invention is to provide a kind of preparation method of the composite absorbed layer of perovskite battery.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of composite absorbed layer of perovskite battery of the present invention, the composite absorbed layer are to be coated on base The film in core shell structure on bottom；Including nanogold particle and the CH being wrapped in outside the nanogold particle3NH3PbX3Material Material, wherein the mol ratio of gold and lead is 1:5-1:100, the X are halogen.
Preferably, the mol ratio of the gold and lead is 1:5-1:20.
Preferably, the mol ratio of the gold and lead is 1:10.
The preparation method of composite absorbed layer of the present invention, comprises the following steps：
Step 1：Prepare nano-Au solution：Using gold chloride as raw material, using nitrogen azoles polyethylene glycol as part, NaBH is utilized4 As reducing agent, using organic solvent as solvent, nanogold organic solution is obtained；
Step 2：Prepare the precursor solution of composite：A certain amount of lead halogen is added into the nanogold organic solution Compound and methylamine, stir, the nanogold/CH being uniformly mixed3NH3PbX3The precursor solution of composite；
Step 3：Coating, dry：The precursor solution is coated on transparent conducting glass, then at 30-120 DEG C of condition Lower dry 1-15h, nanogold are combined as a whole by part and perovskite material, obtain the nanogold of core shell structure/ CH3NH3PbX3Composite absorbed layer.
Preferably, in the step 1, the mol ratio of the gold chloride and nitrogen azoles polyethylene glycol part is 1:5, the chlorine Auric acid and NaBH4Mol ratio be 1:10, the organic solvent is methanol, ethanol, isopropanol, the tert-butyl alcohol, chloroform, ethene two Alcohol, dimethyl acetamide, dimethyl sulfoxide, benzyl ether, 1-METHYLPYRROLIDONE, N- ethyl pyrrolidones, N, N- dimethyl formyls Any one or more in amine, the organic solution counts its concentration as 0.1% using gold chloride.
Preferably, the lead halide in the step 2 is one or two kinds of in lead iodide, lead bromide.
Preferably, in the step 3, precursor solution is entered by the way of vacuum, nitrogen or argon atmosphere Row drying.
Compared with prior art, the invention has the advantages that：
The Au/CH of the present invention3NH3PbX3The uniformity of composite absorbed layer electrode is good, absorbance is strong, photoelectric conversion effect Rate is high.
Nanogold is incorporated into CH by the present invention3NH3PbX3Synthesis Au/CH is prepared in system3NH3PbX3Core shell structure composite wood Expect extinction body, using the surface plasmon resonance effect of nanogold, absorb the sun that will do not absorbed by metal organohalogen compounds Light, absorbed for metal organohalogen compounds, absorption intensity and its spectral bandwidth of extension to sunshine are improved, so as to improve battery Optoelectronic transformation efficiency.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive Feature and/or step beyond, can combine in any way.Any feature disclosed in this specification, except non-specifically chatting State, can alternative features equivalent by other or with similar purpose replaced.I.e., unless specifically stated otherwise, each feature It is an example in a series of equivalent or similar characteristics.
A kind of composite absorbed layer of perovskite battery of the present invention, the composite absorbed layer are to be coated on base The film in core shell structure on bottom；Including nanogold particle and the CH being wrapped in outside the nanogold particle3NH3PbX3Material Material, wherein the mol ratio of gold and lead is 1:5-1:100, the X are halogen.
Preferably, the mol ratio of the gold and lead is 1:5-1:20.
Preferably, the mol ratio of the gold and lead is 1:10.
A kind of composite absorbed layer of perovskite battery of the present invention, the composite absorbed layer are to be coated on base The film in core shell structure on bottom；Including nanogold particle and the CH being wrapped in outside the nanogold particle3NH3PbX3Material Material, wherein the mol ratio of gold and lead is 1:5-1:100, the X are halogen.
Preferably, the mol ratio of the gold and lead is 1:5-1:20.
Preferably, the mol ratio of the gold and lead is 1:10.
The preparation method of composite absorbed layer of the present invention, comprises the following steps：
Step 1：Prepare nano-Au solution：Using gold chloride as raw material, using nitrogen azoles polyethylene glycol as part, NaBH is utilized4 As reducing agent, using organic solvent as solvent, nanogold organic solution is obtained；
Step 2：Prepare the precursor solution of composite：A certain amount of lead halogen is added into the nanogold organic solution Compound and methylamine, stir, the nanogold/CH being uniformly mixed3NH3PbX3The precursor solution of composite；
Step 3：Coating, dry：The precursor solution is coated on transparent conducting glass, then at 30-120 DEG C of condition Lower dry 1-15h, nanogold are combined as a whole by part and perovskite material, obtain the nanogold of core shell structure/ CH3NH3PbX3Composite absorbed layer.
Preferably, in the step 1, the mol ratio of the gold chloride and nitrogen azoles polyethylene glycol part is 1:5, the chlorine Auric acid and NaBH4 mol ratio are 1:10, the organic solvent is methanol, ethanol, isopropanol, the tert-butyl alcohol, chloroform, ethene two Alcohol, dimethyl acetamide, dimethyl sulfoxide, benzyl ether, 1-METHYLPYRROLIDONE, N- ethyl pyrrolidones, N, N- dimethyl formyls Any one or more in amine, the concentration (in terms of gold chloride) of the organic solution is 0.1%.
Preferably, the lead halide in the step 2 is one or two kinds of in lead iodide, lead bromide.
Preferably, in the step 3, precursor solution is entered by the way of vacuum, nitrogen or argon atmosphere Row drying.
Embodiment 1
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer, specifically include following step Suddenly：
Step 1：Prepare nano-Au solution：With gold chloride (HAuCl4) it is raw material, using nitrogen azoles polyethylene glycol as part, profit Use NaBH4As reducing agent, using ethanol as solvent, nanogold organic solution is obtained；Wherein gold chloride is matched somebody with somebody with nitrogen azoles polyethylene glycol The mol ratio of body is 1:5, gold chloride and NaBH4Mol ratio be 1:10, the concentration of organic solution is (in terms of gold chloride) 0.1%；
Step 2：Prepare the precursor solution of composite：According to Jin Heqian mol ratio 1：10 ratio, to nanogold Lead halide and methylamine are added in organic solution, stirs, obtains nanogold/CH3NH3PbX3The presoma of composite is molten Liquid；Wherein lead halide is PbCl2With PbBr2, mol ratio PbCl2：PbBr2For 1:0.2；
Step 3：Dry：Compacted zone TiOx is prepared in the FTO spin-on-glass cleaned up, then in TiOx layer surface spin coatings Precursor solution obtained by step 2,5h is dried under 70 DEG C of temperature argon gas atmosphere, obtain the nanogold of core shell structure/ CH3NH3PbX3Composite absorbed layer.
The present embodiment additionally provides nanogold/CH using core shell structure3NH3PbX3The calcium titanium electricity of composite absorbed layer The preparation method in pond, it is specially：
In nanogold/CH3NH3PbX3Composite absorbs layer surface one layer of spiro-OMeTAD hole transmission layer of spin coating, then One layer of gold electrode of vacuum evaporation, is produced on hole transmission layer.
Embodiment 2
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, the organic solvent in step 1 is methanol to the present embodiment, Gold and lead mol ratio are 1 in step 2:100, PbCl2With PbBr2Mol ratio is 1:0, remaining each condition all same.
Embodiment 3
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, the organic solvent in step 1 is tertiary fourth to the present embodiment Alcohol, gold and lead mol ratio are 1 in step 2:5, PbCl2With PbBr2Mol ratio is 1:1, remaining each condition all same.
Embodiment 4
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, the organic solvent in step 1 is N, N- to the present embodiment Dimethylformamide, remaining each condition all same.
Embodiment 5
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, the organic solvent in step 1 is N- first to the present embodiment Base pyrrolidones, gold and lead mol ratio are 1 in step 2:20, remaining each condition all same.
Embodiment 6
The present embodiment is comparative example.
Present embodiments provide CH3NH3PbX3Composite absorbed layer and the perovskite electricity using the composite absorbed layer The preparation method in pond, specifically includes following steps：
Step 1：Lead halide and methylamine are dissolved in ethanol, stirred, obtain CH3NH3PbX3The presoma of material Solution；The amount of wherein lead halide, methylamine and ethanol is same as Example 1；
Step 2：With the step 3 in embodiment 1.
Embodiment 7
The present embodiment is comparative example.
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, gold and lead mol ratio are 1 to the present embodiment in step 2: 200, remaining each condition all same.
Embodiment 8
The present embodiment is comparative example.
Present embodiments provide Nano Silver/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, the gold chloride in step 1 is replaced with for the present embodiment Silver nitrate, presoma is used as using the ethanol solution of silver nitrate in step 2, the mol ratio of silver and lead is 1:20, remaining each condition All same.
Embodiment 9
Perovskite battery made from embodiment 1-8 is measured to the photoelectric properties of the battery under a standard sunshine, tied Fruit is as shown in table 1 below.
The heterogeneity composite absorbed layer electrode battery performance of table 1
As it can be seen from table 1 changing the composition of presoma, the battery performance of composite can be directly affected.Particularly receive When the golden ratio of rice is suitable, nanogold/CH of prepared core shell structure3NH3PbX3The performance of composite absorbed layer has 20% Improve.
Embodiment 10
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 30 DEG C to the present embodiment in step 3 Temperature nitrogen atmosphere under dry 1h, remaining each condition all same.
Embodiment 11
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 120 DEG C to the present embodiment in step 3 Temperature argon gas atmosphere under dry 15h, remaining each condition all same.
Embodiment 12
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 70 DEG C to the present embodiment in step 3 Temperature argon gas atmosphere under dry 8h, remaining each condition all same.
Embodiment 13
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 70 DEG C to the present embodiment in step 3 Temperature Vacuum under dry 8h, remaining each condition all same.
Embodiment 14
The present embodiment is comparative example.
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 30 DEG C to the present embodiment in step 3 Temperature argon gas atmosphere under dry 0.5h, remaining each condition all same.
Embodiment 15
The present embodiment is comparative example.
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 120 DEG C to the present embodiment in step 3 Temperature argon gas atmosphere under dry 0.5h, remaining each condition all same.
Embodiment 16
The present embodiment is comparative example.
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 20 DEG C to the present embodiment in step 3 Temperature argon gas atmosphere under dry 15h, remaining each condition all same.
Embodiment 17
The present embodiment is comparative example.
Present embodiments provide nanogold/CH of core shell structure3NH3PbX3Composite absorbed layer and use the composite wood Expect the preparation method of the perovskite battery of absorbed layer.Compared with Example 1, drying condition is in 150 DEG C to the present embodiment in step 3 Temperature argon gas atmosphere under dry 1h, remaining each condition all same.
Embodiment 18
Perovskite battery made from embodiment 1, embodiment 10-17 is measured into the battery under a standard sunshine Photoelectric properties, it is as a result as shown in table 2 below.
Combination electrode battery performance obtained by 2 different drying conditions of table
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in, It should all be included within the scope of the present invention.The present invention expands to any new feature disclosed in this manual or any New combination, and disclose any new method or process the step of or any new combination.

Claims (7)

1. a kind of composite absorbed layer of perovskite battery, it is characterised in that the composite absorbed layer is to be coated on base The film in core shell structure on bottom；Including nanogold particle and the CH being wrapped in outside the nanogold particle3NH3PbX3Material Material, wherein the mol ratio of gold and lead is 1:5-1:100, the X are halogen.
2. the composite absorbed layer of a kind of perovskite battery according to claim 1, it is characterised in that the gold and lead Mol ratio be 1:5-1:20.
3. the composite absorbed layer of a kind of perovskite battery according to claim 1, it is characterised in that the gold and lead Mol ratio be 1:10.
4. the preparation method of the composite absorbed layer according to claim 1-3 any one, it is characterised in that including following step Suddenly：
Step 1：Prepare nano-Au solution：Using gold chloride as raw material, using nitrogen azoles polyethylene glycol as part, NaBH is utilized4As also Former agent, using organic solvent as solvent, obtain nanogold organic solution；
Step 2：Prepare the precursor solution of composite：A certain amount of lead halide is added into the nanogold organic solution And methylamine, stir, the nanogold/CH being uniformly mixed3NH3PbX3The precursor solution of composite；
Step 3：Coating, dry：The precursor solution is coated on transparent conducting glass, done under the conditions of 30-120 DEG C Dry 1-15h, nanogold are combined as a whole by part and perovskite material, obtain nanogold/CH of core shell structure3NH3PbX3It is multiple Condensation material absorbed layer.
5. preparation method according to claim 4, it is characterised in that in the step 1, the gold chloride and nitrogen azoles polyethylene glycol The mol ratio of part is 1:5, the gold chloride and NaBH4Mol ratio be 1:10, the organic solvent is methanol, ethanol, different Propyl alcohol, the tert-butyl alcohol, chloroform, ethylene glycol, dimethyl acetamide, dimethyl sulfoxide, benzyl ether, 1-METHYLPYRROLIDONE, N- ethyls Any one or more in pyrrolidones, DMF, the organic solution its concentration in terms of gold chloride is 0.1%.
6. preparation method according to claim 5, it is characterised in that：Lead halide in the step 2 is lead iodide, lead bromide In it is one or two kinds of.
7. preparation method according to claim 6, it is characterised in that in the step 3, to precursor solution using vacuum, nitrogen The mode of gas or argon atmosphere is dried.
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CN105489769A (en) * 2016-01-07 2016-04-13 苏州大学 Preparation method of cathode and anode-modified perovskite solar cell
CN105609588A (en) * 2016-01-22 2016-05-25 南京理工大学 Au nanoparticle-enhanced high-performance inorganic perovskite CsPbX<3> nanocrystalline visible-light detector
CN105870328A (en) * 2016-04-08 2016-08-17 天津市职业大学 Preparation method for stable perovskite solar cell light absorption layer

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103904218A (en) * 2014-03-28 2014-07-02 中国科学院上海技术物理研究所 Perovskite thin-film solar cell structure based on metal particles
CN104465992A (en) * 2014-11-30 2015-03-25 浙江大学 Perovskite planar heterojunction solar battery based on self-assembled monolayer
CN105226187A (en) * 2015-11-15 2016-01-06 河北工业大学 Film crystal silicon perovskite heterojunction solar cell and preparation method thereof
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CN105870328A (en) * 2016-04-08 2016-08-17 天津市职业大学 Preparation method for stable perovskite solar cell light absorption layer

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