CN109110824A - Nano-nickel oxide and preparation for perovskite solar battery hole mobile material - Google Patents
Nano-nickel oxide and preparation for perovskite solar battery hole mobile material Download PDFInfo
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- CN109110824A CN109110824A CN201810919869.4A CN201810919869A CN109110824A CN 109110824 A CN109110824 A CN 109110824A CN 201810919869 A CN201810919869 A CN 201810919869A CN 109110824 A CN109110824 A CN 109110824A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
Nano-nickel oxide and preparation for perovskite solar battery hole mobile material, are related to the preparation of nano material.Nano-nickel oxide is graininess nano-nickel oxide, and crystal grain diameter is 10~20nm, there is the preferred orientation of (111) crystal orientation.Metallic nickel target and baffle are loaded onto magnetic control sputtering device cathode, substrate is placed in magnetic control sputtering device cavity on base station, closes cavity, starts magnetic control sputtering device vacuum pump, initial gas pressure is down in air pressure in cavity；It allows base station to rotate, O is passed through into cavity2With the mixed gas of Ar, make 6~10mTorr of total gas pressure in cavity, controls O2Pressure accounts for the 50%~100% of total gas pressure；Magnetron sputtering power supply is opened, sputtering general power is risen into 60~100W, baffle is opened after pre-sputtering, 30~120min is sputtered, obtains the nano-nickel oxide for perovskite solar battery hole mobile material.
Description
Technical field
The present invention relates to the preparation of nano material, more particularly, to perovskite solar battery hole mobile material is received
Rice nickel oxide and preparation.
Background technique
Perovskite solar battery is a kind of emerging high efficiency solar cell, it is the calcium by hybrid inorganic-organic
What titanium ore crystal form light absorbent, hole and electron transporting materials and electrode material were constituted.Compared to traditional silica-based solar
Battery, perovskite solar battery have the advantages that manufacture craft is simple, low cost, can make flexible device, and short
In several years, efficiency of the silicon solar cell between decades is broken through efficiency progress shoulder to shoulder, and the photoelectricity that authenticates at present turns
It changes efficiency and reaches 22.1%, therefore be widely regarded as the solar battery of the following great potential.
The rapid development of perovskite solar battery, to the transmission material in its hole and electronics, more stringent requirements are proposed,
The hole mobile material that wherein carrier transport is high-efficient, stability is good, inexpensive, environmental-friendly is present and following research
Emphasis.
A large amount of efficient perovskite solar batteries are still using expensive organic material as carrier at present
Transmission material.Poly- (3,4- ethene dioxythiophene)-polystyrolsulfon acid (PEDOT:PSS) is due to its good hole transport performance
It is widely used always.At present home and abroad studies have shown that the hygroscopicity of PEDOT:PSS itself can dramatically speed up perovskite suction
The decomposition of photosphere seriously endangers the stability during battery, hinders the marketing development of perovskite solar battery.In order to solve
The problem of stability, people also seek in exploration other than carrying out Improvement to encapsulation technology and perovskite light absorbent itself
Look for other chemical stabilization, cheap hole mobile material, such as NiO, CuO, MoO3Equal metal oxides.They not only have
There is the ability of transporting holes, and resourceful, chemical stabilization, price is low, is considered as potential alternative materials.Wherein nickel oxide
For being used as hole mobile material in perovskite solar battery, the effect obtained at present is best.
Nano-nickel oxide has different morphologies, such as nano wire, nano-powder, nanometer sheet and nanometer rods, preparation method
Mainly there are spray pyrolysis, hydrothermal synthesis method, pulsed laser deposition and magnetron sputtering etc., wherein spray pyrolysis, hydrothermal synthesis
Equal liquid-phase synthesis process include the process of calcination process at a high temperature of several hundred degrees Celsius.
The patent document of Publication No. CN201310326357.4 discloses a kind of preparation method of nano-nickel oxide, including
Following steps: it using Nickel dichloride hexahydrate and choline chloride base depth congruent melting solvent as raw material, after 120~150 DEG C of hybrid reactions, sinks
Starch is after washing, drying again through 250~400 DEG C of 2~5h of calcining.
Such as the technique of this high-temperature process provided in above-mentioned document is not suitable for the extensive and flexible perovskite sun
The production of energy battery.And magnetron sputtering, since deposition rate is fast, the ingredient ratio of easily controllable nickel oxide, industrial production is at low cost,
And can carry out at room temperature, it is current most popular method.The nickel oxide property of magnetron sputtering is by substrate temperature, sputtering
The influence of the factors such as atmosphere, pressure, power, the chemical constituent of the nickel oxide material obtained under different process, translucency and
The properties such as cavity transmission ability are all made a world of difference, therefore explore a kind of simple and stable, meet efficient perovskite solar-electricity
The nickel oxide magnetron sputtering preparation method of pond application requirement has far-reaching application value.
Summary of the invention
The purpose of the present invention is to provide metallic nickel target is used, nanometer is prepared in reactive sputtering under pure oxygen atmosphere
The nickel oxide of sheet, it is time-consuming it is short, production cost is low, substrate does not need heating, be suitble to large-scale industrial production for calcium titanium
The nano-nickel oxide and preparation method thereof of mine solar battery hole mobile material.
The nano-nickel oxide for perovskite solar battery hole mobile material is graininess nano-nickel oxide,
Crystal grain diameter is 10~20nm, there is the preferred orientation of (111) crystal orientation.
The preparation method of the nano-nickel oxide for perovskite solar battery hole mobile material includes following step
It is rapid:
1) metallic nickel target and baffle are loaded onto magnetic control sputtering device cathode, substrate is placed on base station in magnetic control sputtering device cavity
On, cavity is closed, starts magnetic control sputtering device vacuum pump, initial gas pressure is down in air pressure in cavity；
2) it allows base station to rotate, O is passed through into cavity2With the mixed gas of Ar, make 6~10mTorr of total gas pressure in cavity,
Control O2Pressure accounts for the 50%~100% of total gas pressure；
3) magnetron sputtering power supply is opened, sputtering general power is risen into 60~100W, baffle, sputtering 30 are opened after pre-sputtering
~120min obtains the nano-nickel oxide for perovskite solar battery hole mobile material.
In step 1), the purity of the nickel target can be banged in magnetron sputtering process for 99.9% metallic nickel target
Hit the Ni ion come or atom and the intracorporal O ion of chamber or O2Molecule reaction generates nickel oxide, is passed through O by control2Flow
The ingredient ratio for generating nickel oxide is just adjustable with bias, thus the property of nickel oxide has controllability；During the preparation process if you need to
High-temperature process, perovskite solar cell substrates flexible cannot be applicable in, preferably, the substrate is heated,
Easy process simultaneously saves the energy；Described that air pressure in cavity is down to initial gas pressure as E-6torr, low vacuum degree means cavity
Interior impurity molecule is less.
In step 2), the O2Pressure can account for the 90%~100% of total gas pressure, oxygen present in nickel oxide material is filled out
The defect with nickel vacancy is filled, natural p-type semiconductor property is made it have, is passed through O2Amount can be reduced to less nickel oxide oxygen lack
Density is fallen into, its hole transporting property is unfavorable for；The speed of the base station rotation can be 15 °/s, and substrate is conducive to base station rotation
The uniformity of nickel oxide deposition, but too fast rotation speed may then be such that substrate moves in rotary course.
In step 3), the sputtering general power can be 80~100W, and sputtering power is higher, and the deposition rate of nickel oxide is got over
Fastly, in higher O2Under bias, the fine tuning of deposition rate influences less nickel oxide property, and too low deposition rate needs longer
Working time, increase the loss of equipment；The sputtering time can be 30~60min, preferably 10~15min, pre-sputtering process
The impurity that target material surface can be bombarded improves the quality of nickel oxide material；The shielding power supply can be radio frequency (RF) power supply,
Under radio-frequency power supply, the rate that Ni atom or ion are shelled out is lower, is conducive to and O ion or O2Molecule reaction production oxidation
Nickel.
Compared with prior art, the invention has the following outstanding advantages:
The present invention uses the target of metallic nickel, with O2Reaction magnetocontrol sputtering is carried out, is not related to liquid, raw materials of compound, makes
All raw materials are nontoxic and pollution-free, therefore entire preparation engineering is controllable and environmentally protective；Whole process of the present invention is in room temperature
Lower progress is not related to the complex steps such as heating, and the requirement to equipment is low, and time-consuming short, energy consumption is few, and capital investment is few, is suitble to big rule
The industrialized production of mould；The nickel oxide crystal for the Nanoparticulate that the present invention obtains has the preferred orientation of (111) crystal orientation, partial size
In 10~15nm, particle diameter distribution is uniform；Using the nano-nickel oxide that the present invention is prepared as the perovskite of hole mobile material
Solar battery, short circuit current reach 21.5mA/cm2, there is the photoelectric conversion efficiency close to 17%.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of the embodiment of the present invention 1.
Fig. 2 is test result of the embodiment of the present invention.
Specific embodiment
Following embodiment will the present invention is further illustrated in conjunction with attached drawing.
Embodiment 1
Metallic nickel target and baffle are loaded onto magnetic control sputtering device cathode, clean substrate is placed on base in magnetic control sputtering device cavity
On platform, cavity is closed, starts magnetic control sputtering device vacuum pump, is down to low initial gas pressure (being less than E-6Torr) to air pressure in cavity
Later, setting allows base station with 15 °/s rotation, and pure O is passed through into cavity2(O in cavity2Pressure account for the 100% of total gas pressure), always
Air pressure is shown as 9mTorr, opens magnetron sputtering radio-frequency power supply, power is risen to 80W, baffle is opened after pre-sputtering 10min, splashes
1h is penetrated to get the nano-nickel oxide arrived for perovskite solar battery hole mobile material.
For its electron scanning micrograph as shown in Figure 1, as can be seen from Figure, the grain size of NiO is 10~15nm,
There is the nickel oxide crystal preferential growth of (111) crystal orientation to be orientated.
Embodiment 2
Metallic nickel target and baffle are loaded onto magnetic control sputtering device cathode, clean substrate is placed on base in magnetic control sputtering device cavity
On platform, cavity is closed, starts magnetic control sputtering device vacuum pump, is down to low initial gas pressure (being less than E-6Torr) to air pressure in cavity
Later, setting allows base station with 15 °/s rotation, and O is passed through into cavity2And Ar, total gas pressure are shown as 10mTorr, O2Bias be
9mTorr (accounts for total gas pressure 90%), opens magnetron sputtering radio-frequency power supply, and power is risen to 80W, opens gear after pre-sputtering 10min
Plate sputters 1h to get nano-nickel oxide, and particle size is 8~15nm.
Embodiment 3
Metallic nickel target and baffle are loaded onto magnetic control sputtering device cathode, clean substrate is placed on base in magnetic control sputtering device cavity
On platform, cavity is closed, starts magnetic control sputtering device vacuum pump, is down to low initial gas pressure (being less than E-6Torr) to air pressure in cavity
Later, setting allows base station with 15 °/s rotation, and O is passed through into cavity2And Ar, total gas pressure are shown as 10mTorr, O2Bias be
9mTorr (accounts for total gas pressure 90%), opens magnetron sputtering radio-frequency power supply, and power is risen to 100W, opens gear after pre-sputtering 10min
Plate sputters 0.5h to get nano-nickel oxide, and particle size is 10~18nm.
Performance test of the invention is given below.
Perovskite solar battery, preparation side are prepared using the nano-nickel oxide that embodiment 1 obtains as hole mobile material
Method is as follows: FTO electro-conductive glass successively uses deionized water, acetone, dehydrated alcohol ultrasonic cleaning, and magnetic control sputtering device base is placed on after drying
On platform, nano-nickel oxide hole transmission layer is prepared on FTO substrate with the preparation method of embodiment 1；It is being covered with nanometer
On the FTO substrate of nickel oxide, the successive spin coating PbI of the method for spin coating is used2Dimethylformamide (DMF) solution and methylpyridinium iodide
Amine (CH3NH3I aqueous isopropanol) is placed in 150 DEG C of thermal station and heats 0.5h, and reaction obtains CH3NH3PBI3Calcium titanium ore bed；?
Successively the toluene solution of spin coating PCBM and the aqueous isopropanol of BCP obtain electron transfer layer on calcium titanium ore bed；Substrate is put into very
Ag electrode is plated in empty thermal evaporation system to get complete perovskite solar battery is arrived.
Battery is connected into 2400 source table of Keithley, in the AM1.5 of simulation, 1kW/m2Sunlight irradiation under test its J-V
Curve, test scope is from -0.2V to 1.1V.Test results are shown in figure 2, and short circuit current reaches 21.5mA/cm2, photoelectric conversion effect
Rate is close to 17%.
Present invention process is simple, does not need heating substrate, is suitble to large-scale industrial production；The nano oxidized Nickel particle of preparation
Diameter is less than 10nm, has higher short circuit current using it as the perovskite solar battery of hole mobile material preparation, efficiency is close
17%.
Claims (9)
1. being used for the nano-nickel oxide of perovskite solar battery hole mobile material, it is characterised in that it is graininess nano oxygen
Change nickel, crystal grain diameter is 10~20nm, there is the preferred orientation of (111) crystal orientation.
2. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as described in claim 1,
Characterized by the following steps:
1) metallic nickel target and baffle are loaded onto magnetic control sputtering device cathode, substrate is placed in magnetic control sputtering device cavity on base station, closed
Closed chamber body starts magnetic control sputtering device vacuum pump, initial gas pressure is down in air pressure in cavity；
2) it allows base station to rotate, O is passed through into cavity2With the mixed gas of Ar, make 6~10mTorr of total gas pressure in cavity, controls
O2Pressure accounts for the 50%~100% of total gas pressure；
3) magnetron sputtering power supply is opened, sputtering general power is risen into 60~100W, opens baffle after pre-sputtering, sputtering 30~
120min obtains the nano-nickel oxide for perovskite solar battery hole mobile material.
3. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 2,
It is characterized in that in step 1), metallic nickel target that the purity of the nickel target is 99.9%.
4. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 2,
It is characterized in that in step 1), it is described that air pressure in cavity is down to initial gas pressure as E-6torr.
5. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 2,
It is characterized in that in step 2), the O2Pressure account for the 90%~100% of total gas pressure.
6. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 2,
It is characterized in that the speed of the base station rotation is 15 °/s in step 2).
7. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 2,
It is characterized in that the sputtering general power is 80~100W in step 3), sputtering time is 30~60min.
8. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 7,
It is characterized in that the sputtering time is 10~15min.
9. the preparation method for the nano-nickel oxide of perovskite solar battery hole mobile material as claimed in claim 2,
It is characterized in that the shielding power supply is radio-frequency power supply in step 3).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715958A (en) * | 2022-03-08 | 2022-07-08 | 华能新能源股份有限公司 | Spray pyrolysis method of nickel oxide and perovskite solar cell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08129721A (en) * | 1994-09-08 | 1996-05-21 | Sumitomo Metal Ind Ltd | Production of nio antiferromagnetic film, production of magnetoresistance effect element and its element |
| US20110108116A1 (en) * | 2009-11-11 | 2011-05-12 | Korea Institute Of Machinery And Materials | P-type NiO conducting film for organic solar cell, a method for preparation of NiO conducting film, and an organic solar cell with enhanced light-to-electric energy conversion using the same |
| CN104507870A (en) * | 2012-08-01 | 2015-04-08 | 独立行政法人产业技术综合研究所 | Joined structure comprising cube-or quadratic prism-shaped rock salt-type oxide nanoparticle with fine metal particle, and method for producing same |
-
2018
- 2018-08-14 CN CN201810919869.4A patent/CN109110824A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08129721A (en) * | 1994-09-08 | 1996-05-21 | Sumitomo Metal Ind Ltd | Production of nio antiferromagnetic film, production of magnetoresistance effect element and its element |
| US20110108116A1 (en) * | 2009-11-11 | 2011-05-12 | Korea Institute Of Machinery And Materials | P-type NiO conducting film for organic solar cell, a method for preparation of NiO conducting film, and an organic solar cell with enhanced light-to-electric energy conversion using the same |
| CN104507870A (en) * | 2012-08-01 | 2015-04-08 | 独立行政法人产业技术综合研究所 | Joined structure comprising cube-or quadratic prism-shaped rock salt-type oxide nanoparticle with fine metal particle, and method for producing same |
Non-Patent Citations (1)
| Title |
|---|
| XIN YAN ET AL.: ""Optimization of sputtering NiOx films for perovskite solar cell applications"", 《MATERIALS RESEARCH BULLETIN》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715958A (en) * | 2022-03-08 | 2022-07-08 | 华能新能源股份有限公司 | Spray pyrolysis method of nickel oxide and perovskite solar cell |
| CN114715958B (en) * | 2022-03-08 | 2024-04-02 | 华能新能源股份有限公司 | Spray pyrolysis method of nickel oxide and perovskite solar cell |
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