CN104628025A - Solvothermal preparation method of silicon-surface vertically-assembled CeO2 nanorod film - Google Patents
Solvothermal preparation method of silicon-surface vertically-assembled CeO2 nanorod film Download PDFInfo
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- CN104628025A CN104628025A CN201510079775.7A CN201510079775A CN104628025A CN 104628025 A CN104628025 A CN 104628025A CN 201510079775 A CN201510079775 A CN 201510079775A CN 104628025 A CN104628025 A CN 104628025A
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Abstract
The invention relates to a solvothermal preparation method of a silicon-surface vertically-assembled CeO2 nanorod film, which comprises the following steps: preparing a precursor solution by using ethanol as a solvent, and reacting the raw materials CeCl3 and CO(NH2)2 under the solvothermal conditions of 160-200 DEG C by using a clean silicon chip as a base to prepare the film formed by vertically assembling CeO2 nanorods on the silicon chip surface. The method has the advantages of simple equipment and low film-preparation cost, and does not need to perform high-temperature treatment on the silicon base and film. The prepared film is vertically assembled from the CeO2 nanorods, is thin and uniform, has the advantages of high visible light transparency, favorable adhesiveness and high ultraviolet resistance, has very strong emission peak at 380-390nm, and has wide application prospects in the aspect of crystalline silicon solar cell ultraviolet resistance.
Description
Technical field
The present invention relates to one and vertically assemble CeO on silicon chip matrix
2the solvothermal preparation method of nano-rod film, belongs to novel texture nano materials research technical field.
Background technology
In high altitude localities, because ozonosphere is thin, ultraviolet is strong, causes the average life-span to be the solar cell of about 15 years, is reduced to about 5 years in the work-ing life of high altitude localities.The effective way that uvioresistant film improves solar cell work-ing life is increased in solar cell surface, on the other hand for crystal silicon solar batteries, the UV-light that accounts for sunlight total energy 43% and infrared light is had not to be absorbed and used, people seek to turn light, can have again the functional materials of shielding effect to ultraviolet.Nano Ce O
2have visible light transmissivity high, the advantages such as ultraviolet absorption ability is strong receive much attention.
(albumen assisting alcohol-hydrothermal method prepares CeO to Zou Yunling etc.
2nanometer rod and luminescent properties [J] thereof. chemical research and application, 2010.22(3): 316-319.) with Cerium II Chloride and sodium hydroxide for reaction raw materials, with fresh egg white for complexing agent, in hydrothermal system, prepare the CeO that length is 200nm, diameter is about tens nanometers
2nanometer rod, and in hyacinthine luminous zone, there is stronger luminescence.(the Synthesis and characterization of CeO such as Yong Chen
2nano-rods [J] .Ceramics International, 2013.39(6): be 6607-6610) that raw material adopts water heat transfer diameter for 30nm length is for 100nmCeO with six nitric hydrate ceriums and sodium phosphate
2nanometer rod, with hydrate cerium acetate and the sodium hydrogen phosphate diameter that has been Material synthesis for 10nm length is for 400nmCeO
2nanometer rod, with other irregular CeO
2particle Phase ratio, these two kinds of nanometer rod have better ultraviolet absorption ability.
(the hydro-thermal legal system nano Ce O such as Zhou Li
2film and uv absorption property research [J]. chemical research and application, 2012.24(2): 237-241.) with cerous nitrate and urea for raw material, adopt hydrothermal method to prepare thickness with the condition of 130 DEG C of heating 7h in glass matrix and reach 100nm, crystal formation is better, film surface finish is higher, and has excellent visible light permeability and the nano thin-film of ultraviolet absorption characteristic.
But silicon chip is severely eroded under hydrothermal system, therefore nano Ce O can not be prepared by hydrothermal method at silicon chip surface
2film.There is not yet both at home and abroad at present and adopt solvent-thermal method vertically to assemble CeO at silicon chip surface
2the report of nano-rod film.
Summary of the invention
Goal of the invention:
The present invention proposes a kind of silicon face and vertically assemble CeO
2the solvothermal preparation method of nano-rod film, its object is to strong to ultraviolet absorption ability, that luminous is strong CeO
2nanometer rod is assembled on silicon chip, to make nanometer rod crystal formation better, and film surfacing.
Technical scheme:
The present invention implements by the following technical programs:
A kind of silicon face vertically assembles CeO
2the solvothermal preparation method of nano-rod film, is characterized in that: step is as follows:
(1) by raw material CeCl
37H
2o is dissolved in dehydrated alcohol, obtains 0.01-0.02mol/L CeCl
3ethanol solution, add the CO (NH of 0.02-0.04mol/L
2)
2, stir, obtain precursor solution;
(2) silicon chip of cleaning being put into liner is tetrafluoroethylene reactor, adds precursor liquid, and sealing, is placed in baking oven, at 160-200 DEG C of temperature, reacts 2-6h; Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
In step (2), the compactedness of precursor liquid is 70-80%.
Urea and CeCl in step (1)
3mol ratio be 2:1.
Advantage and effect:
The invention provides a kind of silicon face and vertically assemble CeO
2the solvothermal preparation method of nano-rod film, tool has the following advantages and beneficial effect:
The method equipment is simple, and masking is with low cost, does not need to carry out pyroprocessing to silicon matrix and film, and obtained film is thin is by CeO
2nanometer rod vertically assembles, and evenly, visible transparency is high, tack good, anti-ultraviolet property is strong, and has very strong emission peak (see figure 4) at 380-390nm, is widely used in crystal silicon solar batteries anti-ultraviolet property.
Accompanying drawing explanation
Fig. 1 gained CeO
2the SEM photo of nano-rod film.
Fig. 2 gained CeO
2the XRD spectra of nano-rod film.
Fig. 3 gained CeO
2the ultraviolet spectrogram of nano-rod film; In figure, a is the curve of sample strip; B is the curve of sky silicon chip.
Fig. 4 gained CeO
2the utilizing emitted light spectrogram (excitation wavelength 310nm) of nano-rod film.
Embodiment
The invention provides a kind of silicon face and vertically assemble CeO
2the solvothermal preparation method of nano-rod film, equipment is simple, and masking cost is low, does not need to carry out pyroprocessing to silicon matrix and film, strong to ultraviolet absorption ability, that luminous is strong CeO
2nanometer rod is assembled on silicon chip, and obtained film is thin is by CeO
2(XRD spectra of film as shown in Figure 2) nanometer rod vertically assembles (the SEM photo of film as shown in Figure 1), evenly, visible transparency is high, tack good, anti-ultraviolet property strong (ultraviolet spectrogram as shown in Figure 3), and have very strong emission peak (utilizing emitted light spectrogram is as shown in Figure 4) at 380-390nm, be widely used in crystal silicon solar batteries anti-ultraviolet property.The CeO that silicon chip surface is vertically assembled
2nano-rod film, diameter is 30-50nm, and film thickness can reach about 170 nm, and crystal formation is better, film surfacing.
Above-mentioned silicon face vertically assembles CeO
2the solvothermal preparation method of nano-rod film, step is as follows:
(1) by raw material CeCl
37H
2o is dissolved in dehydrated alcohol, obtains 0.01-0.02mol/L CeCl
3ethanol solution, add the CO (NH of 0.02-0.04mol/L
2)
2, stir, obtain precursor solution;
(2) silicon chip of cleaning being put into liner is tetrafluoroethylene reactor, adds precursor liquid, and sealing, is placed in baking oven, at 160-200 DEG C of temperature, reacts 2-6h; Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
In step (2), the compactedness of precursor liquid is 70-80%.
Urea (CO (NH in step (1)
2)
2) and CeCl
3mol ratio be 2:1.
Below in conjunction with specific embodiment, the present invention is specifically described:
embodiment 1
By raw material CeCl
37H
2o is dissolved in dehydrated alcohol, obtains 0.01mol/L CeCl
3ethanol solution, add 0.02mol/L CO (NH
2)
2, urea and CeCl
3mol ratio be 2:1, stir, obtain precursor solution.It is tetrafluoroethylene reactor that the silicon chip of cleaning is put into liner, adds precursor liquid (compactedness is 70%), and sealing, is placed in baking oven, at 200 DEG C of temperature, reacts 3h.Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
embodiment 2
By raw material CeCl
37H
2o is dissolved in dehydrated alcohol, obtains 0.015mol/LCeCl
3ethanol solution, add 0.03mol/L CO (NH
2)
2, urea and CeCl
3mol ratio be 2:1, stir, obtain precursor solution.It is tetrafluoroethylene reactor that the silicon chip of cleaning is put into liner, adds precursor liquid (compactedness is 70%), and sealing, is placed in baking oven, at 180 DEG C of temperature, reacts 4h.Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
embodiment 3
By raw material CeCl
37H
2o is dissolved in the dehydrated alcohol of certain volume, obtains 0.02mol/L CeCl
3ethanol solution, add 0.04mol/L CO (NH
2)
2, urea and CeCl
3mol ratio be 2:1, stir, obtain precursor solution.It is tetrafluoroethylene reactor that the silicon chip of cleaning is put into liner, adds precursor liquid (compactedness is 80%), and sealing, is placed in baking oven, at 160 DEG C of temperature, reacts 6h.Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
embodiment 4
By raw material CeCl
37H
2o is dissolved in dehydrated alcohol, obtains 0.02mol/L CeCl
3ethanol solution, add 0.04mol/L CO (NH
2)
2, urea and CeCl
3mol ratio be 2:1, stir, obtain precursor solution.It is tetrafluoroethylene reactor that the silicon chip of cleaning is put into liner, adds precursor liquid (compactedness is 75%), and sealing, is placed in baking oven, at 200 DEG C of temperature, reacts 2h.Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
Claims (3)
1. a silicon face vertically assembles CeO
2the solvothermal preparation method of nano-rod film, is characterized in that: step is as follows:
(1) by raw material CeCl
37H
2o is dissolved in dehydrated alcohol, obtains 0.01-0.02mol/L CeCl
3ethanol solution, add the CO (NH of 0.02-0.04mol/L
2)
2, stir, obtain precursor solution;
(2) silicon chip of cleaning being put into liner is tetrafluoroethylene reactor, adds precursor liquid, and sealing, is placed in baking oven, at 160-200 DEG C of temperature, reacts 2-6h; Reaction terminates, and takes out silicon chip after Temperature fall to room temperature, uses ethanol, water washing respectively totally, is drying to obtain product.
2. silicon face according to claim 1 vertically assembles CeO
2the solvothermal preparation method of nano-rod film, is characterized in that: in step (2), the compactedness of precursor liquid is 70-80%.
3. silicon face according to claim 1 vertically assembles CeO
2the solvothermal preparation method of nano-rod film, is characterized in that: urea and CeCl in step (1)
3mol ratio be 2:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000586A (en) * | 2015-08-03 | 2015-10-28 | 攀钢集团攀枝花钢铁研究院有限公司 | One-step synthesizing method of high-dispersion and weak-agglomeration doped ceria |
| WO2020080620A1 (en) * | 2018-10-17 | 2020-04-23 | 창원대학교 산학협력단 | Preparation method of metal ion-doped ceria using solvothermal synthesis |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01167290A (en) * | 1987-12-22 | 1989-06-30 | Kawasaki Steel Corp | Method for carrying out oxidation resistance traeatment of carbon material |
| CN102162127A (en) * | 2011-01-27 | 2011-08-24 | 湘潭大学 | Method for preparing rutile single crystal superfine titanium dioxide nano wire array grown vertical to substrate |
| CN102442834A (en) * | 2011-10-13 | 2012-05-09 | 华东师范大学 | Semiconductor material with Cu2O nano bamboo shoot structure and preparation method thereof |
| CN102534609A (en) * | 2012-01-12 | 2012-07-04 | 南京工业大学 | Method for preparing mesoporous titanium oxide film loaded on substrate |
| CN103449496A (en) * | 2012-12-31 | 2013-12-18 | 深圳信息职业技术学院 | Nano cerium oxide and preparation method thereof |
| CN103539193A (en) * | 2013-09-24 | 2014-01-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cerium-praseodymium composite oxide nanoparticle and nanorod |
-
2015
- 2015-02-15 CN CN201510079775.7A patent/CN104628025B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01167290A (en) * | 1987-12-22 | 1989-06-30 | Kawasaki Steel Corp | Method for carrying out oxidation resistance traeatment of carbon material |
| CN102162127A (en) * | 2011-01-27 | 2011-08-24 | 湘潭大学 | Method for preparing rutile single crystal superfine titanium dioxide nano wire array grown vertical to substrate |
| CN102442834A (en) * | 2011-10-13 | 2012-05-09 | 华东师范大学 | Semiconductor material with Cu2O nano bamboo shoot structure and preparation method thereof |
| CN102534609A (en) * | 2012-01-12 | 2012-07-04 | 南京工业大学 | Method for preparing mesoporous titanium oxide film loaded on substrate |
| CN103449496A (en) * | 2012-12-31 | 2013-12-18 | 深圳信息职业技术学院 | Nano cerium oxide and preparation method thereof |
| CN103539193A (en) * | 2013-09-24 | 2014-01-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cerium-praseodymium composite oxide nanoparticle and nanorod |
Non-Patent Citations (1)
| Title |
|---|
| 周丽: "水热法制纳米CeO2膜及紫外吸收性能研究", 《化学研究与应用》, vol. 24, no. 2, 29 February 2012 (2012-02-29) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000586A (en) * | 2015-08-03 | 2015-10-28 | 攀钢集团攀枝花钢铁研究院有限公司 | One-step synthesizing method of high-dispersion and weak-agglomeration doped ceria |
| WO2020080620A1 (en) * | 2018-10-17 | 2020-04-23 | 창원대학교 산학협력단 | Preparation method of metal ion-doped ceria using solvothermal synthesis |
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| CN104628025B (en) | 2016-06-08 |
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