CN106744973B - Method for preparing amorphous silicon nano material by ultrasonic chemistry - Google Patents
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- CN106744973B CN106744973B CN201611023122.8A CN201611023122A CN106744973B CN 106744973 B CN106744973 B CN 106744973B CN 201611023122 A CN201611023122 A CN 201611023122A CN 106744973 B CN106744973 B CN 106744973B
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 28
- 229910021417 amorphous silicon Inorganic materials 0.000 title abstract 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 45
- 239000010703 silicon Substances 0.000 claims abstract description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 9
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000002604 ultrasonography Methods 0.000 claims description 15
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 235000003270 potassium fluoride Nutrition 0.000 claims description 7
- 239000011698 potassium fluoride Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 5
- 150000004673 fluoride salts Chemical group 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 7
- 230000009471 action Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract 2
- 239000001257 hydrogen Substances 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- 239000000047 product Substances 0.000 description 23
- 238000009835 boiling Methods 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical compound O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 4
- 239000007773 negative electrode material Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- -1 hydroxyl free radical Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Silicon Compounds (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a method for preparing amorphous silicon nano material by ultrasonic chemistry, which is characterized in that silicon dioxide and sodium fluoride aqueous solution are used for preparing amorphous silicon nano material under the ultrasonic action: firstly, fluoride reacts with solid silicon dioxide to generate water-soluble fluosilicic acid ions; then, decomposing hydrogen free radicals and hydroxyl free radicals by utilizing the cavitation generated by water under the action of ultrasonic waves; finally, the decomposed hydrogen free radicals reduce fluosilicic acid ions in the water to obtain the amorphous simple substance silicon nano material. In the process of preparing the elemental silicon, the fluoride plays the role of a catalyst and can be recycled, and the silicon dioxide and the water participate in the reaction. The invention adopts a milder and safer ultrasonic chemical method to synthesize the elemental silicon nano material. The preparation method has the advantages of simple equipment, low energy consumption, rapid synthesis and safe process.
Description
Technical field
The invention belongs to battery material technical fields, and in particular to a kind of sonochemistry prepares unformed silicon nano material
Method.
Background technique
Currently, elemental silicon has very important application in material, information and energy field, as photovoltaic produces
Its demand of the development of industry constantly expands.Due to the increasingly increasing with mobile electronic equipment to high capacity, long-life batteries demand
Long, more stringent requirements are proposed for performance of the people to lithium ion battery.Relatively low have become of capacity of lithium ion battery restricts battery work
One bottleneck of industry development, the negative electrode material for finding more height ratio capacity have become an important development side in battery material field
To.At present commercialization negative electrode material be carbon, from lithium ion battery commercialization since, the research of carbon material obtain it is considerable into
Step, is difficult the space for having promotion again.The negative electrode material for thus finding substitution carbon becomes an important developing direction.It is numerous can
In the negative electrode material of selection, silicon is due to its specific capacity (theoretical value: 4200mAh/g) with higher and lower removal lithium embedded voltage
It attracts attention.
Application No. is 201010567832.3 patents to disclose a kind of preparation method of elemental silicon, by SiO2It is dissolved in and containing
In the molten chloride for having alkali or alkaline earth metal oxide, or the silicate of alkali or alkaline earth metal is dissolved in chloride
In fused salt, the temperature of the molten chloride is 600-1000o C, using graphite or silicon or metal as cathode, with graphite or inertia
Material is that anode is electrolysed, so that the electro-deposition of silicate, the isolated elemental silicon of electro-deposition product occurs in cathode.But
The invention will also refine silicon by electro-deposition, and method is complicated.
Summary of the invention
The defect of elemental silicon method in practical applications is prepared for tradition, the invention proposes a kind of preparations of sonochemistry
The method of unformed silicon nano material is reacted with fluoride aqueous solution by silica, generates simple substance under the action of ultrasound
Silicon nano material.Relative to currently used elementary silicon preparation method, sonochemical method is a kind of mild, safe, green system
The method of standby silicon nano material.
The invention particularly discloses a kind of methods that sonochemistry prepares unformed silicon nano material, in ultrasonic wave and catalysis
Under the action of agent, is reacted by silicon source with water and generate unformed silicon nano material.Sonochemistry is a kind of ultrasound using high intensity
The method that wave (20k-10MHz) is chemically reacted.Sonochemistry is mostly derived from ultrasonic cavitation, the shape of liquid cavitation bubble
At, oscillation, growth, shrink and the caused physics and chemical phenomenon of collapse.Liquid ultrasonic cavitation processes are to concentrate sound field energy
And the process discharged rapidly, when cavitation bubble collapses, in very short time, generate 5000K or more high temperature and about 5.05 ×
108The high pressure of Pa.The high temperature and pressure of part can lead to the chemical bond recombination of precursor and solvent, so that living radical is generated,
This free radical is as the intermediate product for forming final stable nano material.These free radical intermediate products otherwise be derived from solvent,
Derived from the stabilization agent molecule of addition, water is as solvent, and under the action of ultrasound, water is broken down into hydroperoxyl radical and hydrogen-oxygen certainly
By base, hydroperoxyl radical has reproducibility, can show that unique activity restores precursor, to obtain required target
Product.
Preferably, the catalyst is fluoride.
Any of the above-described scheme is preferably, and is included the following steps:
The preparation of step (a), reaction solution: it selects water as solvent, dissolves fluoride, silicon source is added, is configured to solution；
Step (b) generates unformed silicon nano material: after carrying out ultrasound with solution of the ultrasonic method to above-mentioned configuration, carrying out
Centrifuge separation, being placed in 60 DEG C of drying boxes can obtain.Centrifugation 10 minutes, 8000 revs/min of revolving speed.
Any of the above-described scheme is preferably, the silicon source in the step (a) be silica, fluoride be sodium fluoride and/
Or potassium fluoride.
Any of the above-described scheme is preferably, and silicon source and the molar ratio of fluoride are 1:6-1:24 in the step (a).
Any of the above-described scheme is preferably, and temperature when ultrasonic in the step (b) is 50-90 DEG C, ultrasonic time 1-
4h, supersonic frequency are 20-50 kHz, ultrasonic power 100-800W.
Beneficial effects of the present invention are as follows: the invention discloses the sides that a kind of sonochemistry prepares unformed silicon nano material
Method, this method are that unformed silicon nano material is prepared under ultrasonication with silica and sodium fluoride aqueous solution: firstly, fluorination
Object is reacted with solid silica generates water-soluble fluosilicic acid ion；The cavitation for recycling water to generate under ultrasonic wave effect
Effect, decomposites hydroperoxyl radical and hydroxyl free radical；The fluosilicic acid ion in hydroperoxyl radical reductive water finally decomposited obtains
Amorphous simple substance silicon nano material:
(1), for traditional hydrothermal reduction method for preparing elemental silicon and high temperature reduction method, the present invention provides one
The method that the novel sonochemistry of kind prepares simple substance silicon nano material；
(2), preparation method provided by the invention is horn formula sonochemical method, the preparation method mild condition, green peace
Entirely, equipment is simple, low energy consumption, synthesizes quick and process safety.
Detailed description of the invention
Fig. 1 is that the unformed silicon that the method that sonochemistry according to the invention prepares unformed silicon nano material is prepared is received
The infrared spectrum spectrogram of rice material sample.
Fig. 2 is that the unformed silicon that the method that sonochemistry according to the invention prepares unformed silicon nano material is prepared is received
The high-resolution-ration transmission electric-lens figure of rice material sample.
Specific embodiment
Following embodiments are further explanations for the content of present invention using as the explaination to the technology of the present invention content, but
Substantive content of the invention is not limited in described in following embodiments, those skilled in the art can with and should know appoint
What simple change or replacement based on true spirit should belong to protection scope of the presently claimed invention.
Embodiment 1
(1) configuration of reaction solution: 0.01 mole of silica and 0.06 mole of sodium fluoride are weighed in boiling flask, is added
Enter the water dissolution of 90ml；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 60 DEG C, ultrasonic function
Rate is 700W.Ultrasound was centrifuged product after 4 hours, and black product can be obtained in drying in 60 DEG C of baking oven.Such as
Shown in Fig. 1, Fig. 1 is the infrared spectrum spectrogram for the unformed silicon nano material sample prepared；In the figure, it is evident that about
500cm-1There is the characteristic peak of Si-Si bond, illustrates the presence for having elemental silicon in product.As shown in Fig. 2, Fig. 2 is the nothing prepared
The high-resolution-ration transmission electric-lens figure of sizing silicon nano material sample；In the figure, it can be seen that sample obtained does not have obvious lattice fringe,
It is amorphous state.
Embodiment 2
(1) configuration of reaction solution: 0.01 mole of silica and 0.06 mole of potassium fluoride are weighed in boiling flask, is added
Enter the water dissolution of 90ml；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 60 DEG C, ultrasonic function
Rate is 700W.Ultrasound was centrifuged product after 4 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 3
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.06 mole of sodium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 80 DEG C, ultrasonic function
Rate is 700W.Ultrasound was centrifuged product after 2 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 4
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.06 mole of sodium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 50 DEG C, ultrasonic function
Rate is 500W.Ultrasound was centrifuged product after 3 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 5
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.12 sodium fluoride in boiling flask, is added
The water of 90ml dissolves；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 60 DEG C, ultrasonic function
Rate is 600W.Ultrasound was centrifuged product after 2 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 6
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.06 mole of sodium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 90 DEG C, ultrasonic function
Rate is 800W.Ultrasound was centrifuged product after 1 hour, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 7
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.06 mole of potassium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 80 DEG C, ultrasonic function
Rate is 700W.Ultrasound was centrifuged product after 2 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 8
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.06 mole of potassium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 50 DEG C, ultrasonic function
Rate is 500W.Ultrasound was centrifuged product after 3 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 9
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.12 mole of potassium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 60 DEG C, ultrasonic function
Rate is 600W.Ultrasound was centrifuged product after 2 hours, and black product can be obtained in drying in 60 DEG C of baking oven.
Embodiment 10
(1) configuration of reaction solution: weighing 0.005 mole of silica and 0.06 mole of potassium fluoride in boiling flask,
The water dissolution of 90ml is added；
(2) ultrasonic reaction solution: reaction solution is placed in horn formula Vltrasonic device, and setting temperature is 90 DEG C, ultrasonic function
Rate is 800W.Ultrasound was centrifuged product after 1 hour, and black product can be obtained in drying in 60 DEG C of baking oven.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that those skilled in the art without
It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical solution, all should be within the scope of protection determined by the claims.
Claims (4)
1. a kind of method that sonochemistry prepares unformed silicon nano material, which is characterized in that in the work of ultrasonic wave and catalyst
Under, is reacted by silicon source with water and generate unformed silicon nano material；The catalyst is fluoride；Specifically include the following steps:
The preparation of step (a), reaction solution: it selects water as solvent, dissolves fluoride, silicon source is added, is configured to solution；
Step (b) generates unformed silicon nano material: after carrying out ultrasound with solution of the ultrasonic method to above-mentioned configuration, being centrifuged
Separation, being placed in 60 DEG C of drying boxes can obtain.
2. preparing the method for unformed silicon nano material as described in claim 1, which is characterized in that the silicon in the step (a)
Source is silica, and fluoride is sodium fluoride and/or potassium fluoride.
3. preparing the method for unformed silicon nano material as described in claim 1, which is characterized in that silicon source in the step (a)
Molar ratio with fluoride is 1:6-1:24.
4. preparing the method for unformed silicon nano material as described in claim 1, which is characterized in that ultrasonic in the step (b)
When temperature be 50-90 DEG C, ultrasonic time 1-4h, supersonic frequency be 20-50 kHz, ultrasonic power 100-800W.
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| US7244513B2 (en) * | 2003-02-21 | 2007-07-17 | Nano-Proprietary, Inc. | Stain-etched silicon powder |
| CN101979712A (en) * | 2010-12-01 | 2011-02-23 | 武汉大学 | Method for preparing elemental silicon |
| CN102951642A (en) * | 2011-08-31 | 2013-03-06 | 常州诺瑞格纳米科技有限公司 | Water-soluble silicon nanoparticles and preparation method thereof |
| CN103288088B (en) * | 2012-02-23 | 2016-02-17 | 苏州宝时得电动工具有限公司 | A kind of preparation method of polysilicon |
| JP6057424B2 (en) * | 2013-03-06 | 2017-01-11 | 学校法人東京電機大学 | Method for producing silicon nanoparticles |
| US20150125601A1 (en) * | 2013-11-04 | 2015-05-07 | Systems And Materials Research Corporation | Method and apparatus for producing nanosilicon particles |
| CN105271239B (en) * | 2015-10-28 | 2017-10-03 | 内江师范学院 | A kind of method that using plasma method prepares nano-metal silicon |
| CN106044777A (en) * | 2016-06-01 | 2016-10-26 | 北京大学 | Novel method for preparing nanometer silicon from silicon dioxide |
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Non-Patent Citations (1)
| Title |
|---|
| Optical properties of silicon nanoparticles by ultrasound-induced solution method;Lee, S et al;《JAPANESE JOURNAL OF APPLIED PHYSICS PART 2-LETTERS & EXPRESS LETTERS》;20040604;第43卷(第6B期);全文 * |
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