CN103601194B - A method of regulation nano-silicon pattern and structure - Google Patents
A method of regulation nano-silicon pattern and structure Download PDFInfo
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- CN103601194B CN103601194B CN201310578786.0A CN201310578786A CN103601194B CN 103601194 B CN103601194 B CN 103601194B CN 201310578786 A CN201310578786 A CN 201310578786A CN 103601194 B CN103601194 B CN 103601194B
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Abstract
The invention discloses a kind of simple regulation nanometer Silicon forms and the methods of structure, and using crystalline silicon as presoma, using water-ethanol-ammonium hydroxide mixed solution as reaction system, constant temperature is stirred to react.By control water and ethyl alcohol volume when reaction time, the silicon/oxidative silicon composite nanometer particle for being respectively provided with nucleocapsid, yolk eggshell and hollow structure is obtained.This method for silica-base material lithium ion battery, catalyst, drug release agents and in terms of large-scale application provide a kind of new approach.
Description
Technical field
The present invention relates to the regulation method of nano-silicon pattern and structure, it can regulate and control to obtain nucleocapsid, yolk eggshell and hollow
Structure belongs to chemosynthesis technical field.
Background technique
Silicon has been widely used in the fields such as chip and memory device as traditional semiconductor material.Silicon is because have
Be currently known highest theoretical capacity, be equally treated as great potential cathode material for high capacity lithium ion battery [Wu H,
Cui Y. Designing nanostructured Si anodes for high energy lithium ion
batteries[J]. Nano Today, 2012].In recent years, the synthesis of silica receives the extensive of people with preparation
Pay close attention to [Zhang T, Ge J, Hu Y, et al. Formation of hollow silica colloids through
a spontaneous dissolution–regrowth process] [Wong Y J, Zhu L, Teo W S, et al.
Revisiting the stober method: inhomogeneity in silica shells[J]. Journal of
the American Chemical Society, 2011, 133(30): 11422-11425].Due to nontoxic and excellent life
Object compatibility, silica is in biochemistry especially in administering pharmaceutical substances, gene delivery [Slowing I I, Vivero-
Escoto J L, Wu C W, et al. Mesoporous silica nanoparticles as controlled
release drug delivery and gene transfection carriers[J]. Advanced drug
Delivery reviews, 2008,60 (11): 1278-1288] and cell imaging [Wang L, Zhao W, Tan W.
Bioconjugated silica nanoparticles: development and applications[J]. Nano
Research, 2008,1 (2): 99-115] etc. fields have a good application prospect.The silicon and silica of different shape
Material is successfully prepared, these structures include core-shell structure [Guerrero-Mart í nez A, P é rez-Juste J,
Liz‐Marzán L M. Recent progress on silica coating of nanoparticles and
Related nanomaterials [J] Advanced Materials, 2010,22 (11): 1182-1195], yolk egg
Shell structure [Liu J, Qiao S Z, Chen J S, et al. Yolk/shell nanoparticles:new
platforms for nanoreactors, drug delivery and lithium-ion batteries[J].
Chemical Communications, 2011,47 (47): 12578-12591] and hollow structure [Lou X W D,
Archer L A, Yang Z. Hollow Micro‐/Nanostructures: Synthesis and Applications
[J]. Advanced Materials, 2008, 20(21): 3987-4019].Yin et al. has found in research work, nothing
The silica of sizing is in NaBH4It is handled in aqueous solution, after living through a spontaneous dissolution regrowth process, will form egg
Yellow eggshell and hollow structure [Zhang T, Ge J, Hu Y, et al. Formation of hollow silica
colloids through a spontaneous dissolution–regrowth process[J]. Angewandte
Chemie, 2008, 120(31): 5890-5895.].In the work of other researchers, made using polyvinylpyrrolidone
For protective agent, using NaOH solution as etching agent, being prepared has yolk eggshell [Zhang Q, Ge J, Goebl
J, et al. Rattle-type silica colloidal particles prepared by a surface-
Protected etching process [J] Nano Research, 2009,2 (7): 583-591.] and it is hollow
[Zhang Q, Zhang T, Ge J, et al. Permeable silica shell through surface-
Protected etching [J] Nano letters, 2008,8 (9): 2867-2871.] structure silica
Grain.But these preparation methods will point multistep carry out, the condition for controlling form is relative complex；Simultaneously to introduce etching agent or
Protective agent, and these reagents need to carry out post-processing, otherwise can cause environmental pollution.
Summary of the invention
In view of the above-mentioned problems, the object of the present invention is to provide a kind of method of simpler regulation nano-silicon appearance structure,
Silica-base material with nucleocapsid, yolk eggshell and hollow structure is made as follows:
Step 1: the nano silicon particles of certain mass being added in the mixed solution that ethanol/water volume ratio is 0 ~ 12:1,
Ultrasonic disperse；
Step 2: being added concentrated ammonia liquor in the above solution, and constant temperature stirs 10min ~ 96h；
Step 3: the product after stirring is centrifugated immediately, is washed till neutrality with ethyl alcohol, is then dried in vacuum drying oven
It is dry.
The further preferred embodiment of the present invention is: the silicon nanoparticle preferable particle size is between 30 ~ 1000nm.
The further preferred embodiment of the present invention is: ethanol water mixed reaction solution preferred volume ratio is 12:1 ~ 4:1.
The further preferred embodiment of the present invention is: the concentration that concentrated ammonia liquor is added is 20% ~ 30%, and ammonium hydroxide is preferred with reaction solution
Volume ratio is 1:120 ~ 3:120.
The further preferred embodiment of the present invention is: preferred mixing time is 10min ~ 96h.
The invention has the following advantages that process flow is simple, when the volume by simply controlling water-ethanol is when reacted
Between, so that it may achieve the purpose that control silicon particle form.Low solvent in reaction process is required to consersion unit and reaction condition
It is easy to remove with reaction reagent, obtained product purity is high.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) figure with Core-shell structure material.
Fig. 2 is graphene transmission electron microscope (TEM) figure with yolk eggshell structural material.
Fig. 3 is graphene transmission electron microscope (TEM) figure with hollow structure material.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples:
Embodiment 1
The silicon particle that 80mg partial size is 100nm is added in 20ml water and 120ml alcohol mixed solution, ultrasonic disperse
20min.The ammonium hydroxide that 2ml concentration is 30% is added in the above solution, constant temperature stirs 10min.Product after stirring is centrifuged immediately
Separation, is washed till neutrality with a large amount of ethyl alcohol, then dries in vacuum drying oven.
As shown in 1 transmission electron microscope of attached drawing (TEM), obtained silicon/silicon dioxide material has core-shell structure.
Embodiment 2
The silicon particle that 80mg partial size is 100nm is added in 20ml water and 120ml alcohol mixed solution, ultrasonic disperse
20min.The ammonium hydroxide that 2ml concentration is 30% is added in the above solution, constant temperature stirs 1h.Product after stirring is centrifuged immediately and is divided
From being washed till neutrality with a large amount of ethyl alcohol, then dried in vacuum drying oven.
As shown in 2 transmission electron microscope of attached drawing (TEM), obtained silicon/silicon dioxide material has yolk eggshell structure.
Embodiment 3
The silicon particle that 80mg partial size is 100nm is added in 20ml water and 120ml alcohol mixed solution, ultrasonic disperse
20min.The ammonium hydroxide that 2ml concentration is 30% is added in the above solution, constant temperature stirs for 24 hours.Product after stirring is centrifuged immediately and is divided
From being washed till neutrality with a large amount of ethyl alcohol, then dried in vacuum drying oven.
As shown in 3 transmission electron microscope of attached drawing (TEM), earth silicon material is obtained with hollow structure.
Embodiment 4
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 100nm, the volume of water is 10ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 30%, constant temperature mixing time is for 24 hours.Obtained silicon/silicon dioxide material has core-shell structure.
Embodiment 5
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 100nm, the volume of water is 15ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 30%, constant temperature mixing time is for 24 hours.Obtained silicon/silicon dioxide material has core-shell structure.
Embodiment 6
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 100nm, the volume of water is 30ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 30%, constant temperature mixing time is for 24 hours.Earth silicon material is obtained with hollow structure.
Embodiment 7
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 100nm, the volume of water is 30ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 30%, constant temperature mixing time is 10min.Obtained silicon/silicon dioxide material has nucleocapsid knot
Structure.
Embodiment 8
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 100nm, the volume of water is 10ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 30%, constant temperature mixing time is 1h.Earth silicon material is obtained with hollow structure.
Embodiment 9
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 30nm, the volume of water is 20ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 30%, constant temperature mixing time is 1h.Obtained silicon/silicon dioxide material has yolk eggshell knot
Structure.
Embodiment 10
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 1000nm, the volume of water is 20ml, ethyl alcohol
Volume is 120ml, and ammonia concn 30%, constant temperature mixing time is 1h.Obtained silicon/silicon dioxide material has yolk eggshell
Structure.
Embodiment 11
Operating method is with embodiment 1, the difference is that the partial size of silicon particle is 100nm, the volume of water is 20ml, the body of ethyl alcohol
Product is 120ml, and ammonia concn 20%, constant temperature mixing time is 1h.Obtained silicon/silicon dioxide material has yolk eggshell knot
Structure.
Presently preferred embodiments of the present invention is illustrated above, but the present invention is not limited to the embodiment,
Those skilled in the art can also make various equivalent variation or replacement on the premise of without prejudice to spirit of the invention,
These equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (4)
1. a kind of method of regulation nano-silicon pattern and structure, it is characterised in that be made as follows:
Step 1: the nano silicon particles of certain mass are added in the mixed solution that ethanol/water volume ratio is 4~12:1, are surpassed
Sound dispersion；
Step 2: being added concentrated ammonia liquor in the above solution, and constant temperature stirs 10min~96h；
Step 3: the product after stirring is centrifugated immediately, is washed till neutrality with ethyl alcohol, is then dried in vacuum drying oven.
2. the method for regulation nano-silicon pattern and structure as described in claim 1, it is characterised in that: the silicon nanoparticle
Partial size is between 30~1000nm.
3. the method for regulation nano-silicon pattern and structure as described in claim 1, it is characterised in that: the concentration of concentrated ammonia liquor is added
It is 20%~30%, ammonium hydroxide volume and reaction solution volume are 1:120~3:120.
4. the method for regulation nano-silicon pattern and structure as described in claim 1, it is characterised in that: under steady temperature, stirring
Time is 10min~for 24 hours.
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| US20150162617A1 (en) * | 2013-12-09 | 2015-06-11 | Nano And Advanced Materials Institute Limited | Si@C core/shell Nanomaterials for High Performance Anode of Lithium Ion Batteries |
| CN112960676B (en) * | 2019-12-12 | 2022-11-01 | 中国科学院大连化学物理研究所 | Preparation method of nano silicon dioxide core-shell structure particles |
| CN114300667A (en) * | 2021-12-21 | 2022-04-08 | 惠州锂威新能源科技有限公司 | Preparation method, product and application of silicon negative electrode material |
| CN115057448B (en) * | 2022-07-14 | 2023-06-09 | 青岛大学 | Ultrathin silica nanosheets and preparation method thereof |
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| WO2007086367A1 (en) * | 2006-01-27 | 2007-08-02 | Konica Minolta Medical & Graphic, Inc. | Si/Si3N4 NANOPARTICLE, BIOSUBSTANCE LABELING AGENT BASED ON THE SAME, AND PROCESS FOR PRODUCING THE NANOPARTICLE |
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Effective date of registration: 20181119 Address after: 100000 Hongzhuang International Cultural Bonded Innovation Park D-2-6, No. 1 Baijialou Jia, Chaoyang North Road, Chaoyang District, Beijing Applicant after: Xiao Yanshe Address before: 100029, No. 15 East Third Ring Road, Chaoyang District, Beijing Applicant before: Beijing University of Chemical Technology |
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Effective date of registration: 20210113 Address after: 100020 d-2-8 (1-3 floors), Beijing Hongzhuang international cultural bonded Innovation Park, No.1, baijialou, Chaoyang North Road, Chaoyang District, Beijing Patentee after: BEIJING HUAKE XUNNENG GRAPHENE NEW TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. Address before: 100000 Hongzhuang International Cultural Bonded Innovation Park D-2-6, No. 1 Baijialou Jia, Chaoyang North Road, Chaoyang District, Beijing Patentee before: Xiao Yanshe |