CN106299284A - A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires - Google Patents

A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires Download PDF

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CN106299284A
CN106299284A CN201610807393.6A CN201610807393A CN106299284A CN 106299284 A CN106299284 A CN 106299284A CN 201610807393 A CN201610807393 A CN 201610807393A CN 106299284 A CN106299284 A CN 106299284A
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attapulgite
quito
hole
silicon nanowires
mixture
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侯建华
窦倩
王雪
蒋欣
王小治
鄢碧鹏
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Yangzhou University
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Yangzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires, belongs to the preparing technical field of nano-electrode material.To filter after solution supersound process containing attapulgite or centrifugal, be then dried and obtain the attapulgite being dried, then by dry attapulgite and aluminum chloride, aluminium powder or aluminium powder and the mixture of magnesium powder, obtain the mixture containing attapulgite；Mixture containing attapulgite is heated under air-proof condition 180～280 DEG C react 0.5～40 hour；Reaction is cooled to greenhouse after terminating, collect product, after soaking with dilute hydrochloric acid, with distilled water wash, obtains hole, attapulgite Quito silicon nanowires.Process of the present invention is simple, and the prices of raw materials are cheap, productivity is high, and is that solid state reaction preparation is conducive to industrialized production, and obtains the achievement of the chemical property of excellence.

Description

A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires
Technical field
The invention belongs to the preparing technical field of nano-electrode material.
Background technology
At present, along with socioeconomic fast development, the demand of the energy is grown with each passing day by the mankind, simultaneously fossil energy and its Gradually using up of the primary energy that he is non-renewable, makes environmental quality decline to a great extent, and ecological environment problem is the most increasingly serious, and this is all It it is a difficult problem the most urgently to be resolved hurrily.In this context, new chemical energy storage device (such as secondary cell) has obtained great concern And development.
Silicon/carbon/graphite in lithium ion batteries carbon negative pole material theoretical specific capacity only has 372 mAh/g, and high rate performance is poor, jolt ramming Density is little, it is impossible to meet the demand of energy-density lithium ion battery.Thus, the negative material finding height ratio capacity substitutes graphite Imperative.Silicon has the theoretical specific capacity of up to 4200 mAh/g and moderate voltage platform, is most to be hopeful to substitute stone One of lithium ion battery negative material of ink.But, silicon exist in cyclic process serious Volumetric expansion (reach 300% with On), it is easily caused silicon grain and pulverizes and force electrode structure avalanche, and the poorly conductive of silicon, thus, the reality of silicon based anode material Border application is by the biggest obstruction.It addition, the preparation cost of silicon is higher at present, technique mixes, it is difficult to large-scale production.Nearest grinds Studying carefully and show, prepare silicon materials and typically require higher temperature, i.e. use magnesiothermic reduction technology, temperature is also required to high higher than 550 DEG C Temperature, and the method condition is harsh.Such as: Zhihao Bao etc. (RSC Adv., 2013,3 (26): 10145-10149) and Yi Cui etc. (Sci.Rep., 2013,3:1919-1925) Liu Shu and (Kunming University of Science and Technology's journal (natural science edition) 6 such as grade : 14-18) etc. (39) problem is with rice husk in agricultural product for silicon source, uses magnesiothermic reduction technology to prepare silicon materials, and obtains excellence Chemical property.
For problem above, this paper is based on the environmentally friendly preparation method simplified and selects inexpensive raw material, special It it not the low temperature method of preparing silicon materials.The preferable chemical molecular formula of attapulgite is: Mg5Si8O20(OH)2(OH2)4·4H2O, Its unique stratiform, chain structure give its special performance.Attapulgite is a kind of natural non-metallic clay mineral, has specific surface The advantages such as long-pending big, good, the high adsorption capacity of chemical stability.Chinese scholar Xu Jiquan in 1976 etc. are in Jiangsu Province, China Luhe County bamboo Little winding discovery attapulgite ore deposit, town, finds this ore deposit on the ground such as Xuyi Jiangsu, Mingguang, anhui the most in succession.Attapulgite form in Hair-like or fibrous, usually woollen blanket shape or earthy aggregation.Attapulgite structure exists crystal lattice, crystal contains Variable amount of Fe3+、Al3+、Na+、Ca2+, crystal is needle-like, threadiness or fiber collection shape.Mohs' hardness 2～3, is heated to 700～800 DEG C, hardness > 5, proportion is 2.05～2. 32.
Summary of the invention
The present invention provides a kind of method that low temperature prepares hole, attapulgite Quito silicon nanowires.
The present invention comprises the steps:
1) will filter after the solution supersound process containing attapulgite or centrifugal, be then dried and obtain the attapulgite being dried, then By dry attapulgite and aluminum chloride, aluminium powder or aluminium powder and the mixture of magnesium powder, obtain the mixture containing attapulgite；
2) mixture containing attapulgite is heated under air-proof condition 180～280 DEG C react 0.5～40 hour；
3) reaction is cooled to greenhouse after terminating, and collects product, after soaking with dilute hydrochloric acid, with distilled water wash, obtains attapulgite Hole, Quito silicon nanowires.
It is simple that the whole synthesis technique of the present invention has process, and the prices of raw materials are cheap, productivity advantages of higher, and are that solid phase is anti- Beneficially industrialized production should be prepared, and obtain the achievement of the chemical property of excellence.
Concrete beneficial effect:
1, present invention process is simple, cost is relatively low, and is substantially reduced reaction temperature, and the productivity of final products is high, can realize Large-scale production.
2, the material prepared by the present invention may be used for high-capacity lithium ion cell, catalyst carrier, ultracapacitor, urges Agent, adsorbent, gas store, medicament transport, the numerous areas such as bio-imaging and water process.
3, the material prepared with the present invention forms lithium ion battery, after 300 times circulate, and 0.744 A/g and 3.72A/g electricity Under current density, reversible capacity is up to 2045.85mAh/g and 1432.08mAh/g respectively.The chemical property of this material excellence obtains Benefit the pattern of silicon nanowires in material alleviate the bulk effect of silicon and decrease Li+Diffusion rate.
Further, the mixture of aluminium powder of the present invention or aluminium powder and magnesium powder and the attapulgite being dried, tri-chlorination The mixing quality ratio of aluminum is 1～50: 1: 1～100.The ratio of aluminum chloride is for aluminum chloride more than the purpose of attapulgite High-temperature fusion salt can fully wrap up attapulgite, so can reduce high price aluminium powder or aluminium powder and magnesium powder mixture make Amount for reducing agent.
In described step 3) the concentration of dilute hydrochloric acid for soaking be 0.1M effect be remove unreacted aluminium powder or (with) magnesium powder and the corresponding impurity such as aluminum silicide or magnesium silicide.
In order to obtain hole, purity higher attapulgite Quito silicon nanowires, after described step 3), then with Fluohydric acid. or The aqueous slkali of the dense heat of person removes remaining Si oxide, obtains refined hole, attapulgite Quito silicon nanowires.
Accompanying drawing explanation
Fig. 1 is the XRD figure of prepared hole, attapulgite Quito silicon nanowires in embodiment 1.
Fig. 2 is scanning electron microscope (SEM) figure of prepared hole, attapulgite Quito silicon nanowires in embodiment 1.
Fig. 3 is transmission electron microscope (TEM) figure of prepared hole, attapulgite Quito silicon nanowires in embodiment 1.
Fig. 4 be the lithium ion battery that in embodiment 1 prepared by prepared hole, attapulgite Quito silicon nanowires in difference times Rate constant current charge-discharge cycle life figure.
Fig. 5 is scanning electron microscope (SEM) figure of prepared hole, attapulgite Quito silicon nanowires in embodiment 2.
Fig. 6 is scanning electron microscope (SEM) figure of prepared hole, attapulgite Quito silicon nanowires in embodiment 3.
Detailed description of the invention
Embodiment 1:
Step one: the attapulgite of 100g is joined after filtering after ultrasonic 1 hour in 200mL aqueous solvent or being centrifugal dry Dry, obtain attapulgite, then with the mass ratio of 1: 9: 1, attapulgite and aluminum chloride, aluminium powder are mixed, obtain containing attapulgite The mixture of soil.
Step 2: said mixture is loaded in stainless steel autoclave, sealing autoclave post-heating to 200 DEG C and guarantor Temperature reaction 10 hours.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, obtain hole, attapulgite Quito silicon nanowires.
Product and performance test:
From the XRD figure spectrum that Fig. 1 is prepared hole, attapulgite Quito silicon nanowires embodiment 1, the XRD of the sample obtained spreads out Penetrating peak as it is shown in figure 1, only there is diffraction maximum at 28.6 °, 46.9 °, 56.2 °, 69.4 ° and 76.3 °, these diffraction maximums are brilliant The diffraction maximum of body silicon, therefore attapulgite is after the technique of embodiment 1, can obtain pure silicon materials.The specifically side of reaction Formula is as follows:
Al + Mg5Si8O20(OH)2(OH2)4+AlCl3→8Si +AlOCl+MgAl2Cl8+5H2O
By-product AlOCl, MgAl in this reaction system2Cl8Easily process.
It is scanning electron microscope (SEM) figure of prepared hole, attapulgite Quito silicon nanowires embodiment 1 from Fig. 2, can see Going out, porous silicon is interconnective nano wire shape and nano-particle composition, and the length of the nano wire of some porous silicon is more than 4 Micron.
It is that embodiment 1 observes table in transmission electron microscope (TEM) figure of prepared hole, attapulgite Quito silicon nanowires from Fig. 3 Bright: porous silicon presents interconnective irregular loose structure, porous silicon is crystal structure, and interlamellar spacing is 0. 31 nm, corresponding (111) interplanar distance in crystalline silicon.
Hole, the attapulgite Quito silicon nanowires using the example method to make makes lithium ion battery, further from Fig. 4's Visible at different multiplying constant current charge-discharge cycle life figure, after 300 times circulate, 0.744 A/g and 3.72A/g electric current density Under, reversible capacity is up to 2045.85mAh/g and 1432.08mAh/g respectively.The chemical property of this material excellence has benefited from material In material, the pattern of silicon nanowires alleviates the bulk effect of silicon and decreases Li+Diffusion rate.
Embodiment 2:
Step one: with the ratio that mass ratio is 1: 1, aluminium powder and magnesium powder are mixed in advance, form aluminium powder and the mixture of magnesium powder.
In the dilute hydrochloric acid solvent of the 0.1M that the attapulgite of 100g is joined 200 mL after ultrasonic 0.5 hour filter or It is dried after person is centrifugal, obtains attapulgite, the most again by the mixture of attapulgite and aluminum chloride and aluminium powder and magnesium powder the most again With the mass ratio mixing that mass ratio is 1: 9: 2, obtain the mixture containing attapulgite.
Step 2: said mixture is loaded in stainless steel autoclave, sealing autoclave post-heating to 200 DEG C and guarantor Temperature reaction 8 hours.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, obtain hole, attapulgite Quito silicon nanowires.
The SEM of prepared material is shown in Fig. 5, as seen from Figure 5, it can be seen that porous silicon is interconnective nano wire shape Form with nano-particle, and the length of the nano wire of some porous silicon is more than 1 micron.
Embodiment 3:
Step one: the attapulgite of 100 g is joined after filtering after ultrasonic 1 hour in 200 mL aqueous solvents or being centrifugal dry Dry, obtain attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 8: 1, obtain containing recessed The mixture of convex rod soil.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 220 DEG C and insulation is anti- Answer 7 hours；
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, wash with distilled water back mixing Wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, i.e. can get porous silicon nano wire.
The SEM of prepared material is shown in Fig. 6, and porous silicon is interconnective nano wire shape and nano-particle as seen from Figure 6 Composition, and the length of the nano wire of some porous silicon is more than 2 microns.
Embodiment 4:
Step one: with the ratio that mass ratio is 3: 1, aluminium powder and magnesium powder are mixed in advance, form aluminium powder and the mixture of magnesium powder.
The attapulgite of 100g is joined in the dilute hydrochloric acid solvent of 200mL, 0.1M filter after ultrasonic 0.6 hour or It is dried after Li Xin, obtains attapulgite, more dried attapulgite will add aluminum chloride, aluminium powder or aluminium powder and magnesium powder Mixture, the mass ratio of these three mixture is 1: 10: 2.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 190 DEG C and insulation 12 Hour.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, i.e. can get porous silicon nano wire.
Embodiment 5:
Step one: the attapulgite of 100g is joined 200 mL, in the dilute hydrochloric acid of 0.1M after ultrasonic 0.5 hour filter or It is dried after person is centrifugal, obtains attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 16: 1 Close, obtain the mixture containing attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 240 DEG C and insulation 5 Hour；
Step 3: naturally cool to greenhouse and collect product, after soaking with 0.1M dilute hydrochloric acid, washs with distilled water back mixing, finally uses 4% hydrofluoric acid solution removes remaining Si oxide, i.e. can get porous silicon nano wire.
Embodiment 6:
Step one: the attapulgite of 100g is joined after filtering after ultrasonic 1 hour in 200 mL aqueous solvents or being centrifugal dry Dry, obtain attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 15: 12, acquirement contains The mixture of attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 270 ° of C and insulation 4 Hour；
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, wash with distilled water back mixing Wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, i.e. can get porous silicon nano wire.
Embodiment 7:
Step one: the attapulgite of 100 g is joined 200 mL, mistake after ultrasonic 0.5 hour in the dilute hydrochloric acid solvent of 0.1M Filter or centrifugal after be dried, obtain attapulgite, the most again by attapulgite and aluminum chloride, aluminium powder with 1: 15: 15 quality Ratio mixes, and obtains the mixture containing attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 180 DEG C and insulation 10 Hour.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, i.e. can get porous silicon nano wire.
Embodiment 8:
Step one: the attapulgite of 100 g is joined after filtering after ultrasonic 1.5 hours in 200 mL aqueous solvents or being centrifugal It is dried, obtains attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 30: 20, obtain Mixture containing attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 220 DEG C and insulation 4 Hour.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, finally remove remaining Si oxide by the 2M NaOH solution of 70 DEG C, i.e. can get the porous silicon nano wire of fine work.
Embodiment 9:
Step one: the attapulgite of 100g is joined after filtering after ultrasonic 2 hours in 200 mL aqueous solvents or being centrifugal dry Dry, obtain attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 20: 0.5, obtain Mixture containing attapulgite；
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 180 DEG C and insulation 15 is little Time；
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, wash with distilled water back mixing Wash, finally remove remaining Si oxide with 3% hydrofluoric acid solution, i.e. can get porous silicon nano wire.
Embodiment 10:
Step one: the attapulgite of 100g is joined in the dilute hydrochloric acid solvent of 200mL, 0.1M and filter after ultrasonic 0.5 hour Or be dried after Li Xin, obtain attapulgite, the most again by attapulgite and aluminum chloride, aluminium powder with 1: 24: 25 mass ratio Example mixes, and obtains the mixture containing attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 200 DEG C and insulation 13 Hour.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, i.e. can get porous silicon nano wire.
Embodiment 11:
Step one: the attapulgite of 100g is joined in the dilute hydrochloric acid solvent of 200mL, 0.1M filter after ultrasonic 1 hour or It is dried after person is centrifugal, obtains attapulgite；The most again by attapulgite and aluminum chloride, aluminium powder with 1: 20: 50 mass ratio Mixing, obtains the mixture containing attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 180 DEG C and insulation 3 Hour；
Step 3: naturally cool to greenhouse and collect product, after soaking with 0.1M dilute hydrochloric acid, washs with distilled water back mixing, To porous silicon nano wire.
Embodiment 12:
Step one: the attapulgite of 100g is joined after filtering after ultrasonic 2 hours in 200mL aqueous solvent or being centrifugal dry Dry, obtain attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 30: 20, acquirement contains The mixture of attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 210 ° of C and insulation 12 hours.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffling and wash, the 2M NaOH solution of last 70 DEG C removes remaining Si oxide, i.e. can get the porous silicon nano wire of fine work.
Embodiment 13:
Step one: the attapulgite of 100g is joined 200 mL, filters after ultrasonic 0.5 hour in the dilute hydrochloric acid solvent of 0.1M Or be dried after Li Xin, obtain attapulgite, the most again by attapulgite and aluminum chloride, aluminium powder with 1: 30: 30 mass ratio Example mixes, and obtains the mixture containing attapulgite；
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 240 DEG C and insulation 12 is little Time；
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, wash with distilled water back mixing Wash, i.e. can get the porous silicon nano wire of doped silicon oxide.
Embodiment 14:
Step one: the attapulgite of 100g is joined after filtering after ultrasonic 1 hour in 200 mL aqueous solvents or being centrifugal dry Dry, obtain attapulgite, the most again attapulgite and aluminum chloride, aluminium powder are mixed with the mass ratio of 1: 80: 40, acquirement contains The mixture of attapulgite.
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 240 DEG C and insulation 4 Hour.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, i.e. can get the porous silicon nano wire of doped silicon oxide.
Embodiment 15:
Step one: the attapulgite of 100g is joined in the dilute hydrochloric acid solvent of 200mL, 0.1M mistake after ultrasonic 0.5 hour Filter or centrifugal after be dried, obtain attapulgite, the most again by attapulgite and aluminum chloride, aluminium powder with 1: 100: 50 quality Ratio mixes, and obtains the mixture containing attapulgite；
Step 2: be loaded in stainless steel autoclave by said mixture, sealing autoclave is heated to 280 DEG C and insulation 2 is little Time.
Step 3: reaction naturally cools to greenhouse and collects product after terminating, after soaking with 0.1M dilute hydrochloric acid, anti-with distilled water Shuffle and wash, i.e. can get the porous silicon nano wire of doped silicon oxide.

Claims (4)

1. a kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires, it is characterised in that comprise the following steps:
1) will filter after the solution supersound process containing attapulgite or centrifugal, be then dried and obtain the attapulgite being dried, then By dry attapulgite and aluminum chloride, aluminium powder or aluminium powder and the mixture of magnesium powder, obtain the mixture containing attapulgite；
2) mixture containing attapulgite is heated under air-proof condition 180～280 DEG C react 0.5～40 hour；
3) reaction is cooled to greenhouse after terminating, and collects product, after soaking with dilute hydrochloric acid, with distilled water wash, obtains attapulgite Hole, Quito silicon nanowires.
A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires, it is characterised in that institute Stating the mixture of aluminium powder or aluminium powder and magnesium powder with the mixing quality ratio of dry attapulgite, aluminum chloride is 1～50: 1: 1 ～100.
A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires, it is characterised in that institute State in step 3) for the concentration of dilute hydrochloric acid soaked be 0.1M.
A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires, it is characterised in that After described step 3), then remove remaining Si oxide with the aqueous slkali of Fluohydric acid. or dense heat, obtain refined attapulgite soil matrix Porous silicon nano wire.
CN201610807393.6A 2016-09-07 2016-09-07 A kind of low temperature preparation method of hole, attapulgite Quito silicon nanowires Pending CN106299284A (en)

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