CN105060306A - Preparation method of silica nanotube - Google Patents
Preparation method of silica nanotube Download PDFInfo
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- CN105060306A CN105060306A CN201510488587.XA CN201510488587A CN105060306A CN 105060306 A CN105060306 A CN 105060306A CN 201510488587 A CN201510488587 A CN 201510488587A CN 105060306 A CN105060306 A CN 105060306A
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- silica nanotube
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002071 nanotube Substances 0.000 title claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 239000002070 nanowire Substances 0.000 claims abstract description 8
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 8
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 238000003837 high-temperature calcination Methods 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000877 morphologic effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 3
- 239000000243 solution Substances 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 150000001298 alcohols Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
A preparation method of a silica nanotube is characterized by comprising steps as follows: 1), 1-5 parts of tellurium nanowires are weighed in parts by mass and added to a beaker containing 25-50 parts of absolute ethanol, and the mixture is magnetically stirred for 30-50 minutes to be uniformly dispersed; 2), 6-10 parts of a mixed solution of TEOS (tetraethoxysilane) and anhydrous ethanol in the volume ratio being 1:10 are dropwise added to the solution obtained in the step 1); 3), after the solution is dropwise added, the mixture is stirred for 2-5 hours without light; 4), the mixture is subjected to reduced pressure distillation for 10-40 minutes at the temperature of 45 DEG C-70 DEG C under the pressure of 0.06 MPa-0.1 MPa after stirring ends; 5), a thick liquid obtained from the step 4) is dried and calcined at the high temperature, and a silica nanotube material is obtained. The preparation method has the benefits as follows: 1), the prepared silica nanotube material has good firmness and high morphological plasticity; 2), the product preparation process is simple, the conditions are easy to control, and scale production is facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of Silica Nanotube, belong to field of nano material preparation.
Technical background
Nano silicon is a kind of inorganic chemical industry material, and owing to being ultrafine nanometer, size range, at 1 ~ 100nm, therefore has the character of many uniquenesses, as having anti-ultraviolet optical property, can improve that other materials is anti-aging, intensity and chemical resistance.And nano silicon has undersized effect, high-strength, the strangeness such as high-ductility, good stability of surface-interface effect, quantum size effect and macroscopic quantum channel effect and special optical and electrical properties, high Magnetoresistance Phenomena, nonlinear resistance phenomenon and at high temperature still tool, be widely used every field.Because Silica Nanotube material has superior self film-formed, and anticorrosive, transparent, and the advantages such as physical and chemical performance is stable, can be applicable to for the aspect such as dress of fabric or coating.But there is fastness difference, the problems such as pattern plasticity-is low in the Silica Nanotube product of preparation at present.
Summary of the invention
The object of the invention is to overcome the problems such as the Silica Nanotube fastness difference of producing in prior art, and provide a kind of size uniformity, the preparation method of the titania nanotube that pattern is interweaved.
For achieving the above object, present invention employs following technical scheme:
A preparation method for Silica Nanotube, it comprises the steps:
1) by mass fraction, the tellurium nano-wire taking 1-5 part joins in the beaker containing 25-50 part dehydrated alcohol, within magnetic agitation 30-50 minute, makes to be uniformly dispersed;
2) by mass fraction, be that the tetraethoxy TEOS/ dehydrated alcohol mixing solutions of 1:10 is dropwise added drop-wise in step 1) solution by 6-10 part volume ratio;
3), after dropwising, 2-5 hour is stirred in above-mentioned system shading;
4) stir terminate after at temperature 45-70 DEG C, underpressure distillation 10-40 minute under pressure 0.06-0.1Mpa;
5), after the slurry of gained in step 4) being carried out oven dry and high-temperature calcination, Silica Nanotube material had both been obtained.
The invention has the beneficial effects as follows:
1) what the present invention prepared is good based on Silica Nanotube material fastness, and morphological plasticity is high.
2) this product preparation process is simple, and condition is easy to control, and is convenient to scale production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Silica Nanotube of the present invention.
Fig. 2 is the transmission electron microscope picture of Silica Nanotube of the present invention.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Be scanning electron microscope (SEM) photograph and the transmission electron microscope picture of inventive silica nanotube as shown in Figure 1, 2, it is by the surface adsorption layer of silicon dioxide of distillation under vacuum in tellurium nano-wire template.Subsequently after lyophilize plastotype and high-temperature calcination, size uniformity can be obtained, the Silica Nanotube that pattern is interweaved.
A preparation method for Silica Nanotube, it comprises the steps:
1) by mass fraction, the tellurium nano-wire taking 1-5 part joins in the beaker containing 25-50 part dehydrated alcohol, within magnetic agitation 30-50 minute, makes to be uniformly dispersed;
2) by mass fraction, be that the tetraethoxy TEOS/ dehydrated alcohol mixing solutions of 1:10 is dropwise added drop-wise in step 1) solution by 6-10 part volume ratio;
3), after dropwising, 2-5 hour is stirred in above-mentioned system shading;
4) stir terminate after at temperature 45-70 DEG C, underpressure distillation 10-40 minute under pressure 0.06-0.1Mpa;
5), after the slurry of gained in step 4) being carried out oven dry and high-temperature calcination, Silica Nanotube material had both been obtained.
Embodiment 1:
A preparation method for Silica Nanotube, it comprises the steps:
1) by mass fraction, the tellurium nano-wire taking 1 part joins in the beaker containing 25 parts of dehydrated alcohols, and magnetic agitation makes to be uniformly dispersed for 30 minutes;
2) by mass fraction, be that the tetraethoxy TEOS/ dehydrated alcohol mixing solutions of 1:10 is dropwise added drop-wise in step 1) solution by 6 parts of volume ratios;
3), after dropwising, above-mentioned system shading is stirred 2 hours;
4) stir terminate after at temperature 45 C, underpressure distillation 10 minutes under pressure 0.06Mpa;
5), after the slurry of gained in step 4) being carried out oven dry and high-temperature calcination, Silica Nanotube material had both been obtained.
Embodiment 2:
A preparation method for Silica Nanotube, it comprises the steps:
1) by mass fraction, the tellurium nano-wire taking 3 parts joins in the beaker containing 40 parts of dehydrated alcohols, and magnetic agitation makes to be uniformly dispersed for 40 minutes;
2) by mass fraction, be that the tetraethoxy TEOS/ dehydrated alcohol mixing solutions of 1:10 is dropwise added drop-wise in step 1) solution by 8 parts of volume ratios;
3), after dropwising, above-mentioned system shading is stirred 3 hours;
4) stir terminate after at temperature 60 C, underpressure distillation 20 minutes under pressure 0.08Mpa;
5), after the slurry of gained in step 4) being carried out oven dry and high-temperature calcination, Silica Nanotube material had both been obtained.
Embodiment 3:
A preparation method for Silica Nanotube, it comprises the steps:
1) by mass fraction, the tellurium nano-wire taking 5 parts joins in the beaker containing 50 parts of dehydrated alcohols, and magnetic agitation makes to be uniformly dispersed for 50 minutes;
2) by mass fraction, be that the tetraethoxy TEOS/ dehydrated alcohol mixing solutions of 1:10 is dropwise added drop-wise in step 1) solution by 10 parts of volume ratios;
3), after dropwising, above-mentioned system shading is stirred 5 hours;
4) stir terminate after at temperature 70 C, underpressure distillation 40 minutes under pressure 0.1Mpa;
5), after the slurry of gained in step 4) being carried out oven dry and high-temperature calcination, Silica Nanotube material had both been obtained.
Claims (1)
1. a preparation method for Silica Nanotube, is characterized in that it comprises the steps:
1) by mass fraction, the tellurium nano-wire taking 1-5 part joins in the beaker containing 25-50 part dehydrated alcohol, within magnetic agitation 30-50 minute, makes to be uniformly dispersed;
2) by mass fraction, be that the tetraethoxy TEOS/ dehydrated alcohol mixing solutions of 1:10 is dropwise added drop-wise in step 1) solution by 6-10 part volume ratio;
3), after dropwising, 2-5 hour is stirred in above-mentioned system shading;
4) stir terminate after at temperature 45-70 DEG C, underpressure distillation 10-40 minute under pressure 0.06-0.1Mpa;
5), after the slurry of gained in step 4) being carried out oven dry and high-temperature calcination, Silica Nanotube material had both been obtained.
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| CN201510488587.XA CN105060306B (en) | 2015-08-11 | 2015-08-11 | Preparation method of silica nanotube |
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| CN105060306B CN105060306B (en) | 2017-04-19 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106975756A (en) * | 2017-04-07 | 2017-07-25 | 厦门大学 | A kind of preparation method of rhodium tellurium alloy hollow nanotube |
| CN109970070A (en) * | 2017-12-27 | 2019-07-05 | 中国科学技术大学 | A kind of Silica Nanotube and preparation method thereof |
| CN110642280A (en) * | 2019-11-09 | 2020-01-03 | 王杰 | alpha-Al2O3Nanotube and method for preparing the same |
| CN110862089A (en) * | 2019-12-09 | 2020-03-06 | 徐少晨 | Preparation method of mesoporous hollow silicon spheres |
| CN112072098A (en) * | 2020-09-22 | 2020-12-11 | 福州大学 | Nanotube-shaped silicon-based material for lithium battery and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318658A (en) * | 2008-07-01 | 2008-12-10 | 上海大学 | Method for preparing silicon dioxide nano-tube with multi-walled carbon nanotube |
| KR20110002387A (en) * | 2009-07-01 | 2011-01-07 | (주)씽크루트 | Preparation methods for silicon dioxide nano-wire |
| CN104692398A (en) * | 2015-02-03 | 2015-06-10 | 天津大学 | Preparation method for three-dimensional continuous silicon dioxide nanotube |
-
2015
- 2015-08-11 CN CN201510488587.XA patent/CN105060306B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318658A (en) * | 2008-07-01 | 2008-12-10 | 上海大学 | Method for preparing silicon dioxide nano-tube with multi-walled carbon nanotube |
| KR20110002387A (en) * | 2009-07-01 | 2011-01-07 | (주)씽크루트 | Preparation methods for silicon dioxide nano-wire |
| CN104692398A (en) * | 2015-02-03 | 2015-06-10 | 天津大学 | Preparation method for three-dimensional continuous silicon dioxide nanotube |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106975756A (en) * | 2017-04-07 | 2017-07-25 | 厦门大学 | A kind of preparation method of rhodium tellurium alloy hollow nanotube |
| CN106975756B (en) * | 2017-04-07 | 2019-02-15 | 厦门大学 | A kind of preparation method of rhodium tellurium alloy hollow nanotube |
| CN109970070A (en) * | 2017-12-27 | 2019-07-05 | 中国科学技术大学 | A kind of Silica Nanotube and preparation method thereof |
| CN109970070B (en) * | 2017-12-27 | 2022-09-06 | 中国科学技术大学 | Silicon dioxide nanotube and preparation method thereof |
| CN110642280A (en) * | 2019-11-09 | 2020-01-03 | 王杰 | alpha-Al2O3Nanotube and method for preparing the same |
| CN110862089A (en) * | 2019-12-09 | 2020-03-06 | 徐少晨 | Preparation method of mesoporous hollow silicon spheres |
| CN112072098A (en) * | 2020-09-22 | 2020-12-11 | 福州大学 | Nanotube-shaped silicon-based material for lithium battery and preparation method thereof |
| CN112072098B (en) * | 2020-09-22 | 2021-06-29 | 福州大学 | Nanotube-shaped silicon-based material for lithium battery and preparation method thereof |
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| CN105060306B (en) | 2017-04-19 |
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Effective date of registration: 20180122 Address after: 315806 north side of No. 1, No. 1, West Avenue, Zhejiang Free Trade Zone Patentee after: NINGBO TONGJING ZIZAI ENVIRONMENT TECHNOLOGY CO.,LTD. Address before: 310000 room 8613, main building, Hangzhou platinum Hotel Irene Co., Ltd., Jianggan District hang Hai Road, Jianggan District, Hangzhou, Zhejiang Patentee before: HANGZHOU YUJING ENVIRONMENTAL SCIENCE AND TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20200318 Address after: Room 501, qixianqiao village, Liangzhu street, Yuhang District, Hangzhou City, Zhejiang Province Patentee after: HANGZHOU TONG KING ENVIRONMENT TECHNOLOGY Co.,Ltd. Address before: 315806 north side of No. 1, No. 1, West Avenue, Zhejiang Free Trade Zone Patentee before: NINGBO TONGJING ZIZAI ENVIRONMENT TECHNOLOGY CO.,LTD. |
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Application publication date: 20151118 Assignee: Shenzhen Titanium and New Material Technology Co.,Ltd. Assignor: HANGZHOU TONG KING ENVIRONMENT TECHNOLOGY Co.,Ltd. Contract record no.: X2023990000617 Denomination of invention: A Preparation Method of Silicon Dioxide Nanotubes Granted publication date: 20170419 License type: Exclusive License Record date: 20230619 |