CN101607714A - A kind of preparation method of chrysotile nanotubes in direction arrangement - Google Patents
A kind of preparation method of chrysotile nanotubes in direction arrangement Download PDFInfo
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- CN101607714A CN101607714A CNA2009100895078A CN200910089507A CN101607714A CN 101607714 A CN101607714 A CN 101607714A CN A2009100895078 A CNA2009100895078 A CN A2009100895078A CN 200910089507 A CN200910089507 A CN 200910089507A CN 101607714 A CN101607714 A CN 101607714A
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Abstract
The invention discloses a kind of preparation method of chrysotile nanotubes in direction arrangement, comprise step: 1) NaOH solution is inserted in the hydrothermal reaction kettle; 2) preparation is mixed with the aqueous solution of magnetic ion, adds in the hydrothermal reaction kettle; 3) press MgO and SiO
2Mol ratio is that 3: 2 ratio takes by weighing active MgO and nanometer SiO respectively
2Powder joins in the hydrothermal reaction kettle successively, adds distilled water then in this reaction system, and the pH value of regulating this reaction system is 11～13.8; 4) seal this hydrothermal reaction kettle, and place magnetic field; Simultaneously with hydrothermal reaction kettle heating and under constant temperature, react 15～80h postcooling; Cooled hydrothermal reaction kettle is opened, slowly blotted the supernatant liquid body, and add distilled water slowly and wash until the washing water of sucking-off till the neutrality; The post-heating drying that opens it forms.Its method is simple, and the chrysotile nano-tubes of generation is pure and crystalline texture is perfect, and suitable nanometer assembling also is applied to nanometer superminiature preparation of devices.
Description
Technical field
The present invention relates to a kind of preparation method's of chrysotile nano-tubes, particularly a kind of chrysotile nanotubes in direction arrangement preparation method, belong to field of inorganic nano material.
Background technology
In the prior art, mainly concentrate on for the preparation research of chrysotile nano-tubes and to adopt on the pure or unordered chrysotile nano-tubes that mixes of Hydrothermal Preparation; Disclosed technology comprises employing Hydrothermal Preparation chrysotile monocrystalline, adopts the Hydrothermal Preparation chrysotile nano-tubes and adopt Hydrothermal Preparation doped F e
3+The relevant research report of chrysotile nano-tubes; In recent years, research Fe has also appearred
3+Occupy-place in prepared chrysotile lattice is with the control mechanism of seeking its internal diameter and the growth mechanism of chrysotile nano-tubes; The technical qualification and the product feature of assembled Cds quantum dot in the pure chrysotile nano-tubes that adopts Hydrothermal Preparation are to improve the content of chrysotile nano-tubes at the aspects such as application efficiency aspect the quantum assembling.
Aspect the assembling research of chrysotile nano-tubes, also mainly be at present the method for utilizing physics and chemistry, liquid state or gasiform metal simple-substance and compound are entered in the chrysotile nano-tubes under the effect of external pressure; The method of using has melt injection method, Metalorganic Chemical Vapor Deposition, heating anneal method, sonochemical method and electrochemical deposition method.The material of assembling in the chrysotile pipe has GaAs, Pb, Sn, Hg, InP, CdS, ZnS, NiO.But, make the power that is assembled into of above method all be lower than 5%, and can not obtain the successive quantum wire owing to have impurity in the lack of alignment of chrysotile nano-tubes, pipe; Thereby have influence on the application of chrysotile nano-tubes aspect the quantum assembling.
Summary of the invention
In order to overcome above-mentioned defective of the prior art, the purpose of this invention is to provide a kind of preparation method who is ordered arrangement, the interior inclusion-free of pipe and is chrysotile nanotubes in direction arrangement.
To achieve these goals, the present invention adopts following technical scheme, a kind of preparation method of chrysotile nanotubes in direction arrangement, and it comprises the steps:
1) prepares NaOH solution, and it is inserted in the hydrothermal reaction kettle;
2) by magnetic ion/(Mg+Si) mol ratio is the aqueous solution that 1%～2% preparation is mixed with magnetic ion, it is added in the hydrothermal reaction kettle of step 1);
3) press MgO and SiO
2Mol ratio is that 3: 2 ratio takes by weighing active MgO and nanometer SiO respectively
2Powder joins in the described hydrothermal reaction kettle successively, forms reaction system; Add distilled water then in this reaction system, the pH value of regulating this reaction system is 11～13.8, and keeping total liquor capacity is 65～70% of described hydrothermal reaction kettle cavity volume;
4), and place a magnetic field with the sealing of the described hydrothermal reaction kettle of step 3), to this hydrothermal reaction kettle internal heating and under constant temperature, react 15～80h, naturally cooling then; Cooled hydrothermal reaction kettle is opened, slowly blotted the supernatant liquid body, and add distilled water slowly and wash;
5) repeating step 4) clarification and washing step, until the washing water of sucking-off till the neutrality; With 105 ℃ of dry 10h of described hydrothermal reaction kettle heating, grown along field direction and be chrysotile nanotubes in direction arrangement in the bottom, chamber within it then.
Above-mentioned steps 2) magnetic ion in can be selected Fe for use
3+, Ni
2+, Cr
3+Or Co
2+In any; The aqueous solution that is mixed with magnetic ion can be selected in sulfate liquor, chloride soln or the nitrate aqueous solution any for use.
Above-mentioned steps 3) magneticstrength in is 0.2～0.8T;
Above-mentioned steps 4) the heat drying temperature in is 140～220 ℃.
The present invention adopts as above technical scheme, and it has following advantage: 1) the present invention is by active MgO and SiO cheap and easy to get
2Be raw material, mixed the salts solution of magnetic ion, and reaction system is applied directional magnetic field induce, make chrysotile nano-tubes along the field direction oriented growth.This preparation method is simple, processing condition are easy to control; The chrysotile nano-tubes that is prepared from is pure and crystalline texture is perfect.2) chrysotile nano-tubes of the present invention's preparation is pencil, and regularly arranged, interior pure, the inclusion-free of pipe, and interior external diameter is about ten nm and tens of nm respectively, is about hundreds of nm.This nanotube that aligns is except that the character with conventional monodimension nanometer material, itself also has weak magnetic, and easily by the control of outfields such as electricity, magnetic realization to its performance, thereby make it be more suitable for carrying out nanometer assembling and be applied to nanometer superminiature preparation of devices, have huge potential using value aspect the quantum assembling.
Embodiment
The invention provides a kind of preparation method of chrysotile nanotubes in direction arrangement, it comprises that step is as follows:
1) preparation NaOH solution is inserted in the hydrothermal reaction kettle;
2) be the aqueous solution that 1%～2% requirement preparation is mixed with magnetic ion by the mol ratio of magnetic ion/(Mg+Si), and it is added in the NaOH solution of step 1); Wherein, magnetic ion can be selected Fe for use
3+, Ni
2+, Cr
3+Or Co
2+In any; The aqueous solution is selected in sulfate liquor, chloride soln or the nitrate aqueous solution any for use;
3) press MgO and SiO
2Mol ratio is respectively to take by weighing active MgO and nanometer SiO at 3: 2
2Powder joins step 2 successively) hydrothermal reaction kettle in; Add distilled water again, the pH value of regulating this reaction system maintains 11～13.8, and keeping total liquor capacity is 65～70% of hydrothermal reaction kettle cavity volume;
4) with the sealing of the described hydrothermal reaction kettle of step 3), be placed in the magnetic field that magneticstrength is 0.2～0.8T, and be heated to 140～220 ℃, and under a certain specified temp of this temperature range isothermal reaction 15～80h, naturally cooling then; Then cooled hydrothermal reaction kettle is opened, the supernatant liquid body is slowly blotted, and add distilled water slowly and wash; Repeat clarification and washing step, until the washing water of sucking-off till the neutrality;
5) hydrothermal reaction kettle with step 4) heats 105 ℃ of dry 10h under open state, and having grown along field direction in the hydrothermal reaction kettle bottom is chrysotile nanotubes in direction arrangement.
Below by specific examples technical scheme of the present invention is described in further detail.
Example 1:
1) takes by weighing the 16gNaOH pressed powder and insert in the 200ml volumetric flask, add the NaOH solution of distilled water constant volume preparation 2mol/L; And this solution inserted in the hydrothermal reaction kettle;
2) with magnetic Fe
3+Ion is made dopant ion, presses Fe
3+/ (Mg+Si) mol ratio is that 1% requirement preparation is mixed with Fe
3+Ferric chloride Solution, and it is added in the described NaOH solution of step 1); Press MgO and SiO
2Mol ratio is respectively to take by weighing active MgO and nanometer SiO at 3: 2
2Powder joins in the hydrothermal reaction kettle successively; Add distilled water again, the pH value of regulating its reaction system is 13～13.8, and keeping total liquor capacity is 70% of reactor cavity volume;
3) with step 2) described hydrothermal reaction kettle sealing, be placed in the magnetic field that magneticstrength is 0.5T, and be heated to 220 ℃ of isothermal reaction 72h, naturally cooling then;
4) the described refrigerative hydrothermal reaction kettle of step 3) is opened, the supernatant liquid body is slowly blotted, and add distilled water slowly and wash; Repeat this step until the washing water of sucking-off till the neutrality;
5) with the 105 ℃ of heating 10h under open state of the hydrothermal reaction kettle after the step 4) suction, make this hydrothermal reaction kettle drying, obtaining in the hydrothermal reaction kettle bottom having grown along field direction is chrysotile nanotubes in direction arrangement.
Example 2:
1) this step does not repeat them here with the step 1) in the example 1;
2) with magnetic Fe
3+Ion is made dopant ion, presses Fe
3+/ (Mg+Si) mol ratio is that 1% requirement prepares ferrum sulfuricum oxydatum solutum, and it is added in the described NaOH solution of step 1); Press MgO and SiO
2Mol ratio is respectively to take by weighing active MgO and nanometer SiO at 3: 2
2Powder joins in the hydrothermal reaction kettle successively; Add distilled water again, the pH value of regulating its reaction system is 13～13.8, and keeping total liquor capacity is 70% of reactor cavity volume;
3) with step 2) described hydrothermal reaction kettle sealing, be placed in the magnetic field that magneticstrength is 0.8T, and be heated to 140 ℃ of isothermal reaction 80h, naturally cooling then;
4) the described refrigerative hydrothermal reaction kettle of step 3) is opened, the supernatant liquid body is slowly blotted, and add distilled water slowly and wash; Repeat this step until the washing water of sucking-off till the neutrality;
5) with the 105 ℃ of heating 10h under the opening condition of the hydrothermal reaction kettle after the step 4) suction, make this hydrothermal reaction kettle drying, obtaining in the hydrothermal reaction kettle bottom having grown along field direction is chrysotile nanotubes in direction arrangement.
Example 3:
1) this step does not repeat them here with the step 1) in the example 1;
2) with magnetic Cr
3+Ion is made dopant ion, presses Cr
3+/ (Mg+Si) mol ratio is that 1% requirement prepares CrCl
3Solution, and it is added in the described NaOH solution of step 1); Press MgO and SiO
2Mol ratio is respectively to take by weighing active MgO and nanometer SiO at 3: 2
2Powder joins in the hydrothermal reaction kettle successively; Add distilled water again, the pH value of regulating its reaction system is 11～11.8, and keeping total liquor capacity is 70% of reactor cavity volume;
3) with step 2) described hydrothermal reaction kettle sealing, be placed in the magnetic field that magneticstrength is 0.8T, and be heated to 140 ℃ of isothermal reaction 15h, naturally cooling then;
4) the described refrigerative hydrothermal reaction kettle of step 3) is opened, the supernatant liquid body is slowly blotted, and add distilled water slowly and wash; Repeat this step until the washing water of sucking-off till the neutrality;
5) with the 105 ℃ of heating 10h under the opening condition of the hydrothermal reaction kettle after the step 4) suction, make this hydrothermal reaction kettle drying, obtaining in the hydrothermal reaction kettle bottom having grown along field direction is chrysotile nanotubes in direction arrangement.
Example 4:
1) this step does not repeat them here with the step 1) in the example 1;
2) with magnetic Ni
2+Ion is made dopant ion, presses Ni
2+/ (Mg+Si) mol ratio is that 1% requirement prepares NiCl
2Solution, and it is added in the described NaOH solution of step 1); Press MgO and SiO
2Mol ratio is respectively to take by weighing active MgO and nanometer SiO at 3: 2
2Powder joins in the hydrothermal reaction kettle successively; Add distilled water again, the pH value of regulating its reaction system is 12, and keeping total liquor capacity is 65% of reactor cavity volume;
3) with step 2) described hydrothermal reaction kettle sealing, be placed in the magnetic field that magneticstrength is 0.8T, and be heated to 140 ℃ of isothermal reaction 15h, naturally cooling then;
4) the described refrigerative hydrothermal reaction kettle of step 3) is opened, the supernatant liquid body is slowly blotted, and add distilled water slowly and wash; Repeat this step until the washing water of sucking-off till the neutrality;
5) with the 105 ℃ of heating 10h under the opening condition of the hydrothermal reaction kettle after the step 4) suction, make this hydrothermal reaction kettle drying, obtaining in the hydrothermal reaction kettle bottom having grown along field direction is chrysotile nanotubes in direction arrangement.
Example 5:
1) this step does not repeat them here with the step 1) in the example 1;
2) with magnetic Ni
2+Ion is made dopant ion, presses Ni
2+/ (Mg+Si) mol ratio is that 2% requirement prepares Ni (NO
3)
2Solution, and it is added in the described NaOH solution of step 1); Press MgO and SiO
2Mol ratio is respectively to take by weighing active MgO and nanometer SiO at 3: 2
2Powder joins in the hydrothermal reaction kettle successively; Add distilled water again, the pH value of regulating its reaction system is 13～13.8, and keeping total liquor capacity is 68% of reactor cavity volume;
3) with step 2) described hydrothermal reaction kettle sealing, be placed in the magnetic field that magneticstrength is 0.2T, and be heated to 220 ℃ of isothermal reaction 24h, naturally cooling then;
4) the described refrigerative hydrothermal reaction kettle of step 3) is opened, the supernatant liquid body is slowly blotted, and add distilled water slowly and wash; Repeat this step until the washing water of sucking-off till the neutrality;
5) with the 105 ℃ of heating 10h under the opening condition of the hydrothermal reaction kettle after the step 4) suction, make this hydrothermal reaction kettle drying, obtain along the field direction growth in the hydrothermal reaction kettle bottom and be chrysotile nanotubes in direction arrangement.
Claims (5)
1, a kind of preparation method of chrysotile nanotubes in direction arrangement comprises the steps:
1) prepares NaOH solution, and it is inserted in the hydrothermal reaction kettle;
2) preparation is mixed with the aqueous solution of magnetic ion, and it is added in the hydrothermal reaction kettle of step 1);
3) press MgO and SiO
2Mol ratio is that 3: 2 ratio takes by weighing active MgO and nanometer SiO respectively
2Powder joins in the described hydrothermal reaction kettle successively, forms reaction system; Add distilled water then in this reaction system, the pH value of regulating this reaction system is 11～13.8, and keeping total liquor capacity is 65～70% of described hydrothermal reaction kettle cavity volume;
4) with the sealing of the described hydrothermal reaction kettle of step 3), and place a magnetic field, to this hydrothermal reaction kettle internal heating and under constant temperature, react 15～80h postcooling; Then cooled hydrothermal reaction kettle is opened, slowly blotted the supernatant liquid body, and add distilled water slowly and wash;
5) repeating step 4) clarification and washing step, until the washing water of sucking-off till the neutrality; Then with described hydrothermal reaction kettle heat drying, having grown along field direction at the intracavity bottom of this hydrothermal reaction kettle is chrysotile nanotubes in direction arrangement.
2, preparation method according to claim 1 is characterized in that: step 2) described magnetic ion is Fe
3+, Ni
2+, Cr
3+Or Co
2+In any;
3, preparation method according to claim 1 is characterized in that: step 2) the described aqueous solution that is mixed with magnetic ion be in sulfate liquor, chloride soln or the nitrate aqueous solution any.
4, preparation method according to claim 1 is characterized in that: the intensity in the described magnetic field of step 3) is 0.2～0.8T.
5, according to the described preparation method of claim 1-4, it is characterized in that: the described naturally cooling that is cooled to of step 4); Described Heating temperature is 140～220 ℃.
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| CN 200910089507 CN101607714B (en) | 2009-07-22 | 2009-07-22 | Preparation method of chrysotile nanotube in direction arrangement |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910089507 CN101607714B (en) | 2009-07-22 | 2009-07-22 | Preparation method of chrysotile nanotube in direction arrangement |
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| CN101607714A true CN101607714A (en) | 2009-12-23 |
| CN101607714B CN101607714B (en) | 2010-12-08 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534745A (en) * | 2011-12-26 | 2012-07-04 | 西南科技大学 | Preparation method for nanometer tube of anti-chrysotile structure |
| CN103466647A (en) * | 2013-09-10 | 2013-12-25 | 合肥工业大学 | Method for preparing magnetic chrysotile nanotube |
| CN105679799A (en) * | 2016-01-25 | 2016-06-15 | 京东方科技集团股份有限公司 | Large-size AMOLED display substrate and manufacturing method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100560490C (en) * | 2008-06-18 | 2009-11-18 | 湖南大学 | The method of alkali-free Hydrothermal Preparation chrysotile nano-tubes |
-
2009
- 2009-07-22 CN CN 200910089507 patent/CN101607714B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534745A (en) * | 2011-12-26 | 2012-07-04 | 西南科技大学 | Preparation method for nanometer tube of anti-chrysotile structure |
| CN102534745B (en) * | 2011-12-26 | 2015-03-04 | 西南科技大学 | Preparation method for nanometer tube of anti-chrysotile structure |
| CN103466647A (en) * | 2013-09-10 | 2013-12-25 | 合肥工业大学 | Method for preparing magnetic chrysotile nanotube |
| CN103466647B (en) * | 2013-09-10 | 2015-03-11 | 合肥工业大学 | Method for preparing magnetic chrysotile nanotube |
| CN105679799A (en) * | 2016-01-25 | 2016-06-15 | 京东方科技集团股份有限公司 | Large-size AMOLED display substrate and manufacturing method thereof |
| CN105679799B (en) * | 2016-01-25 | 2018-09-04 | 京东方科技集团股份有限公司 | A kind of large scale AMOLED display base plates and preparation method thereof |
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| CN101607714B (en) | 2010-12-08 |
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