CN107501895A - A kind of preparation method of composite nanometer conductive material - Google Patents
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Abstract
The invention provides a kind of preparation method of composite nanometer conductive material, comprise the following steps:Stirring after copper chloride, alchlor, calcium chloride, ferric chloride (FeCl36H2O) and ethylene glycol ultrasound is added into anhydrous sodium acetate and polyethylene glycol;Add in polytetrafluoroethylene (PTFE) and reacted in kettle, washing and drying obtains product A;Nano zine oxide, polyoxyethylene sorbitan monoleate, Aerosol OT, lauroyl diethanolamine and distilled water are mixed, add product A, ultrasonic disperse;Stood after stopping stirring, add cocinic acid, phytic acid and pyrrole monomer, stirring reaction after cooling, filtration washing drying, obtain product B;Product B and distilled water are mixed, iron pentacarbonyl, piperidines and ammonium metavanadate is added, formic acid, stirring reaction, filtration washing drying is added under water-bath.Material easy processing shaping prepared by the preparation method of this composite nanometer conductive material, electric conductivity is splendid, all has potential application value in terms of electric transducer, solar cell, ultracapacitor.
Description
Technical field
The present invention relates to a kind of preparation method of composite nanometer conductive material.
Background technology
Nanometer technology is emerging in the last few years, has a kind of technology with broad prospects for development, at present to a certain degree
On be used for the industries such as medicine, chemistry, electronic information and machinery.Nanometer technology refers to manufacture material with single atom, molecule
Science and technology, research structure the size property of material and application in 0.1 to 100 nanometer range.And so-called nano material, refer to
It is at least one-dimensional in nano-scale (0.1-100 nm) or by the material that they are formed as elementary cell in three dimensions,
This is about as much as the yardstick that 10-100 atom is arranged closely together.Because its size is already close to the relevant length of electronics
Degree, great changes will take place because strong relevant caused self-organizing causes property for its property, also, its yardstick is close to light
Wavelength, has the special effects of large surface plus it, therefore its characteristic for being showed, such as fusing point, magnetic, optics, heat conduction, conduction
Characteristic etc., the property often showed different from the material in integrality.At present, existing a variety of nano materials are closed
Into such as nano semiconductor material and metal nano material.In recent years, nanometer conductive material is also included into nano materials research model
Enclose, but nanometer conductive material processing is whard to control, the lattice structure not determined, therefore, it is also desirable to largely next pair of research
It is controlled and improved.
The content of the invention
Technical problems to be solved:It is an object of the invention to provide a kind of preparation method of composite nanometer conductive material, institute
The composite nanometer conductive material easy processing shaping of preparation, electric conductivity is splendid, in electric transducer, solar cell, ultracapacitor
Aspect all has potential application value.
Technical scheme:A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:By 2-4 parts copper chloride, 1-3 parts alchlor, 1-2 parts calcium chloride, 1-2 parts ferric chloride (FeCl36H2O) and 80-100 parts
Ethylene glycol is mixed, and 7-9 part nothings are added while stirring under rotating speed 200-400r/min with magnetic stirrer after ultrasonic 20-30 minutes
Water sodium acetate and 2-3 part polyethylene glycol, continue to stir 30-40 minutes;
Step 2:Add in polytetrafluoroethylene (PTFE) in kettle, 7-9 hours are reacted at 220-240 DEG C, are entered respectively with distilled water and ethanol
Row washing, is put into baking oven and dries, obtain product A;
Step 3:By 0.2-0.5 parts nano zine oxide, 0.3-0.7 parts Tween-80,0.2-0.4 part butanedioic acid di-isooctyls
Sodium sulfonate, 0.1-0.3 parts lauroyl diethanolamine and 80-120 parts distilled water mix, and add product A, are put into Ultrasound Instrument
Carry out ultrasonic disperse 2-3 hours;
Step 4:10-15 minutes are stood after stopping stirring, add 0.5-1 parts cocinic acid, 0.2-0.4 parts phytic acid and 1-2 part pyrroles
Monomer is coughed up, is put into refrigerator, 5-10 minutes are cooled down at 0-5 DEG C of temperature, stirring reaction 2-3 hours after taking-up, filtering, are used respectively
Distilled water and ethanol are washed, and are put into baking oven and are dried, and obtain product B;
Step 5:Product B and 20-30 part distilled water is mixed, carries out ultrasonic disperse, adds 1-2 parts iron pentacarbonyl, 0.1-0.2 parts
Piperidines and 0.1-0.2 part ammonium metavanadates, water-bath at being 80-100 DEG C in temperature, add 2-5 part formic acid, 30-50 points of stirring reaction
Clock;
Step 6:Continue at normal temperatures stirring reaction 2-3 hours, filtering, washed respectively with distilled water and ethanol, be put into baking
Drying in case.
It is further preferred that ultrasonic time is 25 minutes, rotating speed 250-350r/min in step 1, mixing time is 35 points
Clock.
It is further preferred that temperature is 230 DEG C in step 2, the reaction time is 8 hours.
It is further preferred that jitter time is 2.5 hours in step 3.
It is further preferred that temperature is 1-3 DEG C in step 4, cool time is 7-9 minutes, and the normal-temperature reaction time is 2.5 small
When.
It is further preferred that bath temperature is 85-95 DEG C in step 5, the reaction time is 35-45 minutes.
It is further preferred that the stirring reaction time is 2.5 hours in step 6.
Beneficial effect:With the composite nanometer conductive material prepared by the present invention, particle diameter is between 5.5-5.7nm, easy processing
Shaping, electric conductivity is splendid, and electrical conductivity reaches as high as 211S/cm, in terms of electric transducer, solar cell, ultracapacitor all
With potential application value.
Embodiment
Embodiment 1
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:2 parts of copper chlorides, 1 part of alchlor, 1 part of calcium chloride, 1 part of ferric chloride (FeCl36H2O) and 80 parts of ethylene glycol are mixed,
Ultrasound adds 7 parts of anhydrous sodium acetates and 2 parts of poly- second two with magnetic stirrer while stirring after 20 minutes under rotating speed 200r/min
Alcohol, continue stirring 30 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7 hours at 220 DEG C, washed respectively with distilled water and ethanol,
It is put into baking oven and dries, obtains product A;
Step 3:By 0.2 part of nano zine oxide, 0.3 part of Tween-80,0.2 part of Aerosol OT, 0.1 part
Lauroyl diethanolamine and 80 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 2 hours;
Step 4:10 minutes are stood after stopping stirring, 0.5 part of cocinic acid, 0.2 part of phytic acid and 1 part of pyrrole monomer is added, is put into
In refrigerator, cool down 5 minutes, stirring reaction 2 hours after taking-up, filtering, washed respectively with distilled water and ethanol at 0 DEG C of temperature
Wash, be put into baking oven and dry, obtain product B;
Step 5:Product B and 20 parts of distilled water are mixed, carry out ultrasonic disperse, adds 1 part of iron pentacarbonyl, 0.1 part of piperidines and 0.1
Part ammonium metavanadate, water-bath at being 80 DEG C in temperature, adds 2 parts of formic acid, stirring reaction 30 minutes;
Step 6:Continue stirring reaction at normal temperatures 2 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven
Middle drying.
Embodiment 2
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:By 2.5 parts of copper chlorides, 1.5 parts of alchlors, 1.5 parts of calcium chloride, 1.5 parts of ferric chloride (FeCl36H2O)s and 85 parts of second two
Alcohol mixes, and ultrasound adds 8 parts of anhydrous sodium acetates and 2.5 with magnetic stirrer while stirring after 25 minutes under rotating speed 250r/min
Part polyethylene glycol, continues stirring 35 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7.5 hours at 225 DEG C, washed respectively with distilled water and ethanol
Wash, be put into baking oven and dry, obtain product A;
Step 3:By 0.3 part of nano zine oxide, 0.4 part of Tween-80,0.25 part of Aerosol OT, 0.15
Part lauroyl diethanolamine and 90 parts of distilled water mix, and add product A, and it is small to be put into progress ultrasonic disperse 2.5 in Ultrasound Instrument
When;
Step 4:11 minutes are stood after stopping stirring, 0.6 part of cocinic acid, 0.25 part of phytic acid and 1.5 parts of pyrrole monomers is added, puts
Enter in refrigerator, cooled down 6 minutes at 1 DEG C of temperature, stirring reaction 2.5 hours after taking-up, filtering, entered respectively with distilled water and ethanol
Row washing, is put into baking oven and dries, obtain product B;
Step 5:Product B and 25 parts of distilled water are mixed, carry out ultrasonic disperse, add 1.2 parts of iron pentacarbonyls, 0.15 part of piperidines and
0.12 part of ammonium metavanadate, water-bath at being 90 DEG C in temperature, adds 3 parts of formic acid, stirring reaction 35 minutes;
Step 6:Continue stirring reaction at normal temperatures 2.5 hours, filtering, washed respectively with distilled water and ethanol, be put into baking
Drying in case.
Embodiment 3
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:3 parts of copper chlorides, 2 parts of alchlors, 1.5 parts of calcium chloride, 1.5 parts of ferric chloride (FeCl36H2O)s and 90 parts of ethylene glycol are mixed
Close, ultrasound adds 8 parts of anhydrous sodium acetates while stirring under rotating speed 300r/min with magnetic stirrer after 25 minutes and 2.5 parts poly-
Ethylene glycol, continue stirring 35 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 8 hours at 230 DEG C, washed respectively with distilled water and ethanol,
It is put into baking oven and dries, obtains product A;
Step 3:By 0.35 part of nano zine oxide, 0.5 part of Tween-80,0.3 part of Aerosol OT, 0.2 part
Lauroyl diethanolamine and 100 parts of distilled water mix, and add product A, and it is small to be put into progress ultrasonic disperse 2.5 in Ultrasound Instrument
When;
Step 4:13 minutes are stood after stopping stirring, 0.7 part of cocinic acid, 0.3 part of phytic acid and 1.5 parts of pyrrole monomers is added, puts
Enter in refrigerator, cooled down 7 minutes at 3 DEG C of temperature, stirring reaction 2.5 hours after taking-up, filtering, entered respectively with distilled water and ethanol
Row washing, is put into baking oven and dries, obtain product B;
Step 5:Product B and 25 parts of distilled water are mixed, carry out ultrasonic disperse, add 1.5 parts of iron pentacarbonyls, 0.15 part of piperidines and
0.15 part of ammonium metavanadate, water-bath at being 90 DEG C in temperature, adds 3.5 parts of formic acid, stirring reaction 40 minutes;
Step 6:Continue stirring reaction at normal temperatures 2.5 hours, filtering, washed respectively with distilled water and ethanol, be put into baking
Drying in case.
Embodiment 4
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:By 3.5 parts of copper chlorides, 2.5 parts of alchlors, 1.5 parts of calcium chloride, 1.5 parts of ferric chloride (FeCl36H2O)s and 95 parts of second two
Alcohol mixes, and ultrasound adds 8 parts of anhydrous sodium acetates and 2.5 with magnetic stirrer while stirring after 25 minutes under rotating speed 350r/min
Part polyethylene glycol, continues stirring 35 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 8.5 hours at 235 DEG C, washed respectively with distilled water and ethanol
Wash, be put into baking oven and dry, obtain product A;
Step 3:By 0.4 part of nano zine oxide, 0.6 part of Tween-80,0.35 part of Aerosol OT, 0.25
Part lauroyl diethanolamine and 110 parts of distilled water mix, and add product A, and it is small to be put into progress ultrasonic disperse 2.5 in Ultrasound Instrument
When;
Step 4:14 minutes are stood after stopping stirring, 0.9 part of cocinic acid, 0.35 part of phytic acid and 1.5 parts of pyrrole monomers is added, puts
Enter in refrigerator, cooled down 9 minutes at 4 DEG C of temperature, stirring reaction 2.5 hours after taking-up, filtering, entered respectively with distilled water and ethanol
Row washing, is put into baking oven and dries, obtain product B;
Step 5:Product B and 25 parts of distilled water are mixed, carry out ultrasonic disperse, add 1.5 parts of iron pentacarbonyls, 0.15 part of piperidines and
0.15 part of ammonium metavanadate, water-bath at being 95 DEG C in temperature, adds 4 parts of formic acid, stirring reaction 45 minutes;
Step 6:Continue stirring reaction at normal temperatures 2.5 hours, filtering, washed respectively with distilled water and ethanol, be put into baking
Drying in case.
Embodiment 5
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:4 parts of copper chlorides, 3 parts of alchlors, 2 parts of calcium chloride, 2 parts of ferric chloride (FeCl36H2O)s and 100 parts of ethylene glycol are mixed,
Ultrasound adds 9 parts of anhydrous sodium acetates and 3 parts of poly- second two with magnetic stirrer while stirring after 30 minutes under rotating speed 400r/min
Alcohol, continue stirring 40 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 9 hours at 240 DEG C, washed respectively with distilled water and ethanol,
It is put into baking oven and dries, obtains product A;
Step 3:By 0.5 part of nano zine oxide, 0.7 part of Tween-80,0.4 part of Aerosol OT, 0.3 part
Lauroyl diethanolamine and 120 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 3 hours;
Step 4:15 minutes are stood after stopping stirring, 1 part of cocinic acid, 0.4 part of phytic acid and 2 parts of pyrrole monomers is added, is put into ice
In case, cool down 10 minutes, stirring reaction 3 hours after taking-up, filtering, washed respectively with distilled water and ethanol at 5 DEG C of temperature
Wash, be put into baking oven and dry, obtain product B;
Step 5:Product B and 30 parts of distilled water are mixed, carry out ultrasonic disperse, adds 2 parts of iron pentacarbonyls, 0.2 part of piperidines and 0.2
Part ammonium metavanadate, water-bath at being 100 DEG C in temperature, adds 2-5 part formic acid, stirring reaction 50 minutes;
Step 6:Continue stirring reaction at normal temperatures 3 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven
Middle drying.
Comparative example 1
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:2 parts of copper chlorides, 1 part of alchlor, 1 part of calcium chloride, 1 part of ferric chloride (FeCl36H2O) and 80 parts of ethylene glycol are mixed,
Ultrasound adds 7 parts of anhydrous sodium acetates and 2 parts of poly- second two with magnetic stirrer while stirring after 20 minutes under rotating speed 200r/min
Alcohol, continue stirring 30 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7 hours at 220 DEG C, washed respectively with distilled water and ethanol,
It is put into baking oven and dries, obtains product A;
Step 3:By 0.2 part of nano zine oxide, 0.3 part of Tween-80,0.2 part of Aerosol OT, 0.1 part
Lauroyl diethanolamine and 80 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 2 hours;
Step 4:Stands 10 minutes after stopping stirring, add 1 part of pyrrole monomer, be put into refrigerator, 5 points of the cooling at 0 DEG C of temperature
Clock, stirring reaction 2 hours after taking-up, filtering, washed respectively with distilled water and ethanol, be put into baking oven and dry, obtain product
B;
Step 5:Product B and 20 parts of distilled water are mixed, carry out ultrasonic disperse, adds 1 part of iron pentacarbonyl, 0.1 part of piperidines and 0.1
Part ammonium metavanadate, water-bath at being 80 DEG C in temperature, adds 2 parts of formic acid, stirring reaction 30 minutes;
Step 6:Continue stirring reaction at normal temperatures 2 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven
Middle drying.
Comparative example 2
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:3 parts of copper chlorides, 2 parts of ferric chloride (FeCl36H2O)s and 80 parts of ethylene glycol are mixed, ultrasound uses magnetic agitation after 20 minutes
Machine adds 7 parts of anhydrous sodium acetates and 2 parts of polyethylene glycol while stirring under rotating speed 200r/min, continues stirring 30 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7 hours at 220 DEG C, washed respectively with distilled water and ethanol,
It is put into baking oven and dries, obtains product A;
Step 3:By 0.2 part of nano zine oxide, 0.3 part of Tween-80,0.2 part of Aerosol OT, 0.1 part
Lauroyl diethanolamine and 80 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 2 hours;
Step 4:10 minutes are stood after stopping stirring, 0.5 part of cocinic acid, 0.2 part of phytic acid and 1 part of pyrrole monomer is added, is put into
In refrigerator, cool down 5 minutes, stirring reaction 2 hours after taking-up, filtering, washed respectively with distilled water and ethanol at 0 DEG C of temperature
Wash, be put into baking oven and dry, obtain product B;
Step 5:Product B and 20 parts of distilled water are mixed, carry out ultrasonic disperse, adds 1 part of iron pentacarbonyl, 0.1 part of piperidines and 0.1
Part ammonium metavanadate, water-bath at being 80 DEG C in temperature, adds 2 parts of formic acid, stirring reaction 30 minutes;
Step 6:Continue stirring reaction at normal temperatures 2 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven
Middle drying.
Each embodiment is compared with comparative example, comparing result is as shown in the table, it may be seen that prepared by the present invention
Material particle size is between 5.5-5.7nm, and easy processing shaping, electric conductivity is splendid, and electrical conductivity reaches as high as 211S/cm, in fax sense
All there is potential application value in terms of device, solar cell, ultracapacitor.
The partial properties index of the composite nanometer conductive material of table 1
Name of product | Material particle size(nm) | Electrical conductivity(S/cm) |
Embodiment 1 | 5.5 | 205 |
Embodiment 2 | 5.5 | 208 |
Embodiment 3 | 5.7 | 209 |
Embodiment 4 | 5.6 | 211 |
Embodiment 5 | 5.5 | 208 |
Comparative example 1 | 5.5 | 201 |
Comparative example 2 | 5.8 | 189 |
Claims (7)
- A kind of 1. preparation method of composite nanometer conductive material, it is characterised in that:Comprise the following steps:Step 1:By 2-4 parts copper chloride, 1-3 parts alchlor, 1-2 parts calcium chloride, 1-2 parts ferric chloride (FeCl36H2O) and 80-100 parts Ethylene glycol is mixed, and 7-9 part nothings are added while stirring under rotating speed 200-400r/min with magnetic stirrer after ultrasonic 20-30 minutes Water sodium acetate and 2-3 part polyethylene glycol, continue to stir 30-40 minutes;Step 2:Add in polytetrafluoroethylene (PTFE) in kettle, 7-9 hours are reacted at 220-240 DEG C, are entered respectively with distilled water and ethanol Row washing, is put into baking oven and dries, obtain product A;Step 3:By 0.2-0.5 parts nano zine oxide, 0.3-0.7 parts Tween-80,0.2-0.4 part butanedioic acid di-isooctyls Sodium sulfonate, 0.1-0.3 parts lauroyl diethanolamine and 80-120 parts distilled water mix, and add product A, are put into Ultrasound Instrument Carry out ultrasonic disperse 2-3 hours;Step 4:10-15 minutes are stood after stopping stirring, add 0.5-1 parts cocinic acid, 0.2-0.4 parts phytic acid and 1-2 part pyrroles Monomer is coughed up, is put into refrigerator, 5-10 minutes are cooled down at 0-5 DEG C of temperature, stirring reaction 2-3 hours after taking-up, filtering, are used respectively Distilled water and ethanol are washed, and are put into baking oven and are dried, and obtain product B;Step 5:Product B and 20-30 part distilled water is mixed, carries out ultrasonic disperse, adds 1-2 parts iron pentacarbonyl, 0.1-0.2 parts Piperidines and 0.1-0.2 part ammonium metavanadates, water-bath at being 80-100 DEG C in temperature, add 2-5 part formic acid, 30-50 points of stirring reaction Clock;Step 6:Continue at normal temperatures stirring reaction 2-3 hours, filtering, washed respectively with distilled water and ethanol, be put into baking Drying in case.
- A kind of 2. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 1 Middle ultrasonic time is 25 minutes, rotating speed 250-350r/min, and mixing time is 35 minutes.
- A kind of 3. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 2 Middle temperature is 230 DEG C, and the reaction time is 8 hours.
- A kind of 4. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 3 Middle jitter time is 2.5 hours.
- A kind of 5. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 4 Middle temperature is 1-3 DEG C, and cool time is 7-9 minutes, and the normal-temperature reaction time is 2.5 hours.
- A kind of 6. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 5 Middle bath temperature is 85-95 DEG C, and the reaction time is 35-45 minutes.
- A kind of 7. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 6 The middle stirring reaction time is 2.5 hours.
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CN102161764A (en) * | 2011-02-25 | 2011-08-24 | 东华大学 | Method for preparing cobalt-zinc ferrite/polypyrrole nano composite material |
CN105632586A (en) * | 2016-03-22 | 2016-06-01 | 苏州捷德瑞精密机械有限公司 | Nano conductive composite material and preparation method therefor |
CN106340401A (en) * | 2016-11-28 | 2017-01-18 | 中物院成都科学技术发展中心 | Preparing method of composite electrode material and application thereof |
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2017
- 2017-09-19 CN CN201710843835.7A patent/CN107501895A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102161764A (en) * | 2011-02-25 | 2011-08-24 | 东华大学 | Method for preparing cobalt-zinc ferrite/polypyrrole nano composite material |
CN105632586A (en) * | 2016-03-22 | 2016-06-01 | 苏州捷德瑞精密机械有限公司 | Nano conductive composite material and preparation method therefor |
CN106340401A (en) * | 2016-11-28 | 2017-01-18 | 中物院成都科学技术发展中心 | Preparing method of composite electrode material and application thereof |
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