CN106669555A - Preparation method of carbon nanotube conductive ball - Google Patents
Preparation method of carbon nanotube conductive ball Download PDFInfo
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- CN106669555A CN106669555A CN201611111742.7A CN201611111742A CN106669555A CN 106669555 A CN106669555 A CN 106669555A CN 201611111742 A CN201611111742 A CN 201611111742A CN 106669555 A CN106669555 A CN 106669555A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
Abstract
The invention provides a preparation method of a carbon nanotube conductive ball. According to the preparation method provided by the invention, by combining the advantages of stability of polymeric microspheres and SiO2 microspheres and high conductivity of a carbon nanotube, the spherical carbon nanotube conductive ball is obtained by coating the polymeric microspheres or SiO2 microspheres as a matrix with a carbon nanotube material, wherein before coating with the carbon nanotube material, surface modification is performed on the polymeric microspheres or SiO2 microspheres by way of acid oxidation. The treatment method is simple and feasible, and can effectively generate oxygen-containing groups on the surfaces of the polymeric microspheres or SiO2 microspheres. Due to the adsorption action of the oxygen-containing groups, the follow-up carbon nanotube can effectively coat the polymeric microspheres or SiO2 microspheres so as to obtain the carbon nanotube conductive ball with a good carbon nanotube coating property.
Description
Technical field
The present invention relates to flat-panel screens field, more particularly to a kind of preparation method of carbon nanotube conducting ball.
Background technology
Conductive gold spacer (Au ball) as the important materials in electronic industry, by commonly used colloidal materials in, at present,
Commonly use mixed with the frame glue of conductive gold spacer to turn on up and down in liquid crystal display (Liquid Crystal Display, LCD) industry
Substrate, forms conductive path.After baseplate-laminating, the gold/nickel integument of conductive gold spacer outer layer can transmit electronics, and (electrical conductivity will
Ask and reach 2.4 × 105S/cm), conductive gold spacer kernel has resilient resin balls can buffer the pressure after laminating.Practical application
When, gold goal is used with frame glue hybrid modulation into gold size, the gold size mainly by conductive gold spacer, resin matrix, dispersant, firming agent,
Accelerator etc. constitutes.The production of conventional conductive gold goal is that the resin ball surface using electroless plating method at a diameter of 5~8 μm is carried out
The parcel of gold/nickel, this method power consumption is big, and complex process, the gold salt used in gold plating process is mostly cyanide, and toxicity is very big,
During be also easy to produce heavy metal pollution, and gold is expensive, increased cost.With the enhancing of people's environmental consciousness, electricity
Plating makes the technique of conductive gold spacer, is gradually substituted by new material new process.
CNT (Carbon Nanotube, CNT) is common one-dimensional carbon nano material, with excellent electrical property
Energy and mechanical performance, are soluble in different solvents in the presence of strength ultrasound, are conducive to industrialized production.In addition,
With the fast development of CNT industrial chains, CNT costs are gradually lowered, Costco Wholesale be no longer able to hinder CNT industrialization and
Large-scale application.Patent document CN105199641 discloses a kind of preparation method of carbon nanotube conducting ball, by by polymer
Microsphere or SiO2Microsphere is added in CNT dispersion, ultrasound, centrifugation, filtration and dried is then carried out, so as to obtain CNT
Parcel polymer microballoon or SiO2The carbon nanotube conducting ball (CNT ball) with superior electrical conductivity of microsphere, the method letter
It is single, environmental protection and energy saving.But in encapsulation process, although possessing the CNT of high specific surface area can wrap microsphere, but due to
Microsphere surface hydrophilic is poor, in follow-up ultrasound or centrifugation processing procedure, the risk of CNT disengagings can be all produced, so as to cause
CNT can not effectively wrap up microsphere.
The method of polymer surface modification is a lot, can substantially be divided into two classes：Chemical modification and physical modification.Chemical modification
Method mainly has chemical oxidization method, chemical etching method, Low Temperature Plasma Treating method, surface grafting method, ion implantation etc..Thing
Reason is modified to include mechanically modifying and surface coating modified etc..In chemical oxidization method, acid oxidase is at a kind of modal surface
Reason method, can oxypolymer surface, generate a series of oxy radical such as hydroxyl, carbonyl, carboxyl, sulfonic group and unsaturated bonds
Etc. oxygen containing polar group, the generation of these groups, polymer surface activation can be made, from oil-wetted surface water-wetted surface is activated into,
Reach the purpose for improving polymer surfaces tension force.
The content of the invention
It is an object of the invention to provide a kind of preparation method of carbon nanotube conducting ball, poly- by the way of acid oxidase
Compound microsphere or SiO2Microsphere surface produces oxy radical so that it is micro- that follow-up CNT can effectively wrap polymer
Ball or SiO2Microsphere and form the good carbon nanotube conducting ball of encapsulation.
For achieving the above object, the present invention provides a kind of preparation method of carbon nanotube conducting ball, comprises the following steps：
Step 1, offer polymer microballoon or SiO2Microsphere, by the way of acid oxidase to the polymer microballoon or
SiO2Microsphere carries out surface modification treatment, in polymer microballoon or SiO2Microsphere surface produces oxy radical, obtains at acid oxidase
The polymer microballoon or SiO of reason2Microsphere；
Step 2, offer carbon nano tube dispersion liquid, by the polymer microballoon or SiO of acid oxidase process2Microsphere is added
In carbon nano tube dispersion liquid, carry out supersound process, be then centrifuged, filtered, rinsing, drying process, obtain CNT and lead
Electric ball.
In the step 1, the mode of the acid oxidase refers to use the mode of chemical reagent acid oxidase, wherein describedization
Reagent is anhydrous chromic acid-sym-tetrachloroethane system oxidation solution, chromic acid-acetic acid system oxidation solution, chloric acid-sulphuric acid system oxidation solution, dichromic acid
The mixed solution of one or more in salt-sulphuric acid system oxidation solution, concentrated nitric acid, concentrated sulphuric acid and hydrogen peroxide.
The chemical reagent is standard chromic acid solution, comprising potassium dichromate, concentrated sulphuric acid and water, wherein potassium dichromate, dense sulfur
The mass ratio of acid and water is 5:100:8.
To the polymer microballoon or SiO by the way of acid oxidase in the step 12Microsphere carries out the modified place in surface
The detailed process of reason is to take polymer microballoon or SiO2Microsphere adds standard chromic acid solution, at 15 DEG C~100 DEG C in beaker
At a temperature of, 0.1min~180min is processed, filter out polymer microballoon or SiO2Microsphere, then using deionized water rinsing, obtains
To the polymer microballoon or SiO of acid oxidase process2Microsphere.
In the step 1, the mode of the acid oxidase refers to the side of the mode or oxonium ion bombardment of ozone acid oxidase
Formula.
The concrete preparation process of carbon nano tube dispersion liquid provided in the step 2 is, there is provided carbon nanotube powder and molten
Agent, the carbon nanotube powder is added in solvent, by ultrasound, stir process, centrifugation, takes supernatant, obtains concentration range
For the carbon nano tube dispersion liquid of 0.01mg/mL~10mg/mL.
The solvent include water, ethanol, ethylene glycol, isopropanol, acetone, chloroform, N-Methyl pyrrolidone, tetrahydrofuran,
One or more in dimethylformamide, toluene.
The concrete preparation process of the carbon nano tube dispersion liquid is additionally included in solvent and adds surfactant.
The surfactant includes sodium lauryl sulphate, ammonium lauryl sulfate, dodecyl sodium sulfate, dodecane
One or more in base benzene sulfonic acid sodium salt, sodium tetradecyl sulfate.
In the step 1, the polymer microballoon includes polystyrene, polyaniline, polypyrrole, polythiophene, polyacrylic acid
One or more in polymer microballoon, the polymer microballoon size uniformity, the particle size range of the polymer microballoon is 1 μm
~50 μm.
Beneficial effect：The present invention provides a kind of preparation method of carbon nanotube conducting ball, conjugated polymer microsphere, SiO2It is micro-
The stability of ball and the high conductivity advantage of CNT, with polymer microballoon or SiO2Based on microsphere, CNT is wrapped up
Material, obtains spherical carbon nanotube conducting ball, wherein, before parcel carbon nano-tube material, by the way of acid oxidase pair
The polymer microballoon or SiO2Microsphere carries out surface modification treatment, and this processing method is simple, can effectively in polymerization
Thing microsphere or SiO2Microsphere surface produces oxy radical, due to the adsorption of oxy radical, and then causes follow-up CNT
Polymer microballoon or SiO can effectively be wrapped2Microsphere and obtain the good carbon nanotube conducting ball of CNT encapsulation.
In order to be able to be further understood that the feature and technology contents of the present invention, refer to below in connection with the detailed of the present invention
Illustrate and accompanying drawing, but accompanying drawing only provides with reference to and illustrates to use, not for being any limitation as to the present invention.
Description of the drawings
Below in conjunction with the accompanying drawings, described in detail by the specific embodiment to the present invention, technical scheme will be made
And other beneficial effects are apparent.
In accompanying drawing,
Fig. 1 is the flow chart of the preparation method of the carbon nanotube conducting ball of the present invention；
Fig. 2 is the carbon nanotube conducting ball obtained by the embodiment 1 of the preparation method of the carbon nanotube conducting ball of the present invention
Stereoscan photograph；
Fig. 3 is the carbon nanotube conducting ball obtained by the embodiment 2 of the preparation method of the carbon nanotube conducting ball of the present invention
Stereoscan photograph；
Fig. 4 is the carbon nanotube conducting ball obtained by the embodiment 3 of the preparation method of the carbon nanotube conducting ball of the present invention
Stereoscan photograph.
Specific embodiment
Further to illustrate the technological means taken of the invention and its effect, below in conjunction with being preferable to carry out for the present invention
Example and its accompanying drawing are described in detail.
Fig. 1 is referred to, present invention firstly provides a kind of preparation method of carbon nanotube conducting ball, comprises the following steps：
Step 1, offer polymer microballoon or SiO2Microsphere, by the way of acid oxidase to the polymer microballoon or
SiO2Microsphere carries out surface modification treatment, in polymer microballoon or SiO2Microsphere surface produces oxy radical, obtains at acid oxidase
The polymer microballoon or SiO of reason2Microsphere.
Specifically, in the step 1, refer to use the mode, smelly of chemical reagent acid oxidase by the way of acid oxidase
The mode of oxygen acid oxidase or the mode of oxonium ion bombardment；Wherein, the chemical reagent belongs to Strong oxdiative liquid, can be conventional
Anhydrous chromic acid-sym-tetrachloroethane system oxidation solution, chromic acid-acetic acid system oxidation solution, chloric acid-sulphuric acid system oxidation solution, bichromate-sulphuric acid system
Oxidation solution, concentrated nitric acid, concentrated sulphuric acid and hydrogen peroxide or other reagents with oxidisability, then or can also be above-mentioned
Various mixed solution in solution.
Preferably, polymer microballoon is provided in the step 1, and the mode of the acid oxidase is referred to using chemistry
The mode of reagent acid oxidase, the chemical reagent of Strong oxdiative liquid can oxypolymer microsphere surface, generate a series of oxy radicals
Such as hydroxyl, carbonyl, carboxyl, sulfonic group and unsaturated bond isopolarity group, the generation of these groups, polymer surfaces can be made to live
Change, from oil-wetted surface water-wetted surface is activated into, the purpose for improving polymer surfaces tension force is reached, while the weak side of polymer microballoon
Interlayer is broken to rough structure because being dissolved in Strong oxdiative liquid, so as to increased surface roughness, improves follow-up
The parcel effect of CNT.
It is further preferred that the chemical reagent is standard chromic acid solution, it is by potassium dichromate, concentrated sulphuric acid and water institute structure
Into wherein the mass ratio of potassium dichromate, concentrated sulphuric acid and water is 5:100:8；The step 1 specifically, weigh polymer microballoon in
In beaker, standard chromic acid solution is added, at a temperature of 15 DEG C~100 DEG C, process 0.1min~180min, be then filtered off polymerization
Thing microsphere, using deionized water rinsing polymer microballoon, obtains the polymer microballoon of acid oxidase process, now polymer microballoon table
The oxy radical of carboxyl, hydroxyl and carbonyl is contained in face, so as to contribute to the parcel of follow-up CNT.
Specifically, in the step 1, the polymer microballoon includes polystyrene, polyaniline, polypyrrole, polythiophene, poly-
One or more in acrylate copolymer microsphere, the polymer microballoon size uniformity, the particle diameter model of the polymer microballoon
Enclose for 1 μm~50 μm.
Step 2, offer carbon nano tube dispersion liquid, by the polymer microballoon or SiO of acid oxidase process2Microsphere is added
In carbon nano tube dispersion liquid, carry out supersound process, be then centrifuged, filtered, rinsing, drying process, obtain CNT and lead
Electric ball.
Specifically, the concrete preparation process of the carbon nano tube dispersion liquid of offer is in the step 2, there is provided carbon nanotube powders
End and solvent, the carbon nanotube powder is added in solvent, by ultrasound, stir process, centrifugation, takes supernatant, is obtained dense
Degree scope is the carbon nano tube dispersion liquid of 0.01mg/mL~10mg/mL.
Specifically, the solvent include water, ethanol, ethylene glycol, isopropanol, acetone, chloroform, N-Methyl pyrrolidone, four
One or more in hydrogen furan, dimethylformamide, toluene, polar solvent.
Specifically, the concrete preparation process of the carbon nano tube dispersion liquid is also alternative includes adding surface in a solvent
Activating agent；The surfactant includes sodium lauryl sulphate, ammonium lauryl sulfate, dodecyl sodium sulfate, dodecane
One or more in base benzene sulfonic acid sodium salt, sodium tetradecyl sulfate.
In addition, the present invention can also select the surface oxidation treatment CNT by the way of acid oxidase, then using acid
The CNT of oxidation processes is wrapping up polymer microballoon or SiO2Microsphere, can shadow yet with oxidation is carried out to CNT
Ring CNT electric conductivity, so the present invention preferentially wrapped up using CNT acid oxidase process polymer microballoon or
SiO2The mode of microsphere.
It is below the preferred embodiment of the preparation method of the carbon nanotube conducting ball of the present invention.
Embodiment 1：
Polymer microballoon 1g is taken in beaker, then 20ml standard chromic acid solutions is poured in beaker into, is stirred at 15 DEG C
Reaction 3h, filters out polymer microballoon, using deionized water rinsing polymer microballoon, after dried, obtains acid oxidase process
Polymer microballoon.Then the polymer microballoon stirring ultrasound for processing carbon nano tube dispersion liquid and acid oxidase, is then centrifuged for, Jing
Repeatedly rinse, get rid of the impurity of ball surface, after being dried, as shown in Fig. 2 obtain the good CNT of CNT encapsulation leading
Electric ball.
Embodiment 2：
Polymer microballoon 1g is taken in beaker, then 20ml standard chromic acid solutions is poured in beaker into, is stirred at 60 DEG C
Reaction 10min, filters out polymer microballoon, using deionized water rinsing polymer microballoon, after dried, obtains at acid oxidase
The polymer microballoon of reason.Then the polymer microballoon stirring ultrasound for processing carbon nano tube dispersion liquid and acid oxidase, is then centrifuged for,
Many flushings of Jing, get rid of the impurity of ball surface, after being dried, as shown in figure 3, obtaining the good CNT of CNT encapsulation
Conducting sphere.
Embodiment 3：
Polymer microballoon 1g is taken in beaker, then 20ml standard chromic acid solutions is poured in beaker into, is stirred at 80 DEG C
Reaction 5min, filters out polymer microballoon, using deionized water rinsing polymer microballoon, after dried, obtains at acid oxidase
The polymer microballoon of reason.Then the polymer microballoon stirring ultrasound for processing carbon nano tube dispersion liquid and acid oxidase, is then centrifuged for,
Many flushings of Jing, get rid of the impurity of ball surface, after being dried, as shown in figure 4, obtaining the good CNT of CNT encapsulation
Conducting sphere.
Embodiment 4：
Polymer microballoon 1g is taken in beaker, then 20ml standard chromic acid solutions is poured in beaker into, is stirred at 100 DEG C
Reaction 6s, filters out polymer microballoon, using deionized water rinsing polymer microballoon, after dried, obtains acid oxidase process
Polymer microballoon.Then the polymer microballoon stirring ultrasound for processing carbon nano tube dispersion liquid and acid oxidase, is then centrifuged for, Jing
Repeatedly rinse, get rid of the impurity of ball surface, after being dried, obtain the good carbon nanotube conducting ball of CNT encapsulation.
In sum, the preparation method of carbon nanotube conducting ball of the invention, conjugated polymer microsphere, SiO2Microsphere it is steady
The high conductivity advantage of qualitative and CNT, with polymer microballoon or SiO2Based on microsphere, carbon nano-tube material is wrapped up,
Spherical carbon nanotube conducting ball is obtained, wherein, before parcel carbon nano-tube material, to described poly- by the way of acid oxidase
Compound microsphere or SiO2Microsphere carries out surface modification treatment, and this processing method is simple, can be effectively micro- in polymer
Ball or SiO2Microsphere surface produces oxy radical, due to the adsorption of oxy radical, and then enables follow-up CNT
Effectively wrap polymer microballoon or SiO2Microsphere and obtain the good carbon nanotube conducting ball of CNT encapsulation.
The above, for the person of ordinary skill of the art, can be with technology according to the present invention scheme and technology
Other various corresponding changes and deformation are made in design, and all these changes and deformation should all belong to the claims in the present invention
Protection domain.
Claims (10)
1. a kind of preparation method of carbon nanotube conducting ball, it is characterised in that comprise the following steps：
Step 1, offer polymer microballoon or SiO2Microsphere, to the polymer microballoon or SiO by the way of acid oxidase2It is micro-
Ball carries out surface modification treatment, in polymer microballoon or SiO2Microsphere surface produces oxy radical, obtains the poly- of acid oxidase process
Compound microsphere or SiO2Microsphere；
Step 2, offer carbon nano tube dispersion liquid, by the polymer microballoon or SiO of acid oxidase process2Microsphere adds carbon nanometer
In pipe dispersion liquid, carry out supersound process, be then centrifuged, filtered, rinsing, drying process, obtain carbon nanotube conducting ball.
2. the preparation method of carbon nanotube conducting ball as claimed in claim 1, it is characterised in that in the step 1, the acid
The mode of oxidation refers to use the mode of chemical reagent acid oxidase, wherein the chemical reagent is anhydrous chromic acid-sym-tetrachloroethane
It is oxidation solution, chromic acid-acetic acid system oxidation solution, chloric acid-sulphuric acid system oxidation solution, bichromate-sulphuric acid system oxidation solution, concentrated nitric acid, dense
The mixed solution of one or more in sulphuric acid and hydrogen peroxide.
3. the preparation method of carbon nanotube conducting ball as claimed in claim 2, it is characterised in that the chemical reagent is standard
Chromic acid solution, comprising potassium dichromate, concentrated sulphuric acid and water, the wherein mass ratio of potassium dichromate, concentrated sulphuric acid and water is 5:100:8.
4. the preparation method of carbon nanotube conducting ball as claimed in claim 3, it is characterised in that using acid in the step 1
The mode of oxidation is to the polymer microballoon or SiO2It is to take polymer micro- that microsphere carries out the detailed process of surface modification treatment
Ball or SiO2Microsphere adds standard chromic acid solution in beaker, at a temperature of 15 DEG C~100 DEG C, process 0.1min~
180min, filters out polymer microballoon or SiO2Microsphere, then using deionized water rinsing, obtains the polymerization of acid oxidase process
Thing microsphere or SiO2Microsphere.
5. the preparation method of carbon nanotube conducting ball as claimed in claim 1, it is characterised in that in the step 1, the acid
The mode of oxidation refers to the mode of the mode of ozone acid oxidase or oxonium ion bombardment.
6. the preparation method of carbon nanotube conducting ball as claimed in claim 1, it is characterised in that provide in the step 2
The concrete preparation process of carbon nano tube dispersion liquid is, there is provided carbon nanotube powder and solvent, and the carbon nanotube powder is added
In solvent, by ultrasound, stir process, centrifugation, supernatant is taken, the carbon for obtaining concentration range for 0.01mg/mL~10mg/mL is received
Mitron dispersion liquid.
7. the preparation method of carbon nanotube conducting ball as claimed in claim 6, it is characterised in that the solvent includes water, second
One kind in alcohol, ethylene glycol, isopropanol, acetone, chloroform, N-Methyl pyrrolidone, tetrahydrofuran, dimethylformamide, toluene
Or it is various.
8. the preparation method of carbon nanotube conducting ball as claimed in claim 6, it is characterised in that the carbon nano tube dispersion liquid
Concrete preparation process be additionally included in solvent and add surfactant.
9. the preparation method of carbon nanotube conducting ball as claimed in claim 8, it is characterised in that the surfactant includes
Sodium lauryl sulphate, ammonium lauryl sulfate, dodecyl sodium sulfate, dodecylbenzene sodium sulfonate, sodium tetradecyl sulfate
In one or more.
10. the preparation method of carbon nanotube conducting ball as claimed in claim 1, it is characterised in that described in the step 1
Polymer microballoon includes one or more in polystyrene, polyaniline, polypyrrole, polythiophene, acrylic acid polymer microsphere,
The polymer microballoon size uniformity, the particle size range of the polymer microballoon is 1 μm~50 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107102489A (en) * | 2017-06-20 | 2017-08-29 | 深圳市华星光电技术有限公司 | A kind of anisotropic conductive adhesive paste, conducting sphere and preparation method thereof |
| CN108441151A (en) * | 2018-03-19 | 2018-08-24 | 深圳市华星光电技术有限公司 | A kind of carbon nanotube conducting ball, carbon nanotube conducting glue and liquid crystal display |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107102489A (en) * | 2017-06-20 | 2017-08-29 | 深圳市华星光电技术有限公司 | A kind of anisotropic conductive adhesive paste, conducting sphere and preparation method thereof |
| CN108441151A (en) * | 2018-03-19 | 2018-08-24 | 深圳市华星光电技术有限公司 | A kind of carbon nanotube conducting ball, carbon nanotube conducting glue and liquid crystal display |
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