CN109096756B - Preparation method and application of polyaniline-polyamideimide single-side conductive nano composite film - Google Patents
Preparation method and application of polyaniline-polyamideimide single-side conductive nano composite film Download PDFInfo
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Abstract
The invention belongs to the technical field of modification of high polymer materials and preparation of nano composite materials, and discloses a high-strength and high-modulus single-sided conductive film based on polyamide-imide and a preparation method thereof. The preparation method of the single-sided conductive film comprises the following steps: firstly, soluble polyaniline (poly-o-toluidine and poly-o-anisidine) is synthesized and then doped with organic acid (p-toluenesulfonic acid) to obtain the soluble conductive polyaniline. Then, pouring soluble conductive polyaniline on the upper surface of the polyamide-imide to prepare the polyaniline-polyamide-imide single-sided conductive composite film. The polyaniline-polyamide imide single-sided conductive composite film provided by the invention has higher conductivity and mechanical property, and can be used as an electrical contact material.
Description
Technical Field
The invention belongs to the technical field of preparation of nano composite materials, and particularly relates to a preparation method and application of a polyaniline-polyamide imide single-side conductive nano composite film.
Background
The metal conductive material is easy to oxidize in high-temperature and humid environments, so that overheating and open circuit are easily caused, the service life of electronic product parts is influenced, and safety accidents are caused; and the metal product has heavier mass, higher price and limited resources. With the rapid development of society, a single metal conductive material cannot meet the high requirements of the high-precision industry, and more conductive high polymer materials are discovered. The polymer conductive material is widely applied to the markets of aerospace, transportation, medical and industrial equipment, automobiles, household appliances and electronics. The conductive polyaniline has the advantages of stable chemical properties, difficult oxidation, high and low temperature resistance, high conductivity, easy processing and the like.
The Cu-W alloy and Ag-based contact material (AgSnO) are the most representative of the current electric contact materials2AgCdO, Ag-W series, etc.). W, Ag, etc. are all precious metals, so the resource reserves are limited, and the cost of the electric contact material is too high by using the precious metals as raw materials, which is not beneficial to popularization and application. In addition, the contact material has poor wear resistance and is difficult to use on sliding contacts.
Disclosure of Invention
The single-sided conductive composite film is prepared by adopting soluble polyaniline (poly-o-toluidine or poly-o-anisidine) as a conductive material and polyamide-imide as a flexible high-strength high-modulus mechanical material, so that the cost is reduced, and the problems of increased contact resistance and the like in the use process of a metal material electric contact are solved. The soluble polyaniline has stable chemical property, difficult oxidation, light weight, good conductivity and low price. The polyamide-imide is a flexible material, can be attached to any surface, and has high strength and high modulus. The polyaniline-polyamide imide single-side conductive nano composite film prepared by combining the polyaniline and the polyamide imide can be used for preparing key electric contact materials which are not easy to oxidize, can be attached to any surface and are light in weight.
The polyaniline-polyamide imide single-side conductive nano composite film provided by the invention is a double-layer material compounded by non-conductive polyamide imide and conductive polyaniline.
The preparation method of the polyaniline-polyamide imide single-side conductive nano composite film provided by the invention comprises the following steps:
(1) selection of polyamideimides
Selecting a high-strength and high-modulus polyamide-imide material.
(2) Preparation of polyaniline
Respectively adding newly distilled o-methylaniline or o-anisidine into 0.2mol/L hydrochloric acid solution, stirring at 0-5 ℃ for 0.5-2h, slowly dripping into aqueous solution of ammonium persulfate at the speed of 1-3s per drop, and reacting at 0-5 ℃ for 6-10 h; carrying out suction filtration on the reaction liquid to obtain a green solid, then respectively carrying out soxhlet extraction on the green solid by using methanol, normal hexane and chloroform, and taking a chloroform dissolved part; vacuum drying at 60 deg.C for 12h to obtain hydrochloric acid doped poly-o-toluidine (POT) or poly-o-anisidine (POMA), i.e. soluble polyaniline, which is green powder.
(3) Preparation of p-toluenesulfonic acid doped soluble conductive polyaniline
Adding soluble polyaniline powder into ammonia water with the mass concentration of 10%, stirring at normal temperature for 12-16h, washing with water to be neutral, and vacuum drying at 60 ℃ for 12h to obtain the intrinsic soluble polyaniline powder with the character of purple powder. And then, solution blending is adopted to obtain the soluble polyaniline doped with the p-toluenesulfonic acid, namely, the p-toluenesulfonic acid (TSA) is ground, the intrinsic soluble polyaniline is added, the m-cresol is added, the stirring is continuously carried out for 60min at 90 ℃, and finally, the drying is carried out at 90 ℃ to obtain the soluble conductive polyaniline doped with the p-toluenesulfonic acid.
(4) Preparation of soluble polyaniline-polyamide imide single-side conductive nano composite film
Preparing a solution from soluble conductive polyaniline doped with p-toluenesulfonic acid and chloroform, pouring the solution onto the upper surface of preselected polyamide-imide, and drying at 80-95 ℃ to obtain the soluble polyaniline-polyamide-imide single-side conductive nano composite film.
The polyamide-imide in the step (1) is a flexible material and can be attached to any surface; the thickness of the high-strength high-modulus polyamide-imide layer is 0.2 mm. The structural formula of the polyamide-imide resin is shown as the following formula:
wherein 10< n < 200.
The mol ratio of the o-methylaniline or the o-methoxyaniline in the step (2) to the ammonium persulfate is 1: 1; the prepared polyaniline has stable chemical property, difficult oxidation, light weight and good conductivity.
The p-toluenesulfonic acid doped soluble polyaniline in the step (3) is poly-o-toluidine (POT-TSA) or poly-o-anisidine (POMA-TSA) with the following structural formula.
Wherein 0< y < 1; wherein 10< n.
The mass ratio of the soluble polyaniline to the ammonia water in the step (3) is 1: 20.
The mass ratio of the soluble polyaniline and p-toluenesulfonic acid doping in the step (3) is 1:0.8-1: 2.
The invention also provides application of the prepared polyaniline-polyamideimide single-side conductive nano composite film, and the prepared polyaniline-polyamideimide single-side conductive nano composite film is used as an electric contact material.
Has the advantages that:
the selected polyamide-imide is a flexible high-strength high-modulus mechanical material, is convenient to process and die cut, and can be attached to any surface and curved surface; the material can be used at a high temperature for a long time by utilizing the characteristic of stable chemical property; the material has light weight and high conductivity, and can be used as an electric contact material for long-term use at high temperature.
When the prepared polyaniline-polyamide imide single-side conductive nano composite film is applied to an electric contact, the polyaniline conductive layer can resist high temperature and has good oxidation resistance, the formation of an oxide layer can be reduced, the total contact resistance is reduced, the heat generation in the use process is reduced, the reliability of the electric contact material is improved, and the service life of the electric contact material is prolonged.
Drawings
Fig. 1 is a schematic diagram of a soluble polyaniline-polyamideimide single-sided conductive nanocomposite film.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
The structural formula of the selected polyamide-imide resin (PAI-AU) is shown as follows:
the structural formula of the selected poly-o-toluidine (POT-TSA) or poly-o-anisidine (POMA-TSA) is shown as follows:
example 1
(1) Selection of polyamideimides
Selecting a high-strength and high-modulus polyamide-imide material;
(2) preparation of polyaniline
Respectively adding newly distilled o-toluidine into 0.2mol/L hydrochloric acid solution, stirring at 0 ℃ for 2h, slowly dripping the solution into aqueous solution of ammonium persulfate at the speed of 1-3s per drop, and reacting at 0 ℃ for 10 h; carrying out Soxhlet extraction on green solids obtained by suction filtration of reaction liquid by using methanol, normal hexane and chloroform respectively, taking chloroform dissolved parts, and carrying out vacuum drying at 60 ℃ for 12h to obtain hydrochloric acid doped poly-o-toluidine (POT);
(3) preparation of soluble conductive polyaniline (doped with an organic acid)
Adding soluble polyaniline powder into 10% ammonia water, stirring at normal temperature for 12h, washing with water to neutrality, and vacuum drying at 60 deg.C for 12h to obtain intrinsic soluble polyaniline powder with purple characteristic. Then adopting solution blending to dope poly-o-toluidine and p-toluenesulfonic acid according to the mass ratio of 1:0.8 to obtain soluble polyaniline, namely grinding p-toluenesulfonic acid (TSA), then adding intrinsic soluble polyaniline, adding m-cresol, continuously stirring at 90 ℃ for 60min, and finally drying at 90 ℃ to obtain p-toluenesulfonic acid doped soluble conductive polyaniline;
(4) preparation of soluble polyaniline-polyamide imide single-side conductive nano composite film
And dissolving the soluble conductive polyaniline doped with the p-toluenesulfonic acid in a chloroform solution to prepare a solution of 10mg/ml, stirring for 12 hours, pouring the solution onto a polyamide-imide film with the thickness of 0.2mm, and drying to obtain the conductive polyaniline film with the thickness of 0.02 mm. The conductivity of the soluble polyaniline-polyamide imide single-side conductive nano composite film is 3.02S/m; the tensile strength was 63.5MPa, and the Young's modulus was 1.9 GPa.
Example 2
The difference between the present example and example 1 is that in the preparation step of the soluble polyaniline-polyamideimide single-sided conductive nanocomposite film, the mass ratio of poly-o-toluidine to p-toluenesulfonic acid is 1:1.1, and other treatment means are the same as those in example 1, so that the thickness of the conductive polyaniline layer obtained is 0.02 mm. The conductivity of the soluble polyaniline-polyamide imide single-side conductive nano composite film is 2.51S/m; the tensile strength was 59.6MPa, and the Young's modulus was 1.7 GPa.
Example 3
The difference between the present example and example 1 is that in the preparation step of the soluble polyaniline-polyamideimide single-sided conductive nanocomposite film, poly-o-toluidine and p-toluenesulfonic acid are dissolved in a chloroform solution according to a mass ratio of 1:0.9 to prepare a 40mg/ml solution, and other treatment means are consistent with example 1, so that the thickness of the conductive polyaniline layer obtained is 0.03 mm. The conductivity of the soluble polyaniline-polyamide imide single-side conductive nano composite film is 5.10S/m; the tensile strength was 58.4MPa, and the Young's modulus was 1.6 GPa.
Example 4
The difference between this example and example 1 is that poly-o-anisidine is replaced with poly-o-anisidine in the preparation step of the soluble polyaniline-polyamideimide single-sided conductive nanocomposite film, and the thickness of the conductive polyaniline layer obtained by other treatment methods is 0.02mm, which is the same as that in example 1. The conductivity of the soluble polyaniline-polyamide imide single-side conductive nano composite film is 72.02S/m; the tensile strength was 62.1MPa, and the Young's modulus was 1.8 GPa.
Example 5
The difference between this example and example 1 is that poly-o-anisidine is replaced with poly-o-anisidine and dissolved in chloroform solution in the preparation step of the soluble polyaniline-polyamideimide single-sided conductive nanocomposite film, a 40mg/ml solution is prepared, and other treatment means are the same as those in example 1, and the thickness of the conductive polyaniline layer obtained is 0.03 mm. The conductivity of the soluble polyaniline-polyamide imide single-sided conductive nano composite film is 103.22S/m; the tensile strength was 58.1MPa, and the Young's modulus was 1.3 GPa.
From the results in table 1, it can be seen that: the materials obtained in example 4 and example 5 have high conductivity and low resistance compared with those obtained in examples 1 to 3, which shows that the conductivity of the conductive layer of the composite thin film obtained by the invention can be controlled.
TABLE 1
| Examples | 1 | 2 | 3 | 4 | 5 |
| Conductivity (S/m) | 3.02 | 2.51 | 5.10 | 72.02 | 103.22 |
| Resistivity (omega. m) | 3.31×10-1 | 3.98×10-1 | 1.96×10-1 | 1.39×10-2 | 9.69×10-3 |
| Tensile Strength (MPa) | 63.5 | 59.6 | 58.4 | 62.1 | 58.1 |
| Young's modulus (GPa) | 1.9 | 1.7 | 1.6 | 1.8 | 1.3 |
The above embodiments are only used for illustrating the present invention, and the parameters, implementation conditions and the like of the steps can be changed, and all equivalent changes and improvements based on the technical scheme of the present invention should not be excluded from the protection scope of the present invention.
In conclusion, the polyamideimide-based single-sided conductive composite material disclosed by the invention has excellent conductive performance and mechanical strength, and can be applied to an electrical contact material.
Claims (4)
1. A polyaniline-polyamide imide single-side conductive nano composite film is characterized in that: the single-sided conductive nano composite film is a double-layer material compounded by a non-conductive polyamide imide layer and a conductive polyaniline layer;
the preparation method of the polyaniline-polyamide imide single-side conductive nano composite film comprises the following steps:
(1) selection of polyamideimide:
selecting a high-strength and high-modulus polyamide-imide material;
the polyamide-imide is a flexible material with the thickness of 0.2mm, and the structural formula of the polyamide-imide is shown as the following formula:
wherein 10< n < 2000;
(2) preparing polyaniline:
adding newly distilled o-anisidine into 0.2mol/L hydrochloric acid solution, stirring at 0-5 deg.C for 0.5-2h, slowly dripping into aqueous solution of ammonium persulfate at a speed of 1-3s per drop, and reacting at 0-5 deg.C for 6-10 h; carrying out Soxhlet extraction on green solids obtained by suction filtration of reaction liquid by using methanol, normal hexane and chloroform respectively, taking a chloroform dissolved part, and carrying out vacuum drying for 12h at the temperature of 60 ℃ to obtain hydrochloric acid-doped poly-o-anisidine, namely soluble polyaniline powder;
(3) preparation of p-toluenesulfonic acid doped soluble conductive polyaniline:
adding soluble polyaniline powder into ammonia water with the mass concentration of 10%, stirring at normal temperature for 12-16h, washing with water to be neutral, and vacuum drying at 60 ℃ for 12h to obtain intrinsic soluble polyaniline; grinding p-toluenesulfonic acid, adding eigenstate soluble polyaniline, adding m-cresol, continuously stirring at 50 ℃ for 60min, and finally drying at 90 ℃ to obtain p-toluenesulfonic acid doped soluble conductive polyaniline;
(4) preparing a soluble polyaniline-polyamide imide single-side conductive nano composite film:
preparing a solution of soluble conductive polyaniline doped with p-toluenesulfonic acid and chloroform, pouring the solution onto the upper surface of the selected polyamide-imide in the step (1), and drying to obtain a soluble polyaniline-polyamide-imide single-sided conductive nano composite film;
the thickness of the poured soluble conductive polyaniline layer is 0.02-0.03 mm;
the polyaniline-polyamide imide single-sided conductive nano composite film is used as an electric contact material.
2. The polyaniline-polyamideimide single-sided conductive nanocomposite film according to claim 1, wherein: in the step (2), the molar ratio of the o-anisidine to the ammonium persulfate is 1:1.
3. The polyaniline-polyamideimide single-sided conductive nanocomposite film according to claim 1, wherein: the mass ratio of the soluble polyaniline to the ammonia water in the step (3) is 1: 20.
4. The polyaniline-polyamideimide single-sided conductive nanocomposite film according to claim 1, wherein: in the step (3), the mass ratio of the soluble polyaniline to the p-toluenesulfonic acid is 1:0.8-1: 2.
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