CN105199378A - Anti-abrasion conductive polyimide film and preparation method thereof - Google Patents
Anti-abrasion conductive polyimide film and preparation method thereof Download PDFInfo
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- CN105199378A CN105199378A CN201510615397.XA CN201510615397A CN105199378A CN 105199378 A CN105199378 A CN 105199378A CN 201510615397 A CN201510615397 A CN 201510615397A CN 105199378 A CN105199378 A CN 105199378A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention provides an anti-abrasion conductive polyimide film which is prepared from, by weight, 30-50 parts of cyclobutanetetracarboxylic dianhydride, 20-40 parts of 3,3'4,4'-benzophenone tetracarboxylic acid dianhydride, 25-50 parts of p-phenylenediamine, 20-35 parts of 3,4-diaminodiphenyl ether, 3-10 parts of polyphosphoric acid, 2-8 parts of triethylamine, 1-6 parts of chlorinated paraffin, 5-15 parts of zinc peroxide, 3-12 parts of barium sulfate, 2-10 parts of graphite powder, 2-10 parts of conductive mica powder, 1-7 parts of recycled silver colloids, 1-5 parts of molybdenum powder, 2-10 parts of palm oil, 18-35 parts of organic solvents and 1-5 parts of coupling agents. The invention further provides a preparation method of the anti-abrasion conductive polyimide film. The prepared polyimide film has good abrasion resistance and conductivity, the service life of the polyimide film can be prolonged, and equipment and electronic products are better protected.
Description
Technical field
The present invention relates to field of electronic materials, particularly a kind of wear-resistant conductive Kapton and preparation method thereof.
Background technology
Containing multiple aromatic heterocycle structural unit in polyimide molecule, therefore its thermotolerance is splendid, and its second-order transition temperature is more than 260 DEG C usually, is applicable to the circuit that temperature is high.In addition, polyimide has excellent low temperature resistant, high creep resistance, high dimensional stabilizing, low thermal coefficient of expansion, high electric insulation, low-k and loss, radiation hardness, the advantage such as corrosion-resistant due to it, is widely used in electron trade.But polyimide material to have high electrical insulating properties therefore non-conductive, be easy to assemble electric charge and form electrostatic thus bring unnecessary loss; In addition its lower rub resistance, limits it and applies more widely.
Summary of the invention
The technical problem solved is: in order to deficiencies such as the low electric conductivity and rub resistance that solve Kapton are low, provide a kind of wear-resistant conductive Kapton and preparation method thereof.
Technical scheme: in order to solve the problem, the invention provides a kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 30 ~ 50 parts, 3, 3 ' 4, 4 '-benzophenone tetracarboxylic dianhydride 20 ~ 40 parts, Ursol D 25 ~ 50 parts, 3, 4-diaminodiphenyl oxide 20 ~ 35 parts, polyphosphoric acid 3 ~ 10 parts, triethylamine 2 ~ 8 parts, clorafin 1 ~ 6 part, zinc peroxide 5 ~ 15 parts, 3 ~ 12 parts, barium sulfate, Graphite Powder 99 2 ~ 10 parts, conductive mica powder 2 ~ 10 parts, reclaim elargol 1 ~ 7 part, molybdenum powder 1 ~ 5 part, plam oil 2 ~ 10 parts, organic solvent 18 ~ 35 parts and coupling agent 1 ~ 5 part.
Preferably, a kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 38 ~ 50 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 25 ~ 40 parts, Ursol D 32 ~ 50 parts, 3,4-diaminodiphenyl oxide 27 ~ 35 parts, polyphosphoric acid 6 ~ 10 parts, triethylamine 4 ~ 8 parts, clorafin 2 ~ 6 parts, zinc peroxide 8 ~ 15 parts, 5 ~ 12 parts, barium sulfate, Graphite Powder 99 2 ~ 6 parts, conductive mica powder 2 ~ 8 parts, recovery elargol 3 ~ 7 parts, molybdenum powder 2 ~ 5 parts, plam oil 4 ~ 10 parts, organic solvent 22 ~ 35 parts and coupling agent 2 ~ 5 parts.
Preferably, a kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 42 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 30 parts, Ursol D 36 parts, 3,4-diaminodiphenyl oxide 32 parts, polyphosphoric acid 7 parts, triethylamine 6 parts, clorafin 4 parts, zinc peroxide 9 parts, 7 parts, barium sulfate, Graphite Powder 99 4 parts, conductive mica powder 5 parts, recovery elargol 4 parts, molybdenum powder 3 parts, plam oil 6 parts, organic solvent 28 parts and coupling agent 3 parts.
Preferably, described organic solvent is phenylate, dimethyl formamide or phenol.
Preferably, described coupling agent is silane coupling agent or titanate coupling agent.
A preparation method for a kind of wear-resistant conductive Kapton described above, the method comprises the steps:
(1) raw materials weighing by a certain percentage;
(2) organic solvent is added in there-necked flask, then in flask, add tetramethylene tetracarboxylic dianhydride, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride, Ursol D and 3,4-diaminodiphenyl oxide, in a nitrogen atmosphere, stirring and dissolving, then adds polyphosphoric acid and triethylamine, continues to stir;
(3) after clorafin, zinc peroxide, barium sulfate, Graphite Powder 99, conductive mica powder, recovery elargol, molybdenum powder and plam oil being mixed, add in there-necked flask, at 3 DEG C ± 2 DEG C, stir 5 ~ 10h;
(4) mixed solution stirred in step (3) is coated on substrate, is taken up in order of priority the baking oven dry solidification being placed in 100 DEG C and 320 DEG C, be cooled to room temperature and take off and get final product.
The present invention has following beneficial effect: test result shows, and the volume specific resistance of the polyamide layer prepared by the present invention is 5.6 × 10
5~ 2.4 × 10
8Ω cm; Surface resistivity is 2.17 × 10
6~ 3.65 × 10
8Ω/squar, far below commercially available common polyamide film; In addition, the frictional dissipation rate of the polyamide layer prepared by the present invention is 3.2 × 10
-6~ 6.3 × 10
-6mm/Nm is also less than the value of commercially available common polyamide film.Therefore, the polyamide layer prepared by the present invention has the work-ing life that good electroconductibility and rub resistance can improve polyamide layer, plays better provide protection to equipment and electronic product.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, invention preferred embodiment is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
A kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 30 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 20 parts, Ursol D 25 parts, 3,4-diaminodiphenyl oxide 20 parts, polyphosphoric acid 3 parts, triethylamine 2 parts, clorafin 1 part, zinc peroxide 5 parts, 3 parts, barium sulfate, Graphite Powder 99 2 parts, conductive mica powder 2 parts, recovery elargol 1 part, molybdenum powder 1 part, plam oil 2 parts, organic solvent 18 parts and coupling agent 1 part.
Described organic solvent is phenylate.Described coupling agent is silane resin acceptor kh-550.
A preparation method for wear-resistant conductive Kapton, the method comprises the steps:
(1) raw materials weighing by a certain percentage;
(2) organic solvent is added in there-necked flask, then in flask, add tetramethylene tetracarboxylic dianhydride, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride, Ursol D and 3,4-diaminodiphenyl oxide, in a nitrogen atmosphere, stirring and dissolving, then adds polyphosphoric acid and triethylamine, continues to stir;
(3), after clorafin, zinc peroxide, barium sulfate, Graphite Powder 99, conductive mica powder, recovery elargol, molybdenum powder and plam oil being mixed, add in there-necked flask, at 3 DEG C ± 2 DEG C, stir 8h;
(4) mixed solution stirred in step (3) is coated on substrate, is taken up in order of priority the baking oven dry solidification being placed in 100 DEG C and 320 DEG C, be cooled to room temperature and take off and get final product.
Embodiment 2
A kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 50 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 40 parts, Ursol D 50 parts, 3,4-diaminodiphenyl oxide 35 parts, polyphosphoric acid 10 parts, triethylamine 8 parts, clorafin 6 parts, zinc peroxide 15 parts, 12 parts, barium sulfate, Graphite Powder 99 10 parts, conductive mica powder 10 parts, recovery elargol 7 parts, molybdenum powder 5 parts, plam oil 10 parts, organic solvent 35 parts and coupling agent 5 parts.
Described organic solvent is dimethyl formamide.Described coupling agent is Silane coupling reagent KH-570.
A preparation method for wear-resistant conductive Kapton, the concrete steps of the method, see embodiment 1, do not repeat them here.
Embodiment 3
A kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 40 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 30 parts, Ursol D 38 parts, 3,4-diaminodiphenyl oxide 27 parts, polyphosphoric acid 6 parts, triethylamine 5 parts, clorafin 3 parts, zinc peroxide 10 parts, 7 parts, barium sulfate, Graphite Powder 99 6 parts, conductive mica powder 6 parts, recovery elargol 4 parts, molybdenum powder 3 parts, plam oil 6 parts, organic solvent 26 parts and coupling agent 3 parts.
Described organic solvent is phenol.Described coupling agent is titanate coupling agent KR-TTS.
A preparation method for wear-resistant conductive Kapton, the concrete steps of the method, see embodiment 1, do not repeat them here.
Embodiment 4
A kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 42 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 30 parts, Ursol D 36 parts, 3,4-diaminodiphenyl oxide 32 parts, polyphosphoric acid 7 parts, triethylamine 6 parts, clorafin 4 parts, zinc peroxide 9 parts, 7 parts, barium sulfate, Graphite Powder 99 4 parts, conductive mica powder 5 parts, recovery elargol 4 parts, molybdenum powder 3 parts, plam oil 6 parts, organic solvent 28 parts and coupling agent 3 parts.
Described organic solvent is dimethyl formamide.Described coupling agent is silane coupling agent KH-560.
A preparation method for wear-resistant conductive Kapton, the concrete steps of the method, see embodiment 1, do not repeat them here.
Embodiment 5
A kind of wear-resistant conductive Kapton, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 38 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 25 parts, Ursol D 32 parts, 3,4-diaminodiphenyl oxide 27 parts, polyphosphoric acid 6 parts, triethylamine 4 parts, clorafin 2 parts, zinc peroxide 8 parts, 5 parts, barium sulfate, Graphite Powder 99 6 parts, conductive mica powder 8 parts, recovery elargol 3 parts, molybdenum powder 2 parts, plam oil 4 parts, organic solvent 22 parts and coupling agent 2 parts.
Described organic solvent is phenylate.Described coupling agent is silane resin acceptor kh-550.
A preparation method for wear-resistant conductive Kapton, the concrete steps of the method, see embodiment 1, do not repeat them here.
Performance test
Carry out performance test to the electroconductibility of the Kapton prepared by above each embodiment and wear resistance below, test result sees the following form:
Wherein, volume specific resistance adopts ZC90E type resistance measuring instrument (Shanghai section Fitow), and surface resistivity adopts RTS-5 type four point probe resistance-meter (Guangzhou four point probe); Frictional dissipation rate adopts GB3960-83 to carry out test determination.
As seen from the above table, the volume specific resistance of the polyamide layer prepared by embodiment 1 ~ 5, surface resistivity and frictional dissipation rate are all better than common polyamide film, show good electroconductibility and rub resistance.
Claims (6)
1. a wear-resistant conductive Kapton, it is characterized in that, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 30 ~ 50 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 20 ~ 40 parts, Ursol D 25 ~ 50 parts, 3,4-diaminodiphenyl oxide 20 ~ 35 parts, polyphosphoric acid 3 ~ 10 parts, triethylamine 2 ~ 8 parts, clorafin 1 ~ 6 part, zinc peroxide 5 ~ 15 parts, 3 ~ 12 parts, barium sulfate, Graphite Powder 99 2 ~ 10 parts, conductive mica powder 2 ~ 10 parts, recovery elargol 1 ~ 7 part, molybdenum powder 1 ~ 5 part, plam oil 2 ~ 10 parts, organic solvent 18 ~ 35 parts and coupling agent 1 ~ 5 part.
2. a kind of wear-resistant conductive Kapton as claimed in claim 1, it is characterized in that, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 38 ~ 50 parts, 3, 3 ' 4, 4 '-benzophenone tetracarboxylic dianhydride 25 ~ 40 parts, Ursol D 32 ~ 50 parts, 3, 4-diaminodiphenyl oxide 27 ~ 35 parts, polyphosphoric acid 6 ~ 10 parts, triethylamine 4 ~ 8 parts, clorafin 2 ~ 6 parts, zinc peroxide 8 ~ 15 parts, 5 ~ 12 parts, barium sulfate, Graphite Powder 99 2 ~ 6 parts, conductive mica powder 2 ~ 8 parts, reclaim elargol 3 ~ 7 parts, molybdenum powder 2 ~ 5 parts, plam oil 4 ~ 10 parts, organic solvent 22 ~ 35 parts and coupling agent 2 ~ 5 parts.
3. a kind of wear-resistant conductive Kapton as claimed in claim 1, it is characterized in that, be prepared from by following raw material according to parts by weight: tetramethylene tetracarboxylic dianhydride 42 parts, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride 30 parts, Ursol D 36 parts, 3,4-diaminodiphenyl oxide 32 parts, polyphosphoric acid 7 parts, triethylamine 6 parts, clorafin 4 parts, zinc peroxide 9 parts, 7 parts, barium sulfate, Graphite Powder 99 4 parts, conductive mica powder 5 parts, recovery elargol 4 parts, molybdenum powder 3 parts, plam oil 6 parts, organic solvent 28 parts and coupling agent 3 parts.
4. a kind of wear-resistant conductive Kapton as claimed in claim 1, is characterized in that, described organic solvent is phenylate, dimethyl formamide or phenol.
5. a kind of wear-resistant conductive Kapton as claimed in claim 1, is characterized in that, described coupling agent is silane coupling agent or titanate coupling agent.
6. a preparation method for a kind of wear-resistant conductive Kapton as described in any one of claim 1 ~ 5, it is characterized in that, the method comprises the steps:
(1) raw materials weighing by a certain percentage;
(2) organic solvent is added in there-necked flask, then in flask, add tetramethylene tetracarboxylic dianhydride, 3,3 ' 4,4 '-benzophenone tetracarboxylic dianhydride, Ursol D and 3,4-diaminodiphenyl oxide, in a nitrogen atmosphere, stirring and dissolving, then adds polyphosphoric acid and triethylamine, continues to stir;
(3) after clorafin, zinc peroxide, barium sulfate, Graphite Powder 99, conductive mica powder, recovery elargol, molybdenum powder and plam oil being mixed, add in there-necked flask, at 3 DEG C ± 2 DEG C, stir 5 ~ 10h;
(4) mixed solution stirred in step (3) is coated on substrate, is taken up in order of priority the baking oven dry solidification being placed in 100 DEG C and 320 DEG C, be cooled to room temperature and take off and get final product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615397.XA CN105199378A (en) | 2015-09-24 | 2015-09-24 | Anti-abrasion conductive polyimide film and preparation method thereof |
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| CN201510615397.XA CN105199378A (en) | 2015-09-24 | 2015-09-24 | Anti-abrasion conductive polyimide film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924648A (en) * | 2016-04-19 | 2016-09-07 | 安徽鑫柏格电子股份有限公司 | Polyimide hybrid film with low surface resistance and preparation method thereof |
| CN111100458A (en) * | 2019-11-15 | 2020-05-05 | 无锡顺意锐新材料研究有限公司 | Long-acting antistatic polyimide film and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1101641A (en) * | 1964-01-20 | 1968-01-31 | Du Pont | Amino polyamides |
| JPH0755539B2 (en) * | 1987-12-09 | 1995-06-14 | エヌオーケー株式会社 | Manufacturing method of conductive composite material |
| JPH07207024A (en) * | 1994-01-18 | 1995-08-08 | Shin Etsu Chem Co Ltd | Polyimide resin composition |
| JP2002275281A (en) * | 2001-03-21 | 2002-09-25 | Sumitomo Bakelite Co Ltd | Polyimide resin film |
| CN1772812A (en) * | 2005-11-17 | 2006-05-17 | 复旦大学 | Reinforced toughened antiwear composite polyimide material |
| CN101831175A (en) * | 2010-04-01 | 2010-09-15 | 辽宁科技大学 | Colorless and transparent polyimide nano-composite material membrane and preparation method thereof |
| CN103772983A (en) * | 2014-01-24 | 2014-05-07 | 江苏亚宝绝缘材料股份有限公司 | Transparent flexible conductive polyimide film |
| CN103768864A (en) * | 2014-01-24 | 2014-05-07 | 中国科学院重庆绿色智能技术研究院 | Method for preparing anti-static and high-performance flue gas purification filter material |
-
2015
- 2015-09-24 CN CN201510615397.XA patent/CN105199378A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1101641A (en) * | 1964-01-20 | 1968-01-31 | Du Pont | Amino polyamides |
| JPH0755539B2 (en) * | 1987-12-09 | 1995-06-14 | エヌオーケー株式会社 | Manufacturing method of conductive composite material |
| JPH07207024A (en) * | 1994-01-18 | 1995-08-08 | Shin Etsu Chem Co Ltd | Polyimide resin composition |
| JP2002275281A (en) * | 2001-03-21 | 2002-09-25 | Sumitomo Bakelite Co Ltd | Polyimide resin film |
| CN1772812A (en) * | 2005-11-17 | 2006-05-17 | 复旦大学 | Reinforced toughened antiwear composite polyimide material |
| CN101831175A (en) * | 2010-04-01 | 2010-09-15 | 辽宁科技大学 | Colorless and transparent polyimide nano-composite material membrane and preparation method thereof |
| CN103772983A (en) * | 2014-01-24 | 2014-05-07 | 江苏亚宝绝缘材料股份有限公司 | Transparent flexible conductive polyimide film |
| CN103768864A (en) * | 2014-01-24 | 2014-05-07 | 中国科学院重庆绿色智能技术研究院 | Method for preparing anti-static and high-performance flue gas purification filter material |
Non-Patent Citations (3)
| Title |
|---|
| 周祥兴: "《中国塑料制品配方大全》", 31 May 1999 * |
| 朱洪法 等: "《无机化工产品手册》", 31 December 2008 * |
| 李克友 等: "《高分子合成原理及工艺学》", 31 October 1999 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924648A (en) * | 2016-04-19 | 2016-09-07 | 安徽鑫柏格电子股份有限公司 | Polyimide hybrid film with low surface resistance and preparation method thereof |
| CN111100458A (en) * | 2019-11-15 | 2020-05-05 | 无锡顺意锐新材料研究有限公司 | Long-acting antistatic polyimide film and preparation method thereof |
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Application publication date: 20151230 |