CN103772704A - Method for preparing polyimide thin film with low friction coefficient and high cohesive force - Google Patents
Method for preparing polyimide thin film with low friction coefficient and high cohesive force Download PDFInfo
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Abstract
The invention discloses a method for preparing a polyimide thin film with low friction coefficient and high cohesive force, and belongs to the technical field of electronic thin film insulating material preparation. During the preparation process, a composition of a filtering material and a dispersing agent of which the mass ratio is (10:1)-(1:1) is used, the filtering material is microscale or nanoscale spherical organosilicone, silicate, aluminum-oxygen compound or calcium phosphate filtering material and the like; the dispersing agent is polyphosphate or polyacrylic acid compound or composition; every 100 parts of a polyamide acid resin liquid (solid content) by weight uses 10-20 parts of the composition of the filtering material and the dispersing agent by weight. Through the addition of the microscale filtering material, the internal performance of the thin film is improved, the surface roughness of the thin film is increased, the mechanical occlusion action of the thin film and the coating surface and the adhesive force of the thin film and the coating are enhanced, the wettability and the adhesion are greatly improved, so that the working efficiency is effectively improved, the product quality is optimized, and the suitability and the reliability of the thin film in various fields can be improved.
Description
Technical field
The present invention relates to the manufacturing technology of the high cohesive force Kapton of a kind of low-friction coefficient, particularly the formula preparation method of the high cohesive force polyamic acid of a kind of low-friction coefficient, belongs to speciality polymer Material Field.
Background technology
Along with the development of the most advanced and sophisticated new technologies such as aerospace cause and electronic industry, the demand of Kapton is constantly expanded.In present stage China's Kapton product development process, exist many technical barriers: electron trade requires the quality of Kapton, and especially film surface quality is very high, and therefore requiring steel band is minute surface steel band.But because minute surface steel band smooth finish is very high, Ra value reaches 0.02, and the film surface of producing is very smooth, film is easily adhesion between layers, and rolling rear film surface is easily wrinkling, and surface tension is little, is unfavorable for surface bonding; In resin synthetic technology, because a large amount of fillers adds, bring very large difficulty to resin is synthetic, react unstable, molecular weight is difficult to control; In dispersion technology, filler disperses uneven in resin, and when salivation, manufacturability performance poor and film is inhomogeneous unstable.
Du pont company is the main manufacturer of Kapton, and due to the huge commercial promise of product, the said firm takes strict secrecy provision to Kapton production technology.Therefore, from disclosed document and patent, obtain about the fabricating technology information of Kapton limited.Since realizing the commercialization of Kapton the sixties in last century, China's Kapton still adopts backward production technique, and kind is more single, can only be used for common motor, electrical apparatus insulation, is difficult to meet high-performance motor and electronic industry needs.
The Kapton cohesive force of the film surface processing such as classical acid alkaline purification, plasma treatment and surface grafting is bad, and surfaceness is low, frictional coefficient is large, film layer by layer between adhesion, surface irregularity.The present invention can increase the mechanical snap effect on film and coating interface, improves film surface tension force, and the materials such as the small molecules of film surface are polluted in removal simultaneously.The surface tension of film and wetting property are not subject to the impact of time and environment, and cohesive force is high and have a persistence.
The present invention meets the particular requirement of domestic and international every profession and trade and needs, has invented the Kapton of the high cohesive force of a kind of low-friction coefficient, has widened Kapton Application Areas, has optimized the quality of product, has improved working efficiency.。The problems such as fundamentally having changed Kapton surface can be low, wetting ability is poor, and poor with the adhesive property of other material, and film frictional force is between layers large, the not smooth generation adhesion of relative movement.For above-mentioned technological difficulties, the present invention has carried out the research and development of the high cohesive force Kapton of low-friction coefficient.Adopt in synthetic resins and add micron order calcium phosphate and spherical silicoorganic compound, to increase roughness and the smooth degree of film surface, fundamentally solved the little problem that is unsuitable for gluing of film surface adhesion and surface tension.
Summary of the invention
The present invention is can be low in order to overcome the surface of polyamides Kapton in prior art, the poor adhesive property poor (copper-clad plate industry, coating and ink printing) that causes itself and other material of wetting ability, Kapton surface is very smooth simultaneously, film frictional force is between layers very large, close contact and completely isolated air almost between film surface, when separation, form parital vacuum, produce adhesion, affect the rolling of film and unreel and the planeness of outward appearance.The large more smooth film surface of frictional coefficient is very unfavorable to coating etc. simultaneously, and after applying, between coating and film, sticking power is little, and cohesive force also can decline.So just limit the use of Kapton or reduced working efficiency.
Further, described object of the present invention is the Kapton of the high cohesive force of a kind of low-friction coefficient of development, has widened Kapton Application Areas, improves the quality of product, meets customer need, and increases work efficiency.
In order to realize foregoing invention object, the invention provides following technical scheme:
Overall plan of the present invention is that filler and dispersion agent are added in organic solvent and disperseed, after dispersion, add organic tetracarboxylic dianhydride and aromatic diamine, react, generate polyamic acid solution, salivation film forming on steel band, self-supporting Polyamic Acid Film, horizontal, vertical stretching high temperature imidization, last film take-up, eliminate stress, pack after the assay was approved.
The filler of using in the high cohesive force Kapton of low-friction coefficient preparation process and a composition for dispersion agent, be made up of filler and the dispersion agent of 10:1～1:1 weight ratio.Described filler is one or more.
Described dispersion agent is acroleic acid macromolecular compound and poly-phosphate or its composition.
Wherein comprise the filler of 10～20 mass parts (with respect to the polyamic acid resin fluid solid content of 100 mass parts), filler is conducive to increase the mechanical snap effect on film and coating interface, improve film surface tension force, the wettability of film and adhesivity are increased.Simultaneously film surface tension force and wetting property are not subject to the impact of time and environment, and cohesive force is high and have a weather resistance.
The dispersion agent that simultaneously also comprises 1～10 part (with respect to polyamic acid resin fluid solid content of 100 mass parts) in composition, suitable dispersive agent ratio has important impact to the performance of film.
Further, described filler is silicone based, it is characterized in that, organosilicon is microspheric form, and film surface is smooth, and film surface does not produce adhesion between layers, and frictional coefficient is low, have higher roughness simultaneously.
Further, described filler is preferably organosilicon and calcium phosphate.Especially, select above-mentioned substance as filler, taken into full account various weighting agents to the issuable impact of the high cohesive force Kapton of low-friction coefficient performance.
Consider from filler particle size, performance, cost and being easy to get property etc., optimal selection organosilicon of the present invention, is characterized in that, organosilicon microspheric form makes film surface smooth, and film surface does not produce adhesion between layers, thereby effectively reduces frictional coefficient; Preferably micron order calcium phosphate is filler simultaneously, makes film surface have higher roughness.Except special instruction.
Further, described dispersion agent is polyethylene salt base polymer, polyacrylic polymer, methylcellulose gum and poly-phosphate and derivative thereof.
Preferred dispersion agent is that acroleic acid macromolecular and phosphoric acid salt are used in combination.Select above-mentioned dispersion agent, with polyamic acid system good dispersity, and be retained between polyimide molecule and occur without side reaction after adding, do not affect the stability of final polyimide.
Particularly preferably, the following material composition that filler, disperser composition are weight part: 10～20.
Further, above-mentioned filler, disperser composition use after disperseing by the N,N-dimethylacetamide of 0.5～1.5 times of its total mass.
The present invention adopts particularly preferred filler, the disperser composition of this combination, and the film quality of production is good, and stable performance, and can significantly reduce the frictional coefficient on Kapton surface, increases its surfaceness.
In addition, the invention solves and roll off the production line that to occur that because frictional force is large film draws motionless or because film and film friction cause the damaged phenomenon of even breaking after gluing in use procedure, printing and winding around; The film surface of preparation is smooth, can not cause because storage period is long the bad order phenomenons such as film surface gauffer; Quality product and production efficiency are improved significantly.
The present invention also provides a kind of preparation method of Kapton of mixing type, comprises step:
After evenly polyamic acid rear and 18～25% solid contents mixes according to 1:4～8 weight ratio by filler, dispersant, salivate or apply into polyamides filler, the dispersant polyamic acid resin liquid that evenly rear and solid content is 18%～25% is mixed according to 1:10～20 mass ratio.
Further, described resin is through secondary filtration salivation or apply into film, under 65～100 ℃, 70～140 ℃, 100～200 ℃ three temperature sections, carry out hot imidization, to obtain solid content be 25～40% polyamic acid glued membrane peeling off, by 300～450 ℃ of high temperature imidizations.
Further, above-mentioned after the two-way stretch of 1.01～1.10 stretch ratios, rolling obtains the high cohesive force Kapton of low-friction coefficient.
Described imidization temperature is 300 ℃, 350 ℃, 400 ℃, 450 ℃ and 250 ℃ of five temperature sections.
Further, described filler, dispersion agent mix in the hold-up vessel of 20～50 ℃.
In addition, the frictional coefficient of common Kapton is greatly about more than 0.5, and therefore film frictional force is between layers very large, relative movement is not smooth, close contact and completely isolated air almost between film surface, the parital vacuum forming when separation, can produce adhesion.
Compared with prior art, the rolling of film and unreel and the planeness of outward appearance bad, even because frictional force there will be tensile phenomenon.The present invention is directed to this problem, Kapton internal performance is carried out to modification, and subsequent technique is carried out to corresponding research and development and improve.
Useful optimal effectiveness of the present invention: the Kapton of preparation has good mechanical property, resistant of high or low temperature, high-insulativity and lower frictional coefficient, from having improved in essence operation performance and the reliability of Kapton.Can be used as High Performance Insulation material and be applied to electric power electric field and copper-clad plate industry, also can be used as in the basement membrane of metallic film and tectum and apply, on Kapton, apply sizing agent film and Copper Foil be combined with each other, compound evenly, cohesive force is strong; The Kapton of the high cohesive force of low-friction coefficient that the present invention develops, has wide Application Areas, has optimized the quality of product, has improved working efficiency.
Embodiment
Below in conjunction with test example and specific implementation method, the present invention is described in further detail.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on content of the present invention all belong to scope of the present invention.
The technology of the present invention overall plan: filler and dispersion agent are added in organic solvent and disperseed, after dispersion, organic tetracarboxylic dianhydride and aromatic diamine are added, react, generate polyamic acid solution, salivation film forming on steel band, self-supporting Polyamic Acid Film, horizontal, vertical stretching high temperature imidization, Kapton rolling, eliminate stress, pack after the assay was approved, finally obtain the high cohesive force Kapton of the low friction of finished product.
Each workshop section, process in following embodiment all carry out under normal pressure, the amount of all substances is all based on mass percent, all parts are mass parts (by the solid content of the polyamic acid resin of 100 mass parts), all temperature condition are degree Celsius, all viscosity all refers to that polyamic acid solid content is 20% N, the viscosity number of N-dimethylacetamide solution in the time of 20 ℃, all raw material is electronic-grade ultra-pure chemicals, except as otherwise noted.
Embodiment 1
Be to add N in the hold-up vessel of 10 ± 2 ℃ to temperature, N-N,N-DIMETHYLACETAMIDE 750kg, in synthetic resins process, add filler calcium phosphate 7kg and nano level organosilicon 10kg, dispersion agent 3kg, after being uniformly mixed, the viscosity that is 20% by itself and solid content is 250, 000 polyamic acid solution is after 1:7.5 mass ratio mixes, after filtration, after nature froth breaking, apply (interior is airtight clean system) on the minute surface steel band that is placed in the wide 50～70cm of being by extruding the device salivation of getting to know, with the speed of a motor vehicle of 6m/min in 75 ℃, 130 ℃, dry film forming for 175 ℃ three sections, again the film after part hot imidization is separated to steel band through stripper roll, send into 300 ℃ through two-way stretch (stretch ratio is 1.10) again, 350 ℃, 400 ℃, in the High Temperature Furnaces Heating Apparatus of five temperature sections of 450 ℃ and 250 ℃, carry out complete imidization processing, in film, residual solvent amount is 0.1%～1.0%, finally by the processing of corona film, plant limit, rolling makes the high cohesive force Kapton of low-friction coefficient.
Embodiment 2
Be to add N in the hold-up vessel of 10 ± 2 ℃ to temperature, N-N,N-DIMETHYLACETAMIDE 750kg, in synthetic resins process, add filler calcium phosphate 7kg and nano level organosilicon 15kg, dispersion agent 3kg, after being uniformly mixed, the viscosity that is 20% by itself and solid content is 250, 000 polyamic acid solution is after 1:6 mass ratio mixes, after filtration, after nature froth breaking, apply (interior is airtight clean system) on the minute surface steel band that is placed in the wide 50～70cm of being by extruding the device salivation of getting to know, with the speed of a motor vehicle of 6m/min in 75 ℃, 130 ℃, dry film forming for 175 ℃ three sections, again the film after part hot imidization is separated to steel band through stripper roll, send into 300 ℃ through two-way stretch (stretch ratio is 1.10) again, 350 ℃, 400 ℃, in the High Temperature Furnaces Heating Apparatus of five temperature sections of 450 ℃ and 250 ℃, carry out complete imidization processing, in film, residual solvent amount is 0.1%～1.0%, finally by the processing of corona film, plant limit, rolling makes the high cohesive force Kapton of low-friction coefficient.
Embodiment 3
Be to add N in the hold-up vessel of 10 ± 2 ℃ to temperature, N-N,N-DIMETHYLACETAMIDE 750kg, in synthetic resins process, add filler calcium phosphate 17kg, dispersion agent 3kg, after being uniformly mixed, the viscosity that is 20% by itself and solid content is 250, 000 polyamic acid solution is after 1:7.5 mass ratio mixes, after filtration, after nature froth breaking, apply (interior is airtight clean system) on the minute surface steel band that is placed in the wide 50～70cm of being by extruding the device salivation of getting to know, with the speed of a motor vehicle of 6m/min in 75 ℃, 130 ℃, dry film forming for 175 ℃ three sections, again the film after part hot imidization is separated to steel band through stripper roll, send into 300 ℃ through two-way stretch (stretch ratio is 1.10) again, 350 ℃, 400 ℃, in the High Temperature Furnaces Heating Apparatus of five temperature sections of 450 ℃ and 250 ℃, carry out complete imidization processing, in film, residual solvent amount is 0.1%～1.0%, finally by the processing of corona film, plant limit, rolling makes the high cohesive force Kapton of low-friction coefficient.
Embodiment 4
Be to add N in the hold-up vessel of 10 ± 2 ℃ to temperature, N-N,N-DIMETHYLACETAMIDE 750kg, in synthetic resins process, add filler nanometer level organosilicon 17kg and dispersion agent 3kg, after being uniformly mixed, the viscosity that is 18%～25% by itself and solid content is 250, 000 polyamic acid solution is after 1:7.5 mass ratio mixes, after filtration, after nature froth breaking, apply (interior is airtight clean system) on the minute surface steel band that is placed in the wide 50～70cm of being by extruding the device salivation of getting to know, with the speed of a motor vehicle of 6m/min in 75 ℃, 130 ℃, dry film forming for 175 ℃ three sections, again the film after part hot imidization is separated to steel band through stripper roll, send into 300 ℃ through two-way stretch (stretch ratio is 1.10) again, 350 ℃, 400 ℃, in the High Temperature Furnaces Heating Apparatus of five temperature sections of 450 ℃ and 250 ℃, carry out complete imidization processing, in film, residual solvent amount is 0.1%～1.0%, finally by the processing of corona film, plant limit, rolling makes the high cohesive force Kapton of low-friction coefficient.
Reference examples
The polyamic acid solution that is 20% by solid content after filtration, after vacuum outgas bubble, be coated on and be placed on the Stainless Steel Band for no reason that airtight clean system infolding footpath is 40～60cm by extruding the device salivation of getting to know, with the speed of a motor vehicle of 6m/min in 75 ℃, 130 ℃, dry film forming for 175 ℃ three sections, again the film after part hot imidization is separated to steel band for no reason through stripper roll, send into rubber roll, or after the two-way stretch of 1.10 stretch ratios, send into 300 ℃, 350 ℃, 400 ℃, in the High Temperature Furnaces Heating Apparatus of five temperature sections of 450 ℃ and 250 ℃, carry out complete imidization processing, in film, residual solvent amount is 0.1%～1.0%, finally by the processing of corona film, plant limit, rolling makes the high cohesive force Kapton of low-friction coefficient.
Test
The performance that adopts the Kapton of relevant test method test preparation, the results are shown in Table 1
Table 1 is the performance of prepared Kapton
The present invention is by adding micron order filler, and resin liquid is effectively disperseed, prepare the Kapton of the high cohesive force of a kind of low-friction coefficient, change film surface property, increase surfaceness, the mechanical snap effect on enhanced film and coating interface, improves film surface tension force, remove polluting the materials such as the small molecules of film surface in film simultaneously, make the wettability of film and adhesivity have large increase.
In addition, film surface tension force prepared by employing the present invention and wetting property are not subject to the impact of time and environment, and film surface tension force and wettability have had large increase, the Adhesion enhancement between coating and film; Improved significantly suitability and reliability that film uses in every field, improved quality and the working efficiency of film production, cohesive force is high has weather resistance.
Claims (10)
1. the filler of using in the Kapton preparation process of the high cohesive force of low-friction coefficient, a composition for dispersion agent, is characterized in that, is made up of filler and the dispersion agent of 10:1～1:1 weight ratio;
Described filler is silicone based, silicates, aluminum oxide class, calcium phosphate etc.;
Described dispersion agent is polyphosphoric acid salt, polyacrylic macromolecular compound or its composition;
Filler and the disperser composition of 10～20 mass parts for every 100 mass parts polyamic acid resin liquid (solid content);
The solid content of described polyamic acid resin liquid is 18～25%.
2. the composition of filler and dispersion agent according to claim 1, is characterized in that, described filler is any one or its composition in silicone based, silicates, aluminum oxide class and calcium phosphate.
3. the composition of filler and dispersion agent according to claim 1, described filler is micron order or nano-level sphere is silicone based, silicates etc., it is characterized in that, micron order or nano-level sphere compound can be evenly distributed in film surface, form " concavo-convex " interface (microcosmic) thin film layer, between layer, have " space ".
4. the composition of filler and dispersion agent according to claim 1, it is characterized in that, described dispersion agent is any one or its composition in polymer (comprising high, normal, basic molecular weight) polyvalent alcohol-many ethyleneimines segmented copolymer and acrylate polymeric.
5. the composition of filler and dispersion agent according to claim 1, is characterized in that, described dispersion agent is any one or its composition in polyester-polyurethane, polyacrylic ester lipid acid oxyethane, polyethylene glycol type polyvalent alcohol and polyethylenimine derivates.
6. in addition, the composition of filler and dispersion agent, is characterized in that according to claim 1, and described dispersion agent also comprises in inorganic salt (phosphoric acid, silicate) and acrylate polymeric polymkeric substance any one or its composition.
7. the composition of filler and dispersion agent according to claim 1, is characterized in that, the N,N-dimethylacetamide of 0.5～1.5 times of its total mass is used after disperseing for described filler and disperser composition.
8. the thermochemistry imidization method that physics is mixed the polyamic acid of pattern, comprise the following steps, by filler, the dispersant polyamic acid resin liquid that evenly rear and solid content is 18wt%～25wt% mixes according to 1:10～20 mass ratio, resin is through secondary filtration curtain coating or apply into film, through 65～100 ℃, 70～140 ℃, under 100～200 ℃ of three temperature sections, carry out hot imidization, obtain the polyamic acid glued membrane that solid content is 25～40%wt% peeling off, by 300～400 ℃ of high temperature imidizations, simultaneously after the two-way stretch of 1.01～1.10 stretch ratios, rolling obtains the high cohesive force Kapton of low-friction coefficient.
9. the high cohesive force Kapton of low-friction coefficient of preparing according to claim 8, it is characterized in that, in described polyamic acid preparation process, adopt high pressure homogenizer take high pressure reciprocating pump as transmission of power and material conveying mechanism, by mass transport to operating valve (one-level homogenizing valve and secondary Emulsified valve) part.Want material handling by the process of operating valve, under high pressure produce strong shearing, shock and cavitation, thereby make the solid particulate take liquid as carrier obtain ultra micro refinement.
10. the high cohesive force Kapton of low-friction coefficient of preparing according to claim 8, it is characterized in that, described salivation process resin needs hot blast to heat, and described hot-blast heat exchange device is to adopt stacked the forming of staggered form corrugation aluminium sheet, volume is little, heat interchanging area is large, and windage is little.The present invention adopts air intake technology, and the hot blast of the oven dry road discharge that the cold wind of introducing is come in through interchanger and side from one side carries out after heat exchange from another side out, and cold wind is preheated, hot blast is by tentatively cooling, save the energy, extended the work-ing life of equipment, improved efficiency.
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| C06 | Publication | ||
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Application publication date: 20140507 |