CN111364280A - Mica membrane and preparation method thereof - Google Patents
Mica membrane and preparation method thereof Download PDFInfo
- Publication number
- CN111364280A CN111364280A CN202010334927.4A CN202010334927A CN111364280A CN 111364280 A CN111364280 A CN 111364280A CN 202010334927 A CN202010334927 A CN 202010334927A CN 111364280 A CN111364280 A CN 111364280A
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- Prior art keywords
- layer
- mica
- aramid fiber
- mica paper
- iii
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- 239000010445 mica Substances 0.000 title claims abstract description 123
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 123
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- 229920006231 aramid fiber Polymers 0.000 claims abstract description 59
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 23
- 239000004917 carbon fiber Substances 0.000 claims abstract description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 22
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- 239000000126 substance Substances 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
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- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 4
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 4
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- 206010070834 Sensitisation Diseases 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
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- KZKGLGIVGQYOTG-UHFFFAOYSA-N [F].[Au] Chemical compound [F].[Au] KZKGLGIVGQYOTG-UHFFFAOYSA-N 0.000 claims 1
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- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 3
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- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 2
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- 241001391944 Commicarpus scandens Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- Chemical & Material Sciences (AREA)
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- Laminated Bodies (AREA)
Abstract
The invention discloses a mica membrane and a preparation method thereof, wherein the mica membrane comprises a base mica paper layer, a reinforcing layer is formed on one side surface of the base mica paper layer, the reinforcing layer comprises an aramid fiber layer and a carbon fiber film layer, the aramid fiber adopted in the aramid fiber layer is short-cut aramid fiber III subjected to nickel plating treatment in a chemical mode, during preparation, the short-cut aramid fiber III is subjected to pretreatment modification, then is matched with chemical plating solution for surface metallization treatment, then is filled in the aramid fiber layer, is covered with the carbon fiber film layer provided with honeycomb grid holes and is subjected to hot pressing to form the reinforcing layer, and then a reinforcing mica paper layer is formed on the outer surface of the reinforcing layer. The mica membrane has better stability and secondary processability while having mica thermal property and dielectric property, and can effectively solve the problems of safe use and long service life of an electric heating element.
Description
Technical Field
The invention relates to the field of mica material processing, in particular to a mica membrane with high temperature resistance, better surface strength and deformation resistance and a preparation method thereof.
Background
Mica, as a naturally occurring phyllosilicate mineral, has excellent physical and electrical properties and the properties of maintaining the properties at high temperature, and has the characteristics of complete chemical inertness, high voltage resistance, corona discharge resistance and radiation protection, thus having applications in numerous fields. Mica paper is one of the most extensive application approaches of the current mica, and is a paper-based insulating material which is prepared by taking the mica as a main raw material, splitting the mica into fine mica flakes through thermochemistry or waterpower and then manufacturing the mica flakes through a modern papermaking wet method, so that the mica paper has high temperature resistance and reprocessing performance which are obvious to the outside, and can be used as a film material of an electric heating element to carry out external protection on the electric heating element, thereby improving the safety use performance of the electric heating element and improving the heat utilization rate of the electric heating element by assisting the corresponding electric heating element.
At present, a mica electric heating film prepared by wrapping mica paper on a commercially available electric heating element is generally simple in structure, the mica paper is not subjected to adaptive improvement, and the mica paper is directly wrapped on the surface of the electric heating element during use, so that the adhesion performance is poor, and displacement is easy to generate. Because the traditional mica paper is formed mainly by Van der Waals force and electrostatic force among mica sheets, the mechanical strength of the formed paper is low, so that the mica paper is easy to break and has insufficient impact resistance. However, in the actual use process, if the heat efficiency of the mica electric heating film needs to be improved, the mica paper needs to reduce the thickness of the mica electric heating film, but the production of the mica electric heating film is difficult to meet the use requirement, the defective rate is high, and the production efficiency is low; if the thickness of the mica paper is increased, the surface temperature of the product is uneven, the total power of the product is attenuated due to the heat conductivity of the mica paper in the long-term use process, and meanwhile, the mechanical property and the electrical insulation property of the mica paper cannot meet the satisfactory requirements and the service life of the product is directly influenced. In addition, the problem is alleviated by adopting the additionally arranged heat-conducting metal foil or heat-conducting alloy foil or high-temperature-resistant heat-conducting resin layer to be matched with the insulating glue for fixing, but the structure of the insulating glue material has low heat conductivity coefficient, the heat conduction efficiency of the outer packaging structure is limited, the heat generated by the electric heating element cannot be led out quickly, and the application range of the electric heating element is greatly limited.
Disclosure of Invention
The invention aims to provide a mica membrane and a preparation method thereof, the mica membrane has controllable membrane thickness, high mechanical strength, good insulation property and high temperature resistance, is not easy to peel and deform even an electric heating element is continuously used for a long time, and can be used for solving the defects in the background technology.
The technical problem solved by the invention is realized by adopting the following technical scheme:
the utility model provides a mica diaphragm, includes basic mica paper layer, the shaping has the enhancement layer on one side surface of basic mica paper layer, the enhancement layer includes one deck aramid fiber layer and one deck carbon fiber film layer, the aramid fiber who adopts in the aramid fiber layer is for carrying out nickel plating treatment's short aramid fiber III through chemical mode, and it has honeycomb mesh to open on the carbon fiber film layer, and the carbon fiber film layer shaping is on aramid fiber's surface, and the surface of enhancement layer still the shaping has one deck reinforcement mica paper layer.
As a further limitation, the mica paper substrate is a natural muscovite paper layer or natural phlogopite paper or synthetic fluorphlogopite paper.
By way of further limitation, the reinforced mica paper layer is a natural muscovite paper layer.
Further, the ratio of the thickness of the mica paper substrate to the thickness of the reinforced mica paper layer after molding is 2:1 to 3: 1.
The thickness of the aramid fiber layer is 30-80 mu m, the monofilament diameter of the adopted chopped aramid fiber III is 10-25 mu m, the thickness of a nickel plating layer on the chopped aramid fiber III in the aramid fiber layer is 0.15-0.35 mu m, and the nickel content in the nickel plating layer is more than 85%.
As a further limitation, the thickness of the single layer of the carbon fiber film layer is 0.2-2 μm.
The invention also discloses a preparation method of the mica membrane, which comprises the following operation steps:
s1, purchasing or adopting self-made mica paper as a mica paper base material, and cutting the mica paper into a proper size for later use;
s2, carrying out short-cut treatment on the aramid fiber III or directly purchasing a finished product of the short-cut aramid fiber III, sequentially carrying out pre-treatment of cleaning, oil removal, coarsening, neutralization, sensitization, activation and reduction on the short-cut aramid fiber III, and then putting the pre-treated fiber into a chemical plating solution for carrying out surface metallization treatment to form the short-cut aramid fiber III with a nickel-plated layer;
s3, uniformly spraying the chopped aramid fiber III with the nickel-plated layer prepared in the step S2 on the surface of a mica paper substrate, covering a carbon fiber film layer with honeycomb-shaped grid holes after spraying, manufacturing a reinforced mica paper layer on the surface of the carbon fiber film layer by mica paper pulp after hot pressing, stabilizing, and forming to obtain the finished mica membrane.
Has the advantages that: the mica film prepared by the invention has better physical properties while having the properties of mica paper, has excellent bending resistance and impact resistance, has better physical strength, secondary processing performance and structural stability under the condition of the same thickness compared with the traditional single mica paper, has certain toughness and flexibility, is easier to form on small and miniature components, can effectively keep the structural stability under the condition of long-time use, and simultaneously can effectively improve the heat conversion efficiency, the soaking effect and the electrical property through the arrangement of the carbon fiber film layer, thereby bearing stronger over-current, realizing planar heating on the surface of an electric heating element when being applied to the electric heating element and improving the heat conduction efficiency.
Drawings
FIG. 1 is a sectional detail view of a preferred embodiment of the present invention.
Wherein: 1. a reinforced mica paper layer; 2. a carbon fiber film layer; 3. an aramid fiber layer; 4. a base mica paper layer; 5. and (4) cellular grid holes.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings.
In the following examples, it will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Referring to fig. 1, in the present embodiment, the mica film includes a base mica paper layer 4 and a reinforced mica paper layer 1, wherein the base mica paper layer 4 and the reinforced mica paper layer 1 are both natural white mica paper and have a thickness ratio of 3:1, and a carbon fiber layer 2 and an aramid fiber layer 3 are further formed between the base mica paper layer 4 and the reinforced mica paper layer 1, wherein the aramid fiber layer 3 has a thickness of 60 μm, the aramid fiber layer 3 is filled with chopped aramid iii fiber monofilaments having a monofilament diameter of 15 to 22 μm, the chopped aramid iii fiber monofilaments are chemically plated with a nickel plating layer having a thickness of 0.15 to 0.35 μm, and the total nickel content in the nickel plating layer is 89.5%; the carbon fiber film layer 2 is a single-layer carbon fiber film layer with 1.6 mu m thickness and provided with honeycomb-shaped grid holes 5, and is directly molded on the surface of the aramid fiber.
The mica membrane is prepared by the following steps:
preparation of mica paper substrate: selecting muscovite sheets with uniform and impurity-free surfaces as raw materials, washing and drying the mica sheets to obtain dry mica sheets, roasting the dry mica sheets at the temperature of 800 ℃ for 9min, cooling the dry mica sheets to normal temperature along with a furnace, uniformly delivering the cooled mica sheets to a high-pressure hydraulic crusher to be crushed into mica flakes, washing, filtering and screening the crushed mica flakes, controlling the particle size of the mica flakes to be-50 meshes to +200 meshes to obtain pulp flakes, carrying out hydraulic classification on the screened pulp flakes to obtain papermaking pulp, and storing the pulp and boiling the pulp at high temperature and high pressure; and (3) stabilizing the pressure of part of paper pulp in the paper making pulp after the pulp boiling is finished as a raw material, then carrying out size mixing and sizing, making part of pulp into mica paper to obtain a mica paper base material, and reserving part of pulp for later use.
Preparing aramid fibers: carrying out short-cut treatment on aramid fiber III, adding the short-cut aramid fiber III into 50% of acetone according to the mass ratio of feed liquid of 1:80, carrying out ultrasonic-assisted soaking to complete cleaning and oil removal treatment, and cleaning with deionized water after treatment for 2-3 h; then, the resultant was immersed in a 45g/L potassium hydroxide solution in a water bath at 50 ℃ to conduct a roughening treatment, washed with deionized water after 2 hours of treatment, and then neutralized with a 10% sulfuric acid solution.
Using 20g/L stannous chloride solution and 45ml/L hydrochloric acid (d is 119 g/cm)3) Soaking, adding sufficient stannous chloride powder, reacting for 3h, cleaning with deionized water, and completing sensitization treatment; adjusting the pH value of the sensitized chopped aramid III fiber to be 2-3 by using hydrochloric acid, adding a 0.35g/L palladium chloride solution and sufficient palladium chloride, stirring for reacting for 3 hours, and then cleaning by using deionized water to complete activation treatment; and then, carrying out water bath for 3min in warm water by using 100ml/L hydrochloric acid, wherein the water bath ratio is 1:200, treating by using 15g/L sodium hypophosphite after the water bath is finished, the bath ratio is 1:200, cleaning by using deionized water after 10min, finishing reduction treatment, and drying to obtain the pretreated chopped aramid fiber III.
Carrying out surface metallization treatment on the pretreated chopped aramid fiber III in chemical plating solution to form the chopped aramid fiber III with a nickel plating layer, wherein the chemical plating solution comprises 40g/L nickel sulfate, 35g/L sodium hypophosphite, 1.5mg/L sodium tartrate, 5g/L sodium citrate and 6g/L ammonium phosphate; wherein, nickel sulfate is main electroplating salt, sodium hypophosphite is a reducing agent, sodium tartrate and sodium citrate are combined complexing agents, sodium citrate is an auxiliary stabilizer, and ammonium phosphate is an enhanced stabilizer; and (3) reacting the pretreated chopped aramid fiber III in the chemical plating solution, and obtaining the modified chopped aramid fiber III for filling in the aramid fiber layer 3 after the reaction is completed.
Adding the modified chopped aramid fiber III into a coating machine, uniformly spraying the modified chopped aramid fiber III on the surface of a mica paper substrate 4, controlling the spraying thickness to be 60 mu m, covering a carbon fiber film layer 2 pre-opened with honeycomb grid holes after the spraying is finished, carrying out hot pressing stabilization on the surface of the carbon fiber film layer, then using standby mica paper pulp to manufacture a reinforced mica paper layer 1 on the surface of the carbon fiber film layer, carrying out hot pressing and dehydration on the reinforced mica paper layer 1 to form the mica paper layer with the water content of 0.2-0.5%, and then carrying out edge cutting treatment to obtain the finished mica membrane, wherein the reinforced mica paper layer 1 of the mica membrane has no bubbling and peeling phenomena, and the like, so that the bonding force of the.
In the present invention, mica is a material frequently used in the chemical and electronic industries. The mica scales are not beneficial to metal surface treatment because of the atomically flat surface, and meanwhile, the mica scales forming the mica paper depend on Van der Waals force and electrostatic acting force among mica sheets, so that the mechanical strength of the finished paper is small, the mica paper is easy to break, the impact resistance is insufficient, in order to improve the mechanical strength of the mica paper and ensure the insulating property of the mica paper, the adopted reinforcement method uses aramid fibers as a reinforcing material of the mica paper, and the reinforcement method is also an important direction for the insulation development of the high-quality composite mica paper.
However, the aramid fiber body commonly used in the prior art has limited heat resistance, is difficult to meet the requirements of C-level insulation grade and above materials, and is difficult to meet the use in high-end electric heating fields, and meanwhile, because the aramid fiber has smooth surface and poor surface wettability, and when the aramid fiber is compounded with a matrix, the bonding strength of two phase interfaces is weak, the application range of the aramid fiber is greatly limited, mainly because the aramid fiber has a high-crystallization and high-orientation molecular structure and is of an obvious skin-core structure, the wettability is poor, the surface lattice is compact, the active points are few, and the bonding energy of the fiber and the matrix interface is low, so that the surface modification treatment is needed. However, even if the aramid fiber is subjected to surface modification treatment of short cutting and metallization, the aramid fiber under the prior art still has use defects and strength which is difficult to reach the standard, while the aramid fiber III is a para-aromatic heterocyclic copolyamide fiber series product, has excellent performances of low density, ultrahigh strength, ultrahigh modulus, high temperature resistance, good impact resistance, good wear resistance, good wave permeability and the like due to unique molecular structure and process technology, is one of organic fibers with the best comprehensive performance, can effectively utilize the own fiber performance of the aramid fiber III and the surface performance after metallization by utilizing the aramid fiber III as a raw material for surface modification, improves the heat conduction and heat soaking efficiency of mica paper, effectively improves the strength and stability of the mica paper, and can effectively prevent large local expansion coefficient caused by uneven local surface heat distribution by matching with a carbon fiber film layer with honeycomb grid holes, The deformation and fracture conditions can effectively meet the application of mica paper in the aspect of high-end electric heating elements.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The utility model provides a mica diaphragm, its characterized in that, includes basic mica paper layer, the shaping has the enhancement layer on one side surface of basic mica paper layer, the enhancement layer includes one deck aramid fiber layer and one deck carbon fiber film layer, aramid fiber who adopts in the aramid fiber layer is for carrying out nickel plating treatment's short aramid fiber III through the chemical mode, and it has honeycomb grid hole to open on the carbon fiber film layer, and the carbon fiber film layer shaping is on aramid fiber's surface, and the surface of enhancement layer still the shaping has one deck reinforcement mica paper layer.
2. The mica film according to claim 1, wherein the mica paper substrate is a natural white mica paper layer or a natural gold mica paper or an artificial synthetic fluorine gold mica paper.
3. The mica film of claim 1, wherein said reinforcing mica paper layer is a natural white mica paper layer.
4. The mica film according to claim 1, wherein the ratio of the thickness of the mica paper substrate to the thickness of the reinforced mica paper layer after molding is 2:1 to 3: 1.
5. The mica film according to claim 1, wherein the thickness of the aramid fiber layer is 30 to 80 μm, the monofilament diameter of the adopted chopped aramid III is 10 to 25 μm, the thickness of the nickel-plated layer on the chopped aramid III in the aramid fiber layer is 0.15 to 0.35 μm, and the nickel content in the nickel-plated layer is more than 85%.
6. The mica film sheet according to claim 1, wherein the carbon fiber film layer has a single layer thickness of 0.2 to 2 μm.
7. A method for preparing a mica membrane with the technical characteristics of claim 1, which specifically comprises the following operation steps:
s1, purchasing or adopting self-made mica paper as a mica paper base material, and cutting the mica paper into a proper size for later use;
s2, carrying out short-cut treatment on the aramid fiber III or directly purchasing a finished product of the short-cut aramid fiber III, sequentially carrying out pre-treatment of cleaning, oil removal, coarsening, neutralization, sensitization, activation and reduction on the short-cut aramid fiber III, and then putting the pre-treated fiber into a chemical plating solution for carrying out surface metallization treatment to form the short-cut aramid fiber III with a nickel-plated layer;
s3, uniformly spraying the chopped aramid fiber III with the nickel-plated layer prepared in the step S2 on the surface of a mica paper substrate, covering a carbon fiber film layer with honeycomb-shaped grid holes after spraying, manufacturing a reinforced mica paper layer on the surface of the carbon fiber film layer by mica paper pulp after hot pressing, stabilizing, and forming to obtain the finished mica membrane.
8. The method for preparing mica film sheet according to claim 1, wherein the chemical plating solution comprises 40g/L nickel sulfate, 35g/L sodium hypophosphite, 1.5mg/L sodium tartrate, 5g/L sodium citrate and 6g/L ammonium phosphate.
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