CN115447222B - Preparation method of compact PVDF-based composite membrane - Google Patents
Preparation method of compact PVDF-based composite membrane Download PDFInfo
- Publication number
- CN115447222B CN115447222B CN202210636410.XA CN202210636410A CN115447222B CN 115447222 B CN115447222 B CN 115447222B CN 202210636410 A CN202210636410 A CN 202210636410A CN 115447222 B CN115447222 B CN 115447222B
- Authority
- CN
- China
- Prior art keywords
- pvdf
- film
- based composite
- glass substrate
- chemical anchor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002033 PVDF binder Substances 0.000 title claims abstract description 86
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 86
- 239000002131 composite material Substances 0.000 title claims abstract description 76
- 239000012528 membrane Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 43
- 239000000945 filler Substances 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- 238000012360 testing method Methods 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 239000010408 film Substances 0.000 description 56
- 238000000034 method Methods 0.000 description 14
- 238000001723 curing Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 229910002113 barium titanate Inorganic materials 0.000 description 5
- 230000006399 behavior Effects 0.000 description 4
- 230000001066 destructive effect Effects 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 238000004873 anchoring Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229920005570 flexible polymer Polymers 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
- B32B3/08—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B2038/0052—Other operations not otherwise provided for
- B32B2038/0076—Curing, vulcanising, cross-linking
Landscapes
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
The invention discloses a preparation method of a compact PVDF-based composite membrane, wherein a test device comprises a glass substrate and a chemical anchor side layer which is attached to the upper surface of the glass substrate and can form a rigid structure with the PVDF-based composite membrane, and the middle part of the chemical anchor side layer is provided with a hollowed-out area for pouring casting solution; the preparation method comprises the following steps: s1, adding filler into a solvent for dissolving PVDF according to a designed proportion, and uniformly dispersing; s2, putting PVDF powder into the dispersion liquid according to a designed proportion, and heating and dissolving; s3, pouring PVDF film casting solution into the hollow area of the chemical anchor edge layer, and heating and curing to form a film; s4, cutting along the boundary of the hollowed-out area of the chemical anchor edge layer to obtain the compact PVDF-based composite membrane. The invention solves the problem that the film is difficult to be leveled due to large cohesion in the preparation process of the PVDF-based composite film.
Description
Technical Field
The invention belongs to the technical field of flexible polymer composite membrane preparation in the electronic industry, and particularly relates to a preparation method of a compact PVDF-based composite membrane.
Background
Polyvinylidene fluoride (PVDF) is a ferroelectric polymer with good chemical stability, corrosion resistance, high temperature resistance, radiation resistance, and special energy conversion properties such as piezoelectricity, dielectric property, and thermoelectric property. Unlike traditional piezoelectric/dielectric materials such as ceramics, PVDF has the characteristics of mechanical flexibility, low density, easy regulation and control of performance and the like, so that the PVDF has great application potential in numerous electronic industry subdivision fields such as flexible electronic equipment, dielectric capacitors, organic field effect transistors, actuators and the like.
The preparation method of the polyvinylidene fluoride (PVDF) pure film mainly comprises two main flow schemes of melt coextrusion and solution casting in the industrial application process. In the process of preparing the pure PVDF film, the guarantee of the flatness of the film is not very big in practice. If the PVDF composite film is prepared by adopting melt coextrusion, the method has the advantages that the cost of melt coextrusion equipment required by the method is high and the equipment volume is large in spite of higher density, and the PVDF composite precursor master batch can be obtained by blending and granulating dissolved PVDF and inorganic/organic filler particles in advance, so that the steps are complicated. Therefore, the melt coextrusion process is not the best choice for preparing PVDF composite films, both from the standpoint of economic cost and technical ease of operation. For PVDF composite membranes, the solution casting preparation process is clearly superior to melt coextrusion. However, when a solution casting process is used for preparing the PVDF composite film, the strong in-plane cohesive effect can be generated in the process of thermocuring film formation of the PVDF composite film casting solution due to the strong dimensional and size uniformity of the adopted filler, and the cohesive force and the uneven stress distribution in the film formation of the composite film can cause the composite film to generate destructive physical behaviors such as curling, kneading and the like.
The points of interest in conventional solution casting processes are more in three aspects, namely the nature of the solution itself and the choice of material for the base film (casting solution carrier material), and the curing film forming process (e.g., temperature). However, in practice, solution casting processes have found a practical limitation. When the prepared PVDF composite film is thinner (for example, less than or equal to 50 mu m) and the size uniformity of filler particles is high, the PVDF composite film with higher flatness can be prepared by a solution casting method. However, with the increase of the preparation thickness and the occurrence of the conditions of low uniformity of the size of filler particles and high dimensional diversity of the filler, even composite films can be hardly obtained after the curing of PVDF composite casting solution if the conventional solution casting process is still adopted without any technical improvement.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a compact PVDF-based composite membrane. The method for preparing the PVDF-based composite membrane comprises the steps of firstly, creatively providing a chemical anchor side layer, forcibly inhibiting a strong in-plane cohesive effect caused by the diversity of the dimension and the size uniformity of the filler by means of strong covalent bond or hydrogen bond action between the chemical anchor side layer and the PVDF and the composite membrane, so as to achieve the purpose of inhibiting destructive physical behaviors such as curling and kneading of the composite membrane, improving the universality of filler particles in PVDF composite membrane casting liquid, namely reducing the requirements on the dimension and dimension uniformity of the filler particles, and realizing effective controllability of the flatness, thickness and transverse dimension of the PVDF-based composite membrane.
In order to solve the technical problems, the invention is realized by the following technical scheme:
The test device comprises a glass substrate and a chemical anchor edge layer which is attached to the upper surface of the glass substrate and can form a rigid structure with PVDF casting solution, wherein the middle part of the chemical anchor edge layer is provided with a hollowed-out area for casting the casting solution; the preparation method comprises the following steps:
S1, adding a filler into a solvent for dissolving PVDF according to a designed proportion, uniformly dispersing, and dispersing liquid;
S2, putting PVDF powder into the dispersion liquid according to a designed proportion, and heating and dissolving to obtain PVDF casting film liquid;
s3, pouring PVDF film casting solution into the hollowed-out area, and heating, curing and forming a film;
S4, cutting along the boundary of the hollowed-out area, and separating the cut PVDF-based composite film from the glass substrate to obtain the compact PVDF-based composite film.
Preferably, in step S1, the filler is added to the solvent in an amount of 0 to 50% by volume of the PVDF-based composite film after curing.
Preferably, in step S1, the solvent is an organic solvent, which includes at least one of N, N-dimethylformamide, N-methylpyrrolidone and acetone.
Preferably, in step S2, the PVDF powder is added in an amount of 1 to 30% by mass based on the dispersion.
Preferably, in step S3, the heating temperature does not exceed 170 ℃.
Preferably, the filler comprises inorganic or organic solid particles, the dimensions of which comprise 0-dimensional micro-nano particles, 1-dimensional micro-nano wire rods and 2-dimensional micro-nano sheets. The uniformity of the dimensions of the filler means that the dimensions of the filler in the directions of x, y and z dimensions are less than 1mm, and the dimensions of the filler can be freely combined.
Preferably, the chemical anchor edge layer is made of organic glass or inorganic glass. Wherein, covalent bond can be generated between the organic glass and the PVDF-based composite membrane, and hydrogen bond can be generated between the inorganic glass and the PVDF-based composite membrane.
Preferably, the thickness of the chemical anchoring edge layer is 30-1000 μm.
Compared with the prior art, the preparation method of the compact PVDF-based composite membrane has the following beneficial effects:
(1) The universality against filler particles is very high. Various inorganic or organic solid particles can be selected; the dimension of the filler can comprise 0-dimensional micro-nano particles, 1-dimensional micro-nano wire rods and 2-dimensional micro-nano sheets; the dimensions and dimensions of the filler may be unlimited, any combination; the concentration of filler loading can be up to 50% by volume.
(2) On the premise that the flatness of the PVDF-based composite film is effectively controlled, the method is not limited by the transverse dimension in the plane and the shape of the composite film. The clean glass substrate is selected as a casting solution bearing table, the thickness of the glass substrate is not limited, and the transverse size can be adjusted without limit according to application requirements; the chemical anchor side layer is enclosed on the glass substrate according to the shape and the size of the application requirement to form a closed loop; the physical destructive behaviors such as curling, kneading and the like in the heat curing process can be strongly restrained due to the strong covalent bond or hydrogen bond acting force between the chemical anchor edge layer and the PVDF composite film.
(3) The thickness of the PVDF-based composite film can be simply, conveniently and effectively controlled. The thickness of the compact PVDF-based composite membrane can be adjusted according to the thickness of the chemical anchoring edge layer, and the preferable thickness is 30-1000 mu m.
Drawings
FIG. 1 is a schematic plan view of a test apparatus according to an embodiment of the present invention.
Fig. 2 is a cross-sectional view taken along A-A in fig. 1.
FIG. 3 is a PVDF/BaTiO 3 composite membrane prepared in example 1 of the present invention.
FIG. 4 is a PVDF/Ag rod composite film prepared in example 2 of the present invention.
FIG. 5 is a PVDF/C 3N4 composite membrane prepared in example 3 of the present invention.
In the figure: 1-a glass substrate; 2-chemical anchor edge layer; 21-hollowed-out area.
Detailed Description
During the experiments to which the invention relates, we found that the uneven phenomenon of the PVDF-based composite film (namely, the situation that the uniformity of the size of filler particles is low and the dimensional diversity of the filler is high along with the increase of the preparation thickness, if the traditional solution casting technology is still adopted, no technical improvement is made, the even composite film can be hardly obtained after the PVDF composite film casting liquid is solidified) is caused because a large amount of two-phase interfaces are generated in the PVDF composite film casting liquid due to the introduction of the filler. Because of the significant difference in dimensions of these two-phase interfaces and the large number of two-phase interfaces, the solvent evaporation rate in the PVDF composite casting is greatly different at each two-phase interface in the plane when the composite casting is cured by heating. From a macroscopic point of view, in the drying and film forming process of the PVDF composite casting film liquid, the film in the peripheral area is always completely dried, the film in the adjacent area is still in a solution state, the film forming states of different areas in the surface are also quite different, and finally, the film starts to curl from the periphery of the composite film until the film is completely dried, and the composite film finally kneads and gathers into a group due to uneven stress.
In order that those skilled in the art will better understand the technical solution of the present invention, preferred embodiments of the present invention will be described below with reference to specific examples, but should not be construed as limiting the present patent, but merely as examples.
The test methods or test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are obtained from conventional commercial sources or prepared in conventional manner.
Example 1
The preparation method of the compact PVDF-based composite membrane comprises the following steps: ①PVDF/BaTiO3 Preparing a composite casting solution: adding 0-dimensional 60-100 nm barium titanate filler into DMF solvent according to the volume fraction of 11% of the solidified barium titanate filler in PVDF film, and performing ultrasonic dispersion; then, PVDF powder with the mass fraction of 10% is put into the dispersion liquid, and is fully dissolved under the heating condition of 70 ℃ to obtain PVDF/BaTiO3 composite casting film liquid; ② Setting a casting solution bearing table: selecting a clean organic glass substrate as a bearing table, wherein the thickness of the glass substrate 1 is 1mm, and the transverse dimension is 180mm x 300mm; the outer frame of the chemical anchor edge layer 2 is 180mm x 300mm, the inner frame is 124mm x 104mm (namely the size of the hollowed-out area 21), and the thickness is 1mm, as shown in figures 1 and 2; ③PVDF/BaTiO3 Curing the composite casting solution to form a film: pouring a proper amount of PVDF/BaTiO 3 composite casting solution into the shape surrounded by the chemical anchor edge layer 2, and curing to form a film at 170 ℃; then, cutting along the boundary of the hollowed-out area 21 to obtain the compact PVDF/BaTiO 3 composite membrane, as shown in figure 3.
Example 2
The preparation method of the compact PVDF-based composite membrane comprises the following steps: ① Preparing PVDF/Ag rod composite casting film liquid: putting Ag rod filler with 0-dimensional length-diameter ratio of 10:1 into NMP solvent according to the volume fraction of 1.3% of the solidified Ag rod filler in PVDF film, and performing ultrasonic dispersion; then, PVDF powder with the mass fraction of 10% is put into the dispersion liquid, and is fully dissolved under the heating condition of 90 ℃ to obtain PVDF/Ag rod composite casting film liquid; ② Setting a casting solution bearing table: selecting a clean organic glass substrate as a bearing table, wherein the thickness of the glass substrate is 1mm, and the transverse dimension is 180mm x 300mm; the outer frame of the chemical anchor side layer is 180mm x 300mm, the inner frame is 124mm x 104mm, and the thickness is 30 μm, as shown in figures 1 and 2; ③ And curing the PVDF/Ag rod composite casting solution to form a film: pouring a proper amount of PVDF/Ag rod composite casting solution into the shape surrounded by the chemical anchor edge layer, and curing the solution to form a film at 110 ℃; subsequently, the thin film is cut along the boundary of the hollowed-out area 21, and a compact PVDF/Ag rod composite film is obtained, as shown in FIG. 4.
Example 3
The preparation method of the compact PVDF-based composite membrane comprises the following steps: ①PVDF/C3N4 Preparing a composite casting solution: adding a C 3N4 filler with the 2-dimensional diameter of 4 mu m into DMF/acetone (volume ratio of 7:3) solvent according to the volume fraction of 50% of the solidified C 3N4 filler in the PVDF film, and performing ultrasonic dispersion; then, PVDF powder with the mass fraction of 10% is put into the dispersion liquid, and is fully dissolved under the heating condition of 80 ℃ to obtain PVDF/C 3N4 composite casting film liquid; ② Setting a casting solution bearing table: selecting a clean inorganic glass substrate as a bearing table, wherein the thickness of the glass substrate is 1mm, and the transverse dimension is 180mm x 300mm; the outer frame of the chemical anchor edge layer is a circle with the diameter of 100mm, the inner frame is a circle with the diameter of 70mm, and the thickness is 1000 mu m; ③ PVDF/C3N4 Curing the composite casting solution to form a film: pouring a proper amount of PVDF/C 3N4 composite casting solution into the shape surrounded by the chemical anchor edge layer, and curing the solution to form a film at 80 ℃; subsequently, the compact PVDF/C 3N4 composite membrane is obtained by cutting along the boundary of the hollowed-out area 21, as shown in FIG. 5.
As is evident from fig. 2 to 4, the composite film formed by the filler and PVDF composite with various dimensions and dimensions prepared by the chemical anchoring edge method according to the present invention can maintain high flatness, and overcomes the defect of destructive physical behaviors such as curling and kneading caused by uneven cohesive force and stress distribution during the curing film forming process.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. Accordingly, the present embodiment is merely an exemplary case and is not limiting. The scope of the invention is indicated by the appended claims rather than by the foregoing description, and all changes that come within the meaning and range of equivalency of the claims are intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (1)
1. The preparation method of the compact PVDF-based composite membrane is characterized in that a test device comprises a glass substrate (1) and a chemical anchor edge layer (2) which is attached to the upper surface of the glass substrate (1) and can form a rigid structure with the PVDF-based composite membrane, a hollowed-out area (21) for pouring PVDF casting solution is formed in the middle of the chemical anchor edge layer (2), organic glass is selected as the chemical anchor edge layer (2), and inorganic glass is selected as the glass substrate (1); the thickness of the glass substrate is 1mm, and the transverse dimension is 180mm x 300mm; the outer frame of the chemical anchor edge layer is a circle with the diameter of 100mm, the inner frame is a circle with the diameter of 70mm, and the thickness is 1000 mu m; the preparation method comprises the following steps:
S1, adding 50% of filler in the PVDF-based composite film according to the volume fraction of the filler in the PVDF-based composite film after solidification, and uniformly dispersing to obtain a dispersion liquid; the filler is 2-dimensional C 3N4 filler with the diameter of 4 mu m; the solvent is a mixed solvent of DMF and acetone in a volume ratio of 7:3;
S2, putting PVDF powder with the mass fraction of 10% into the dispersion liquid in the S1, and heating and dissolving at 80 ℃ to obtain a composite casting film liquid of PVDF and C 3N4;
S3, pouring the composite casting film liquid in the S2 into the hollowed-out area (21), and heating and curing at 80 ℃ to form a film;
s4, cutting along the boundary of the hollowed-out area (21), and separating the cut film from the glass substrate to obtain the flat compact PVDF-based composite film.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210636410.XA CN115447222B (en) | 2022-06-07 | 2022-06-07 | Preparation method of compact PVDF-based composite membrane |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210636410.XA CN115447222B (en) | 2022-06-07 | 2022-06-07 | Preparation method of compact PVDF-based composite membrane |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115447222A CN115447222A (en) | 2022-12-09 |
CN115447222B true CN115447222B (en) | 2024-06-04 |
Family
ID=84296142
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210636410.XA Active CN115447222B (en) | 2022-06-07 | 2022-06-07 | Preparation method of compact PVDF-based composite membrane |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115447222B (en) |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105529496A (en) * | 2015-10-23 | 2016-04-27 | 湘潭大学 | Gel polymer electrolyte membrane and preparation method thereof |
CN105771703A (en) * | 2016-03-15 | 2016-07-20 | 北京工业大学 | Preparation method of polyethersulfone-based composite positive permeable membrane |
CN108948390A (en) * | 2018-07-24 | 2018-12-07 | 电子科技大学 | A kind of step curtain coating preparation method of PVDF based polymer film |
WO2018233338A1 (en) * | 2017-06-22 | 2018-12-27 | 南京工业大学 | Preparation method for force-electro-optical conversion enhanced light emitting composite film |
CN109400931A (en) * | 2018-11-22 | 2019-03-01 | 武汉纺织大学 | It is a kind of to be orientated porous polyunsymfluorethylepiezoelectric piezoelectric film and preparation method thereof |
CN109942997A (en) * | 2019-04-03 | 2019-06-28 | 大连大学 | A kind of graphene oxide-barium titanate dielectric composite film and preparation method thereof |
CN110003514A (en) * | 2019-04-16 | 2019-07-12 | 电子科技大学 | Preparation method and application of high-dielectric composite film |
CN111333892A (en) * | 2020-03-19 | 2020-06-26 | 辽宁科京新材料科技有限公司 | Preparation method of organic/inorganic amphoteric ion conduction composite membrane |
CN112111757A (en) * | 2020-09-15 | 2020-12-22 | 中国科学院大连化学物理研究所 | Composite membrane for high-temperature water electrolysis and preparation method and application thereof |
AU2020103787A4 (en) * | 2020-11-30 | 2021-02-11 | Junada (qingdao) Technology Co., Ltd. | SiO2/PVDF-HFP Composite Fiber Membrane and Its Preparation Method and Application |
CN113843937A (en) * | 2021-10-08 | 2021-12-28 | 西安理工大学 | Migration-resistant hydrogel-based freshness colorimetric indication label and preparation method thereof |
-
2022
- 2022-06-07 CN CN202210636410.XA patent/CN115447222B/en active Active
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105529496A (en) * | 2015-10-23 | 2016-04-27 | 湘潭大学 | Gel polymer electrolyte membrane and preparation method thereof |
CN105771703A (en) * | 2016-03-15 | 2016-07-20 | 北京工业大学 | Preparation method of polyethersulfone-based composite positive permeable membrane |
WO2018233338A1 (en) * | 2017-06-22 | 2018-12-27 | 南京工业大学 | Preparation method for force-electro-optical conversion enhanced light emitting composite film |
CN108948390A (en) * | 2018-07-24 | 2018-12-07 | 电子科技大学 | A kind of step curtain coating preparation method of PVDF based polymer film |
CN109400931A (en) * | 2018-11-22 | 2019-03-01 | 武汉纺织大学 | It is a kind of to be orientated porous polyunsymfluorethylepiezoelectric piezoelectric film and preparation method thereof |
CN109942997A (en) * | 2019-04-03 | 2019-06-28 | 大连大学 | A kind of graphene oxide-barium titanate dielectric composite film and preparation method thereof |
CN110003514A (en) * | 2019-04-16 | 2019-07-12 | 电子科技大学 | Preparation method and application of high-dielectric composite film |
CN111333892A (en) * | 2020-03-19 | 2020-06-26 | 辽宁科京新材料科技有限公司 | Preparation method of organic/inorganic amphoteric ion conduction composite membrane |
CN112111757A (en) * | 2020-09-15 | 2020-12-22 | 中国科学院大连化学物理研究所 | Composite membrane for high-temperature water electrolysis and preparation method and application thereof |
AU2020103787A4 (en) * | 2020-11-30 | 2021-02-11 | Junada (qingdao) Technology Co., Ltd. | SiO2/PVDF-HFP Composite Fiber Membrane and Its Preparation Method and Application |
CN113843937A (en) * | 2021-10-08 | 2021-12-28 | 西安理工大学 | Migration-resistant hydrogel-based freshness colorimetric indication label and preparation method thereof |
Non-Patent Citations (4)
Title |
---|
g-C_3N_4/PVDF复合膜的制备及热解性能研究;王慧雅;杭祖圣;卢向明;应三九;;现代化工(第04期);全文 * |
姜在渭.上海建筑材料工作志.上海社会科学院出版社,1997,第99页. * |
李俊寿.新材料概论.国防工业出版社,2004,第188页. * |
邢焰等.国之重器出版工程 航天器材料.人民邮电出版社,2018,第287页. * |
Also Published As
Publication number | Publication date |
---|---|
CN115447222A (en) | 2022-12-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Liao et al. | Misorientation control and functionality design of nanopillars in self-assembled Perovskite− Spinel heteroepitaxial nanostructures | |
CN101322919B (en) | Method for preparing micropore ceramic separation film | |
Lyu et al. | Direct ink writing of programmable functional silicone‐based composites for 4D printing applications | |
KR101678817B1 (en) | Manufacturing method of reduced graphene oxide, reduced graphene oxide, manufacturing method of barrier film using the reduced graphene oxide and barrier film | |
Chen et al. | Tilted aligned epitaxial La0. 7Sr0. 3MnO3 nanocolumnar films with enhanced low-field magnetoresistance by pulsed laser oblique-angle deposition | |
KR101471161B1 (en) | Piezoelectric element having β-phase PVDF film prepared by spray coating | |
CN115447222B (en) | Preparation method of compact PVDF-based composite membrane | |
JP2011145636A (en) | Method for manufacturing flexible display substrate having low moisture and low oxygen permeability | |
CN109694537A (en) | Energy storage composite film material and preparation method containing quantum dot | |
CN109291428B (en) | Method for regulating and controlling arrangement direction of ceramic nanowires in composite material | |
Liu et al. | Effect of the slurry composition on the piezoelectric properties of PZT ceramics fabricated via materials extrusion 3D printing | |
Yabu et al. | Robust anisotropic polymer meshes prepared by stretching and photo-crosslinking of poly (1, 2-butadiene) honeycomb films | |
CN104891426B (en) | A kind of preparation method with the micro-patterned films of selective stimulating recovery function | |
Ko et al. | Selective Template Wetting Routes to Hierarchical Polymer Films: Polymer Nanotubes from Phase-Separated Films via Solvent Annealing | |
CN110628068A (en) | Method for preparing surface pattern structure with magnetic response | |
CN110713645B (en) | Polymer-based two-dimensional topological material and preparation method and application thereof | |
Aoki | Superhydrophobic coating fabricated by electrophoretic deposition using polydimethylsiloxane-based organic–inorganic hybrid materials and ceramic powders | |
Tamura et al. | Tailoring of grain size in textured CaBi 4 Ti 4 O 15 ceramics prepared by templated grain growth process | |
KR101468491B1 (en) | Nano-grid structure of Nanowire and method of fabrication thereof | |
CN107540402A (en) | A kind of preparation method of porous calcium copper titanate film | |
Wen et al. | Fabrication of PZT microspheres for application in electrorheological fluids | |
CN106540758A (en) | Micro-fluidic chip | |
Aoki et al. | One-step fabrication of composites with superhydrophobic surfaces using spin-coating with polydimethylsiloxane/silica/solvent suspension | |
CN114887493B (en) | Three-dimensional porous material and preparation method thereof | |
CN103936425A (en) | Preparation method of ceramic plate |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |