CN115447222A - Preparation method of compact PVDF (polyvinylidene fluoride) -based composite membrane - Google Patents
Preparation method of compact PVDF (polyvinylidene fluoride) -based composite membrane Download PDFInfo
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- CN115447222A CN115447222A CN202210636410.XA CN202210636410A CN115447222A CN 115447222 A CN115447222 A CN 115447222A CN 202210636410 A CN202210636410 A CN 202210636410A CN 115447222 A CN115447222 A CN 115447222A
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- 239000002131 composite material Substances 0.000 title claims abstract description 76
- 239000012528 membrane Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 92
- 238000005266 casting Methods 0.000 claims abstract description 42
- 239000000945 filler Substances 0.000 claims abstract description 29
- 239000011521 glass Substances 0.000 claims abstract description 28
- 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 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229910003480 inorganic solid Inorganic materials 0.000 claims 1
- 230000006399 behavior Effects 0.000 description 4
- 230000001066 destructive effect Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- 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 form; Layered products 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 form; Layered products 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 form; Layered products 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
Abstract
The invention discloses a preparation method of a compact PVDF (polyvinylidene fluoride) -based composite membrane.A 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 the PVDF-based composite membrane, wherein the middle part of the chemical anchor edge layer is provided with a hollow area for pouring a membrane casting solution; the preparation method comprises the following steps: s1, adding a filler into a solvent for dissolving PVDF according to a design proportion, and uniformly dispersing; s2, putting PVDF powder into the dispersion liquid according to a designed proportion, and heating for dissolving; s3, pouring a PVDF film casting solution into the hollow area of the chemical anchor edge layer, and heating and curing to form a film; and S4, cutting along the hollow area boundary of the chemical anchor edge layer to obtain the compact PVDF-based composite membrane. The invention solves the problem that the membrane is difficult to flatten due to large internal cohesion in the preparation process of the PVDF-based composite membrane.
Description
Technical Field
The invention belongs to the technical field of preparation of flexible polymer composite membranes in the electronic industry, and particularly relates to a preparation method of a compact PVDF (polyvinylidene fluoride) -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, dielectricity, pyroelectricity and the like. Different from traditional piezoelectric/dielectric materials such as ceramics, PVDF has the characteristics of mechanical flexibility, low density, easy performance regulation and the like, so that PVDF has great application potential in a plurality of 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 mainstream schemes of melt coextrusion and solution casting in the industrial application process. In both preparation methods, the guarantee of the flatness of the membrane is practically not a great problem in the preparation of pure PVDF membranes. If the PVDF composite membrane is prepared by adopting melt coextrusion, although the compactness is higher, the melt coextrusion equipment required by the method has high cost and large equipment volume, 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 co-extrusion process is not the best choice for the preparation process of the PVDF composite membrane from the viewpoint of economic cost and convenience of technical operation. For PVDF composite films, the solution cast preparation process is clearly superior to melt coextrusion. However, when the PVDF composite film is prepared by using the solution casting process, the PVDF composite casting solution may generate a strong in-plane cohesion effect during the thermosetting film forming process due to the strong diversity of the dimension and size uniformity of the adopted filler, and the composite film may generate destructive physical behaviors such as warping, crumpling and the like due to uneven distribution of cohesion and stress during the film forming process.
The traditional solution casting process focuses more on three aspects, namely the nature of the solution and the material selection of a base film (casting solution bearing material), and the curing film-forming process (such as temperature). However, in practice, it has been found that solution casting processes have one applicable limitation. When the prepared PVDF composite membrane is thin (such as less than or equal to 50 mu m) and the size uniformity of the filler particles is high, the PVDF composite membrane with high flatness can be prepared by a solution casting method. However, with the increase of the preparation thickness, the lower size uniformity of the filler particles and the higher dimensional diversity of the filler, if the traditional solution casting process is still adopted, no technical improvement is made, and a flat composite membrane can hardly be obtained after the PVDF composite casting solution is cured.
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 the chemical anchoring edge layer is creatively provided, and by means of strong covalent bond or hydrogen bond action between the chemical anchoring edge layer and the PVDF and composite membrane, the strong in-plane cohesion effect caused by the diversity of the dimension and dimension uniformity of the filler is forcibly inhibited, so that the aim of inhibiting the composite membrane from generating destructive physical behaviors such as warping, kneading and the like is fulfilled, the universality of the filler particles in the PVDF composite membrane casting solution is improved, namely, the requirements on the dimension and dimension uniformity of the filler particles are reduced, and the effective controllability of the flatness, thickness and transverse dimension of the PVDF-based composite membrane is realized.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a preparation method of a compact PVDF (polyvinylidene fluoride) -based composite membrane comprises a test device and a test device, wherein 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 a PVDF membrane casting solution, and the middle part of the chemical anchor edge layer is provided with a hollow area for casting the membrane casting solution; the preparation method comprises the following steps:
s1, adding a filler into a solvent for dissolving PVDF according to a design proportion, and dispersing uniformly to obtain a dispersion liquid;
s2, putting PVDF powder into the dispersion liquid according to a designed proportion, and heating and dissolving to obtain a PVDF membrane casting liquid;
s3, pouring a PVDF membrane casting solution into the hollow area, and heating and curing to form a membrane;
and S4, cutting along the boundary of the hollow area, and separating the cut film from the glass substrate to obtain the compact PVDF-based composite film.
Preferably, in step S1, the filler is introduced into 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 including 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 in the dispersion liquid.
Preferably, in step S3, the heating temperature does not exceed 170 ℃.
Preferably, the filler comprises inorganic or organic solid particles, and the dimensions of the filler comprise 0-dimensional micro-nano particles, 1-dimensional micro-nano wire rods and 2-dimensional micro-nano sheets. The various size uniformity of the filler means that the dimension and size of the filler can be freely combined without limitation under the condition that the size of the filler in the directions of three dimensions of x, y and z is less than 1 mm.
Preferably, the chemical anchor edge layer is made of organic glass or inorganic glass. Wherein, when organic glass is adopted, covalent bonds can be generated between the organic glass and the PVDF-based composite membrane, and when inorganic glass is adopted, hydrogen bonds 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 for filler particles is 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 dimension and size of the filler can be unlimited and can be combined at will; the filler can be filled up to a concentration of 50% by volume.
(2) Under the premise that the flatness of the PVDF-based composite membrane is effectively controlled, the PVDF-based composite membrane is not limited by the in-plane transverse dimension and the shape of the composite membrane. Selecting a clean glass substrate as a casting solution bearing platform, wherein the thickness of the glass substrate is not limited, and the transverse dimension can be adjusted without limit according to application requirements; the chemical anchoring edge layer is formed into a shape and a size corresponding to the application requirements on the glass substrate according to the shape and the size of the application requirements to form a closed loop; due to the strong covalent bond or hydrogen bond acting force between the chemical anchor edge layer and the PVDF composite film, physical damage behaviors such as warping, crumpling and the like in the thermosetting process can be strongly inhibited.
(3) The thickness of the PVDF-based composite membrane 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 μm.
Drawings
FIG. 1 is a schematic plan view of a testing apparatus according to an embodiment of the present invention.
Fig. 2 isbase:Sub>A sectional view taken along linebase:Sub>A-base:Sub>A in fig. 1.
FIG. 3 is a PVDF/BaTiO prepared in example 1 of the present invention 3 A composite membrane.
FIG. 4 is a PVDF/Ag rod composite membrane prepared in example 2 of the present invention.
FIG. 5 is a PVDF/C prepared in example 3 of the present invention 3 N 4 A composite membrane.
In the figure: 1-a glass substrate; 2-chemical anchoring edge layer; 21-hollowed out area.
Detailed Description
In the experimental process related to the invention, the phenomenon that the PVDF-based composite membrane is not flat (namely, along with the increase of the preparation thickness and the occurrence of the conditions that the size uniformity of filler particles is lower and the dimension diversity of the filler is higher, if the traditional solution casting process is still adopted, no technical improvement is made, and the flat composite membrane can hardly be obtained after the PVDF composite membrane casting solution is cured) is found to be caused because a large amount of two-phase interfaces are generated in the PVDF composite membrane casting solution due to the introduction of the filler. Because of the obvious difference of the scales of the two-phase interfaces and the huge number of the two-phase interfaces, the volatilization rate of the solvent in the PVDF composite casting solution at each two-phase interface in the plane is greatly different when the composite casting solution is heated and cured. From a macroscopic view, in the process of drying and film-forming the PVDF composite casting solution, 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 greatly different, finally, the film starts to curl and warp from the periphery of the composite film until the film is completely dried, and the composite film finally kneads and gathers into a whole due to uneven stress.
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with specific examples, which should not be construed as limiting the present patent, but merely as exemplifications.
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 either commercially available from conventional sources or are prepared in conventional manners.
Example 1
A preparation method of a compact PVDF-based composite membrane comprises the following steps: (1) PVDF/BaTiO 3 Preparing a composite casting solution: adding a 0-dimensional 60-100 nm barium titanate filler into a DMF (dimethyl formamide) solvent according to the volume fraction of 11% occupied in the PVDF film after curing, and performing ultrasonic dispersion; then, putting 10% PVDF powder by mass fraction into the dispersion liquid, and fully dissolving under the heating condition of 70 ℃ to obtain a PVDF/BaTiO3 composite casting solution; (2) setting a casting solution bearing platform: selecting a clean organic glass substrate as a bearing platform, 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, and the inner frame is 124mm x 104mm (i.e. the size of the hollowed-out area 21) with a thickness of 1mm, as shown in fig. 1 and 2; (3) PVDF/BaTiO 3 Curing the composite casting solution to form a film: pouring a proper amount of PVDF/BaTiO into the shape surrounded by the chemical anchoring edge layer 2 3 The composite membrane casting solution is cured to form a membrane at the temperature of 170 ℃; subsequently, cutting along the boundary of the hollow area 21 to obtain compact PVDF/BaTiO 3 Composite membrane, as shown in figure 3.
Example 2
A preparation method of a compact PVDF-based composite membrane comprises the following steps: (1) preparing a PVDF/Ag rod composite casting solution: adding the Ag rod filler with the length-diameter ratio of 0-10 of 1 in the volume fraction of 1.3 percent in the PVDF film after curing into an NMP solvent, and performing ultrasonic dispersion; then, adding 10% of PVDF powder by mass fraction into the dispersion liquid, and fully dissolving under the heating condition of 90 ℃ to obtain a PVDF/Ag rod composite casting solution; (2) setting a membrane casting liquid bearing platform: selecting a clean organic glass substrate as a bearing platform, wherein the thickness of the glass substrate is 1mm, and the transverse dimension of the glass substrate is 180mm x 300mm; the outer frame of the chemical anchor edge layer is 180mm x 300mm, the inner frame is 124mm x 104mm, and the thickness is 30 μm, as shown in fig. 1 and 2; (3) curing the PVDF/Ag rod composite casting solution to form a film: pouring a proper amount of PVDF/Ag rod composite membrane casting solution into the shape enclosed by the chemical anchor edge layer, and curing at 110 ℃ to form a membrane; and then, cutting along the boundary of the hollow area 21 to obtain a compact PVDF/Ag rod composite membrane, as shown in FIG. 4.
Example 3
A preparation method of a compact PVDF-based composite membrane comprises the following steps: (1) PVDF/C 3 N 4 Preparing a composite casting solution: 2-dimensional C with the diameter of 4 mu m 3 N 4 Adding the filler into a DMF/acetone (volume ratio of 7; subsequently, 10 mass% PVDF powder was put into the dispersion and sufficiently dissolved under heating at 80 ℃ to obtain PVDF/C 3 N 4 Compounding the casting solution; (2) setting a casting solution bearing platform: selecting a clean inorganic glass substrate as a bearing table, wherein the thickness of the glass substrate is 1mm, and the transverse dimension of the glass substrate is 180mm x 300mm; the outer frame of the chemical anchor edge layer is straightA circle with the diameter of 100mm, an inner frame of 70mm and the thickness of 1000 mu m; (3) PVDF/C 3 N 4 Curing the composite casting solution to form a film: pouring proper amount of PVDF/C into the shape enclosed by the chemical anchoring edge layer 3 N 4 Compounding the casting solution, and curing at 80 ℃ to form a film; subsequently, cutting along the boundary of the hollow area 21 to obtain compact PVDF/C 3 N 4 Composite membrane, as shown in fig. 5.
From fig. 2 to 4, it is obvious that the composite film of PVDF and filler with various dimensions and size uniformity prepared by the chemical anchor edge method of the present invention can maintain high flatness, and overcome the defect of occurrence of destructive physical behaviors such as warping and crumpling caused by uneven distribution of cohesion and stress 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 any other specific form without departing from the spirit or essential attributes thereof. Thus, the present embodiments are merely exemplary and non-limiting. The scope of the invention is indicated by the appended claims rather than 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 above are only preferred embodiments of the present invention, and it should be noted that the above preferred embodiments should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the 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 should be considered to be within the scope of the invention.
Claims (8)
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 anchoring 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, wherein the middle part of the chemical anchoring edge layer (2) is provided with a hollow area (21) for pouring a PVDF membrane casting solution; the preparation method comprises the following steps:
s1, adding a filler into a solvent for dissolving PVDF according to a design proportion, and uniformly dispersing to obtain a dispersion liquid;
s2, putting PVDF powder into the dispersion liquid according to a designed proportion, and heating and dissolving to obtain a PVDF membrane casting liquid;
s3, pouring a PVDF film casting solution into the hollow area (21), and heating and curing to form a film;
and S4, cutting along the boundary of the hollow area (21), and separating the cut product from the glass substrate to obtain the compact PVDF-based composite membrane.
2. The method of preparing a densified PVDF-based composite film according to claim 1, wherein 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.
3. The process for preparing a dense PVDF-based composite membrane according to claim 1, wherein in step S1, an organic solvent comprising at least one of N, N-dimethylformamide, N-methylpyrrolidone and acetone is used as the solvent.
4. The method for producing a dense PVDF-based composite membrane according to claim 1, wherein in step S2, the PVDF powder is added in an amount of 1 to 30% by mass in the dispersion liquid.
5. The process for the preparation of a dense PVDF-based composite membrane according to claim 1, wherein in step S3, the heating temperature is not more than 170 ℃.
6. The process for the preparation of a densified PVDF-based composite membrane according to claim 1, wherein the filler comprises inorganic solid particles or organic solid particles.
7. The process for the preparation of a dense PVDF-based composite membrane according to claim 1, wherein the chemical anchoring edge layer (2) is made of organic glass or inorganic glass.
8. The process for the preparation of a dense PVDF-based composite membrane according to claim 1, wherein the thickness of the chemical anchoring edge layer (2) is 30 to 1000 μm.
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