CN113426306A - Double-layer hollow ceramic membrane and production process thereof - Google Patents
Double-layer hollow ceramic membrane and production process thereof Download PDFInfo
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- CN113426306A CN113426306A CN202110708809.XA CN202110708809A CN113426306A CN 113426306 A CN113426306 A CN 113426306A CN 202110708809 A CN202110708809 A CN 202110708809A CN 113426306 A CN113426306 A CN 113426306A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 231
- 239000012528 membrane Substances 0.000 title claims abstract description 165
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000012296 anti-solvent Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229920000297 Rayon Polymers 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 44
- 239000002904 solvent Substances 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- 238000001721 transfer moulding Methods 0.000 description 3
- 239000011345 viscous material Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
Abstract
The invention discloses a double-layer hollow ceramic membrane and a production process thereof, and relates to the field of ceramic membranes. The technical scheme mainly comprises the following steps: s100, preparing a first ceramic membrane by a phase transfer method; s200, coating ceramic slurry on the surface of the first ceramic membrane to form a convex part; s300, placing the other first ceramic membrane on the boss, and then pressing to form a double-layer hollow ceramic membrane; s400, sintering and forming the double-layer hollow ceramic membrane. The invention is suitable for ceramic membranes formed by a phase transfer method, and can improve the bonding effect of two layers of membranes after sintering and improve the strength and the pressure-bearing capacity of the double-layer hollow ceramic membrane.
Description
Technical Field
The invention relates to the field of ceramic membranes, in particular to a double-layer hollow ceramic membrane and a production process thereof.
Background
The traditional ceramic membrane is formed by adopting an extrusion method, and a hollow ceramic membrane structure can be formed in one step to enhance the strength of the ceramic membrane. However, the phase transfer method cannot form the hollow ceramic membrane structure in one step.
The prior Chinese patent with the publication number of CN103381338B discloses a ceramic flat membrane support and a preparation method thereof, wherein a half-side membrane containing a convex part is prepared by a phase transfer method, then a layer of viscous substance is coated on the convex part, then two half-side membranes are relatively adhered to form a green body, and finally the ceramic flat membrane support is obtained by sintering; the viscous substance is PVA water solution.
However, the above-mentioned viscous substance merely plays a temporary blocking role, and the aqueous PVA solution is decomposed at the time of high-temperature sintering.
The prior Chinese patent with the publication number of CN105188893B discloses a product with a channel and a manufacturing method thereof, which comprises the following steps: contacting a template having spaced apart openings with a solution comprising a first solvent and a polymer soluble in the first solvent; introducing a second solvent into the solution through the openings of the template to cause phase inversion of the solution and form an article having spaced apart channels extending from the surface of the article to a substantially planar body of the article.
However, the above-described manufacturing method cannot produce a product having a projection.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a production process of a double-layer hollow ceramic membrane, which is suitable for ceramic membranes formed by a phase transfer method and can improve the pressure bearing capacity.
In order to achieve the purpose, the invention provides the following technical scheme:
a production process of a double-layer hollow ceramic membrane comprises the following steps:
s100, preparing a first ceramic membrane by a phase transfer method;
s200, preparing a second ceramic membrane by a phase transfer method, wherein a convex part is integrally formed on the surface of the second ceramic membrane;
s300, coating ceramic slurry on the end face of the bulge of the second ceramic membrane;
s400, placing the first ceramic membrane on the boss of the second ceramic membrane to enable the first ceramic membrane to be in contact with the ceramic slurry on the end face of the boss, and then pressing the first ceramic membrane and the second ceramic membrane to form a double-layer hollow ceramic membrane;
and S500, sintering and molding the double-layer hollow ceramic membrane.
Further, in step S400, the method further includes immersing the double-layered hollow ceramic membrane formed after the pressing in water, and performing a drying process after taking out the membrane.
In order to achieve the purpose, the invention also provides the following technical scheme:
a production process of a double-layer hollow ceramic membrane comprises the following steps:
s100, preparing a first ceramic membrane by a phase transfer method;
s200, coating ceramic slurry on the surface of the first ceramic membrane to form a convex part;
s300, placing the other first ceramic membrane on the boss, and then pressing to form a double-layer hollow ceramic membrane;
s400, sintering and forming the double-layer hollow ceramic membrane.
Further, in step S300, the method further includes immersing the double-layered hollow ceramic membrane formed after the pressing in water, and performing a drying process after taking out the membrane.
Further, the ceramic slurry comprises ceramic powder, an organic solvent and a polymer.
In order to achieve the purpose, the invention also provides the following technical scheme:
a production process of a double-layer hollow ceramic membrane comprises the following steps:
s100, preparing a first ceramic membrane by a phase transfer method;
s200, coating viscose on the surface of the first ceramic film to form a convex part;
and S300, placing another first ceramic membrane on the lug boss, and then carrying out pressing to form the double-layer hollow ceramic membrane.
Further, the preparation process of the first ceramic membrane comprises the following steps:
s01, dipping a template into the ceramic slurry, wherein the template comprises openings spaced from each other;
s02, introducing an anti-solvent into the ceramic slurry to cause phase inversion of the ceramic slurry and form a first ceramic film over the template; the first ceramic membrane comprises a ceramic membrane body formed on top thereof, and spaced apart channels extending from the first ceramic membrane surface to the ceramic membrane body, the channels being dendritic;
s03, removing the template after phase inversion.
Further, in step S01, the depth of the template immersed in the ceramic slurry is defined as H, and H > 0.03 mm.
The invention also aims to provide the double-layer hollow ceramic membrane prepared by the production process, which comprises two ceramic membranes, wherein a bulge part is fixedly arranged between the two ceramic membranes, so that a cavity is formed between the two ceramic membranes.
In conclusion, the invention has the following beneficial effects:
1. the ceramic slurry coated on the bulge forms a bonding layer after sintering, so that the bonding firmness of the two membranes and the strength and pressure-bearing capacity of the double-layer hollow ceramic membrane can be improved;
2. the bulge is directly formed by the ceramic slurry, so that on one hand, the bonding effect of two layers of films after sintering can be improved, the strength and the pressure-bearing capacity of the double-layer hollow ceramic film are improved, on the other hand, a die does not need to be customized, the production cost is reduced, the shape and the arrangement mode of the bulge can be flexibly selected and adjusted, and the production efficiency is improved;
3. the double-layer hollow ceramic membrane greatly reduces the pressure-bearing area of the membrane in the filtering process, so that the pressure-bearing capacity of the membrane is greatly improved.
Drawings
FIG. 1 is a schematic flow chart of a process for producing a double-layered hollow ceramic membrane according to example 1;
FIG. 2 is a schematic flow chart of a process for producing a double-layered hollow ceramic membrane according to example 2;
FIG. 3 is a schematic flow chart of a process for producing a double-layered hollow ceramic membrane according to example 3;
FIG. 4 is a schematic view of a flow chart for preparing the first ceramic film in example 4;
fig. 5 is a scanning electron micrograph image one of a cross section of a first ceramic film in example 4;
fig. 6 is a second scanning electron micrograph image of a cross-section of the first ceramic film of example 4.
In the figure: 1. a first ceramic film; 2. a second ceramic film; 3. a boss portion; 4. an adhesive layer; 51. a mold; 52. a template; 53. a ceramic slurry; 54. an anti-solvent; 55. an article of manufacture.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Example 1:
a double-layer hollow ceramic membrane production process, referring to fig. 1, comprising the following steps:
s100, preparing a first ceramic membrane 1 by a phase transfer method;
s200, preparing a second ceramic membrane 2 by a phase transfer method, wherein a convex part 3 is integrally formed on the surface of the second ceramic membrane 2;
s300, coating ceramic slurry on the end face of the bulge 3 of the second ceramic membrane 2;
s400, placing the first ceramic membrane 1 on the boss 3 of the second ceramic membrane 2, enabling the first ceramic membrane 1 to be in contact with the ceramic slurry on the end face of the boss 3, and then pressing the first ceramic membrane 1 and the second ceramic membrane 2 to form a double-layer hollow ceramic membrane;
and S500, sintering and molding the double-layer hollow ceramic membrane.
In this embodiment, microchannels are formed in both the first ceramic film 1 and the second ceramic film 2, and the preparation processes thereof are all the prior art and are not described herein again; the protrusions 3 integrally formed on the surface of the second ceramic film 2 are used to separate the first ceramic film 1 from the second ceramic film 2, so that a cavity is formed between the first ceramic film 1 and the second ceramic film 2, and the protrusions 3 may be in the form of strips, cylinders, dots, or the like, or may be in a combination of different shapes, which is not limited herein.
In this embodiment, ceramic slurry is prepared for both the first ceramic film 1 and the second ceramic film 2 before the ceramic films are formed by the phase transfer method; in this embodiment, the ceramic slurry includes ceramic powder (e.g., alumina, zirconia, titania, silicon carbide, etc.), an organic solvent (e.g., N-methylpyrrolidone, DMSO, etc.), a binder (e.g., polyethersulfone), and a dispersant (PVP, etc.), and the ceramic slurry is obtained by mixing the above raw materials in a ball mill.
In the embodiment, the first ceramic membrane 1 is a plate-type membrane, the main body part of the second ceramic membrane 2 is also a plate-type membrane, and after phase transfer molding, both the two membranes need to be put into an oven for drying at the temperature of 40-150 ℃.
In the embodiment, ceramic slurry is coated on the convex part 3, and the two films are bonded by the ceramic slurry; the ceramic slurry may be a ceramic slurry used in preparing the first ceramic film 1 or the second ceramic film 2, or may be separately prepared to control the viscosity thereof; the ceramic slurry coated on the convex part 3 forms the bonding layer 4 after sintering, thereby improving the bonding firmness of the two membranes and the strength and the bearing capacity of the double-layer hollow ceramic membrane.
In this embodiment, the ceramic slurry contains an organic solvent, and in order to avoid cracking of the double-layer hollow ceramic membrane during sintering, in step S400, the method further includes the steps of immersing the double-layer hollow ceramic membrane formed after pressing in water, and then taking out the double-layer hollow ceramic membrane, wherein the organic solvent is miscible with water, so that the organic solvent in the ceramic slurry can be removed; taking the double-layer hollow ceramic membrane out of water, and drying the double-layer hollow ceramic membrane in an oven at the temperature of between 30 and 200 ℃; the double-layer hollow ceramic membrane taken out from the water is dried, so that the influence on a kiln is avoided during sintering, and the membrane is prevented from cracking during sintering.
Example 2:
a double-layer hollow ceramic membrane production process, referring to fig. 2, comprising the following steps:
s100, preparing a first ceramic membrane 1 by a phase transfer method, wherein the first ceramic membrane 1 after phase transfer molding needs to be placed in an oven for drying;
s200, coating ceramic slurry on the surface of a first ceramic membrane 1 to form a convex part 3;
s300, placing the other first ceramic membrane 1 on the boss 3, then pressing to form a double-layer hollow ceramic membrane, taking out the double-layer hollow ceramic membrane after pressing after soaking in water, and taking out the double-layer hollow ceramic membrane and drying in an oven;
s400, sintering and forming the double-layer hollow ceramic membrane.
Unlike the production process in embodiment 1, in this embodiment, the projections 3 are formed by painting with ceramic slurry, that is, the projections 3 are formed later; the ceramic slurry used for forming the projections 3 in this embodiment needs a high viscosity so that the ceramic slurry can be maintained in a standing state after being applied to form the projections 3.
In the embodiment, the bulge 3 is directly formed by the ceramic slurry, so that the bonding effect of two layers of films after sintering can be improved, the strength and the pressure-bearing capacity of the double-layer hollow ceramic film are improved, a die does not need to be customized, the production cost is reduced, the shape and the arrangement mode of the bulge 3 can be flexibly selected and adjusted, and the production efficiency is improved.
Example 3:
a double-layer hollow ceramic membrane production process, referring to fig. 3, comprising the following steps:
s100, preparing a first ceramic membrane 1 by a phase transfer method, wherein the first ceramic membrane 1 after phase transfer molding needs to be placed in an oven for drying;
s200, coating viscose on the surface of a first ceramic membrane 1 to form a convex part 3;
s300, another first ceramic film 1 is placed on the convex portion 3, and then, a double-layered hollow ceramic film is formed by pressing.
Different from the production process in the embodiment 2, in the embodiment, the protrusions 3 are directly formed by using viscose glue, and then the two first ceramic membranes 1 are bonded by using the protrusions 3 to form a double-layer hollow ceramic membrane; in the embodiment, the adhesive needs to have certain viscosity and strength, and can be epoxy resin, polyurethane, hot melt adhesive or the like; in the embodiment, the protruding part 3 is formed by adopting viscose glue, so that the production process can be simplified, the production cost is reduced, and the production efficiency is improved.
Example 4:
referring to fig. 4, compared with examples 1 to 3, the present example is different in the preparation process of the first ceramic film 1; the first ceramic film 1 in examples 1 to 3 was prepared by the prior art, and the preparation process of the first ceramic film in this example includes the following steps:
s01, dipping the template 52 into the ceramic slurry 53, wherein the template 52 includes spaced apart openings;
s02, introducing an anti-solvent 54 into the ceramic slurry 53 to cause phase inversion of the ceramic slurry 53 and form the article 55 (i.e., the first ceramic film) over the template 52; the first ceramic membrane includes a ceramic membrane body formed on top thereof, and spaced apart channels extending from the first ceramic membrane surface to the ceramic membrane body, the channels being dendritic;
s03, removing template 52 after phase inversion.
Referring to fig. 4, specifically, the template 52 and the ceramic slurry 53 are both placed in the mold 51, and the template 52 is entirely immersed in the ceramic slurry 53 in this embodiment, and is placed at a deeper position in the ceramic slurry 53 than in the manufacturing method in the background art; then introducing an anti-solvent 54 into the ceramic slurry 53 to cause phase inversion of the ceramic slurry 53 and form a desired article 55 (i.e., a first ceramic film) above the template 52, and then separating the article 55 from the template 52, while the article formed below the template 52 is not desired; in the present embodiment, the depth of the template 52 immersed in the ceramic slurry 53 is defined as H, and then H is greater than 0.03mm and less than or equal to 3mm, but in other alternative embodiments, the depth H may be adjusted as needed, and the desired product 55 may be formed above the template 52, which is not limited herein.
Referring to fig. 5 and 6, in contrast to the related art manufacturing method, in the present embodiment, by changing the depth of the template, a different channel structure is formed in the article; specifically, in the background art, the second solvent passes through the template and enters the solution, so that a regular, uniform and single vertical microchannel is formed in the product; in the embodiment, the template is arranged at a deeper position in the ceramic slurry, the anti-solvent directly enters the ceramic slurry without penetrating through the template, the first ceramic membrane formed above the template after phase conversion also has spaced channels, but a single channel gradually takes the shape of dendritic bifurcation, after several times of bifurcation, the thickness of the spongy pore layer (namely, the first ceramic membrane main body) formed at the top of the first ceramic membrane is greatly reduced, the first ceramic membrane is integrally planar, the thickness is usually 1-10 μm, so that the mass and heat transfer can be greatly accelerated, the material transmission resistance is reduced, and the bifurcated channels are connected with each other, the specific surface area inside the first ceramic membrane is increased, and a good place is provided for chemical reaction.
Example 5:
a double-layer hollow ceramic membrane is prepared by any one of the production processes of the embodiments 1 to 4, and specifically comprises two layers of ceramic membranes, wherein a bulge part is fixedly arranged between the two layers of ceramic membranes, so that a cavity is formed between the two layers of ceramic membranes; in the double-layer hollow ceramic membrane in the embodiment, the pressure-bearing area of the membrane is greatly reduced in the filtering process, so that the pressure-bearing capacity of the membrane can be greatly improved.
Claims (9)
1. The production process of the double-layer hollow ceramic membrane is characterized by comprising the following steps of:
s100, preparing a first ceramic membrane by a phase transfer method;
s200, preparing a second ceramic membrane by a phase transfer method, wherein a convex part is integrally formed on the surface of the second ceramic membrane;
s300, coating ceramic slurry on the end face of the bulge of the second ceramic membrane;
s400, placing the first ceramic membrane on the boss of the second ceramic membrane to enable the first ceramic membrane to be in contact with the ceramic slurry on the end face of the boss, and then pressing the first ceramic membrane and the second ceramic membrane to form a double-layer hollow ceramic membrane;
and S500, sintering and molding the double-layer hollow ceramic membrane.
2. The process for producing a double-layered hollow ceramic membrane according to claim 1, wherein: in step S400, the method further includes immersing the double-layered hollow ceramic membrane formed after the pressing in water, and performing a drying process after taking out the ceramic membrane.
3. The production process of the double-layer hollow ceramic membrane is characterized by comprising the following steps of:
s100, preparing a first ceramic membrane by a phase transfer method;
s200, coating ceramic slurry on the surface of the first ceramic membrane to form a convex part;
s300, placing the other first ceramic membrane on the boss, and then pressing to form a double-layer hollow ceramic membrane;
s400, sintering and forming the double-layer hollow ceramic membrane.
4. The process for producing a double-layered hollow ceramic membrane according to claim 3, wherein: in step S300, the method further includes immersing the double-layered hollow ceramic membrane formed after the pressing in water, and performing a drying process after taking out the ceramic membrane.
5. The process for producing a double-layered hollow ceramic membrane according to claim 1 or 3, wherein: the ceramic slurry comprises ceramic powder, an organic solvent and a polymer.
6. The production process of the double-layer hollow ceramic membrane is characterized by comprising the following steps of:
s100, preparing a first ceramic membrane by a phase transfer method;
s200, coating viscose on the surface of the first ceramic film to form a convex part;
and S300, placing another first ceramic membrane on the lug boss, and then carrying out pressing to form the double-layer hollow ceramic membrane.
7. The process for producing a double-layered hollow ceramic membrane according to claim 1, 3 or 6, wherein: the preparation process of the first ceramic membrane comprises the following steps:
s01, dipping a template into the ceramic slurry, wherein the template comprises openings spaced from each other;
s02, introducing an anti-solvent into the ceramic slurry to cause phase inversion of the ceramic slurry and form a first ceramic film over the template; the first ceramic membrane comprises a ceramic membrane body formed on top thereof, and spaced apart channels extending from the first ceramic membrane surface to the ceramic membrane body, the channels being dendritic;
s03, removing the template after phase inversion.
8. The process for producing a double-layered hollow ceramic membrane according to claim 7, wherein: in step S01, the depth of the template immersed in the ceramic slurry is defined as H, and H > 0.03 mm.
9. A double-layered hollow ceramic membrane prepared by the production process according to claim 1, 3 or 6, wherein: the ceramic membrane comprises two ceramic membranes, wherein a lug boss is fixedly arranged between the two ceramic membranes, so that a cavity is formed between the two ceramic membranes.
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