CN111875907A - PTFE diaphragm doped with glass beads and preparation method thereof - Google Patents
PTFE diaphragm doped with glass beads and preparation method thereof Download PDFInfo
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- CN111875907A CN111875907A CN202010736670.5A CN202010736670A CN111875907A CN 111875907 A CN111875907 A CN 111875907A CN 202010736670 A CN202010736670 A CN 202010736670A CN 111875907 A CN111875907 A CN 111875907A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
- C08K7/20—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
Abstract
The invention discloses a PTFE diaphragm doped with glass beads, which is prepared by uniformly mixing and stirring 60-80 parts by mass of PTFE granules, 5-10 parts by mass of PTFE micro powder and 15-30 parts by mass of glass beads, and then carrying out compression molding, wherein the particle size of the PTFE granules is 100-500 mu m, the particle size of the PTFE micro powder is 0.5-15 mu m, and the particle size of the glass beads is 10-30 mu m. According to the invention, the glass beads are used as the filler, the glass beads have good fluidity and belong to light materials, and on the basis of ensuring the compactness of the diaphragm, the high-density diaphragm not only retains good bending resistance and excellent fatigue resistance, but also obviously reduces the density.
Description
Technical Field
The invention belongs to the technical field of diaphragm sheets, and particularly relates to a PTFE diaphragm sheet doped with glass beads.
Background
The diaphragm is widely applied to diaphragm valves of various specifications at home and abroad, and the diaphragm separates the inner cavity of the lower valve body of the diaphragm valve from the inner cavity of the upper valve cover, so that parts such as a valve rod, the valve cover and the like positioned above the diaphragm are not corroded by media, a packing and sealing structure is omitted, and the leakage of the media is avoided. The method is applied to fermentation tanks, preparation tanks, filling machines, sterile filters, water production equipment, PW and WFI conveying and distribution, sterile fluid conveying, CIP, SIP and the like. The working principle of the pneumatic diaphragm valve is widely applied to the industries of biological medicine, food and beverage, fluid equipment, cosmetics and the like. Diaphragm valves are suitable for switching and throttling purposes. The diaphragm comprises three series of composite diaphragm, rubber diaphragm and PTFE diaphragm. The PTFE diaphragm is widely used due to the excellent characteristics of the PTFE diaphragm in the aspects of heat resistance, chemical resistance and the like, but the creep resistance and bending resistance of the PTFE diaphragm influence the service life of the PTFE diaphragm, and how to further prolong the service life of the PTFE diaphragm is a key technical problem for improving the product quality and market competitiveness of the PTFE diaphragm.
The invention patent CN105972245B previously filed by the applicant discloses a durable PTFE diaphragm sheet, which is obtained by uniformly mixing and stirring 70-90 parts by mass of PTFE granules and 10-30 parts by mass of PTFE micro powder, and then carrying out compression molding, wherein the particle size of the PTFE granules is 100-500 mu m, and the particle size of the PTFE micro powder is 0.5-15 mu m. The performance of the PTFE membrane sheet is improved by doping PTFE micropowder into the PTFE membrane sheet raw material.
Disclosure of Invention
In order to improve the performance of the PTFE diaphragm, the invention provides the PTFE diaphragm doped with the glass beads, and the glass beads are added into the raw material formula of the PTFE diaphragm, so that the flowability of the raw materials in the forming process is improved, and the weight of the PTFE diaphragm can be reduced.
In order to achieve the purpose, the invention adopts the following technical scheme: the PTFE diaphragm sheet doped with the glass beads is obtained by uniformly mixing and stirring 60-80 parts by mass of PTFE granules, 5-10 parts by mass of PTFE micro powder and 15-30 parts by mass of glass beads, and then carrying out compression molding, wherein the particle size of the PTFE granules is 100-500 mu m, the particle size of the PTFE micro powder is 0.5-15 mu m, and the particle size of the glass beads is 10-50 mu m.
Further preferably, the glass beads are plated with soft magnetic particle films, so that the PTFE diaphragm sheet can be sintered at a lower temperature by microwaves.
A preparation method of a PTFE diaphragm doped with glass beads comprises the following steps:
s1, weighing 60-80 parts by mass of PTFE granules, 5-10 parts by mass of PTFE micro powder and 15-30 parts by mass of glass beads, and uniformly mixing by using a stirrer or a ball mill;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, so that solid-phase reaction occurs inside the blank, and sintering to form a compact structure, thereby obtaining a PTFE diaphragm finished product.
Further preferably, the glass beads adopted in step S1 are pre-chemically plated with iron nanoparticles, and in step S3, the PTFE diaphragm blank is placed in a microwave sintering furnace, and the PTFE diaphragm is sintered by microwave sintering to form a dense structure.
The invention has the beneficial effects that: by adopting the glass beads as the filler, the glass beads have good fluidity and belong to light materials, so that on the basis of ensuring the compactness of the diaphragm sheet, the diaphragm sheet not only keeps good bending resistance and excellent fatigue resistance, but also obviously reduces the density, and the iron nanoparticles are plated on the surfaces of the glass beads, so that the diaphragm sheet can be subjected to microwave sintering, has higher dimensional precision and lower sintering temperature.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1:
s1, the particle size of the PTFE granules is 100 microns, the particle size of the PTFE micro powder is 0.5 microns, and the particle size of the glass beads is 10 microns; weighing 80 parts by mass of PTFE granules, 5 parts by mass of PTFE micro powder and 15 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, preserving heat for 60min to enable the blank to have solid-phase reaction inside, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 2:
s1, the particle size of the PTFE granules is 200 microns, the particle size of the PTFE micro powder is 5 microns, and the particle size of the glass beads is 15 microns; weighing 80 parts by mass of PTFE granules, 10 parts by mass of PTFE micro powder and 10 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, preserving heat for 60min to enable the blank to have solid-phase reaction inside, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 3:
s1, the particle size of the PTFE granules is 300 mu m, the particle size of the PTFE micro powder is 10 mu m, and the particle size of the glass beads is 20 mu m; weighing 75 parts by mass of PTFE granules, 5 parts by mass of PTFE micro powder and 20 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, keeping the temperature for 90min to enable the inside of the blank to generate solid-phase reaction, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 4:
s1, the particle size of the PTFE granules is 400 microns, the particle size of the PTFE micro powder is 10 microns, and the particle size of the glass beads is 20 microns; weighing 75 parts by mass of PTFE granules, 5 parts by mass of PTFE micro powder and 20 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, keeping the temperature for 90min to enable the inside of the blank to generate solid-phase reaction, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 5:
s1, the particle size of the PTFE granules is 500 mu m, the particle size of the PTFE micro powder is 15 mu m, and the particle size of the glass beads is 50 mu m; weighing 70 parts by mass of PTFE granules, 10 parts by mass of PTFE micro powder and 20 parts by mass of glass beads, and uniformly mixing by using a ball mill;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, preserving heat for 120min to enable the blank to have solid-phase reaction inside, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 6:
s1, the particle size of the PTFE granules is 200 microns, the particle size of the PTFE micro powder is 10 microns, and the particle size of the glass beads is 30 microns; weighing 70 parts by mass of PTFE granules, 10 parts by mass of PTFE micro powder and 20 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, keeping the temperature for 90min to enable the inside of the blank to generate solid-phase reaction, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 7:
s1, the particle size of the PTFE granules is 200 microns, the particle size of the PTFE micro powder is 10 microns, and the particle size of the glass beads is 30 microns; weighing 60 parts by mass of PTFE granules, 10 parts by mass of PTFE micro powder and 30 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, keeping the temperature for 90min to enable the inside of the blank to generate solid-phase reaction, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 8:
s1, the particle size of the PTFE granules is 200 microns, the particle size of the PTFE micro powder is 10 microns, and the particle size of the glass beads is 30 microns; weighing 80 parts by mass of PTFE granules, 5 parts by mass of PTFE micro powder and 15 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 370 ℃ during sintering, keeping the temperature for 90min to enable the inside of the blank to generate solid-phase reaction, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 9:
s1, the particle size of the PTFE granules is 200 microns, the particle size of the PTFE micro powder is 10 microns, the particle size of the glass beads is 30 microns, and the glass beads are glass beads chemically plated with iron nanoparticles in advance; weighing 70 parts by mass of PTFE granules, 10 parts by mass of PTFE micro powder and 20 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a microwave sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 330 ℃ during sintering, keeping the temperature for 90min to enable the blank to have solid-phase reaction inside, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Example 10:
s1, the particle size of the PTFE granules is 200 microns, the particle size of the PTFE micro powder is 10 microns, the particle size of the glass beads is 30 microns, and the glass beads are glass beads chemically plated with iron nanoparticles in advance; weighing 70 parts by mass of PTFE granules, 10 parts by mass of PTFE micro powder and 20 parts by mass of glass beads, and uniformly mixing by using a stirrer;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank, and doping absolute ethyl alcohol and oleic acid as auxiliaries to better combine PTFE granules, PTFE micro powder and glass beads together;
and S3, transferring the PTFE diaphragm blank to a microwave sintering furnace for sintering, volatilizing ethanol and oleic acid in the heating process, slowly heating to 330 ℃ during sintering, keeping the temperature for 90min to enable the blank to have solid-phase reaction inside, and sintering to form a compact structure to obtain the finished PTFE diaphragm.
Comparative example 1
Carrying out compression molding on PTFE granules to obtain a PTFE diaphragm blank, wherein the particle size of the PTFE granules is 200 mu m; and then transferring the PTFE diaphragm blank to a curing furnace, heating to 370 ℃, preserving heat for 15min, and curing to obtain a PTFE diaphragm finished product.
Comparative example 2
Uniformly mixing 85 parts by mass of PTFE granules and 15 parts by mass of PTFE micro powder, and then carrying out compression molding to obtain a PTFE diaphragm blank, wherein the particle size of the PTFE granules is 200 mu m, and the particle size of the PTFE micro powder is 10 mu m; and then transferring the PTFE diaphragm blank to a curing furnace, heating to 370 ℃, preserving heat for 15min, and curing to obtain a PTFE diaphragm finished product.
The performance test of the PTFE diaphragm product is detailed in table 1, and as can be seen from table 1, the density can be obviously reduced on the basis of maintaining the fatigue resistance of good bending resistance by adding the glass microspheres. From examples 9 and 10, it can be seen that the iron nanoparticles plated on the surfaces of the glass beads can be sintered by microwave, and the size precision is higher and the sintering temperature is lower.
TABLE 1 PTFE DIAPHRAGM PERFORMANCE TEST METER
| Serial number | Sintering temperature/. degree.C | Specific gravity/(g/m)3) | Dimensional qualification rate | Tensile strength/MPa | Elongation at break/% | Number of times of bending |
| Comparative example 1 | 370 | 2.155 | 98.3 | 28.9 | 340 | 463159 |
| Comparative example 2 | 370 | 2.130 | 99.1 | 35.4 | 370 | 1624531 |
| Example 1 | 370 | 1.916 | 99.2 | 34.9 | 370 | 1696576 |
| Example 2 | 370 | 1.967 | 99.6 | 33.6 | 360 | 1593432 |
| Example 3 | 370 | 1.823 | 99.4 | 33.0 | 360 | 1573698 |
| Example 4 | 370 | 1.842 | 99.6 | 34.3 | 350 | 1567983 |
| Example 5 | 370 | 1.804 | 99.6 | 33.6 | 360 | 1597846 |
| Example 6 | 370 | 1.822 | 99.3 | 34.2 | 380 | 1654324 |
| Example 7 | 370 | 1.659 | 98.9 | 32.2 | 350 | 1438583 |
| Example 8 | 370 | 1.891 | 99.0 | 33.5 | 360 | 1574667 |
| Example 9 | 330 | 1.856 | 100.0 | 34.7 | 370 | 1587659 |
| Example 10 | 330 | 1.863 | 100.0 | 34.3 | 360 | 1547645 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A PTFE diaphragm sheet doped with glass beads is characterized in that: the PTFE material is prepared by uniformly mixing and stirring 60-80 parts by mass of PTFE granules, 5-10 parts by mass of PTFE micro powder and 15-30 parts by mass of glass beads, and then performing compression molding, wherein the particle size of the PTFE granules is 100-500 mu m, the particle size of the PTFE micro powder is 0.5-15 mu m, and the particle size of the glass beads is 10-50 mu m.
2. The glass bead-doped PTFE membrane sheet of claim 1, wherein: the glass beads are plated with soft magnetic particle films.
3. The method of making a glass bead-doped PTFE membrane sheet of claim 1, comprising the steps of:
s1, weighing 60-80 parts by mass of PTFE granules, 5-10 parts by mass of PTFE micro powder and 15-30 parts by mass of glass beads, and uniformly mixing by using a stirrer or a ball mill;
s2, carrying out compression molding on the uniformly mixed powder by using a molding press to obtain a PTFE diaphragm blank;
and S3, transferring the PTFE diaphragm blank to a sintering furnace for sintering, so that solid-phase reaction occurs inside the blank, and sintering to form a compact structure, thereby obtaining a PTFE diaphragm finished product.
4. The method of claim 3, wherein the method comprises the following steps: and (3) chemically plating the glass beads adopted in the step S1 with iron nanoparticles in advance, putting the PTFE diaphragm blank in a microwave sintering furnace in the step S3, and sintering the PTFE diaphragm to form a compact structure by adopting a microwave sintering mode.
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| CN202010736670.5A CN111875907B (en) | 2020-07-28 | 2020-07-28 | PTFE diaphragm doped with glass beads and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5922453A (en) * | 1997-02-06 | 1999-07-13 | Rogers Corporation | Ceramic-filled fluoropolymer composite containing polymeric powder for high frequency circuit substrates |
| CN102381844A (en) * | 2011-07-26 | 2012-03-21 | 西安工程大学 | Method for modifying hollow glass microspheres by chemical precipitation process |
| CN105972245A (en) * | 2016-06-06 | 2016-09-28 | 于都海瑞密封防腐科技有限公司 | Durable PTFE diaphragm piece |
-
2020
- 2020-07-28 CN CN202010736670.5A patent/CN111875907B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5922453A (en) * | 1997-02-06 | 1999-07-13 | Rogers Corporation | Ceramic-filled fluoropolymer composite containing polymeric powder for high frequency circuit substrates |
| CN102381844A (en) * | 2011-07-26 | 2012-03-21 | 西安工程大学 | Method for modifying hollow glass microspheres by chemical precipitation process |
| CN105972245A (en) * | 2016-06-06 | 2016-09-28 | 于都海瑞密封防腐科技有限公司 | Durable PTFE diaphragm piece |
Non-Patent Citations (2)
| Title |
|---|
| 张明强等: ""空心玻璃微珠/聚四氟乙烯复合材料的性能研究"", 《塑料工业》 * |
| 曹茂盛等: "《材料合成与制备方法》", 31 July 2018, 哈尔滨工业大学出版社 * |
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