CN114758892A - Preparation method of dielectric gel matrix - Google Patents
Preparation method of dielectric gel matrix Download PDFInfo
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- CN114758892A CN114758892A CN202210500838.1A CN202210500838A CN114758892A CN 114758892 A CN114758892 A CN 114758892A CN 202210500838 A CN202210500838 A CN 202210500838A CN 114758892 A CN114758892 A CN 114758892A
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- 239000011159 matrix material Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000004014 plasticizer Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000002070 nanowire Substances 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920000642 polymer Polymers 0.000 claims abstract description 6
- 239000010453 quartz Substances 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 238000004528 spin coating Methods 0.000 claims abstract description 6
- 238000007493 shaping process Methods 0.000 claims abstract description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 239000004800 polyvinyl chloride Substances 0.000 claims description 13
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 13
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 12
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000003989 dielectric material Substances 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- XTJFFFGAUHQWII-UHFFFAOYSA-N Dibutyl adipate Chemical group CCCCOC(=O)CCCCC(=O)OCCCC XTJFFFGAUHQWII-UHFFFAOYSA-N 0.000 claims description 7
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 claims description 6
- ZWYAVGUHWPLBGT-UHFFFAOYSA-N bis(6-methylheptyl) decanedioate Chemical compound CC(C)CCCCCOC(=O)CCCCCCCCC(=O)OCCCCCC(C)C ZWYAVGUHWPLBGT-UHFFFAOYSA-N 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 3
- 238000009998 heat setting Methods 0.000 claims description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 12
- 235000012239 silicon dioxide Nutrition 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 239000011521 glass Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 229920002595 Dielectric elastomer Polymers 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method of a dielectric gel matrix, which comprises the steps of fully mixing and stirring an organic dielectric main material A which has dielectric property and is easy to dissolve and a certain amount of solvent to obtain slurry; mixing and stirring a plasticizer and the slurry to obtain dielectric gel; mixing and stirring the nanowire slurry with high dielectric property and mechanical flexibility, standing until bubbles disappear to obtain a uniformly mixed gel state high dielectric organic composite material, coating the gel state composite material on a silicon wafer or a quartz wafer in a blade coating or spin coating mode, and finally standing at normal temperature for different times according to different thicknesses and solidifying and shaping to obtain the high dielectric polymer composite film. The invention can prepare dielectric films with different thicknesses. The film prepared by the dielectric gel has the characteristics of high dielectricity, high breakdown voltage value, low dielectric loss value, high flexibility, easiness in preparation, small environmental load and the like.
Description
Technical Field
The invention relates to the technical field of dielectric elastic drivers and capacitors, in particular to a preparation method of a dielectric gel matrix.
Background
If a uniform dielectric medium is placed between the two electrodes as the dielectric medium of the capacitor, the capacitance of the capacitor will be increased several times more than when the vacuum is a dielectric medium due to the polarization of the dielectric medium, which is the dielectric property of the object. Dielectric materials are widely used to control/store electrical charge and energy, and are of great strategic importance in modern electronic and power systems. The traditional dielectric material such as ferroelectric ceramic has high dielectric constant, but the processing temperature is high, the property is fragile, and the traditional dielectric material is difficult to process into a thin film. The polymer dielectric material has high dielectric breakdown strength, high flexibility and excellent processing performance, but the dielectric constant value of the polymer dielectric material is generally lower.
With the development of electronic devices, there is an increasing demand for applications of miniaturization, high frequency, intelligence, and flexibility of conductor devices, and thus a demand for highly elastic dielectric films has arisen. The high elastic dielectric elastomer has compression deformation effect under high field strength, and can be used for developing new generation of electric drive.
The current dielectric film preparation technology mainly breaks through the following steps:
first, as a composition for forming a dielectric thin film, for example, a ferroelectric material such as a barium titanate-based composition or a lead-based composite perovskite-based material has been used, and such ferroelectric ceramics have a high dielectric constant in many cases, but they have a high processing temperature and are brittle and difficult to process into a thin film.
Second, under the circumstances of increasing global environmental protection, development of a novel composition for forming a dielectric thin film with a small load on the environment is desired.
Third, in the case of producing a dielectric thin film-forming composition containing Ba, Pb, etc., special facilities for treating waste liquid generated in the production process are required for environmental protection, which greatly increases the production cost, and therefore, it is also necessary to develop a dielectric thin film-forming composition not containing such a substance requiring special treatment.
Disclosure of Invention
The invention provides a preparation method of a dielectric gel matrix, which solves the technical problems in the prior art.
The scheme for solving the technical problems is as follows: a preparation method of a dielectric gel matrix comprises mixing easily soluble organic dielectric main material A with dielectric property with a certain amount of solvent, stirring to obtain slurry; mixing and stirring a plasticizer and the slurry to obtain dielectric gel; mixing and stirring the nanowire slurry with high dielectric property and mechanical flexibility, standing until bubbles disappear to obtain a uniformly mixed gel state high dielectric organic composite material, coating the gel state composite material on a silicon wafer or a quartz wafer in a blade coating or spin coating mode, and finally standing at normal temperature for different times according to different thicknesses and solidifying and shaping to obtain the high dielectric polymer composite film.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the organic dielectric main material is polyvinyl chloride, and the molecular weight is preferably 5 to 10 ten thousand.
Furthermore, the solvent of the organic dielectric material is tetrahydrofuran, cyclohexanone, ketone and dimethylformamide.
Further, the plasticizer is di-n-butyl adipate (DBA), dibutyl sebacate (DBS), dibutyl phthalate (DBP), dioctyl adipate (DOA) and diisooctyl sebacate (DOS).
Further, the high dielectric nanowire slurry is silicon dioxide, hexagonal boron nitride and silicon dioxide.
Further, the organic dielectric host material polyvinyl chloride is present in an amount of about 5% to about 10% by weight.
Further, the diluent is present in an amount of about 40% to about 60% by weight.
Further, the plasticizer is present in an amount of about 20% to about 70% by weight.
Further, the heat-setting temperature was room temperature.
The beneficial effects of the invention are: the invention provides a preparation method of a dielectric gel matrix, which has the following advantages:
the embodiment of the invention discloses a preparation method of a transparent dielectric gel matrix, which is characterized by comprising the following steps: mixing and stirring the organic material and a quantitative solvent to obtain a PVC thermoplastic polymer matrix gel composition, then adding the conductive material, and uniformly stirring to obtain the high-dielectric composite gel material. And then putting part of the gel on a smooth surface of a quartz plate or a silicon wafer, and uniformly coating the gel in a blade coating or spin coating manner to prepare dielectric films with different thicknesses.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 shows the viscosity and particle size of the slurry, and the dielectric constant, Young's modulus and tensile strength of the prepared film, corresponding to the variation of the distribution ratio of different components (5 groups) in the examples.
Detailed Description
The principles and features of the present invention are described below in conjunction with the accompanying fig. 1, which is provided by way of example only to illustrate the present invention and not to limit the scope of the present invention. The invention is described in more detail in the following paragraphs by way of example with reference to the accompanying drawings. Advantages and features of the present invention will become apparent from the following description and from the claims. It is to be noted that the drawings are in a very simplified form and are not to precise scale, which is provided for the purpose of facilitating and clearly illustrating embodiments of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
As shown in figure 1, the invention provides a preparation method of a dielectric gel matrix, which comprises the steps of fully mixing and stirring an easily soluble organic dielectric main material A with dielectric property and a certain amount of solvent to obtain slurry; mixing and stirring a plasticizer and the slurry to obtain dielectric gel; mixing and stirring the nanowire slurry with high dielectric property and mechanical flexibility, standing until bubbles disappear to obtain a uniformly mixed gel state high dielectric organic composite material, coating the gel state composite material on a silicon wafer or a quartz wafer in a blade coating or spin coating mode, and finally standing at normal temperature for different times according to different thicknesses and solidifying and shaping to obtain the high dielectric polymer composite film.
Preferably, the organic dielectric main material is polyvinyl chloride, and the molecular weight is preferably 5 to 10 ten thousand.
Preferably, the solvent of the organic dielectric material is tetrahydrofuran, cyclohexanone, ketone or dimethylformamide.
Preferably, the plasticizer is di-n-butyl adipate (DBA), dibutyl sebacate (DBS), dibutyl phthalate (DBP), dioctyl adipate (DOA), and diisooctyl sebacate (DOS).
Preferably, the high dielectric nanowire slurry is silicon dioxide, hexagonal boron nitride or silicon dioxide.
Preferably, the organic dielectric host material is polyvinyl chloride present in an amount of about 5% to about 10% by weight.
Preferably, the diluent is present in an amount of about 40% to about 60% by weight.
Preferably, the plasticizer is present in an amount of about 20% to about 70% by weight.
Preferably, the heat-setting temperature is room temperature.
The specific embodiment of the invention is as follows:
the first embodiment is as follows:
1. fixing the beaker on a stirrer, adjusting the position, and pouring 50mL of tetrahydrofuran;
2. slowly pouring 10g of polyvinyl chloride into the stirrer at a speed of 100r/h, and continuously stirring;
3. after stirring uniformly and transparently, pouring 30g of plasticizer DBS, and continuously stirring;
4. then 50mg of silicon dioxide with the content of 95 percent is poured, and the stirring is continuously and uniformly carried out, and then the operation is finished;
5. 6mL of the prepared PVCgel solution is poured into a glass culture dish with the diameter of 10 cm;
6. standing for 24h to solidify into film.
The second embodiment:
1. fixing a beaker on a stirrer, adjusting the position, and pouring 50mL of tetrahydrofuran;
2. slowly pouring 10g of polyvinyl chloride into the stirrer at a speed of 100r/h, and continuously stirring;
3. after stirring uniformly and transparently, pouring 40g of plasticizer DBA, and continuously stirring;
4. then 50mg of silicon dioxide with the content of 95 percent is poured, and the stirring is continuously and uniformly carried out, and then the operation is finished;
5. 6mL of the prepared PVCgel solution is poured into a glass culture dish with the diameter of 10 cm;
6. standing for 24h to solidify into a film.
Example three:
1. fixing the beaker on a stirrer, adjusting the position, and pouring 50mL of tetrahydrofuran;
2. slowly pouring 10g of polyvinyl chloride into the stirrer at a speed of 100r/h, and continuously stirring;
3. after stirring uniformly and transparently, pouring 50g of plasticizer DBS, and continuously stirring;
4. then 50mg of silicon dioxide with the content of 95 percent is poured, and the stirring is continuously and uniformly carried out, and then the operation is finished;
5. 6mL of the prepared PVCgel solution is poured into a glass culture dish with the diameter of 10 cm;
6. standing for 24h to solidify into a film.
Example four:
1. fixing the beaker on a stirrer, adjusting the position, and pouring 50mL of tetrahydrofuran;
2. slowly pouring 10g of polyvinyl chloride into the stirrer at a speed of 100r/h, and continuously stirring;
3. After stirring evenly and transparently, pouring 40g of plasticizer DBS, and continuously stirring;
4. then, 50mg of micron-sized hexagonal boron nitride is poured into the mixture, and the mixture is continuously stirred uniformly;
5. 6mL of the prepared PVCgel solution is poured into a glass culture dish with the diameter of 10 cm;
6. standing for 24h to solidify into film.
Example five:
1. fixing the beaker on a stirrer, adjusting the position, and pouring 50mL of tetrahydrofuran;
2. slowly pouring 10g of polyvinyl chloride into the stirrer at a speed of 100r/h, and continuously stirring;
3. after stirring uniformly and transparently, pouring 40g of plasticizer DBS, and continuously stirring;
4. then 100mg of micron-sized hexagonal boron nitride is poured into the mixture, and the stirring is continuously and uniformly carried out, so that the operation is finished;
5. 6mL of the prepared PVCgel solution is poured into a glass culture dish with the diameter of 10 cm;
6. standing for 24h to solidify into a film.
The embodiment of the invention discloses a preparation method of a transparent dielectric gel matrix, which is characterized by comprising the following steps: mixing and stirring the organic material and a quantitative solvent to obtain a PVC thermoplastic polymer matrix gel composition, then adding the conductive material, and uniformly stirring to obtain the high-dielectric composite gel material. And then putting part of the gel on a smooth surface of a quartz plate or a silicon wafer, and uniformly coating the gel in a blade coating or spin coating manner to prepare dielectric films with different thicknesses.
The foregoing is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting the invention in any way; one of ordinary skill in the art will readily appreciate from the disclosure that the present invention can be practiced as illustrated in the accompanying drawings and described above; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the scope of the invention; meanwhile, any equivalent changes, modifications and evolutions made to the above embodiments according to the substantial technology of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (9)
1. A preparation method of a dielectric gel matrix is characterized by comprising the steps of fully mixing and stirring an organic dielectric main material A which has dielectric property and is easy to dissolve with a certain amount of solvent to obtain slurry; mixing and stirring a plasticizer and the slurry to obtain dielectric gel; mixing and stirring the nanowire slurry with high dielectric property and mechanical flexibility, standing until bubbles disappear to obtain a uniformly mixed gel state high dielectric organic composite material, coating the gel state composite material on a silicon wafer or a quartz wafer in a blade coating or spin coating mode, and finally standing at normal temperature for different times according to different thicknesses and solidifying and shaping to obtain the high dielectric polymer composite film.
2. The method of claim 1, wherein the organic dielectric host material is polyvinyl chloride having a molecular weight of preferably 5 to 10 ten thousand.
3. The method of claim 2, wherein the solvent of the organic dielectric material is tetrahydrofuran, cyclohexanone, methyl ketone, or dimethylformamide.
4. The method of claim 1, wherein the plasticizer is di-n-butyl adipate (DBA), dibutyl sebacate (DBS), dibutyl phthalate (DBP), dioctyl adipate (DOA), or diisooctyl sebacate (DOS).
5. The method of claim 1, wherein the high dielectric nanowire slurry is silica, hexagonal boron nitride, or silica.
6. The method of claim 1, wherein the organic dielectric host material comprises polyvinyl chloride in an amount of about 5% to about 10% by weight.
7. The method of claim 1, wherein the diluent is present in an amount of about 40% to about 60% by weight.
8. The method of claim 4, wherein the plasticizer is present in an amount of about 20% to about 70% by weight.
9. The method of claim 1, wherein the heat-setting temperature is room temperature.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107099117A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of fibre-reinforced aerogel-polymer composites and preparation method thereof |
CN111113380A (en) * | 2019-12-14 | 2020-05-08 | 西安交通大学 | PVC gel driven flexible mechanical gripper and preparation method thereof |
CN112654431A (en) * | 2018-04-02 | 2021-04-13 | 生物动力学公司 | Dielectric material |
CN113717489A (en) * | 2021-08-17 | 2021-11-30 | 宁波聚泰新材料科技有限公司 | Halogen-free flame-retardant thermoplastic elastomer |
JP2022014502A (en) * | 2020-07-07 | 2022-01-20 | AssistMotion株式会社 | Polyvinyl chloride compact, actuator and method for producing polyvinyl chloride compact |
WO2022046405A1 (en) * | 2020-08-28 | 2022-03-03 | Specialty Electronic Materials Belgium, Srl | Electrically conductive compositions |
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- 2022-05-09 CN CN202210500838.1A patent/CN114758892A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107099117A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of fibre-reinforced aerogel-polymer composites and preparation method thereof |
CN112654431A (en) * | 2018-04-02 | 2021-04-13 | 生物动力学公司 | Dielectric material |
CN111113380A (en) * | 2019-12-14 | 2020-05-08 | 西安交通大学 | PVC gel driven flexible mechanical gripper and preparation method thereof |
JP2022014502A (en) * | 2020-07-07 | 2022-01-20 | AssistMotion株式会社 | Polyvinyl chloride compact, actuator and method for producing polyvinyl chloride compact |
WO2022046405A1 (en) * | 2020-08-28 | 2022-03-03 | Specialty Electronic Materials Belgium, Srl | Electrically conductive compositions |
CN113717489A (en) * | 2021-08-17 | 2021-11-30 | 宁波聚泰新材料科技有限公司 | Halogen-free flame-retardant thermoplastic elastomer |
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