KR101859638B1 - Method for manufaturing thermopalsticity carbon fiber composite material - Google Patents
Method for manufaturing thermopalsticity carbon fiber composite material Download PDFInfo
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- KR101859638B1 KR101859638B1 KR1020160174709A KR20160174709A KR101859638B1 KR 101859638 B1 KR101859638 B1 KR 101859638B1 KR 1020160174709 A KR1020160174709 A KR 1020160174709A KR 20160174709 A KR20160174709 A KR 20160174709A KR 101859638 B1 KR101859638 B1 KR 101859638B1
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- South Korea
- Prior art keywords
- carbon fiber
- bundle
- hybrid
- alumina coating
- alumina
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/18—Separating or spreading
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
- D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B19/00—Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00
- D06B19/0005—Fixing of chemicals, e.g. dyestuffs, on textile materials
- D06B19/0011—Fixing of chemicals, e.g. dyestuffs, on textile materials by heated air
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic System; Aluminates
Abstract
A method for producing a thermoplastic carbon fiber composite material, and a method for producing a hybrid alumina coating liquid. According to the present invention, there is provided a carbon fiber bundle including a carbon fiber bundle supplying step of supplying a carbon fiber bundle composed of a plurality of filaments in one direction, a widening slim step of widening and slimming the carbon fiber bundle with a bundle of carbon fiber spreads by a wide- A spray coating step of spraying and coating a hybrid alumina coating liquid on at least one of the upper surface and the lower surface of the bundle, and a hybrid alumina coating layer forming step of drying the hybrid alumina coating liquid coated on the carbon fiber spread bundle to form a hybrid alumina coating layer .
Description
The present invention relates to a method for producing a thermoplastic carbon fiber composite material.
In general, continuous carbon fiber reinforced thermoplastics have reinforced fibers such as glass fiber or carbon fiber embedded in a continuous phase in a plastic having a relatively low mechanical strength. Fiber-reinforced plastics are manufactured from short fiber-reinforced thermoplastics or long fiber-reinforced thermoplastics (LFT), glass mat-reinforced thermoplastics (GMT) It has excellent mechanical strength, stiffness and impact performance compared to long-fiber reinforced plastics of the same 5 ~ 50mm length.
Continuous fiber reinforced plastics are also highly flexible and can be woven in either unidirectional or both directions through which woven continuous fiber reinforced plastic structures can be applied to products that require a variety of mechanical performances.
The continuous fiber-reinforced plastic is usually produced by a pultrusion method, a commingle method, a hot pressing method, or the like.
The pultrusion method is a method in which a continuous bundle of continuous fibers is passed through a liquid or molten resin tank or a die to impregnate a continuous resin bundle with a plastic resin so that the degree of impregnation can be increased by optimizing the process conditions However, it is difficult to control the content of reinforcement fibers and plastic resin such as continuous fibers, and flexibility is low, which makes it difficult to weave.
Further, according to the conventional heating method, there is a problem that the film is melted from the surface and the surface easily bends.
Accordingly, a method for manufacturing a thermoplastic carbon fiber composite material that can overcome the above problems is desperately required.
The present invention relates to a method of manufacturing a high-density thermoplastic polymer pellet by melt-impregnation comprising repeatedly layering, melting and impregnating a film and a wider carbon fiber bundle, The present invention relates to a method for producing a thermoplastic carbon fiber composite material which improves the impregnation property of a resin with respect to a carbon fiber bundle of a carbon fiber bundle of a carbon fiber bundle of 60K, To provide a method for producing an alumina coating liquid.
Also disclosed is a method for producing a thermoplastic carbon fiber composite material capable of increasing the interfacial strength with a matrix resin of a carbon fiber by forming an alumina coating layer on the surface of a carbon fiber by hybrid alumina coating, and a method for producing a hybrid alumina coating liquid I want to.
According to an embodiment of the present invention, there is provided a carbon fiber bundle supply method for supplying a carbon fiber bundle comprising a plurality of filaments in one direction,
A widening slim step of widening and slimming the carbon fiber bundle into a bundle of carbon fiber spun by a widening unit,
A spray coating step of spraying and coating a hybrid alumina coating liquid on at least one of the upper surface and the lower surface of the carbon fiber spread bundle,
And forming a hybrid alumina coating layer by drying the hybrid alumina coating liquid coated on the carbon fiber spread bundle.
A carbon fiber tape forming step of arranging and bonding a thermoplastic film to at least one of the upper surface and the lower surface of the carbon fiber spread bundle on which the hybrid alumina coating layer is formed to form an alumina coated carbon fiber tape,
And a carbon fiber tape bonding step of winding the carbon fiber tape on a reel.
Wherein the width of the carbon fiber bundle is wide at least two times to at most 20 times,
The thickness of the carbon fiber bundle may be slim from a minimum of 1/2 to a maximum of 1/20.
The carbon fiber bundle may be widened and slimmed by colliding with the air current generated by the vacuum and the hot air in the wider portion.
The drying of the hybrid alumina coating liquid may be performed by hot air generated from hot air, halogen lamps or radiant heat generated from an infrared lamp.
And a step of preparing a coating liquid spray-coated on the carbon fiber spread bundle before performing the spray coating step.
The process for producing the coating liquid includes a hydrolysis step of reacting aluminum alkoxide with water and hydrolyzing the aluminum alkoxide with aluminum hydroxide,
A peptization step of adding nitric acid (HNO 3 ) to the aluminum hydroxide and maintaining the pH at 3.0 to 4.0 to decompose the aluminum hydroxide into an AlOOH sol and disperse it on the water to float,
An AlOOH sol stabilization step in which the AlOOH sol is stabilized by heating,
A ball-milling step in which alpha-alumina balls are charged into the AlOOH sol to perform ball milling in order to add alpha alumina seed particles to the AlOOH sol, and
And a step of preparing a hybrid alumina coating liquid in which alpha alumina seed particles broken by mutual friction of alpha alumina seed particles in the ball-milling step are dispersed in AlOOH sol to produce a stable hybrid alumina coating solution.
The ball-milling in the ball-milling step may be performed for 8 to 20 hours for uniform dispersion of the alpha-alumina seed particles.
The size of the alpha alumina seed particles may be larger than 0.05 mu m and smaller than 100 mu m.
According to an embodiment of the present invention, the hybrid alumina coating treatment produces a strongly adsorbed alumina oxide layer on the carbon fiber surface, without chemical modification of the carbon fiber surface, and this hybrid alumina coated surface treatment is characterized by a carbon fiber thermoplastic composite The interfacial strength of the substrate can be improved.
In addition, hybrid alumina coating treatment is a relatively simple manufacturing method in which a hybrid alumina coating solution is sprayed onto a wider carbon fiber bundle, which is then widened and slimmed, and then dried. As compared with conventional surface treatment methods, cost reduction and productivity can be expected.
Since the method can be applied to a high-speed continuous process, it is easy to apply to a mass production process for mass production. In addition, a continuous carbon fiber reinforced semi-prepreg or a fully impregnated prepreg (continuous carbon fiber-containing tape) can be applied to a wide range of carbon fiber bundles (CF spread tow) coated with a hybrid alumina spray coating in one direction A separate resin impregnation process is not required after the uni-directional arrangement or the bi-axial (0 degrees, 90 degrees) arrangement, and the thermoplastic prepreg obtained by the present invention is unidirectionally aligned or woven, It is possible to obtain various types of continuous carbon fiber reinforced thermoplastic type carbon fiber reinforced plate having high strength and light weight by pressing.
Further, according to the present invention, it is possible to obtain a continuous carbon fiber-reinforced thermoplastic prepreg (continuous carbon fiber-containing tape) that is easily woven and has excellent uniformity.
In addition, by maximizing the impregnation rate of the thermoplastic resin having a relatively high viscosity in comparison with the thermosetting resin in manufacturing, minimizing the void in the molded body and maximizing the volume fraction of the carbon fiber, a high strength thermoplastic carbon fiber composite material CFRTP, Carbon Fiber Reinforced Thermo-Plastics) components.
1 is a schematic diagram of a method of manufacturing a thermoplastic carbon fiber composite material according to an embodiment of the present invention.
2 is a view for explaining the progress of each step of the method for producing a thermoplastic carbon fiber composite material according to an embodiment of the present invention.
3 is a photograph showing a TEM (transmission electron microscope) analysis result of the hybrid alumina coating layer produced according to the method for producing a thermoplastic carbon fiber composite material according to an embodiment of the present invention.
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings, so that those skilled in the art can easily carry out the present invention. As will be readily understood by those skilled in the art, the following embodiments may be modified in various ways within the scope and spirit of the present invention. Wherever possible, the same or similar parts are denoted using the same reference numerals in the drawings.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention. The singular forms as used herein include plural forms as long as the phrases do not expressly express the opposite meaning thereto. Means that a particular feature, region, integer, step, operation, element and / or component is specified, and that other specific features, regions, integers, steps, operations, elements, components, and / And the like.
All terms including technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the present invention belongs. Predefined terms are further interpreted as having a meaning consistent with the relevant technical literature and the present disclosure, and are not to be construed as ideal or very formal meanings unless defined otherwise.
1 is a schematic diagram of a method of manufacturing a thermoplastic carbon fiber composite material according to an embodiment of the present invention.
Referring to FIG. 1, a method for manufacturing a thermoplastic carbon fiber composite material according to an embodiment of the present invention includes the steps of unwinding a
A widening slimming step S200 for widening and slimming the
A spray coating step (S300) of spraying and coating the hybrid alumina coating liquid (40) on at least one of the upper surface and the lower surface of the carbon fiber spread bundle (110) by the spray device (30)
After the hybrid alumina coating liquid injection step S300 is performed, the hybrid
The
And a carbon fiber tape bonding step S600 for winding the
The
The carbon fiber bundle supplying step S100 is a step of supplying the carbon fiber bundle from the
The cemented
The
The
In the widening step S200, the width of the carbon
Here, the width of the
The width of the
In the spray coating step (S300), the spray device (30) includes various spray injectors, spray guns, and the like. The spray device (30) is not limited as long as it can spray and coat the hybrid alumina coating liquid (40).
The spray coating step S300 may be performed by supplying the
In the hybrid alumina coating layer formation step (S400), the heater may include a hot wind generating hot wind, a halogen lamp generating radiant heat, an infrared lamp, or the like. That is, the drying of the hybrid
In the hybrid alumina coating layer forming step S400, the hybrid
The hybrid alumina coating layer forming step S400 is performed by supplying the
A
A
The method for producing a thermoplastic carbon fiber composite material may include a process for preparing a coating solution to spray-coat the carbon fiber spread
The coating manufacturing process, the aluminum alkoxide (Al (OC 4 H 9) 3) is reacted with water, the hydrolysis step of hydrolyzing the aluminum hydroxide (Al (OH) 3) ( S10),
(Al (OH) 3 ) is decomposed into AlOOH sol (sol) by adding nitric acid (HNO 3 ) to the aluminum hydroxide at a set temperature (for example, 80 to 100 degrees) (Peptization) step S20,
An AlOOH sol stabilization step (S30) in which the AlOOH sol is stabilized by heating at a set heating time and a heating time,
Alpha alumina ball-milling (ball milling) the friction as alpha-alumina (α-Al 2 O 3) generating the seed particles and the seed particles, alpha-alumina (α-Al 2 O 3) in the AlOOH sol of the ball by (seed particles) A ball-milling step (S40) in which ball milling is performed for a set time period, and
And a step (S50) of preparing a hybrid alumina coating solution in which the alpha alumina seed particles broken by the mutual friction of the alpha-alumina seed particles in the ball-milling step (S40) are dispersed in AlOOH sol to produce a stable hybrid alumina coating solution .
The AlOOH sol may be prepared by a sol-gel process with a solids content of 5 to 20 wt.% (Especially 10 wt.%). For the stability of dispersion of the AlOOH sol, the pH of the AlOOH sol is preferably 3.0 to 4.0 .
The above-mentioned AlOOH sol has a high adhesion property, which is well adhered to the surface of the substrate, and can be strongly adhered to carbon fibers.
In the ball-milling step S40, the ball-milling can be carried out for a predetermined time, for example, 8 hours to 20 hours, so that the alpha alumina seed particles are not only generated by friction between balls but also dispersed uniformly in the AlOOH sol .
In addition, in the ball-milling step (S40), the size of the alpha alumina seed particles may be larger than 0.05 mu m and less than 100 mu m so that the alpha alumina seed particles may float on the AlOOH sol.
Hereinafter, a method of manufacturing a thermoplastic carbon fiber composite material according to an embodiment of the present invention will be described with reference to FIG.
First, a coating liquid manufacturing process for preparing the coating liquid is spray coated on the carbon fiber spread bundles 110 of the method for producing a thermoplastic carbon fiber composite material according to one embodiment of the present invention, aluminum alkoxide (Al (OC 4 H 9) 3 ) Is reacted with water and hydrolyzed with aluminum hydroxide (Al (OH) 3 ) (S10)
Aluminum hydroxide (Al (OH) 3 ) is decomposed into AlOOH sol (sol) by adding nitric acid (HNO 3 ) to the aluminum hydroxide at a predetermined temperature, for example, The AlOOH sol is stabilized by heating at the set heating temperature and heating time (S30).
Ball milling was then performed to add alpha-Al 2 O 3 seed particles to the AlOOH sol by cross-friction fractured particles by ball milling. (S40). Further, the frictionally pulverized alpha alumina seed particles are well dispersed in the AlOOH sol to prepare a stable hybrid alumina coating solution (S50).
At this time, the AlOOH sol is prepared by a sol-gel method at a solid concentration of, for example, 5 to 20 wt.%, And the pH of the AlOOH sol is set to 3.0 to 4.0 for stability of dispersion of the AlOOH sol. The above-mentioned AlOOH sol has a high adhesion property which is well adhered to the surface of the substrate and can be strongly adhered to the carbon fiber.
A method for manufacturing a thermoplastic carbon fiber composite material includes the steps of unfolding a
The hybrid
The hybrid
The
(Example)
AlOOH-sol was prepared by sol-gel method with a solids concentration of 10 wt.% And the pH was set to 3.0 to 4.0 for stability of dispersion. AlOOH-sol has a high adhesiveness that adheres well to the surface of the substrate and can strongly adhere to carbon fibers.
After the ball milling using the alpha-alumina seed particles of alpha-Al 2 O 3 was performed for 12 hours, for example, alpha-Al 2 O 3 ) α-Al 2 O 3 seed particles are dispersed in AlOOH-sol solution by mutual friction of seed particle balls to form a stable hybrid alumina coating solution (α-Al 2 O 3 seed particles dispersed AlOOH-sol solution) (see Fig. 2).
The hybrid alumina coating solution thus prepared is spray-coated on a superfine carbon fiber spread
The hybrid alumina coating layer formed on the carbon fiber surface is a ceramic material having a higher surface energy than that of the conventional carbon fiber, thereby forming a high interfacial bonding force with the thermoplastic resin of the Martrix material.
FIG. 3 is a photograph showing TEM (transmission electron microscopic) analysis results of the hybrid alumina coating layer prepared according to the method for producing a thermoplastic carbon fiber composite material according to an embodiment of the present invention.
Referring to FIG. 3, it can be confirmed that a hybrid alumina coating layer (α-Al 2 O 3 seed particles dispersed AlOOH-sol solution) is uniformly coated on the filaments of the carbon fiber bundle. Therefore, it is possible to form a high interfacial bonding force with a thermoplastic resin as a matrix material.
S100: Carbon fiber bundle feeding step
S200: Wide Slim step
S300: Spray coating step
S400: Hybrid alumina coating layer formation step
S500: Carbon fiber tape forming step
S600: Carbon fiber tape winding stage
Claims (9)
A widening slim step of widening and slimming the carbon fiber bundle into a bundle of carbon fiber spun by a widening unit,
A spray coating step of spraying and coating a hybrid alumina coating solution on at least one of the upper surface and the lower surface of the carbon fiber spread bundle by a spray device,
A hybrid alumina coating layer forming step of forming a hybrid alumina coating layer by drying the hybrid alumina coating solution coated on the carbon fiber spread bundle at a predetermined temperature by a heater,
A carbon fiber tape forming step of arranging and bonding a thermoplastic film to at least one of the upper surface and the lower surface of the carbon fiber spread bundle on which the hybrid alumina coating layer is formed to form an alumina coated carbon fiber tape,
And a carbon fiber tape bonding step of winding the carbon fiber tape on a reel,
A roll for supplying the thermoplastic film to the upper side or the lower side of the carbon fiber spray bundle in the carbon fiber tape forming step,
Wherein the step of forming the hybrid alumina coating layer includes a step of guiding the carbon fiber spread bundle supplied from the spray device to the heater by a third guide roll installed between the spray device and the heater, ≪ / RTI >
Wherein the width of the carbon fiber bundle is wide at least two times to at most 20 times,
Wherein the thickness of the carbon fiber bundle is slim with a ratio of a minimum of 1/2 to a maximum of 1/20.
Wherein the carbon fiber bundle is widened and slimmed by colliding with an air current generated by a vacuum and hot air in the wide width portion.
Wherein the drying of the hybrid alumina coating liquid is performed by one of hot air generated from hot air of the heater, radiant heat generated from a halogen lamp, and radiant heat generated from an infrared lamp.
Wherein the spray coating step comprises spray-coating the carbon fiber spread bundle before performing the spray coating step.
The process for producing the coating liquid includes a hydrolysis step of reacting aluminum alkoxide with water and hydrolyzing the aluminum alkoxide with aluminum hydroxide,
A step of peptization in which nitric acid (HNO 3 ) is added to the aluminum hydroxide and the pH is maintained at 3.0 to 4.0 to decompose the aluminum hydroxide into an AlOOH sol (sol)
Stabilizing the AlOOH sol to stabilize the AlOOH sol by heating,
A ball-milling step in which ball milling is performed by adding alpha alumina seed particles to the AlOOH sol, and
And a step of preparing a hybrid alumina coating liquid in which the alpha alumina seed particles are dispersed in the AlOOH sol by the mutual friction of the alpha alumina seed particle balls to produce a stable hybrid alumina coating liquid. .
Wherein the ball milling in the ball-milling step is performed for 8 to 20 hours for uniform dispersion of the alpha alumina seed particles.
Wherein the size of the alpha alumina seed particles is larger than 0.05 mu m and smaller than 100 mu m.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112712944A (en) * | 2020-12-24 | 2021-04-27 | 武汉肯达科讯科技有限公司 | High-thermal-conductivity insulating gasket and preparation method thereof |
CN114395834A (en) * | 2021-12-23 | 2022-04-26 | 山东非金属材料研究所 | Process and device for preparing continuous combined filament yarn |
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KR19990028647A (en) * | 1996-05-01 | 1999-04-15 | 구리타 유키오 | METHOD FOR MANUFACTURING MULTIFILAMENT SPREAD SHEET, APPARATUS USED IN THE METHOD, AND SPREAD SHEET PRODUCED BY THE SAME |
KR20040023907A (en) * | 2002-09-12 | 2004-03-20 | 한국화학연구원 | Method for forming the alumina powders via sol-gel process |
KR101482452B1 (en) * | 2013-11-15 | 2015-01-14 | 주식회사 포스코 | Manufacturing method of carbon fiber reinforced thermoplastic composite and the composite manufactured by the same |
KR20170055468A (en) * | 2014-10-31 | 2017-05-19 | 재팬 마텍스 컴퍼니 리미티드 | Process for producing carbon-fiber resin tape, and carbon-fiber resin tape |
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KR19990028647A (en) * | 1996-05-01 | 1999-04-15 | 구리타 유키오 | METHOD FOR MANUFACTURING MULTIFILAMENT SPREAD SHEET, APPARATUS USED IN THE METHOD, AND SPREAD SHEET PRODUCED BY THE SAME |
KR20040023907A (en) * | 2002-09-12 | 2004-03-20 | 한국화학연구원 | Method for forming the alumina powders via sol-gel process |
KR101482452B1 (en) * | 2013-11-15 | 2015-01-14 | 주식회사 포스코 | Manufacturing method of carbon fiber reinforced thermoplastic composite and the composite manufactured by the same |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN112712944A (en) * | 2020-12-24 | 2021-04-27 | 武汉肯达科讯科技有限公司 | High-thermal-conductivity insulating gasket and preparation method thereof |
CN114395834A (en) * | 2021-12-23 | 2022-04-26 | 山东非金属材料研究所 | Process and device for preparing continuous combined filament yarn |
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