WO2019112287A1 - Procédé de préparation d'une composition de pâte à rayonnement thermique à l'aide de fibres de carbone usées, procédé de fabrication d'un film mince à rayonnement thermique l'utilisant, et film mince à rayonnement thermique le comprenant - Google Patents

Procédé de préparation d'une composition de pâte à rayonnement thermique à l'aide de fibres de carbone usées, procédé de fabrication d'un film mince à rayonnement thermique l'utilisant, et film mince à rayonnement thermique le comprenant Download PDF

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WO2019112287A1
WO2019112287A1 PCT/KR2018/015239 KR2018015239W WO2019112287A1 WO 2019112287 A1 WO2019112287 A1 WO 2019112287A1 KR 2018015239 W KR2018015239 W KR 2018015239W WO 2019112287 A1 WO2019112287 A1 WO 2019112287A1
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Prior art keywords
waste carbon
carbon fiber
thin film
heat
carbon fibers
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PCT/KR2018/015239
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English (en)
Korean (ko)
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김대업
김광석
정하나
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한국생산기술연구원
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Publication of WO2019112287A1 publication Critical patent/WO2019112287A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/20—Agglomeration, binding or encapsulation of solid waste
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M1/00—Inking and printing with a printer's forme
    • B41M1/12—Stencil printing; Silk-screen printing
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00—Constructional details common to different types of electric apparatus
    • H05K7/20—Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • H05K7/20436—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing
    • H05K7/20445—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing the coupling element being an additional piece, e.g. thermal standoff
    • H05K7/20472—Sheet interfaces

Definitions

  • This technology relates to the restoration of physical properties of waste resources, specifically, a technology of a heat dissipation material for heat dissipation, a technology for manufacturing a heat dissipation material using waste fibers generated in the process, and a technology for manufacturing heat dissipation parts using the same.
  • the carbon fiber is converted into a prepreg, which is an intermediate substrate, to be used in a predetermined shape.
  • a prepreg is a molding material preliminarily impregnated with a matrix resin in a fabric made of reinforcing fibers such as carbon fibers, and a molded product is formed by laminating prepregs, heating and pressing them to cure the resin.
  • Carbon fiber is a fiber made by heating and carbonizing many organic polymer fibers in an inert gas at about 1000 to 3000 ° C. It is an organic polymer fiber that is a raw material of carbon fiber production. Currently, it is made of polyacrylonitrile (PAN) fiber, (Pitch) fibers, and liquid crystal pitch fibers are used. Carbon fiber is excellent in heat resistance, impact resistance, thermal conductivity, strong in chemicals, lighter in weight than metal, but has more elasticity and strength than metal.
  • PAN polyacrylonitrile
  • Pitch pitch fibers
  • Carbon fiber is excellent in heat resistance, impact resistance, thermal conductivity, strong in chemicals, lighter in weight than metal, but has more elasticity and strength than metal.
  • the carbon fiber is converted into a prepreg, which is an intermediate substrate, to be used in a predetermined shape.
  • a prepreg is a molding material preliminarily impregnated with a matrix resin in a fabric made of reinforcing fibers such as carbon fibers, and a molded product is formed by laminating prepregs, heating and pressing them to cure the resin.
  • a method of manufacturing a heat radiation paste composition includes: collecting waste carbon fibers generated in a carbon fiber manufacturing process; A pretreatment step of homogenizing the collected waste carbon fibers; And adding and mixing the prepared binder and dispersant to the pretreated waste carbon fiber.
  • the pretreatment step may further include cutting the waste carbon fibers to a uniform size and then milling and granulating the waste carbon fibers.
  • the milling can maximize the efficiency by using the slices having a uniform average size.
  • the binder is a dispersion in which ethylcellulose is ultrasonically dispersed in a first solvent
  • the dispersant is a dispersion in which polyvinylpyrrolidone is ultrasonically dispersed in a second solvent.
  • the content of the first solvent or the second solvent is preferably adjusted to be 8 to 10 times the solids content of the binder and the dispersant, respectively.
  • the content of the solid content of the binder is greater than the content of the solid content of the dispersing agent.
  • the milling is carried out in the following manner: i) the average length of the waste carbon fibers: 3 mm, ii) the mass of the waste carbon fibers: 15 g, iii) the ball material: zirconia, iv) the ball diameter: Atmosphere and vii) speed: 500 rpm, it is advantageous in terms of the thermal conductivity of the material to be produced to be made for 2.5 to 3.5 hours.
  • the milling is performed so that the size of the pulverized waste carbon fiber has a distribution of 400 to 650 nm.
  • 10 to 30% by weight of waste carbon fiber; 50 to 80% by weight of a binder; And 20 to 40% by weight of a dispersing agent may be mixed.
  • the method of manufacturing a heat-radiating thin film according to an embodiment of the present invention includes the steps of forming the above-described paste composition into a thin film shape, and sintering the composition molded from the thin film.
  • the forming may comprise silk screen printing and, if the waste carbon fiber comprises waste carbon fibers in the cut form, placing and pressing the paste composition at room temperature or in a heated state.
  • the sintering is preferably performed at a temperature of 350 to 450 ° C.
  • the thin film for heat generation according to an embodiment of the present invention is manufactured by the thin film manufacturing method described above and has a thermal conductivity of at least 0.20 W / mk or more.
  • the method for producing a heat-dissipating paste composition according to the present invention is a method for producing a heat-dissipating paste composition which is capable of reducing the deteriorated physical properties of waste carbon fibers through an additional step such as paste- Thereby making it possible to utilize the waste carbon fiber as a material having properties equal to or higher than those of normal carbon fibers.
  • the thin film produced by using the heat-dissipating paste composition can be used for thin-film components for thermal diffusion, and can realize excellent thermal conductivity.
  • the thin film can be produced by pulverized waste carbon fiber or chopped ) Waste carbon fiber and so on, it can be expected to be applied to various industrial fields according to pretreatment of waste carbon fiber.
  • the present invention ultimately restores the deteriorated physical properties of waste carbon fiber and is a very powerful technology capable of realizing the high added value of waste resources through the recycling of waste resources. In the future, new application fields will be discovered and customized properties By developing recovery technology, it is necessary to continuously utilize waste carbon fiber.
  • Fig. 1 is a graph showing the X-ray analysis results showing the mechanical strengths of waste carbon fibers and waste carbon fibers having normal properties.
  • Fig. 2 is a graph showing weight loss rates of carbon fibers and waste carbon fibers with normal properties according to temperature.
  • 3 is a graph showing the thermal decomposition termination temperature of the carbon fibers and the waste carbon fibers having normal properties.
  • Fig. 4 is an electron micrograph showing the morphology of normal carbon fibers and waste carbon fibers.
  • Fig. 5 is an electron micrograph showing tensile test fracture sectional analysis results of normal carbon fiber and waste carbon fiber.
  • 6 is an electron micrograph showing the distribution of diameters of particles according to the milling time.
  • a method of manufacturing a heat radiation paste composition according to an embodiment of the present invention includes a step of collecting waste carbon fibers generated in a carbon fiber manufacturing process, a pretreatment step of uniformizing the collected waste carbon fibers, and a binder prepared in the pretreated waste carbon fiber Adding and mixing a dispersing agent.
  • Carbon fibers are produced through a stabilization process to induce the cyclization of the polymer and a high-temperature carbonization process to form carbon-carbon bonds. Since the temperature and the residence time of the heat treatment in the stabilization process and the carbonization process greatly affect the properties of the carbon fiber finally produced, the physical properties of the carbon fiber show a great difference depending on the process conditions. Defects are generated naturally inside and outside the carbon fiber in the process of radiating the precursor to produce the carbon fiber and the process of stabilizing and carbonizing the spun fiber. Observing defects is an important part of carbon fiber research, because defects present in the fiber cause a decrease in mechanical strength.
  • 'Waste carbon fiber' is defined as meaning a commercially untradeable fiber because it causes such mechanical strength and other plural properties deterioration.
  • the properties of carbon fibers can be broadly classified into mechanical properties, structure and texture properties, and thermal properties.
  • the mechanical properties are linear density, tensile strength, elastic modulus, and structural and structural characteristics are related to crystal structure, surface and fracture characteristics.
  • Thermal properties are evaluated by thermal activation stability, Speed, weight loss, and the like.
  • carbon fibers such as A-carbon (A-CF), B-carbon (B-CF) -CF). ≪ / RTI > Table 1 shows the results of distinguishing between normal carbon fibers and waste carbon fibers according to mechanical property evaluation.
  • Fig. 1 is a graph showing the X-ray analysis results showing the mechanical strengths of waste carbon fibers and waste carbon fibers having normal properties. Referring to FIG. 1, waste carbon fibers exhibit a strength lowered in strength in comparison with A-grade carbon fibers and B-grade carbon fibers due to defects occurring in the process even though they have a similar crystal structure.
  • Fig. 2 is a graph showing weight loss rates of carbon fibers and waste carbon fibers with normal properties according to temperature.
  • FIG. 3 is a graph showing the thermal decomposition termination temperature of the carbon fibers and the waste carbon fibers having normal properties. Referring to FIG. 3, in the case of the waste carbon fiber compared to the carbon fiber having normal properties, the thermal decomposition termination temperature decreases, and it is confirmed that the heat resistance is weak.
  • Fig. 4 is an electron micrograph showing the morphology of normal carbon fibers and waste carbon fibers.
  • Fig. Fig. 5 is an electron micrograph showing tensile test fracture sectional analysis results of normal carbon fiber and waste carbon fiber.
  • the predetermined waste carbon fibers are classified and collected according to the operator's request as described above.
  • the collected waste carbon fibers are subjected to two types of pretreatment steps as a homogenization process for the subsequent process.
  • the waste carbon fiber slice is preferably pretreated so that the size of the slice, that is, the length, on average, is 2.5 to 3.5 mm. If the mean size of the slice is less than 2.5 mm, it is not suitable in terms of process efficiency or economical efficiency, whereas if the average size of the slice exceeds 3.5 mm, the efficiency of the subsequent granulation step may be lowered When used in the paste manufacturing process and the thinning process described later, it is possible to inhibit the subsequent efficiency of forming a thin film, that is, the smoothness of the thin film surface or the stability of the shape in the film forming process.
  • the waste carbon fiber slice itself may be used in a subsequent process, but the waste carbon fiber slab, which has been pretreated first, may be subjected to another type of pretreatment step by milling through a milling process or the like.
  • the waste carbon fiber slices prepared through the cutting process may be subjected to a secondary pretreatment step in which they are granulated by a milling machine.
  • the waste carbon fiber slice or the waste carbon fiber particles as the intermediate material may be independently used in a subsequent process or may be used in a subsequent process in combination depending on the use of the product to be molded or the operator's intention.
  • the size of the particles is preferably milled to have a size distribution of about 400 to 650 nm.
  • the waste carbon fiber pretreated through the pretreatment step may be included as a main component of the heat radiation paste composition having thermal conductivity.
  • the pretreated waste carbon fibers are added to and mixed with the prepared binder and dispersant to form a heat radiation paste composition.
  • the 'binder' and the 'dispersant' refer to a mixture of a solid and a solvent.
  • the binder is a binder resin, that is, a dispersion prepared through dispersion of binder solids and a solvent.
  • Ethylcellulose is used as the binder resin.
  • any binder resin not mentioned in this specification can be used as long as it is a resin favorable in correlation with thermal conductivity, which is a technical problem of the present invention.
  • a solvent for the dispersion of the binder resin for example,? -Terpineol and the like may be used.
  • the dispersant is also included in the composition as a dispersion, and as the solid content of the dispersant, polyvinyl pyrrolidone and the like can be used.
  • the solvent for dispersing the solid content of the dispersant diethylene glycol (DEG) .
  • DEG diethylene glycol
  • other components not mentioned herein may be used, provided that dispersant solids, solvents, and the like are advantageous in correlation with thermal conductivity, which is a technical problem of the present invention.
  • the binder dispersion and the dispersion of the dispersant may be mixed and dispersed by mixing the solid content and the solvent and by an ultrasonic dispersion method.
  • both the binder and the dispersing agent are included in the dispersion so that the respective solvents are contained in an amount of 8 to 10 times the solid content of the respective solids.
  • the solvents have a content of more than 10 times the solid content, the time for volatilization in the subsequent sintering process is long, which may reduce the efficiency of the thin film manufacturing process.
  • the content of the solvent is less than 8 times the solid content, It may not be possible to realize a uniform thin film shape in the molding process.
  • the content of the binder solids is included in the paste composition such that the content of the binder solids is greater than the content of the dispersant solids.
  • This content control has a causal relationship with the characteristics of the thermal conductivity of the thin film described later.
  • the paste composition may comprise from 10 to 30% by weight of waste carbon fiber, from 50 to 80% by weight of binder, and from 20 to 40% by weight of dispersant.
  • the content of the binder may be larger than the content of the dispersant, it is possible to maximize the heat conduction characteristics of the thin film to be produced.
  • the dispersion performance of the composition may be deteriorated and the molding quality may be deteriorated, so that the binder and the dispersing agent must be simultaneously included in the composition.
  • the milling conditions have a significant causal relation to the thermal conductivity of the thin film described later. Therefore, when cut waste carbon fibers are granulated by a milling machine or the like, the control of the milling time is very important, and the thermal conductivity is not directly proportional to or inversely proportional to the milling time.
  • the thin film for heat dissipation is used as a thin film in various fields such as a protective film of a semiconductor device and plays a role of effectively diffusing internal heat.
  • the heat-dissipating paste composition should be formed into a thin film. There are two types of molding process.
  • the composition may be formed into a thin film by being pressed or heated.
  • the pressing may be performed by using a pressing device, and the pressing device may be a device capable of pressing to several tens of micrometers.
  • the slice is cut to have an average size of 2.5 to 3.5 mm and introduced into the molding process as described above.
  • the heat-dissipating paste composition may be formed into a thin film by a method such as silk screen printing.
  • composition for molding includes a waste carbon fiber slice and waste carbon fiber particles at the same time
  • a silk screen printing method or a press method is appropriately selected in consideration of the content of each component to perform a thinning process And, in some cases, other types of thinning processes may be considered.
  • the milling time can be a very important parameter for the thermal conductivity characteristics of the finally produced thin film.
  • the milling time of the waste carbon fibers (average size of 3 mm) cut into a uniform shape is about 3 hours or less, that is, 2.5 to 3.5 hours under the following milling conditions, Do.
  • milled waste carbon fiber particles Even if the milling conditions are changed, it is important for milled waste carbon fiber particles to be milled to have a particle size distribution of about 400 to 650 nm to communicate the thermal conductivity characteristics of the final thin film product.
  • the molded thin film composition can be manufactured as a thin film for heat dissipation through a sintering process.
  • the sintering is carried out at a temperature of 350 ° C to 450 ° C. If the sintering temperature is less than 350 ° C, the formation of the thin film is difficult and the thermal conductivity of the produced thin film can be remarkably lowered. On the other hand, when the sintering temperature exceeds 450 ° C, homogenization of shapes such as uneven surface characteristics of a thin film to be produced can be inhibited.
  • the final thin film heat dissipation component can be manufactured.
  • the thin film produced by the above-described method may have a thermal conductivity of at least 0.2 W / mk.
  • the milling is carried out in an atmosphere of argon gas and in an atmosphere of argon gas and at a pressure of 5 Torr.
  • the average diameter of the waste carbon fiber is 3 mm, the mass of the waste carbon fiber is 15 g, iii) the ball material is zirconia, vii) Speed: 500 rpm.
  • the milling times were set to 30 minutes, 1 hour 30 minutes, 3 hours, and 4 hours, respectively.
  • the screen printing was not smoothly performed after the composition was formed, and the 30 minute milling conditions were excluded from the examples.
  • binder a dispersion in which ethyl cellulose and alpha -terpineol were mixed and dispersed at a ratio of 1: 9 was used, and a dispersion in which polyvinylpyrrolidone and DEG were mixed and dispersed at a ratio of 1: 9 was used.
  • Each of the examples was classified based on those using the binder (B) and the dispersant (D) in a ratio of B0 / D100, B25 / D75, B50 / D25 and B100 / D0.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 1 hour and 30 minutes to be granulated, and the pulverized waste carbon fibers were mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B25 / D75) .
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 1 hour and 30 minutes to be granulated and the granulated waste carbon fibers were mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B50 / D50) .
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 1 hour and 30 minutes to be granulated and the particulate waste carbon fibers were mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B75 / D25) .
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 1 hour and 30 minutes to be granulated, and the particulate waste carbon fibers were mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B100 / D0) .
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 3 hours to be granulated and the granulated waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B25 / D75) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 3 hours to be granulated and the pulverized waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B50 / D50) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 3 hours to be granulated and the granulated waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B75 / D25) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 3 hours to be granulated, and the particulate waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B100 / D0) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 4 hours to be granulated, and the particulate waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B25 / D75) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 4 hours to be granulated and the pulverized waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B50 / D50) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 4 hours to be granulated, and the pulverized waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B75 / D25) to prepare a paste composition Respectively.
  • the waste carbon fiber slice cut to an average length of 3 mm was milled for 4 hours to be granulated and the granulated waste carbon fiber was mixed with the binder / dispersant solution at a weight ratio of 1: 9 (B100 / D0) to prepare a paste composition Respectively.
  • Example 1-1 Examples 1-2 Example 1-3 Examples 1-4 Examples 1-5 3h Example 2-1 Example 2-2 Example 2-3 Examples 2-4 Example 2-5 4h Example 3-1 Example 3-2 Example 3-3 Example 3-4 Example 3-5
  • FIG. 6 is an electron micrograph showing the distribution of diameters of particles according to the milling time. Referring to FIG. 6, it was confirmed that as the milling time elapsed, the uniformity of the particles was improved and the average size of the particles decreased in proportion to time.
  • the thermal conductivity of the thin film prepared in each example was measured by a thin film thermal conductivity meter, and the result is shown in the graph of FIG. 7 is a graph showing the thermal conductivity according to the milling time and the content of the binder / dispersant.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

La présente invention concerne un procédé de préparation d'une composition de pâte à rayonnement thermique, le procédé comprenant : une étape consistant à collecter des fibres de carbone usées générées pendant un processus de fabrication de fibre de carbone; une étape de prétraitement pour rendre uniforme les fibres de carbone usées collectées; et une étape d'ajout d'un liant et d'un dispersant préparés aux fibres de carbone usées pré-traitées, suivi d'un mélange, et un procédé de fabrication d'un film mince à rayonnement thermique l'utilisant. Le film mince à rayonnement thermique fabriqué par de tels procédés présente d'excellentes caractéristiques de conductivité thermique même s'il est fabriqué en utilisant des fibres de carbone usées.
PCT/KR2018/015239 2017-12-04 2018-12-04 Procédé de préparation d'une composition de pâte à rayonnement thermique à l'aide de fibres de carbone usées, procédé de fabrication d'un film mince à rayonnement thermique l'utilisant, et film mince à rayonnement thermique le comprenant WO2019112287A1 (fr)

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KR1020170165063A KR101897110B1 (ko) 2017-12-04 2017-12-04 폐탄소섬유를 이용한 방열용 페이스트 조성물의 제조방법, 이를 이용한 방열용 박막의 제조방법 및 이를 포함하는 방열용 박막
KR10-2017-0165063 2017-12-04

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KR101897110B1 (ko) * 2017-12-04 2018-10-18 한국생산기술연구원 폐탄소섬유를 이용한 방열용 페이스트 조성물의 제조방법, 이를 이용한 방열용 박막의 제조방법 및 이를 포함하는 방열용 박막
KR102335494B1 (ko) * 2020-02-19 2021-12-06 전주대학교 산학협력단 유해물질 제거를 위한 금속함유 활성탄소섬유 및 그 제조방법

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KR20160060853A (ko) * 2014-11-20 2016-05-31 주식회사 알인텍 폐탄소섬유 재처리방법
KR101735819B1 (ko) * 2016-02-05 2017-05-16 이석 탄소계 방열구조체용 재료, 이를 이용한 탄소계 방열구조체의 제조방법 및 이에 의해 제조된 탄소계 방열구조체
KR101897110B1 (ko) * 2017-12-04 2018-10-18 한국생산기술연구원 폐탄소섬유를 이용한 방열용 페이스트 조성물의 제조방법, 이를 이용한 방열용 박막의 제조방법 및 이를 포함하는 방열용 박막

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