WO2019107706A1 - 에어로겔을 포함한 복합 단열 시트 - Google Patents

에어로겔을 포함한 복합 단열 시트 Download PDF

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Publication number
WO2019107706A1
WO2019107706A1 PCT/KR2018/009608 KR2018009608W WO2019107706A1 WO 2019107706 A1 WO2019107706 A1 WO 2019107706A1 KR 2018009608 W KR2018009608 W KR 2018009608W WO 2019107706 A1 WO2019107706 A1 WO 2019107706A1
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WIPO (PCT)
Prior art keywords
sheet
coating layer
sol
airgel
fiber
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PCT/KR2018/009608
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English (en)
French (fr)
Inventor
오경실
이제균
한병욱
전용석
박상우
김중년
Original Assignee
주식회사 엘지화학
엘지전자 주식회사
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Application filed by 주식회사 엘지화학, 엘지전자 주식회사 filed Critical 주식회사 엘지화학
Priority to US16/631,375 priority Critical patent/US11312103B2/en
Priority to CN201880044833.4A priority patent/CN110870395B/zh
Priority to JP2019570394A priority patent/JP7042287B2/ja
Priority to EP18884080.5A priority patent/EP3629689B1/en
Publication of WO2019107706A1 publication Critical patent/WO2019107706A1/ko

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Definitions

  • the present invention relates to a composite heat insulating sheet containing an airgel and a method of manufacturing the same.
  • the present invention attempts to solve the above-mentioned problem by applying Aerogel, which is attracting attention as a high efficiency heat insulating material.
  • Aerogels are high-porosity materials composed of nanoparticles and have high porosity, specific surface area, and low thermal conductivity, and are attracting attention as high-efficiency heat insulation materials and soundproofing materials.
  • an airgel composite in which airgel is impregnated with fibers such as inorganic fibers or organic fibers, which are conventional heat insulating fibers, is manufactured and used. And adhesion of aerogels is weak, so that airgel particles are separated during processing such as cutting and bending, resulting in generation of dust and durability, which may lead to damage of equipment when applied as a heat insulating material for electronic products.
  • the present invention provides an airgel composite sheet having characteristics of low dust, high strength, and high thermal resistance in order to solve the above problems, thereby enhancing the applicability to electronic devices.
  • Patent Document 1 US 8,021,583 B2 (September 20, 2011)
  • the present invention provides an ultra-thin composite insulation sheet having characteristics of low dust, high strength and high thermal insulation so as to be applicable to electronic devices, and a method of manufacturing the same.
  • the present invention relates to an airgel sheet
  • the present invention also provides a method of manufacturing a fiber sheet, comprising the steps of: forming a sol-opaque coating layer on one side of a fiber sheet;
  • the composite heat insulating sheet of the present invention dust generation is reduced by the sol-free coating layer formed on one surface, and high heat insulating efficiency and processability can be provided.
  • the mechanical strength can be improved by the coating layer, and the durability can be increased.
  • Fig. 1 is a graph showing thermal conductivities of composite heat insulating sheets of Examples and Comparative Examples.
  • the present invention intends to use an airgel sheet as a high-efficiency heat insulating material.
  • an object of the present invention to provide an ultra-thin composite heat-insulating sheet having characteristics of low dust, high strength and high thermal insulation so as to be widely used in electronic products and a method of manufacturing the same.
  • the present invention relates to an airgel sheet
  • the composite heat insulating sheet of the present invention is characterized by introducing a sol-free coating layer on one surface of the airgel sheet.
  • the coating layer includes at least one selected from the group consisting of PA (poly amide), PE (poly ethylene), PET (poly ethylene terephthalate), PI (polyimide), and silicon.
  • PA poly amide
  • PE poly ethylene
  • PET poly ethylene terephthalate
  • PI polyimide
  • the coating layer is particularly characterized by being sol-free.
  • the coating layer of the present invention prevents the sol from flowing to the outside through the fibers when the sol is impregnated with the organic or inorganic fibers in the process of producing the airgel sheet to prevent the airgel from being exposed on the surface of the airgel sheet, do.
  • the other surface on which the coating layer is not formed can prevent the airgel from being exposed to the surface by the functional layer to be described later.
  • the coating layer can serve to compensate the mechanical strength of the very low airgel sheet due to the porous structure.
  • the coating layer can increase the mechanical strength of the composite insulation sheet to improve the durability.
  • the thickness of the sol-free coating layer of the present invention is 30 ⁇ ⁇ or less, more specifically 10 to 20 ⁇ ⁇ . If the thickness of the sol-resistant coating layer is thicker than the above range, the heat insulating performance of the composite heat insulating sheet may be deteriorated, and there may be a limit to the use of the heat insulating material in electronic products requiring ultra-thin insulating materials. On the other hand, if it is thinner than the above range, the effect of improving the mechanical strength is insignificant and the durability may not be good.
  • the substance capable of forming the sol may be at least one substance selected from the group consisting of zirconia, yttrium oxide, hafnia, alumina, titania, ceria, silica, magnesium oxide, calcium oxide, magnesium fluoride and calcium fluoride Inorganic material.
  • the silica sol may include a silicon-containing alkoxide compound.
  • TMOS tetramethyl orthosilicate
  • TEOS tetraethyl orthosilicate
  • Tetraethyl orthosilicate but are not limited to, prehydrolyzed TEOS, methyl triethyl orthosilicate, dimethyl diethyl orthosilicate, tetrapropyl orthosilicate, tetraisopropyl orthosilicate tetraisopropyl orthosilicate, tetrabutyl orthosilicate, tetra secondary butyl orthosilicate, tetra tertiary butyl orthosilicate, tetrahexyl orthosilicate, ), Tetracycline Hexyl orthosilicate may be a tetraalkyl silicate such as (tetracyclohexyl orthosilicate), tetra-dodecyl orthosilicate
  • the alcohols usable in the preparation of the silica sol of the present invention are specifically exemplified by monohydric alcohols such as methanol, ethanol, isopropanol, butanol and the like; Or polyhydric alcohols such as glycerol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, and sorbitol, and any one or a mixture of two or more thereof may be used.
  • monohydric alcohols having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol and the like can be used in consideration of compatibility with water and an airgel.
  • the alcohol (polar organic solvent) as described above can be used in an appropriate amount in consideration of the degree of hydrophobization in the silica airgel which is finally produced while promoting the surface modification reaction.
  • composite heat insulating sheet of the present invention may include at least one functional layer on the other surface of the airgel sheet.
  • the present invention can prevent damage to the device due to no occurrence of dust, while having an innovative heat insulating performance by laminating the functional layer on the other surface of the composite insulating sheet on which the sol-free opaque coating layer is not formed, To prevent heat accumulation in the device due to heat insulation, thereby preventing damage to the device.
  • the functional layer may exhibit at least one function selected from the group consisting of thermal diffusion, insulation, sound absorption, vibration resistance, impermeability to water, and permeability to water vapor, and the composite insulation sheet of the present invention is not limited thereto. And a functional layer which exhibits necessary functions in the electronic product.
  • the composite heat-insulating sheet of the present invention prevents water from penetrating into the electronic component, thereby preventing damage to the electronic component.
  • the functional layer is permeable to water vapor, It is possible to prevent the water vapor from condensing and to prevent the electronic parts from being damaged.
  • the layer impermeable to water and permeable to water vapor may comprise a cellulosic material.
  • the sheet may be an inorganic fiber, an organic fiber, or a combination thereof.
  • the sheet may be a film, a sheet, a net, a fiber, a porous body, a foam, a nonwoven fabric, or a laminate of two or more layers thereof. Further, depending on the application, surface roughness may be formed or patterned on the surface thereof.
  • the sheet may be a fiber capable of further improving the heat insulating performance by including spaces or voids into which the sol can be easily inserted into the sheet.
  • the sheet of the present invention may preferably have a low thermal conductivity.
  • the fiber sheet that can be used in the present invention may be at least one selected from the group consisting of polyethylene terephthalate, polyamide, polybenzimidazole, polyaramid, acrylic resin, phenol resin, polyester, polyetheretherketone (PEEK), polyolefin , Polypropylene or copolymers thereof, etc.), cellulose, carbon, cotton, wool, hemp, non-woven fabric, glass fiber or ceramic wool.
  • the thickness of the airgel sheet of the present invention is 3 mm or less, specifically 2 mm or less, more specifically 1 mm or less.
  • the thickness of the airgel sheet is thicker than the above range, there is a limit to the use of the ultra-thin insulating material in electronic products. If the thickness is thinner than the above range, the mechanical strength is very weak and durability may be deteriorated. .
  • the thickness of the composite heat-insulating sheet of the present invention is 3 mm or less, specifically 2 mm or less, more specifically 1 mm or less.
  • the thickness of the composite heat insulating sheet is thicker than the above range, it may be difficult to use it in an electronic product requiring an ultra-thin insulating material, and if it is thinner than the above range, the processability may be lowered.
  • the present invention provides a method for producing the above-mentioned composite insulation sheet.
  • the sol-free opaque coating layer can be formed by placing the fibers on a coating layer to which the release paper is adhered, followed by heat treatment.
  • the releasing paper means to protect the contact surface which comes into contact with the adhesive surface such as the adhesive tape, the adhesive paper or the label, and means to peel off the paper when it is used to achieve the purpose.
  • the use of the release paper is intended to prevent the airgel from being exposed to the surface of the airgel sheet.
  • the fiber sheet when a solution including a sol and a catalyst is impregnated on the other surface of the fiber sheet after forming a coating layer on one surface of the fiber sheet without using the release paper, the fiber sheet can impregnate all of the solution When the solution is excessive, an aerogel is formed on the surface of the coating layer by the sol flowing over the fiber sheet, so that the coating layer may be contaminated, and in this case, the coating layer for preventing generation of dust can not sufficiently serve .
  • a releasing paper including a coating material is prepared, a fiber is placed on the coating material, heat treatment is performed to form a coating layer on one side of the fiber sheet, And the surface of the coating layer is prevented from being contaminated by removing the release paper.
  • a wet gel sheet can be formed by impregnating the other surface of the fiber sheet with a sol and a catalyst, and gelling the impregnated sheet.
  • the catalyst of the present invention enhances the gelation by increasing the pH of the sol.
  • a basic catalyst may be used.
  • the basic catalyst examples include inorganic bases such as sodium hydroxide and potassium hydroxide; Or ammonium hydroxide.
  • inorganic bases such as sodium hydroxide and potassium hydroxide; Or ammonium hydroxide.
  • an organic base may be preferable since metal ions contained in the compound may be coordinated to the Si-OH compound.
  • the organic base is ammonium hydroxide (NH 4 OH), tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TPAH), tetrabutylammonium hydroxide (TBAH), methylamine, ethylamine, isopropylamine, monoisopropylamine, diethylamine, diisopropylamine, dibutylamine, trimethylamine, triethylamine, triisopropylamine, tributylamine, choline, (2-aminoethyl) ethanol, 2- (methylamino) ethanol, N-methyldiethanolamine, dimethylaminoethanol, diethylaminoethanol, nitrilotriethanol, 2 - (2-aminoethoxy) ethanol, 1-amino-2-propanol, triethanolamine, monopropanolamine or di
  • the present invention may further include a step of allowing the gel to be left at an appropriate temperature after the completion of the gelation reaction and aging the gel so that the chemical change is completely performed, thereby enhancing the mechanical stability. Thereafter, It is possible to hydrophobicize the surface to suppress the absorption of moisture in the air to maintain a low thermal conductivity.
  • the wet gel sheet can be dried to form an airgel sheet, and the drying can be performed by atmospheric pressure drying or supercritical drying.
  • one or more functional layers may be formed on the airgel sheet, thereby forming a composite heat insulating sheet including a sol-gel sheet having a sol-opaque coating layer formed on one surface thereof and a functional layer formed on the other surface thereof.
  • Polyethylene terephthalate (organic fiber) was placed on a polyamide film containing release paper and then heat treated at 150 ° C to prepare polyethylene terephthalate having a poly amide coating layer on one side.
  • HTEOS pre-hydrolyzed TEOS having a silica concentration of 20% was prepared by mixing tetraethyl orthosilicate with ethanol, water and HCl.
  • the HTEOS, ethanol and water were mixed in a weight ratio of 1: 2.25: (SiO 2 ) concentration of 4%.
  • the release paper was removed and allowed to stand for 1 hour at a temperature of 50 to 70 ⁇ using 80 to 90% ammonia solution (2 to 3 vol%) based on the volume of the silica sol. To 90% of hexamethyldisilazane (HMDS) solution (2 to 10 vol%) at a temperature of 50 to 70 ° C.
  • HMDS hexamethyldisilazane
  • a graphite sheet was attached to the airgel sheet as a thermal diffusion material to complete a composite heat insulating sheet.
  • a composite thermal insulation sheet was prepared in the same manner as in Example 1, except that Glass fiber (inorganic fiber) was used instead of polyethylene terephthalate (organic fiber) in Example 1.
  • a composite thermal insulation sheet was prepared in the same manner as in Example 1, except that the coating layer was not formed in Example 1.
  • a composite thermal insulation sheet was prepared in the same manner as in Example 2, except that the coating layer was not formed in Example 2.
  • Polyethylene terephthalate having a poly amide coating layer formed thereon was prepared according to the method of Example 1 above.
  • a glass fiber having a poly amide coating layer was prepared by the method of Example 2 above.
  • the polyethylene terephthalate sheet of Example 1 was prepared.
  • the glass fiber sheet of Example 2 was prepared.
  • Example 1 O Polyethylene terephthalate O Example 2 O Glass fiber O Comparative Example 1 O Polyethylene terephthalate X Comparative Example 2 O Glass fiber X Comparative Example 3 X Polyethylene terephthalate O Comparative Example 4 X Glass fiber O Comparative Example 5 X Polyethylene terephthalate X Comparative Example 6 X Glass fiber X
  • Weight reduction rate (%) [(Weight of first composite insulation sheet - Weight of composite insulation sheet after vibration test) / (Weight of first composite insulation sheet)] x 100
  • Example 1 Example 2 Comparative Example 1 Comparative Example 2 Weight reduction rate (%) 0.0 0.0 0.32 0.35
  • the composite heat-insulating sheet of the Examples showed no weight reduction, indicating that there was almost no dust generation.
  • thermo conductivity of each airgel sheet prepared in Examples 1 and 2 and Comparative Examples 1 and 2 and the sheets of Comparative Examples 3 to 6 was measured using a Heat Flow Meter (HFM) 456 instrument manufactured by NETZSCH Co., Are shown in Table 3 and Fig.
  • HFM Heat Flow Meter
  • Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Room temperature thermal conductivity (mW / mK, 25 ° C) 17.9 16.0 19.3 15.5 34.0 29.9 32.5 28.3
  • PET polyethylene terephthalate organic fibers not containing an airgel of Comparative Example 5 and GF (glass fiber) inorganic fibers containing no airgel of Comparative Example 6 were produced according to the present invention It is found that the heat insulation performance is not excellent only by the fiber sheet because the thermal conductivity is comparatively high.
  • the composite heat insulating sheets of Examples 1 and 2 of the present invention had extremely low thermal conductivity and excellent heat insulating performance.
  • the thermal conductivity of the present invention was higher than that of Comparative Examples 1 and 2 It is confirmed that the increase of the thermal conductivity due to the formation of the coating layer does not occur.
  • the composite heat insulating sheet of the present invention can secure low dust and high strength characteristics while preventing deterioration of heat insulating performance.

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Abstract

본 발명은 에어로겔을 포함한 복합 단열 시트 및 이의 제조방법에 관한 것으로서, 저분진, 고강도, 고단열의 특성을 갖는 초박형 에어로겔 복합 시트를 제공하여 전자 기기에 활용가능성을 높일 수 있다.

Description

에어로겔을 포함한 복합 단열 시트
관련출원과의 상호인용
본 출원은 2017년 11월 28일자 한국 특허 출원 제10-2017-0160077호에 기초한 우선권의 이익을 주장하며, 해당 한국 특허 출원의 문헌에 개시된 모든 내용은 본 명세서의 일부로서 포함된다.
기술분야
본 발명은 에어로겔을 포함한 복합 단열 시트 및 이의 제조방법에 관한 것이다.
노트북, OLED 또는 TV 등의 전자제품은 Heat Source에 의한 Hot Spot 이 존재하여 부분적으로 기기 표면으로 열 방출로 인해 소비자가 느끼는 감성 품질이 떨어질 수 있다. 또한 단순 단열재를 사용하여 외부로 적절히 확산시키지 못하는 경우, 과도하게 축적된 열로 인하여 시스템의 장애를 유발하고, 제품의 수명을 단축시키거나, 심한 경우에는 폭발 및 화재의 원인을 제공하기도 한다. 이러한 발열에 의한 문제를 해결하기 위해서 다양한 단열소재들이 적용되었으나, 현재까지도 두께가 얇고 단열 성능이 우수한 최적의 단열 소재가 개발되지 않아 단열에 대한 다양한 연구 및 기술 개발이 이루어지고 있다.
이러한 종래의 문제점들을 해결하기 위한 본 발명은 고효율 단열재 용도로 주목 받고 있는 Aerogel을 적용하여 상기 문제점을 해결하고자 한다.
에어로겔(aerogel)은 나노입자로 구성된 고다공성 물질로서, 높은 기공률과 비표면적, 그리고 낮은 열전도도를 가져 고효율의 단열재, 방음재 등의 용도로 주목 받고 있는 소재이다.
한편, 이러한 에어로겔은 다공성 구조로 인해 매우 낮은 기계적 강도를 갖기 때문에 기존의 단열섬유인 무기섬유 또는 유기섬유 등의 섬유에 에어로겔을 함침하여 결합시킨 에어로겔 복합체를 제조하여 사용하고 있는데, 상기 에어로겔 복합체는 섬유와 에어로겔의 부착력이 약하여 절단, 구부림 등의 가공과정에서 에어로겔 입자가 분리되어 Dust 발생 및 내구성이 저하되어 전자제품 등의 단열재로 적용하는 경우 기기 손상 등을 가져올 수 있다.
이에 본 발명은 상기 문제들을 해결하기 위하여 저분진, 고강도, 고단열의 특성을 갖는 에어로겔 복합 시트를 제공하여 전자 기기에 활용가능성을 높이고자 한다.
[선행기술문헌]
(특허문헌 1) US 8,021,583 B2 (2011.09.20)
본 발명의 해결하고자 하는 과제는 전자기기에 활용할 수 있도록 저분진, 고강도, 고단열의 특성을 갖는 초박형 복합 단열 시트 및 이의 제조방법을 제공하는 것이다.
본 발명은 에어로겔 시트,
상기 에어로겔 시트의 일면에 형성된 졸 불투과성 코팅층, 및
상기 에어로겔 시트의 타면에 형성된 1 이상의 기능성층을 포함하는 복합 단열 시트를 제공한다.
또한, 본 발명은 섬유 시트의 일면에 졸 불투과성 코팅층을 형성시키는 단계;
상기 섬유 시트의 타면에 졸 및 촉매를 함침시키는 단계;
상기 함침된 시트를 겔화시켜 습윤겔 시트를 형성하는 단계;
상기 습윤겔 시트를 건조시켜 에어로겔 시트를 형성하는 단계; 및
상기 에어로겔 시트에 1 이상의 기능성층을 형성시키는 단계를 포함하는 복합 단열 시트 제조방법을 제공한다.
본 발명의 복합 단열 시트에 의하면 일면에 형성된 졸 불투과성 코팅층에 의해 분진 발생이 저감되어 높은 단열 효율 및 가공 편이성을 제공할 수 있다.
또한, 본 발명의 복합 단열 시트에 의하면 상기 코팅층에 의해 기계적 강도가 개선되어 내구성이 증가할 수 있다.
또한, 본 발명의 복합 단열 시트에 의하면 기능성 층에 의해 필요한 기타 기능을 확보할 수 있다.
본 명세서에 첨부되는 다음의 도면은 본 발명의 구체적인 실시예를 예시하는 것이며, 전술한 발명의 내용과 함께 본 발명의 기술사상을 더욱 이해시키는 역할을 하는 것이므로, 본 발명은 그러한 도면에 기재된 사항에만 한정되어 해석되어서는 아니된다.
도 1은 실시예 및 비교예의 복합 단열 시트의 열전도도를 나타낸 그래프이다.
이하, 본 발명에 대한 이해를 돕기 위해 본 발명을 더욱 상세하게 설명한다. 이때, 본 명세서 및 청구범위에 사용된 용어나 단어는 통상적이거나 사전적인 의미로 한정해서 해석되어서는 아니 되며, 발명자는 그 자신의 발명을 가장 최선의 방법으로 설명하기 위해 용어의 개념을 적절하게 정의할 수 있다는 원칙에 입각하여 본 발명의 기술적 사상에 부합하는 의미와 개념으로 해석되어야만 한다.
일반적으로 전자제품들은 Heat Source에 의한 Hot Spot 이 존재하여 부분적으로 기기표면으로 열 방출이 발생하여 품질이 떨어질 수 있다. 이에 본 발명은 고효율 단열재로서 에어로겔 시트를 사용하고자 한다.
그러나, 상기 에어로겔 시트는 섬유와 에어로겔 간의 부착력이 약하여 절단, 구부림 등의 가공 과정에서 에어로겔 입자가 분리되는 등 분진 발생이 심하고, 강도가 약해 내구성이 저하되어 전자제품 등의 단열재로 적용에 한계가 있다.
이에 본 발명은 전자제품에 널리 활용할 수 있도록 저분진, 고강도, 고단열의 특성을 갖는 초박형 복합 단열 시트 및 이의 제조방법을 제공하는 것을 목적으로 한다.
이하, 본 발명의 복합 단열 시트 및 이의 제조방법을 상세히 설명하기로 한다.
본 발명은 에어로겔 시트,
상기 에어로겔 시트의 일면에 형성된 졸 불투과성 코팅층, 및
상기 에어로겔 시트의 타면에 형성된 1 이상의 기능성층을 포함하는 복합 단열 시트를 제공한다.
종래 문제였던 분진 발생을 저감시키기 위하여 본 발명의 복합 단열 시트는 에어로겔 시트 일면에 졸 불투과성 코팅층을 도입하는 것을 특징으로 한다.
구체적으로 상기 코팅층은 PA(Poly amide), PE(Poly Ethylene), PET(Poly Ethylene Terephthalate), PI(Polyimide) 및 실리콘으로 이루어진 군에서 선택된 1 이상을 포함하는 것을 특징으로 한다.
상기 코팅층은 특히 졸 불투과성인 것을 특징으로 한다. 본 발명의 코팅층은 에어로겔 시트 제조과정에서 졸이 유기 또는 무기섬유에 함침될 때 섬유를 투과하여 바깥으로 졸이 흐르는 것을 방지하여 에어로겔 시트 표면에 에어로겔이 노출되지 않게 함으로써, 저분진 특성을 구현할 수 있게 한다. 한편, 상기 코팅층이 형성되지 않은 다른 일면은 후술할 기능성층에 의해 에어로겔이 표면에 노출되는 것을 방지할 수 있다.
또한, 상기 코팅층은 다공성 구조로 인해 매우 낮은 에어로겔 시트의 기계적 강도를 보완하는 역할을 할 수 있다. 상기 코팅층은 복합 단열 시트의 기계적 강도를 증가시켜 내구성을 개선시킬 수 있다.
한편, 본 발명의 상기 졸 불투과성 코팅층의 두께는 30 ㎛ 이하, 보다 구체적으로는 10 내지 20 ㎛ 인 것을 특징으로 한다. 상기 졸 불투과성 코팅층의 두께가 상기 범위보다 두꺼운 경우, 복합 단열 시트의 단열 성능이 저하되는 문제가 있을 수 있으며, 초박형 단열재가 필요한 전자 제품에의 사용에 한계가 있을 수 있다. 반면, 상기 범위보다 얇은 경우, 기계적 강도 개선 효과가 미미하여 내구성이 좋지 않을 수 있다.
본 발명에 있어서, 상기 졸을 형성할 수 있는 물질은 지르코니아, 산화이트륨, 하프니아, 알루미나, 티타니아, 세리아, 실리카, 산화 마그네슘, 산화칼슘, 플루오르화 마그네슘 및 플루오르화 칼슘으로 이루어진 군에서 선택된 1 이상의 무기물질을 포함할 수 있다.
또한, 상기 실리카 졸의 경우 실리콘 함유 알콕사이드계 화합물을 포함할 수 있으며, 구체적으로는 테트라메틸 오르소실리케이트(tetramethyl orthosilicate; TMOS), 테트라에틸 오르소실리케이트(tetraethyl orthosilicate; TEOS), 전가수분해된 테트라에틸 오르소실리케이트 (Prehydrolyzed TEOS), 메틸트리에틸 오르소실리케이트(methyl triethyl orthosilicate), 디메틸디에틸 오르소실리케이트(dimethyl diethyl orthosilicate), 테트라프로필 오르소실리케이트(tetrapropyl orthosilicate), 테트라이소프로필 오르소실리케이트(tetraisopropyl orthosilicate), 테트라부틸 오르소실리케이트 (tetrabutyl orthosilicate), 테트라세컨드리부틸 오르소실리케이트(tetra secondary butyl orthosilicate), 테트라터셔리부틸 오르소실리케이트(tetra tertiary butyl orthosilicate), 테트라헥실오르소실리케이트(tetrahexyl orthosilicate), 테트라시클로헥실 오르소실리케이트(tetracyclohexyl orthosilicate), 테트라도데실 오르소실리케이트(tetradodecyl orthosilicate) 등과 같은 테트라알킬 실리케이트일 수 있다.
또한, 본 발명의 실리카 졸의 제조에 사용 가능한 알코올은 구체적으로 메탄올, 에탄올, 이소프로판올, 부탄올 등과 같은 1가 알코올; 또는 글리세롤, 에틸렌글리콜, 프로필렌글리콜, 디에틸렌글리콜, 디프로필렌글리콜, 및 솔비톨 등과 같은 다가 알코올일 수 있으며, 이들 중 어느 하나 또는 둘 이상의 혼합물이 사용될 수 있다. 이 중에서도 물 및 에어로겔과의 혼화성을 고려할 때 메탄올, 에탄올, 이소프로판올, 부탄올 등과 같은 탄소수 1 내지 6의 1가 알코올일 수 있다. 상기와 같은 알코올(극성 유기 용매)은 표면개질 반응을 촉진시키는 동시에 최종 제조되는 실리카 에어로겔에서의 소수화도를 고려하여 적절한 함량으로 사용될 수 있다.
또한, 본 발명의 복합 단열 시트는 상기 에어로겔 시트의 타면에 1 이상의 기능성층을 포함할 수 있다.
한편, 전자제품들은 단순 단열재를 사용하여 발생한 열을 외부로 적절히 확산시키지 못하는 경우, 과도하게 축적된 열로 인하여 시스템의 장애를 유발하고, 제품의 수명을 단축시키거나, 심한 경우에는 폭발 및 화재의 원인을 제공하기도 한다.
이에 본 발명은 복합 단열 시트의 졸 불투과성 코팅층이 형성되지 않은 다른 한 면에 기능성층을 적층함으로써, 획기적인 단열 성능을 가지면서도, Dust 발생이 없어 기기손상을 방지할 수 있고, 나아가 열확산 또는 절연층과 적층하여, 단열로 인한 기기 내의 열축적을 방지하여 기기 손상을 방지할 수 있는 구조적 특징을 가지는 복합 단열 시트를 제공하고자 한다.
구체적으로 상기 기능성층은 열확산, 절연, 흡음, 내진동, 물에 대해 불투과성 및 수증기에 대해 투과성으로 이루어진 군에서 선택된 1 이상의 기능을 나타낼 수 있으며, 본 발명의 복합 단열 시트는 이에 제한되지 않고 사용되는 전자제품에서 필요한 기능을 나타내는 기능성층을 포함할 수 있다.
한편, 상기 기능성층이 물에 대해 불투과성인 경우 본 발명의 복합 단열 시트는 전자 부품에 물이 침투하는 것을 방지하여 전자 부품의 손상을 방지할 수 있으며, 수증기에 대해 투과성인 경우, 전자 부품에 수증기가 응결되는 것을 방지하여 전자 부품의 손상을 방지할 수 있다. 상기 물에 대해 불투과성이고, 수증기에 대해 투과성인 층은 셀룰로오스 물질을 포함할 수 있다.
본 발명의 복합 단열 시트에 포함되는 에어로겔 시트에 있어서, 상기 시트는 무기섬유, 유기섬유 또는 이의 조합을 사용할 수 있다.
더 구체적으로 상기 시트는 필름, 시트, 네트, 섬유, 다공질체, 발포체, 부직포체 또는 이들의 2 층 이상의 적층체일 수 있다. 또한, 용도에 따라 그 표면에 표면조도가 형성되거나 패턴화된 것일 수도 있다. 상기 시트는 시트 내로 졸의 삽입이 용이한 공간 또는 공극을 포함함으로써 단열 성능을 보다 향상시킬 수 있는 섬유일 수 있다. 또, 본 발명의 시트는 낮은 열전도도를 갖는 것이 바람직할 수 있다.
구체적으로 본 발명에서 사용할 수 있는 섬유 시트는 폴리에틸렌 테레프탈레이트, 폴리아미드, 폴리벤즈이미다졸, 폴리아라미드, 아크릴수지, 페놀수지, 폴리에스테르, 폴리에테르에테르케톤(PEEK), 폴리올레핀(예를 들면, 폴리에틸렌, 폴리프로필렌 또는 이들의 공중합체 등), 셀룰로오스, 카본, 면, 모, 마, 부직포, 유리섬유 또는 세라믹울 등일 수 있다.
한편, 본 발명의 상기 에어로겔 시트의 두께는 3 mm 이하, 구체적으로는 2 mm 이하, 보다 구체적으로는 1 mm 이하인 것을 특징으로 한다. 상기 에어로겔 시트의 두께가 상기 범위보다 두꺼운 경우, 초박형 단열재가 필요한 전자 제품에의 사용에 한계가 있을 수 있으며, 상기 범위보다 얇은 경우, 기계적 강도가 매우 약해 내구성이 떨어질 수 있고, 단열 성능이 좋지 않을 수 있다.
또한, 본 발명의 상기 복합 단열 시트의 두께는 3 mm 이하, 구체적으로는 2 mm 이하, 보다 구체적으로는 1 mm 이하인 것을 특징으로 한다. 복합 단열 시트의 두께가 상기 범위보다 두꺼울 경우, 초박형 단열재가 필요한 전자제품에의 사용이 어려울 수 있으며, 상기 범위보다 얇은 경우 공정성이 떨어질 수 있다.
또한, 본 발명은 상기 복합 단열 시트 제조방법을 제공한다.
구체적으로, 본 발명의 복합 단열 시트 제조방법은,
섬유 시트의 일면에 졸 불투과성 코팅층을 형성시키는 단계;
상기 섬유 시트의 타면에 졸 및 촉매를 함침시키는 단계;
상기 함침된 시트를 겔화시켜 습윤겔 시트를 형성하는 단계;
상기 습윤겔 시트를 건조시켜 에어로겔 시트를 형성하는 단계; 및
상기 에어로겔 시트에 1 이상의 기능성층을 형성시키는 단계를 포함한다.
보다 구체적으로, 상기 졸 불투과성 코팅층은 이형지가 부착된 코팅층 상에 섬유를 위치시킨 뒤, 열처리를 하여 형성할 수 있다.
여기서, 이형지란 점착테이프, 접착지, 라벨 등 점착면에 접촉시켜 접촉된 면을 보호하는 것을 의미하고, 사용할 때는 벗겨내어 목적을 달성할 수 있도록 하는 것을 의미한다.
본 발명의 졸 불투과성 코팅층 형성 방법으로, 상기 이형지를 사용하는 것은 에어로겔 시트의 표면에 에어로겔이 노출되는 것을 원천적으로 방지하기 위해서이다.
구체적으로, 상기 이형지를 사용하지 않고, 단순히 섬유 시트의 일면에 코팅층을 형성한 이후, 상기 섬유 시트의 타면에 졸 및 촉매를 포함하는 용액을 함침시킬 경우, 섬유 시트가 상기 용액을 모두 함침할 수 없을 정도로 상기 용액이 과량일 때, 섬유 시트 바깥으로 흘러넘친 졸에 의해 상기 코팅층 표면에 에어로겔이 형성되어 코팅층이 오염될 수 있고, 이 경우 분진 발생을 방지하는 코팅층의 역할을 충분히 할 수 없기 때문이다.
따라서, 본 발명의 복합 단열 시트 제조방법은 코팅물질을 포함한 이형지를 준비한 뒤, 상기 코팅물질 상에 섬유를 위치시킨 뒤, 열처리를 하여 섬유 시트의 일면에 코팅층을 형성한 이후, 겔화 완료 후에 코팅층에 부착되어 있는 이형지를 제거하여 상기 코팅층 표면의 오염을 방지하는 것을 특징으로 한다.
이후, 상기 섬유 시트의 타면에 졸 및 촉매를 함침시키키고, 상기 함침된 시트를 겔화시켜 습윤겔 시트를 형성할 수 있다.
본 발명의 상기 촉매는 졸의 pH를 증가시켜 겔화를 촉진하는 역할을 수행하며, 구체적으로 염기성 촉매를 사용할 수 있다.
상기 염기성 촉매로는 수산화나트륨, 수산화칼륨 등의 무기 염기; 또는 수산화암모늄과 같은 유기 염기를 들 수 있으나, 무기 염기의 경우 화합물 내 포함된 금속 이온이 Si-OH 화합물에 배위(coordination)될 우려가 있으므로, 유기 염기가 바람직할 수 있다. 구체적으로 상기 유기 염기는 수산화암모늄(NH4OH), 테트라메틸암모늄 히드록시드(TMAH), 테트라에틸암모늄 히드록시드(TEAH), 테트라프로필암모늄 히드록시드(TPAH), 테트라부틸암모늄 히드록시드(TBAH), 메틸아민, 에틸아민, 이소프로필아민, 모노이소프로필아민, 디에틸아민, 디이소프로필아민, 디부틸아민, 트리메틸아민, 트리에틸아민, 트리이소프로필아민, 트리부틸아민, 콜린, 모노에탄올아민, 디에탄올아민, 2-아미노에탄올, 2-(에틸 아미노)에탄올, 2-(메틸 아미노)에탄올, N-메틸 디에탄올아민, 디메틸아미노에탄올, 디에틸아미노에탄올, 니트릴로트리에탄올, 2-(2-아미노에톡시)에탄올, 1-아미노-2-프로판올, 트리에탄올아민, 모노프로판올아민, 또는 디부탄올아민 등을 들 수 있으며, 이들 중 어느 하나 또는 둘 이상의 혼합물이 사용될 수 있다. 보다 구체적으로 본 발명의 경우 상기 염기는 수산화암모늄(NH4OH)일 수 있다.
한편, 본 발명은 상기 겔화 반응 완료 이후, 상기 겔을 적당한 온도에서 방치하여 화학적 변화가 완전히 이루어지도록 숙성하는 단계를 더 포함하여 기계적 안정성을 강화시킬 수 있으며, 이후, 표면개질 단계를 더 포함하여 겔 표면을 소수화시켜 공기 중의 수분 흡수를 억제시켜 낮은 열전도도를 유지하게 할 수 있다.
이후, 상기 습윤겔 시트를 건조시켜 에어로겔 시트를 형성할 수 있으며, 상기 건조는 상압건조 또는 초임계 건조에 의할 수 있다.
마지막으로 상기 에어로겔 시트에 1 이상의 기능성층을 형성시킬 수 있으며, 이를 통해 졸 불투과성 코팅층이 일면에 형성되고, 기능성층이 타면에 형성된 에어로겔 시트를 포함하는 복합 단열 시트를 제조할 수 있다.
이하, 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 용이하게 실시할 수 있도록 본 발명의 실시예에 대하여 상세히 설명한다. 그러나 본 발명은 여러 가지 상이한 형태로 구현될 수 있으며 여기에서 설명하는 실시예에 한정되지 않는다.
실시예 1
이형지가 포함된 Polyamide필름 위에 폴리에틸렌 테레프탈레이트(유기섬유)를 위치시킨 뒤 150 ℃ 에서 열처리하여 일면에 Poly amide 코팅층이 형성된 폴리에틸렌 테레프탈레이트를 제조하였다.
이후, 테트라에틸오르소실리케이트와 에탄올, 물, HCl을 혼합하여 실리카 농도 20 %의 Pre-hydrolyzed TEOS(HTEOS)를 제조하였고, 상기 HTEOS, 에탄올 및 물을 1:2.25:0.35의 중량비로 혼합하여 실리카(SiO2) 농도 4 %의 실리카 졸을 제조하였다.
폴리에틸렌 테레프탈레이트의 Poly amide 코팅층이 형성되지 않은 타면에 상기 실리카 졸과 염기 촉매 용액을 (에탄올:암모니아수 = 210:1의 중량비로 혼합하고 HTEOS 대비 0.44중량%)분사한 뒤, 겔화를 유도하여 습윤겔 시트를 제조하였다. 겔화 완료 시까지는 10 분 정도 소요되었다. 한편, 이때 상기 실리카 졸은 상기 코팅층을 통과하지 못하는 것을 확인할 수 있었다. 겔화 완료 후 상기 이형지를 제거하고, 실리카 졸 부피 대비 80 내지 90 %의 암모니아 용액(2 ~ 3 vol%)을 이용하여 50 내지 70 ℃의 온도에서 1 시간 방치하여 숙성시킨 뒤, 실리카 졸 부피 대비 80 내지 90 %의 헥사메틸디실라잔(HMDS) 용액(2 ~ 10 vol%)을 이용하여 50 내지 70 ℃의 온도에서 4 시간 동안 방치하여 소수화 반응을 진행하였다. 소수화 반응이 끝나면 7.2 L 초임계 추출기(extractor)에 상기 습윤겔 시트를 넣고 CO2 를 주입하고, 50 ℃, 100 bar 도달 시 0.4 L/min의 속도로 CO2를 주입하여 에탄올을 추출하여 건조하였다. 건조가 끝난 후 CO2 를 배출(venting) 하여 에어로겔 시트를 제조하였다.
상기 에어로겔 시트에 열확산 소재로써 그라파이트 시트를 부착하여 복합 단열 시트를 완성하였다.
실시예 2
상기 실시예 1에서 폴리에틸렌 테레프탈레이트(유기섬유) 대신 Glass fiber(무기섬유)를 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 복합 단열 시트를 제조하였다.
비교예 1
상기 실시예 1에서 코팅층을 형성하지 않는 것을 제외하고는 실시예 1과 동일한 방법으로 복합 단열 시트를 제조하였다.
비교예 2
상기 실시예 2에서 코팅층을 형성하지 않는 것을 제외하고는 실시예 2와 동일한 방법으로 복합 단열 시트를 제조하였다.
비교예 3
상기 실시예 1의 방법으로 Poly amide 코팅층이 형성된 폴리에틸렌 테레프탈레이트를 제조하였다.
비교예 4
상기 실시예 2의 방법으로 Poly amide 코팅층이 형성된 Glass fiber를 제조하였다.
비교예 5
상기 실시예 1의 폴리에틸렌 테레프탈레이트 시트를 준비하였다.
비교예 6
상기 실시예 2의 Glass fiber 시트를 준비하였다.
에어로겔 포함 여부 섬유 종류 코팅층 포함 여부
실시예 1 O 폴리에틸렌 테레프탈레이트 O
실시예 2 O Glass fiber O
비교예 1 O 폴리에틸렌 테레프탈레이트 X
비교예 2 O Glass fiber X
비교예 3 X 폴리에틸렌 테레프탈레이트 O
비교예 4 X Glass fiber O
비교예 5 X 폴리에틸렌 테레프탈레이트 X
비교예 6 X Glass fiber X
실험예 1: 분진 발생량 측정
상기 실시예 1 및 2 및 비교예 1 및 2에서 제조한 각 복합 단열 시트를 12 cm x 12 cm 가 되도록 절단하여 샘플을 제조한 뒤, 자체 제작한 진동시험기(ASTMC592-04)를 이용하여 진동 조건을 24 Hz/3mm, 6 hrs 로 하여 진동에 의한 무게 감소율을 측정하여 그 결과를 하기 표 2에 나타내었다.
* 무게 감소율(%) = [(최초 복합 단열 시트 무게 - 진동 실험 후 복합 단열 시트 무게)/(최초 복합 단열 시트 무게)] x 100
실시예 1 실시예 2 비교예 1 비교예 2
무게 감소율(%) 0.0 0.0 0.32 0.35
상기 표 2에서 보는 바와 같이, 실시예의 복합 단열 시트는 무게 감소가 없는 것으로 보아 분진 발생량이 거의 없음을 알 수 있었다.
이는 본 발명의 복합 단열 시트에 포함된 에어로겔 시트의 일면에 형성된 졸 불투과성 코팅층에 의한 것임을 예상할 수 있었다.
실험예 2: 열전도도 측정
상기 실시예 1 및 2 및 비교예 1 및 2에서 제조한 각 에어로겔 시트 및 비교예 3 내지 6의 시트에 대해 NETZSCH社의 Heat Flow Meter(HFM) 456장비를 이용하여 상온 열전도도를 측정하여 그 결과를 하기 표 3 및 도 1에 나타내었다.
실시예 1 실시예 2 비교예 1 비교예 2 비교예 3 비교예 4 비교예 5 비교예 6
상온 열전도도(㎽/mK, 25 ℃) 17.9 16.0 19.3 15.5 34.0 29.9 32.5 28.3
상기 표 3 및 도 1에서 보는 바와 같이, 비교예 5의 에어로겔을 포함하지 않은 PET(폴리에틸렌 테레프탈레이트) 유기섬유 및 비교예 6의 에어로겔을 포함하지 않은 GF(Glass fiber) 무기섬유는 본 발명의 실시예 대비 열전도도가 매우 높아 섬유 시트 만으로는 단열 성능이 우수하지 않은 것을 알 수 있었다.
한편, 상기 비교예 5 및 6 각각에 코팅층을 형성한 비교예 3 및 4의 경우, 열전도도가 오히려 증가하여 단열 성능이 저하되는 것을 알 수 있었다.
반면, 본 발명의 실시예 1 및 2의 복합 단열 시트는 열전도도가 매우 낮아 단열 성능이 우수한 것을 확인할 수 있었으며, 상기 본 발명의 열전도도는 코팅층을 형성하지 않은 비교예 1 및 2 와 비교하여 그와 동등하거나 오히려 더 낮은 것으로 보아 코팅층 형성으로 인한 열전도도의 상승은 일어나지 않음을 확인할 수 있었다.
이를 통해 본 발명의 복합 단열 시트는 단열 성능의 저하를 방지하면서 저분진, 고강도 특성을 확보할 수 있음을 알 수 있었다.
전술한 본 발명의 설명은 예시를 위한 것이며, 본 발명이 속하는 기술분야의 통상의 지식을 가진 자는 본 발명의 기술적 사상이나 필수적인 특징을 변경하지 않고서 다른 구체적인 형태로 쉽게 변형이 가능하다는 것을 이해할 수 있을 것이다. 그러므로 이상에서 기술한 실시예들은 모든 면에서 예시적인 것이며 한정적이 아닌 것으로 이해해야만 한다.

Claims (12)

  1. 에어로겔 시트,
    상기 에어로겔 시트의 일면에 형성된 졸 불투과성 코팅층, 및
    상기 에어로겔 시트의 타면에 형성된 1 이상의 기능성층을 포함하는 것인 복합 단열 시트.
  2. 제1항에 있어서,
    상기 코팅층은 PA(Poly amide), PE(Poly Ethylene), PET(Poly Ethylene Terephthalate), PI(Polyimide) 및 실리콘으로 이루어진 군에서 선택된 1 이상을 포함하는 것을 특징으로 하는 복합 단열 시트.
  3. 제1항에 있어서,
    상기 졸은 지르코니아, 산화이트륨, 하프니아, 알루미나, 티타니아, 세리아, 실리카, 산화 마그네슘, 산화칼슘, 플루오르화 마그네슘 및 플루오르화 칼슘으로 이루어진 군에서 선택된 1 이상을 포함하는 것을 특징으로 하는 복합 단열 시트.
  4. 제1항에 있어서,
    상기 기능성층은 열확산, 절연, 흡음, 내진동, 물에 대해 불투과성 및 수증기에 대해 투과성으로 이루어진 군에서 선택된 1 이상의 기능을 나타내는 것을 특징으로 하는 복합 단열 시트.
  5. 제1항에 있어서,
    상기 시트는 무기섬유, 유기섬유 또는 이들의 조합인 것을 특징으로 하는 복합 단열 시트.
  6. 제1항에 있어서,
    상기 졸 불투과성 코팅층의 두께는 30 ㎛ 이하인 것을 특징으로 하는 복합 단열 시트.
  7. 제1항에 있어서,
    상기 에어로겔 시트의 두께는 2 mm 이하인 것을 특징으로 하는 복합 단열 시트.
  8. 제1항에 있어서,
    상기 복합 단열 시트의 두께는 3 mm 이하인 것을 특징으로 하는 복합 단열 시트.
  9. 섬유 시트의 일면에 졸 불투과성 코팅층을 형성시키는 단계;
    상기 섬유 시트의 타면에 졸 및 촉매를 함침시키는 단계;
    상기 함침된 시트를 겔화시켜 습윤겔 시트를 형성하는 단계;
    상기 습윤겔 시트를 건조시켜 에어로겔 시트를 형성하는 단계; 및
    상기 에어로겔 시트에 1 이상의 기능성층을 형성시키는 단계를 포함하는 복합 단열 시트 제조방법.
  10. 제9항에 있어서,
    상기 복합 단열 시트는 졸 불투과성 코팅층이 일면에 형성되고, 기능성층이 타면에 형성된 에어로겔 시트를 포함하는 것을 특징으로 하는 복합 단열 시트 제조방법.
  11. 제9항에 있어서,
    상기 졸 불투과성 코팅층은 이형지가 부착된 코팅층 상에 섬유를 위치시킨 뒤, 열처리를 하여 섬유 시트의 일면에 형성시키는 것을 특징으로 하는 복합 단열 시트 제조방법.
  12. 제11항에 있어서,
    상기 상기 이형지는 겔화 완료 이후 코팅층에서 제거하는 단계를 더 포함하는 것을 특징으로 하는 복합 단열 시트 제조방법.
PCT/KR2018/009608 2017-11-28 2018-08-21 에어로겔을 포함한 복합 단열 시트 WO2019107706A1 (ko)

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JP2019570394A JP7042287B2 (ja) 2017-11-28 2018-08-21 エアロゲルを含む複合断熱シート
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