KR20220138183A - Method for preparing binder-free boron nitride film and thermal management material comprising boron nitride film prepared thereby - Google Patents
Method for preparing binder-free boron nitride film and thermal management material comprising boron nitride film prepared thereby Download PDFInfo
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 129
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims abstract description 30
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- 239000002245 particle Substances 0.000 claims abstract description 43
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 230000017525 heat dissipation Effects 0.000 claims abstract description 21
- 238000005266 casting Methods 0.000 claims abstract description 8
- 206010040844 Skin exfoliation Diseases 0.000 claims description 20
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- 238000004299 exfoliation Methods 0.000 claims description 8
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 239000011370 conductive nanoparticle Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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Abstract
Description
본 발명은 바인더 무첨가 질화붕소 필름의 제조 방법 및 이에 따라 제조되는 질화붕소 필름을 포함하는 방열 재료에 관한 것으로서, 보다 상세하게는 방열소재 단일 물질인 질화붕소 단일 물질로 구성되는 질화붕소 슬러리를 이용하여 질화붕소 필름을 제조하는 기술에 관한 것이다. The present invention relates to a method for producing a binder-free boron nitride film and a heat dissipation material including a boron nitride film produced thereby, and more particularly, using a boron nitride slurry composed of a single material, boron nitride, which is a single material for a heat dissipation material. It relates to a technique for producing a boron nitride film.
전자 기기의 고기능화, 소형 박형화의 요구에 따른 전자 및 반도체 소자의 방열 문제는 내구성 및 성능에 영향을 미쳐 제품 전체에 기능을 저하시키는 원인으로 지목되고 있다. 이에 따라, 전자 및 반도체 소자에서 발생하는 열을 외부로 방출하는 기술은 전자 및 반도체 소자의 성능과 장기 수명 특성을 확보하는데 중요한 이슈가 되고 있다.The problem of heat dissipation of electronic and semiconductor devices according to the demand for high-functionality and miniaturization of electronic devices has been pointed out as a cause of deterioration of the overall function of the product by affecting durability and performance. Accordingly, technology for emitting heat generated from electronic and semiconductor devices to the outside has become an important issue in securing performance and long-term lifespan characteristics of electronic and semiconductor devices.
이를 위해 방열 부재로 열 전도성 필름, 열전도성 시트, 열전도성 스페이서, 액상 용액에 열전도성 무기 분말이 충전된 열전도성 페이스트, 경화성 물질에 열전도성 무기 분말이 충전된 열전도성 접착제 등이 제시되어 오고 있다.For this purpose, a thermally conductive film, thermally conductive sheet, thermally conductive spacer, thermally conductive paste filled with thermally conductive inorganic powder in a liquid solution, thermally conductive adhesive in which a curable material is filled with thermally conductive inorganic powder, etc. have been proposed as heat dissipation members. .
이들 중 물질의 계면 간의 열 접촉저항을 줄이면서 동시에 높은 열전도율로 전자기기의 방열 기능을 최대화 시킬 수 있는 열 계면 물질(Thermal Interface Material; TIM)은 통상 열전도성 필러와 접착을 도와주는 고분자 계열의 바인더로 이루어진 복합 소재로 이루어져 있다. TIM에서 내부 열전도성 필러로는 구리, 은과 같은 전도성 나노 입자들로 구성되어 있으며, 내재된 열전도도 자체는 높으나 나노입자로 구성되어 그 특성이 저하되고 산화에 취약한 단점이 있다. 또한, 계면을 채우기 위한 유변학적 특성을 확보하기 위해 추가적인 고분자 바인더가 첨가되는데, 이러한 바인더는 열전도율을 저하시켜 TIM의 성능 자체를 저하시키고, 또한 주기적인 온도 변화로 인한 복합소재 내부의 변형 문제도 야기된다.Among them, the Thermal Interface Material (TIM), which can maximize the heat dissipation function of electronic devices with high thermal conductivity while reducing the thermal contact resistance between the interfaces of materials, is a polymer-based binder that helps adhesion with a thermally conductive filler. It is made of a composite material made of The internal thermally conductive filler in the TIM is composed of conductive nanoparticles such as copper and silver, and although the internal thermal conductivity itself is high, it is composed of nanoparticles, so its properties are deteriorated and it is vulnerable to oxidation. In addition, an additional polymer binder is added to secure the rheological properties to fill the interface, which lowers the thermal conductivity and lowers the performance of the TIM itself, and also causes the problem of deformation inside the composite material due to periodic temperature change. do.
한편, 육방정계 질화붕소(Hexagonal boron nitride, hBN, BN) 입자는 흑연 유사의 층 형상 구조를 갖고, 열전도성, 전기 절연성, 화학적 안정성, 고체 윤활성, 내열 충격성 등의 특성이 우수하기 때문에, 이들의 특성을 살려서 절연 방열계, 고체 윤활제, 고체 이형제, hBN 소결체 제조용 원료 등으로서 사용하고 있다.On the other hand, hexagonal boron nitride (hBN, BN) particles have a graphite-like layered structure, and have excellent properties such as thermal conductivity, electrical insulation, chemical stability, solid lubrication, and thermal shock resistance. Taking advantage of its characteristics, it is used as an insulating heat dissipation system, a solid lubricant, a solid mold release agent, and a raw material for manufacturing hBN sintered compacts.
다만, hBN의 층상구조가 박리되지 않은 벌크 입자는 입자간의 결합력이 적어 그 자체로는 분말로서 존재하는데 이는 단독적으로는 TIM으로 가공되기가 어렵고 추가적인 고분자 바인더가 존재하여야만 기계적, 유변학적 특성이 확보된다. 이러한 접근은 전체적인 열전도율을 저하시키는 원인이 되기 때문에 바인더의 사용을 최소화하면서 TIM을 제조하는 기술이 필요하다. However, bulk particles in which the layered structure of hBN is not exfoliated have low bonding strength between the particles and exist as a powder by themselves. . Since this approach causes a decrease in the overall thermal conductivity, a technique for manufacturing the TIM while minimizing the use of a binder is required.
본 발명의 목적은 방열소재 단일 물질 특히, 질화붕소 단일 물질로 구성되는 질화붕소 슬러리와, 이를 포함하여 열 특성 및 유변학적 특성이 열 계면 물질(TIM)로서 사용되기 적합한 방열 페이스트(paste)를 제공하고자 한다.An object of the present invention is to provide a heat dissipation paste suitable for use as a thermal interface material (TIM) having thermal properties and rheological properties including a boron nitride slurry composed of a single heat dissipation material, in particular, a single boron nitride material want to
본 발명의 실시예에 따른 바인더 무첨가 질화붕소 필름의 제조 방법은 유성 볼 밀링(planetary ball milling)을 이용하여 육방정 질화붕소 입자를 드라이 볼 밀링(dry ball milling)하여 1차 박리하는 단계, 상기 1차 박리된 질화붕소 입자를 볼 밀링(wet ball milling)하여 2차 박리하는 단계, 상기 2차 박리된 질화붕소 입자를 종횡비에 따라 선별하여 질화붕소 슬러리를 형성하는 단계 및 상기 질화붕소 슬러리를 주조하는 단계를 포함한다.The method for producing a binder-free boron nitride film according to an embodiment of the present invention comprises the steps of first peeling the hexagonal boron nitride particles by dry ball milling using planetary ball milling; Secondary exfoliation by performing wet ball milling of the secondary exfoliated boron nitride particles, forming a boron nitride slurry by selecting the secondary exfoliated boron nitride particles according to the aspect ratio, and the boron nitride slurry including casting.
본 발명의 실시예에 따른 바인더 무첨가 질화붕소 필름의 제조 방법에 따라 제조되는 질화붕소 필름을 포함하는 방열 재료에 있어서, 상기 바인더 무첨가 질화붕소 필름의 제조 방법은 유성 볼 밀링(planetary ball milling)을 이용하여 육방정 질화붕소 입자를 드라이 볼 밀링(dry ball milling)하여 1차 박리하는 단계, 상기 1차 박리된 질화붕소 입자를 볼 밀링(wet ball milling)하여 2차 박리하는 단계, 상기 2차 박리된 질화붕소 입자를 종횡비에 따라 선별하여 질화붕소 슬러리를 형성하는 단계 및 상기 질화붕소 슬러리를 주조하는 단계를 포함한다.In the heat dissipation material comprising a boron nitride film manufactured according to the method for manufacturing a binder-free boron nitride film according to an embodiment of the present invention, the method for manufacturing the binder-free boron nitride film uses planetary ball milling to dry ball milling the hexagonal boron nitride particles to perform primary exfoliation, performing secondary exfoliation by performing wet ball milling of the primary exfoliated boron nitride particles, the secondary Forming a boron nitride slurry by screening the exfoliated boron nitride particles according to an aspect ratio, and casting the boron nitride slurry.
본 발명의 실시예에 따르면, 고분자 첨가제 없이 높은 열전도율과 고온 안정성, 높은 점도, 다양한 열 전도도의 종횡비를 가지는 질화붕소 슬러리를 제작할 수 있다. 또한, 본 발명의 실시예에 따라서 제조되는 질화붕소 슬러리를 전자기기 간의 접촉 계면에 주조(casting)하였을 때 전자 부품의 작동온도를 낮추어 성능 및 수명을 효율적으로 증진시킬 수 있으며, 열적 안정성이 뛰어난 방열 도료로도 활용이 가능하다. According to an embodiment of the present invention, a boron nitride slurry having high thermal conductivity, high temperature stability, high viscosity, and various thermal conductivity aspect ratios can be prepared without a polymer additive. In addition, when the boron nitride slurry prepared according to the embodiment of the present invention is cast on the contact interface between electronic devices, the operating temperature of electronic components can be lowered to effectively improve performance and lifespan, and heat dissipation with excellent thermal stability It can also be used as a paint.
도 1은 본 발명의 실시예에 따른 바인더 무첨가 질화붕소 필름의 제조 방법에 대한 동작 흐름도를 도시한 것이다.
도 2는 본 발명의 실시예에 따른 질화붕소 슬러리를 형성하는 과정을 설명하기 위해 도시한 것이다.
도 3은 본 발명의 실시예에 따른 볼 밀링의 횟수에 따른 결합력 및 점도의 실험 결과를 도시한 것이다.
도 4는 본 발명의 실시예에 따른 질화붕소 슬러리의 주조 예를 도시한 것이다.
도 5a 및 도 5b는 본 발명의 실시예에 따른 질화붕소 슬러리 및 질화붕소 필름에 대한 실험 결과를 도시한 것이다.
도 6은 본 발명의 실시예에 따른 질화붕소 슬러리의 방열효과를 검증하기 위한 실험 결과를 도시한 것이다.1 shows an operation flow diagram for a method of manufacturing a binder-free boron nitride film according to an embodiment of the present invention.
2 is a view illustrating a process of forming a boron nitride slurry according to an embodiment of the present invention.
3 shows experimental results of binding force and viscosity according to the number of ball milling according to an embodiment of the present invention.
Figure 4 shows a casting example of a boron nitride slurry according to an embodiment of the present invention.
5A and 5B show experimental results for a boron nitride slurry and a boron nitride film according to an embodiment of the present invention.
6 shows experimental results for verifying the heat dissipation effect of the boron nitride slurry according to an embodiment of the present invention.
본 발명의 이점 및 특징, 그리고 그것들을 달성하는 방법은 첨부되는 도면과 함께 상세하게 후술되어 있는 실시예들을 참조하면 명확해질 것이다. 그러나, 본 발명은 이하에서 개시되는 실시예들에 한정되는 것이 아니라 서로 다른 다양한 형태로 구현될 것이며, 단지 본 실시예들은 본 발명의 개시가 완전하도록 하며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 발명의 범주를 완전하게 알려주기 위해 제공되는 것이며, 본 발명은 청구항의 범주에 의해 정의될 뿐이다.Advantages and features of the present invention and methods of achieving them will become apparent with reference to the embodiments described below in detail in conjunction with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but will be embodied in various different forms, and only these embodiments allow the disclosure of the present invention to be complete, and common knowledge in the art to which the present invention pertains It is provided to fully inform those who have the scope of the invention, and the present invention is only defined by the scope of the claims.
본 명세서에서 사용된 용어는 실시예들을 설명하기 위한 것이며, 본 발명을 제한하고자 하는 것은 아니다. 본 명세서에서, 단수형은 문구에서 특별히 언급하지 않는 한 복수형도 포함한다. 명세서에서 사용되는 "포함한다(comprises)" 및/또는 "포함하는(comprising)"은 언급된 구성요소, 단계, 동작 및/또는 소자는 하나 이상의 다른 구성요소, 단계, 동작 및/또는 소자의 존재 또는 추가를 배제하지 않는다.The terminology used herein is for the purpose of describing the embodiments, and is not intended to limit the present invention. In this specification, the singular also includes the plural unless specifically stated otherwise in the phrase. As used herein, "comprises" and/or "comprising" refers to the presence of one or more other components, steps, operations and/or elements mentioned. or addition is not excluded.
다른 정의가 없다면, 본 명세서에서 사용되는 모든 용어(기술 및 과학적 용어를 포함)는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 공통적으로 이해될 수 있는 의미로 사용될 수 있을 것이다. 또한, 일반적으로 사용되는 사전에 정의되어 있는 용어들은 명백하게 특별히 정의되어 있지 않는 한 이상적으로 또는 과도하게 해석되지 않는다.Unless otherwise defined, all terms (including technical and scientific terms) used herein may be used with the meaning commonly understood by those of ordinary skill in the art to which the present invention belongs. In addition, terms defined in a commonly used dictionary are not to be interpreted ideally or excessively unless clearly specifically defined.
이하, 첨부한 도면들을 참조하여, 본 발명의 바람직한 실시예들을 보다 상세하게 설명하고자 한다. 도면 상의 동일한 구성요소에 대해서는 동일한 참조 부호를 사용하고 동일한 구성요소에 대해서 중복된 설명은 생략한다.Hereinafter, preferred embodiments of the present invention will be described in more detail with reference to the accompanying drawings. The same reference numerals are used for the same components in the drawings, and repeated descriptions of the same components are omitted.
본 발명의 실시예들은, 방열소재 단일 물질인 질화붕소 단일 물질로 구성되는 질화붕소 슬러리를 형성하며, 이를 포함하여 열 특성 및 유변학적 특성이 열 계면 물질(TIM)로서 사용되기 적합한 방열 페이스트(paste)를 제공하는 것을 그 요지로 한다.Embodiments of the present invention form a boron nitride slurry composed of a single material, boron nitride, which is a single material for heat dissipation, and thermal properties and rheological properties including this are suitable for use as a thermal interface material (TIM). ) to provide the gist of it.
이를 위해, 본 발명의 실시예들은 육방정 질화붕소 입자를 적정 용매와 유성 볼 밀링 시스템을 이용하여 드라이 밀링 방식 및 밀링 방식으로 박리하며, 질화붕소의 판상 표면과 첨가 용매의 표면 에너지 차이를 이용한 다양한 유변학적 특성을 통해 질화붕소 슬러리를 제조한다. 본 발명의 실시예에 따라서 제조되는 질화붕소 슬러리는 방열특성 및 내열특성을 이용한 열 계면 물질, 방열 도료 등의 여러 분야에 적용 가능하다. To this end, in the embodiments of the present invention, the hexagonal boron nitride particles are exfoliated by dry milling method and milling method using an appropriate solvent and planetary ball milling system, and the difference in surface energy between the plate-shaped surface of boron nitride and the added solvent is measured. A boron nitride slurry is prepared through the various rheological properties used. The boron nitride slurry prepared according to an embodiment of the present invention can be applied to various fields such as a thermal interface material using heat dissipation characteristics and heat resistance characteristics, and a heat dissipation paint.
이하에서는 도 1 내지 도 6을 참조하여 전술한 본 발명의 실시예들에 대해 상세히 설명한다. Hereinafter, the embodiments of the present invention described above with reference to FIGS. 1 to 6 will be described in detail.
도 1은 본 발명의 실시예에 따른 바인더 무첨가 질화붕소 필름의 제조 방법에 대한 동작 흐름도를 도시한 것이다. 또한, 도 2는 본 발명의 실시예에 따른 질화붕소 슬러리를 형성하는 과정을 설명하기 위해 도시한 것이고, 도 3은 본 발명의 실시예에 따른 볼 밀링의 횟수에 따른 결합력 및 점도의 실험 결과를 도시한 것이며, 도 4는 본 발명의 실시예에 따른 질화붕소 슬러리의 주조 예를 도시한 것이다.1 shows an operation flow diagram for a method of manufacturing a binder-free boron nitride film according to an embodiment of the present invention. In addition, Figure 2 is shown to explain the process of forming a boron nitride slurry according to an embodiment of the present invention, Figure 3 is a test result of bonding force and viscosity according to the number of ball milling according to an embodiment of the
도 1을 참조하면, 단계 S110에서, 유성 볼 밀링(planetary ball milling)을 이용하여 육방정 질화붕소 입자를 드라이 볼 밀링(dry ball milling)하여 1차 박리한다. Referring to FIG. 1 , in step S110 , the hexagonal boron nitride particles are dry ball milled using planetary ball milling to perform primary exfoliation.
단계 S110은 육방정 질화붕소 입자를 용매 없이 드라이 볼 밀링하여 1차 박리할 수 있다.In step S110, the hexagonal boron nitride particles may be first peeled by dry ball milling without a solvent.
육방정 질화붕소(Hexagonal boron nitride) 입자는 2차원 구조를 갖는 물질로서, 붕소 원자와 질소 원자의 육각 배열로 이루어진 물질이다. 육방정 질화붕소 입자는 약 5.9eV의 큰 밴드갭으로 인해 전기적 절연특성을 가지는 물리적 및 기계적으로 안정한 물질로 알려져 있다. 또한, 육방정 질화붕소 입자는 반데르발스 힘(van der Waals force)에 의해 적층(또는 재적층)되려는 특성을 갖는 물질이다.Hexagonal boron nitride (Hexagonal boron nitride) particles are a material having a two-dimensional structure, a material consisting of a hexagonal arrangement of boron atoms and nitrogen atoms. Hexagonal boron nitride particles are known as physically and mechanically stable materials having electrical insulating properties due to their large band gap of about 5.9 eV. In addition, the hexagonal boron nitride particles are a material having a property to be stacked (or re-stacked) by van der Waals force.
육방정 질화붕소의 결정은 흑연과 유사한 육각방면의 적층 구조를 가지므로 매우 단단한 결합을 형성하며, 윤활성을 갖는다. 육방정 질화붕소는 원자 번호가 낮은 원소의 공유결합 물질로서 높은 열전도성을 가지며, 융점을 가지지 않고, 약 3000℃에서 승화되어 고온에서 높은 안정성을 가진다. 또한, 전기 저항이 매우 높아 1000℃를 넘는 고온 영역에서 100Ω 내지 110Ω, 예컨대 105Ω의 저항을 가지는 것일 수 있다. Hexagonal boron nitride crystals have a hexagonal lamination structure similar to graphite, so they form a very hard bond and have lubricity. Hexagonal boron nitride is a covalent material of an element with a low atomic number, has high thermal conductivity, does not have a melting point, and is sublimated at about 3000° C. and has high stability at high temperatures. In addition, the electrical resistance is very high, and may have a resistance of 100Ω to 110Ω, for example, 105Ω in a high temperature region exceeding 1000°C.
육방정 질화붕소 입자는 시중에 유통되는 것 또는 공지된 제조 방법에 따라 제조된 것을 사용할 수 있다. 육방정 질화붕소 입자의 알려진 제조 방법으로는 자가연소법, 탄화연소법 등이 있으나, 이에 제한되는 것은 아니다. 또한, 본 출원 이후에 공지되는 제조 방법에 따라 제조되는 것을 사용할 수 있으며, 그 입수 방법에 특별히 제한되는 것은 아니다.The hexagonal boron nitride particles may be commercially available or prepared according to a known manufacturing method. Known methods for producing hexagonal boron nitride particles include, but are not limited to, a self-combustion method, a carbonization combustion method, and the like. In addition, those prepared according to the manufacturing method known after the present application may be used, and the method of obtaining is not particularly limited.
실시예에 따라서, 육방정 질화붕소 입자의 평균 입격(D50)은 0.1μm 내지 10μm인 것을 사용할 수 있으며, 구체적으로 0.5μm 내지 5μm인 것을 사용할 수 있다. 또한, 육방정 질화붕소 입자는 판상형일 수 있고, 그 두께가 1nm 내지 1,000nm, 구체적으로 10nm 내지 100nm인 것을 사용할 수 있다. 다만, 육방정 질화붕소 입자는 전술한 바에 한정되지 않는다. According to an embodiment, the average particle diameter (D 50 ) of the hexagonal boron nitride particles may be 0.1 μm to 10 μm, specifically, 0.5 μm to 5 μm. In addition, the hexagonal boron nitride particles may be plate-shaped, and may have a thickness of 1 nm to 1,000 nm, specifically, 10 nm to 100 nm. However, the hexagonal boron nitride particles are not limited to those described above.
단계 S120에서, 1차 박리된 질화붕소 입자를 볼 밀링(wet ball milling)하여 2차 박리한다. In step S120, the primary exfoliated boron nitride particles are subjected to secondary exfoliation by wet ball milling.
단계 S120은 박리하는 과정에서, 지르코니아 볼이 질화붕소 입자에 가하는 충격을 최소화하면서 유체로 인한 전단력(shear force)을 일으키기 위해 액체 상태에서 볼 밀링(wet ball milling)을 이용하여 2차 박리할 수 있다. 구체적으로, 지르코니아 볼이 질화붕소 입자의 면방향 사이즈를 줄이지 않고, 효율적으로 박리되어 종횡비를 높이게 하기 위해서는 볼의 직접적인 충격은 최소를 하면서 유체로 인한 전단력(shear force)을 일으키도록 하여야 하기 때문에, 단계 S120은 용매와 같은 액체 상태에서의 볼 밀링(wet ball milling)을 수행할 수 있다. Step S120 is to perform secondary peeling using wet ball milling in a liquid state to generate a shear force due to fluid while minimizing the impact applied by the zirconia balls to the boron nitride particles during the peeling process. can Specifically, in order for the zirconia balls to be efficiently exfoliated without reducing the size of the boron nitride particles in the in-plane direction and to increase the aspect ratio, the direct impact of the balls must be minimized while generating a shear force due to the fluid. S120 may perform wet ball milling in a liquid state such as a solvent.
도 2를 참조하여 설명하면, 단계 S120은 오염되지 않은(Pristine) 1차 박리된 육방정 질화붕소 입자와 용매 및 분쇄용 지르코니아 볼(a)을 볼 밀링(b)하여 2차 박리할 수 있다. 유성 볼 밀링 과정에서 박리된 질화붕소는 용매와 혼합되면서 그 자체로 고분자 바인더 없이 서로 상호작용(interconnection)되어 점성이 증가하는 슬러리 형태(c)로 가공될 수 있다.Referring to FIG. 2 , in step S120, the non-contaminated (Pristine) primary exfoliated hexagonal boron nitride particles, solvent, and zirconia balls for grinding (a) may be subjected to secondary exfoliation by ball milling (b). have. The boron nitride exfoliated in the planetary ball milling process can be processed into a slurry form (c) in which the viscosity increases by being mixed with a solvent and interacting with each other without a polymer binder itself.
이때, 상기 용매의 종류는 이소프로필 알코올, 에탄올과 같은 질화붕소와 표면 에너지가 비슷한 용매로 제작이 가능하며, 헥세인 햅테인 및 물과 같이 표면 에너지가 극성/무극성 쪽으로 극단적인 거리에 있는 용매로도 제작이 가능할 수 있다. 또한, 상기 지르코니아 볼은 용매의 유체학적 흐름이 강한 층류(laminar flow)를 일으키기 위해 지름이 약 1mm 이하의 볼인 것을 특징으로 한다. At this time, the type of the solvent can be prepared with a solvent having a similar surface energy to boron nitride, such as isopropyl alcohol and ethanol, and a solvent with a surface energy at an extreme distance toward polar/non-polar, such as hexane, haptane and water. It may also be possible to manufacture. In addition, the zirconia ball is characterized in that the diameter of the ball is less than about 1mm to generate a strong laminar flow (laminar flow) the fluid flow of the solvent.
본 발명의 실시예에 따른 유성 볼 밀링(planetary ball milling) 시스템의 드라이 볼 밀링(dry ball milling)과 볼 밀링(wet ball milling)의 세부적인 과정은 본 발명이 속하는 기술분야에서 통상적으로 사용되는 방법이므로, 상세한 설명을 생략한다. Detailed processes of dry ball milling and wet ball milling of a planetary ball milling system according to an embodiment of the present invention are commonly used in the art to which the present invention pertains. Since it is a method, a detailed description will be omitted.
단계 S130에서, 2차 박리된 질화붕소 입자를 종횡비에 따라 선별하여 질화붕소 슬러리를 형성한다.In step S130, the second exfoliated boron nitride particles are screened according to the aspect ratio to form a boron nitride slurry.
단계 S130은 볼 밀링 횟수가 증가하면서 높은 종횡비로 나노시트의 비율이 증가된 2차 박리된 질화붕소 입자를 선별할 수 있다. 이에, 단계 S130은 볼 밀링 횟수가 증가하면서 고분자 바인더 없이 상호접속(interconnection)되어 점성이 증가하고 전단력있는 전단 박하(shear thinning) 경향이 증가한 질화붕소 슬러리(slurry)를 형성할 수 있다. 이때, 상기 질화붕소 슬러리는 전단 박하(shear thinning) 경향이 있어 바 코팅을 통해 균일하게 코팅되며, 유연기판에 주조(casting) 가능하다.In step S130, the secondary exfoliated boron nitride particles having an increased ratio of nanosheets with a high aspect ratio may be selected as the number of ball milling increases. Accordingly, in step S130, as the number of ball milling increases, interconnection is performed without a polymer binder to form a boron nitride slurry having increased viscosity and increased shear thinning tendency. At this time, the boron nitride slurry has a tendency to shear thinning, so it is uniformly coated through bar coating, and can be cast on a flexible substrate.
박리되지 않은 질화붕소 벌크입자와 이소프로판 알코올 용매의 혼합물은 입자간 결합력이 약해 점도가 낮으나, 볼 밀링의 횟수가 증가할수록 벌크 입자가 박리되면서 종횡비가 높아지며 나노시트의 비율이 증가한다. 이렇게 혼합물 내에서 질화붕소 나노시트의 비율이 높아지면서 서로 간의 결합력 및 부피 비 증가로 인해 점도가 증가하고 전단력한 전단 박하(shear thinning) 경향이 증가하게 되어 질화붕소 슬러리가 형성될 수 있다.The mixture of unexfoliated boron nitride bulk particles and isopropane alcohol solvent has a low viscosity due to weak inter-particle bonding strength. As the ratio of the boron nitride nanosheets in the mixture increases, the viscosity increases due to the increase in the bonding force and the volume ratio between each other, and the shear thinning tendency increases, thereby forming a boron nitride slurry.
도 3에 도시된 바와 같이, 볼 밀링 횟수가 증가할수록 점도(viscosity)는 점점 증가하여 첨가된 고분자 바인더 없이도 질화붕소와 유체만으로도 높은 점도의 질화붕소 슬러리가 제작되는 것을 특징으로 한다.As shown in FIG. 3 , as the number of ball milling increases, the viscosity gradually increases, so that a boron nitride slurry having a high viscosity is produced only with boron nitride and a fluid without an added polymer binder.
단계 S140에서, 질화붕소 슬러리를 주조한다.In step S140, the boron nitride slurry is cast.
단계 S140은 질화붕소 슬러리에 추가 용매를 주입하여 희석한 후, 진공필터링하여 독립(Free-standing) 가능한 질화붕소 필름을 형성할 수 있다. In step S140, an additional solvent is injected into the boron nitride slurry for dilution, and then vacuum-filtered to form a free-standing boron nitride film.
도 4를 참조하면, 본 발명의 실시예에 따른 질화붕소 슬러리는 전단 박하(shear thinning) 경향이 있어 바 코팅(blade coating, (a))을 통해 균일하게 코팅되어 다양한 두께로 대면적 코팅이 용이하다. 또한, 질화붕소 슬러리가 코팅되었을 시 그 결합력이 유지가 되어 유연기판에도 적용 가능하다. Referring to FIG. 4 , the boron nitride slurry according to the embodiment of the present invention has a tendency to shear thinning and is uniformly coated through a bar coating (blade coating, (a)) to facilitate large-area coating with various thicknesses. do. In addition, when the boron nitride slurry is coated, the bonding force is maintained, so that it can be applied to a flexible substrate.
또한, 본 발명의 실시예에 따른 질화붕소 슬러리에 추가로 용매를 넣어 희석시킨 후 진공필터링(Dilution & vacuum filtering, (b))을 진행하면 독립(Free-standing) 가능한 질화붕소 필름이 제작될 수 있다.In addition, if an additional solvent is added to the boron nitride slurry according to the embodiment of the present invention to be diluted and then vacuum filtering (Dilution & vacuum filtering, (b)) is performed, a free-standing boron nitride film can be produced. have.
또한, 본 발명의 실시예에 따른 질화붕소 슬러리를 48시간 이상 침전시켜 상층액을 걷어내면 좀 더 점도가 높은 질화붕소 잉크가 획득되는데, 이는 주사기(Syringe)로 수직 프린팅(Syringe printing, (c))이 될 수 있을 정도로 높은 점도를 가지게 된다. In addition, when the boron nitride slurry according to the embodiment of the present invention is precipitated for more than 48 hours and the supernatant is removed, boron nitride ink having a higher viscosity is obtained, which is vertical printing with a syringe (Syringe printing, (c) ) to have a high enough viscosity.
도 5a 및 도 5b는 본 발명의 실시예에 따른 질화붕소 슬러리 및 질화붕소 필름에 대한 실험 결과를 도시한 것이다.5A and 5B show experimental results for a boron nitride slurry and a boron nitride film according to an embodiment of the present invention.
본 발명의 실시예에 따른 질화붕소 슬러리를 블레이드 코팅(blade coating)하여 SEM(Scanning Electron Microscope)으로 촬영하면, 도 5a에 도시된 바와 같이 약 수십nm의 두께를 가진 높은 종횡비의 질화붕소 나노시트 입자들이 성공적으로 배열되어 있는 것을 확인할 수 있다.When the boron nitride slurry according to an embodiment of the present invention is blade coated and photographed with a scanning electron microscope (SEM), high aspect ratio boron nitride nanosheet particles having a thickness of about several tens of nm as shown in FIG. 5a It can be seen that they are arranged successfully.
도 5b를 참조하면, 본 발명의 실시예에 따라 제작된 질화붕소 필름의 수평 열전도도를 레이저 펄스 방법(Laser flash analysis)으로 측정한 결과, 수평 열전도도가 약 24W/mK으로 측정된 것을 확인할 수 있다. 이 결과는 종래의 은 나노입자 기반의 방열복합 슬러리(slurry)의 열전도율인 4W/mK를 상회하는 수치이다.Referring to FIG. 5b , as a result of measuring the horizontal thermal conductivity of the boron nitride film produced according to an embodiment of the present invention by a laser pulse method (Laser flash analysis), it can be confirmed that the horizontal thermal conductivity was measured to be about 24 W/mK. have. This result is a value exceeding 4W/mK, which is the thermal conductivity of the conventional silver nanoparticle-based heat dissipation composite slurry.
도 6은 본 발명의 실시예에 따른 질화붕소 슬러리의 방열효과를 검증하기 위한 실험 결과를 도시한 것이다.6 shows experimental results for verifying the heat dissipation effect of the boron nitride slurry according to an embodiment of the present invention.
본 발명의 실시예에 따라 제작된 질화붕소 슬러리를 CPU와 쿨러 사이의 계면에 접착하여 방열효과를 관찰하고자 하였다. 보다 상세하게, CPU와 순환용 쿨러를 결합시킨 후, CPU를 오버클럭(overclock)하여 온도를 측정하였고 그 경과를 관찰하였다. 또한, 비교 군으로 기본 제공되는 상용 은나노 입자 복합소재로 구성된 서머그리스(thermal grease)도 같은 방법으로 오버클럭(overclock)을 진행하여 온도를 측정하였다.It was attempted to observe the heat dissipation effect by attaching the boron nitride slurry prepared according to the embodiment of the present invention to the interface between the CPU and the cooler. In more detail, after the CPU and the circulation cooler were combined, the CPU was overclocked to measure the temperature and the progress was observed. In addition, thermal grease composed of a commercial silver nano-particle composite material provided as a comparison group was overclocked in the same way to measure the temperature.
그 결과 도 6에 도시된 바와 같이, CPU의 최대 온도가 약 7 내지 8도 정도 차이가 나는 것을 확인할 수 있다. 이것을 통해 실제 질화붕소 슬러리가 상용 서머그리스(thermal grease)보다 열전도율이 좋아 열 계면 물질로서 성능이 우수한 것을 알 수 있다. As a result, as shown in FIG. 6 , it can be confirmed that the maximum temperature of the CPU differs by about 7 to 8 degrees. Through this, it can be seen that the actual boron nitride slurry has better thermal conductivity than commercial thermal grease, and thus has superior performance as a thermal interface material.
이상과 같이 실시예들이 비록 한정된 실시예와 도면에 의해 설명되었으나, 해당 기술분야에서 통상의 지식을 가진 자라면 상기의 기재로부터 다양한 수정 및 변형이 가능하다. 예를 들어, 설명된 기술들이 설명된 방법과 다른 순서로 수행되거나, 및/또는 설명된 시스템, 구조, 장치, 회로 등의 구성요소들이 설명된 방법과 다른 형태로 결합 또는 조합되거나, 다른 구성요소 또는 균등물에 의하여 대치되거나 치환되더라도 적절한 결과가 달성될 수 있다.As described above, although the embodiments have been described with reference to the limited embodiments and drawings, various modifications and variations are possible by those skilled in the art from the above description. For example, the described techniques are performed in a different order than the described method, and/or the described components of the system, structure, apparatus, circuit, etc. are combined or combined in a different form than the described method, or other components Or substituted or substituted by equivalents may achieve an appropriate result.
그러므로, 다른 구현들, 다른 실시예들 및 특허청구범위와 균등한 것들도 후술하는 특허청구범위의 범위에 속한다.Therefore, other implementations, other embodiments, and equivalents to the claims are also within the scope of the following claims.
Claims (11)
상기 1차 박리된 질화붕소 입자를 볼 밀링(wet ball milling)하여 2차 박리하는 단계;
상기 2차 박리된 질화붕소 입자를 종횡비에 따라 선별하여 질화붕소 슬러리를 형성하는 단계; 및
상기 질화붕소 슬러리를 주조하는 단계
를 포함하는 바인더 무첨가 질화붕소 필름의 제조 방법. Dry ball milling the hexagonal boron nitride particles by using planetary ball milling (planetary ball milling) to primary peeling;
Second exfoliation by performing wet ball milling of the first exfoliated boron nitride particles;
forming a boron nitride slurry by selecting the second exfoliated boron nitride particles according to an aspect ratio; and
Casting the boron nitride slurry
Method for producing a binder-free boron nitride film comprising a.
상기 1차 박리하는 단계는
상기 육방정 질화붕소 입자를 용매 없이 상기 드라이 볼 밀링하여 1차 박리하는 것을 특징으로 하는, 바인더 무첨가 질화붕소 필름의 제조 방법.According to claim 1,
The first peeling step
The method for producing a binder-free boron nitride film, characterized in that the primary peeling by dry ball milling the hexagonal boron nitride particles without a solvent.
상기 2차 박리하는 단계는
상기 1차 박리된 질화붕소 입자와 용매 및 분쇄용 지르코니아 볼을 상기 볼 밀링하여 2차 박리하는 것을 특징으로 하는, 바인더 무첨가 질화붕소 필름의 제조 방법. 3. The method of claim 2,
The second peeling step
The method for producing a binder-free boron nitride film, characterized in that the primary peeled boron nitride particles and the solvent and the zirconia balls for grinding are subjected to secondary peeling by the Ÿ‡ ball milling.
상기 용매는
이소프로필 알코올 및 에탄올, 또는 헥세인 햅테인 및 물 중 어느 하나인 것을 특징으로 하는, 바인더 무첨가 질화붕소 필름의 제조 방법.4. The method of claim 3,
The solvent is
A method for producing a binder-free boron nitride film, characterized in that any one of isopropyl alcohol and ethanol, or hexane haptane and water.
상기 2차 박리하는 단계는
박리하는 과정에서, 상기 지르코니아 볼이 상기 질화붕소 입자에 가하는 충격을 최소화하면서 유체로 인한 전단력(shear force)을 일으키기 위해 액체 상태에서 상기 볼 밀링(wet ball milling)하여 2차 박리하는 것을 특징으로 하는, 바인더 무첨가 질화붕소 필름의 제조 방법.4. The method of claim 3,
The second peeling step
In the peeling process, the Ÿ‡ ball milling (wet ball milling) in the liquid state to generate a shear force due to the fluid while minimizing the impact applied by the zirconia balls to the boron nitride particles is characterized in that the secondary peeling is performed. A method for producing a binder-free boron nitride film.
상기 지르코니아 볼은
용매의 유체학적 흐름이 강한 층류(laminar flow)를 일으키기 위해 지름이 약 1mm 이하의 볼인 것을 특징으로 하는, 바인더 무첨가 질화붕소 필름의 제조 방법.6. The method of claim 5,
The zirconia balls are
A method for producing a binder-free boron nitride film, characterized in that the fluidic flow of the solvent is a ball having a diameter of about 1 mm or less to cause a strong laminar flow.
상기 질화붕소 슬러리를 형성하는 단계는
볼 밀링 횟수가 증가하면서 높은 종횡비로 나노시트의 비율이 증가된 상기 2차 박리된 질화붕소 입자를 선별하는, 바인더 무첨가 질화붕소 필름의 제조 방법.According to claim 1,
Forming the boron nitride slurry is
A method of manufacturing a binder-free boron nitride film for screening the secondary exfoliated boron nitride particles having an increased ratio of nanosheets with a high aspect ratio while the number of ball milling increases.
상기 질화붕소 슬러리를 형성하는 단계는
볼 밀링 횟수가 증가하면서 고분자 바인더 없이 상호접속(interconnection)되어 점성이 증가하고 전단력있는 전단 박하(shear thinning) 경향이 증가한 상기 질화붕소 슬러리(slurry)를 형성하는, 바인더 무첨가 질화붕소 필름의 제조 방법.8. The method of claim 7,
Forming the boron nitride slurry is
A method of producing a binder-free boron nitride film, which is interconnected without a polymer binder as the number of ball milling increases to form the boron nitride slurry having increased viscosity and increased shear thinning tendency.
상기 질화붕소 슬러리는
전단 박하(shear thinning) 경향이 있어 바 코팅을 통해 균일하게 코팅되며, 유연기판에 주조 가능한 것을 특징으로 하는, 바인더 무첨가 질화붕소 필름의 제조 방법.9. The method of claim 8,
The boron nitride slurry is
A method for producing a binder-free boron nitride film, characterized in that it has a tendency to shear thinning and is uniformly coated through bar coating, and can be cast on a flexible substrate.
상기 질화붕소를 주조하는 단계는
상기 질화붕소 슬러리에 추가 용매를 주입하여 희석한 후, 진공필터링하여 독립(Free-standing) 가능한 질화붕소 필름을 형성하는, 바인더 무첨가 질화붕소 필름의 제조 방법.9. The method of claim 8,
The step of casting the boron nitride
After dilution by injecting an additional solvent into the boron nitride slurry, vacuum filtering to form a free-standing boron nitride film, a method for producing a binder-free boron nitride film.
상기 바인더 무첨가 질화붕소 필름의 제조 방법은
유성 볼 밀링(planetary ball milling)을 이용하여 육방정 질화붕소 입자를 드라이 볼 밀링(dry ball milling)하여 1차 박리하는 단계;
상기 1차 박리된 질화붕소 입자를 볼 밀링(wet ball milling)을 이용하여 2차 박리하는 단계;
상기 2차 박리된 질화붕소 입자를 종횡비에 따라 선별하여 질화붕소 슬러리를 형성하는 단계; 및
상기 질화붕소 슬러리를 주조하는 단계
를 포함하는 질화붕소 필름을 포함하는 방열 재료.
In the heat dissipation material comprising a boron nitride film produced according to the method for producing a binder-free boron nitride film,
The method for producing the binder-free boron nitride film is
Dry ball milling the hexagonal boron nitride particles by using planetary ball milling (planetary ball milling) to primary peeling;
Secondary exfoliation of the first exfoliated boron nitride particles using Ÿ‡ ball milling (wet ball milling);
forming a boron nitride slurry by selecting the second exfoliated boron nitride particles according to an aspect ratio; and
Casting the boron nitride slurry
A heat dissipation material comprising a boron nitride film comprising a.
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