KR20230166733A - A prepreg using a liquid ceramic precursor and a photocuring method - Google Patents
A prepreg using a liquid ceramic precursor and a photocuring method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000012700 ceramic precursor Substances 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 title claims abstract description 19
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 8
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 abstract description 18
- 238000000465 moulding Methods 0.000 abstract description 10
- 238000007168 polymer infiltration and pyrolysis Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011153 ceramic matrix composite Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000001723 curing Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 229920000592 inorganic polymer Polymers 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 239000012705 liquid precursor Substances 0.000 description 1
- 238000000626 liquid-phase infiltration Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002990 reinforced plastic Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
본 발명은 액상의 세라믹전구체와 광경화 공법을 이용한 프리프레그에 관한 것으로, 섬유매트 표면에 액상의 세라믹전구체를 도포한 후 광경화시키고, 상기 액상의 세라믹전구체는 폴리카보실란인 것을 포함함으로써 점성과 탄성을 모두 가지므로 프리프레그 형태로 제공하는 것이 가능하고, 프리프레그의 적층성형이 가능하며 가장 많이 사용되는 vacuum bag 공정 등에 적용이 가능하므로 별도의 성형장치가 필요하지 않는 효과가 있는 프리프레그를 제공한다.The present invention relates to a prepreg using a liquid ceramic precursor and a photocuring method. The liquid ceramic precursor is applied to the surface of a fiber mat and then photocured, and the liquid ceramic precursor contains polycarbosilane to increase viscosity and Since it has both elasticity, it is possible to provide it in the form of a prepreg, laminated molding of the prepreg is possible, and it can be applied to the most commonly used vacuum bag process, providing an effective prepreg that does not require a separate molding device. do.
Description
본 발명은 액상의 세라믹전구체와 광경화 공법을 이용한 프리프레그에 관한 것으로, 보다 상세하게는 광경화가 가능한 폴리카보실란(Polycarbosilane, PCS)을 활용한 프리프레그를 제공하기 위한 것이다.The present invention relates to a prepreg using a liquid ceramic precursor and a photocuring method, and more specifically, to provide a prepreg using polycarbosilane (PCS) that can be photocured.
세라믹 기지 복합재료(ceramic matrix composite, CMC)는 일반적으로 CVI(chemical vapour infiltration), SMI(silicon melt infiltration), PIP(Polymer infiltration and pyrolysis) 등의 공정으로 제조가 가능하다. 그러나, 앞서 언급된 공정은 기타 다른 소재에 비해 공정 비용을 상승시키는 문제가 발생하여 시장 성장을 억제하고 있다.Ceramic matrix composite (CMC) can generally be manufactured through processes such as chemical vapor infiltration (CVI), silicon melt infiltration (SMI), and polymer infiltration and pyrolysis (PIP). However, the above-mentioned process has problems that increase the process cost compared to other materials, which is suppressing market growth.
이러한 공정 비용 상승을 낮추기 위해 원료소재의 단가를 낮추거나, 생산 공정을 단순화 할 필요가 있는데 이중 PIP 공정은 미분말을 분산한 슬러리나 무기고분자인 세라믹전구체를 이용할 수 있는 장점이 있어 잘 알려진 FRP(fiber reinforced plastics) 성형 공정을 적용할 수 있다는 장점이 있다.In order to reduce this increase in process cost, it is necessary to lower the unit price of raw materials or simplify the production process. Among these, the PIP process has the advantage of being able to use a slurry with dispersed fine powder or a ceramic precursor, which is an inorganic polymer, and thus the well-known FRP (fiber) process. It has the advantage of being able to apply the reinforced plastics molding process.
무기고분자인 세라믹전구체를 이용하여 PIP 공정으로 복합소재의 성형에 이용할 수 있는데, 폴리카보실란으로 대표되는 세라믹전구체는 열처리 과정에서 열분해-결정화 단계를 거침으로써 세라믹으로 전환되는 것이 특징이다. 따라서 유동성을 가지는 고분자의 특성을 이용하여 세라믹섬유강화재-전구체레진 복합소재 성형 공정을 거친 후 열처리하여 세라믹섬유강화재-세라믹기지재 복합소재로 전환이 될 수 있다.Ceramic precursors, which are inorganic polymers, can be used to mold composite materials through the PIP process. The characteristic of ceramic precursors, represented by polycarbosilane, is that they are converted into ceramics by going through a thermal decomposition-crystallization step during the heat treatment process. Therefore, using the properties of polymers with fluidity, it can be converted into a ceramic fiber reinforcement-ceramic matrix composite material by going through a ceramic fiber reinforcement-precursor resin composite material molding process and then heat treating it.
그러나 복합소재로 성형된 레진 상태의 전구체는 열처리 중에 용융(melting), 끓음(boiling) 등의 상변형에 의해 형상변형이 발생되는 문제가 있다. 이러한 형상변형 발생을 방지하기 위해서는 반드시 세라믹전구체의 경화 기전이 확보되어야 한다.However, resin precursors molded from composite materials have a problem in that shape deformation occurs due to phase transformation such as melting or boiling during heat treatment. In order to prevent such shape deformation, a curing mechanism for the ceramic precursor must be secured.
한편, FRP(섬유강화 플라스틱 복합소재)는 기지재 소재가 플라스틱이며, 고분자의 특성을 이용한 성형 방식을 채용함으로써 산업에서 광범위하게 사용되고 있다. PIP 방식의 세라믹 기지 복합재료 제조는 슬러리나 세라믹 전구체를 infiltration 하는 방식을 쓰고 있지만, 기존의 방식은 FRP 공정에 적용되지 못하고 있다. 이는 고분자인 세라믹전구체가 액상과 고상 두 가지로 공급되고 있고, 고상의 경우에는 용매에 용해시켜 용액 상태로 사용되는 것이 일반적이며, 액상의 경우에는 경화 방식과 조건 확보가 어려워 몰드에 채워넣고 가압성형 하는 것이 일반적이다.Meanwhile, FRP (fiber-reinforced plastic composite) is made of plastic as a base material and is widely used in industry by adopting a molding method that utilizes the properties of polymers. The PIP method of manufacturing ceramic matrix composites uses a method of infiltration of slurry or ceramic precursors, but the existing method is not applicable to the FRP process. Ceramic precursor, which is a polymer, is supplied in both liquid and solid forms. In the case of the solid state, it is generally used in a solution state by dissolving it in a solvent. In the case of the liquid state, it is difficult to secure the curing method and conditions, so it is filled into a mold and pressed. It is common to do so.
가압성형의 경우에도, 세라믹전구체의 용융과 끓는 현상으로 인하여 경화에 앞서 넘침 등의 변형을 제어하지 못하거나, 점도 제어가 어려워 레진의 두께 확보가 불가능하기 때문에 PIP 공정을 7회 이상 반복적으로 시행하게 된다. 따라서 FRP 공정에 적합한 세라믹전구체 레진의 설계(구조, 배합 등)가 필요한 상황이다.Even in the case of pressure molding, deformations such as overflow cannot be controlled prior to curing due to the melting and boiling phenomenon of the ceramic precursor, or viscosity control is difficult to secure the thickness of the resin, so the PIP process must be repeated seven or more times. do. Therefore, the design (structure, formulation, etc.) of a ceramic precursor resin suitable for the FRP process is necessary.
본 발명이 해결하고자 하는 과제는 세라믹 기지 복합재료 제조에 있어 액상의 세라믹전구체를 사용하는 경우 세라믹전구체의 용융과 끓는 현상으로 인해 경화에 앞서 변형을 제어하지 못 하거나 점도 제어가 어려워 레진의 두께 확보가 불가능하여 PIP 공정이 다수 시행되는 어려움이 있다.The problem that the present invention aims to solve is that when using a liquid ceramic precursor in the production of a ceramic matrix composite material, it is difficult to control the deformation prior to curing or control the viscosity due to the melting and boiling phenomenon of the ceramic precursor, making it difficult to secure the thickness of the resin. Since this is not possible, it is difficult to implement many PIP processes.
따라서 본 발명을 통해 FRP 공정에 적합한 세라믹전구체 레진의 설계(구조, 배합 등)를 위한 프리프레그를 제공하고자 한다.Therefore, through the present invention, the aim is to provide a prepreg for the design (structure, formulation, etc.) of ceramic precursor resin suitable for the FRP process.
본 발명이 해결하고자 하는 과제들은 이상에서 언급된 과제로 제한되지 않으며, 언급되지 않은 또 다른 과제들은 아래의 기재로부터 통상의 기술자에게 명확하게 이해될 수 있을 것이다.The problems to be solved by the present invention are not limited to the problems mentioned above, and other problems not mentioned can be clearly understood by those skilled in the art from the description below.
상기와 같은 본 발명의 목적을 달성하기 위해서, 본 발명의 일실시예에 따른 프리프레그는 섬유매트 표면에 액상의 세라믹전구체를 도포한 후 광경화시키고, 상기 액상의 세라믹전구체는 폴리카보실란인 것을 포함할 수 있다.In order to achieve the object of the present invention as described above, the prepreg according to an embodiment of the present invention is photocured after applying a liquid ceramic precursor to the surface of the fiber mat, and the liquid ceramic precursor is polycarbosilane. It can be included.
본 발명에 따른 프리프레그는, 광경화가 가능한 폴리카보실란을 사용함으로써 점성과 탄성을 모두 갖는 특징으로 인해 프리프레그 형태로 제공하는 것이 가능한 효과가 있다.The prepreg according to the present invention has the advantage of being provided in the form of a prepreg due to its characteristics of having both viscosity and elasticity by using photocurable polycarbosilane.
또한 프리프레그의 적층성형이 가능하며 가장 많이 사용되는 vacuum bag 공정 등에 적용이 가능하므로 별도의 성형장치가 필요하지 않는 효과가 있다.In addition, lamination molding of prepreg is possible and can be applied to the most widely used vacuum bag process, so there is no need for a separate molding device.
도 1은 본 발명에 따른 광경화된 폴리카보실란의 DSC 분석 결과를 나타낸 그래프이다.Figure 1 is a graph showing the results of DSC analysis of photocured polycarbosilane according to the present invention.
첨부한 도면을 참조하여 본 발명의 실시예들에 의한 액상의 세라믹전구체와 광경화 공법을 이용한 프리프레그에 대하여 상세히 설명한다. 본 발명은 다양한 변경을 가할 수 있고 여러 가지 형태를 가질 수 있는바, 특정 실시예들을 도면에 예시하고 본문에 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 개시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다.Referring to the attached drawings, a liquid ceramic precursor according to embodiments of the present invention and a prepreg using a photocuring method will be described in detail. Since the present invention can be subject to various changes and can have various forms, specific embodiments will be illustrated in the drawings and described in detail in the text. However, this is not intended to limit the present invention to a specific disclosed form, and should be understood to include all changes, equivalents, and substitutes included in the spirit and technical scope of the present invention.
또한, 제1 및 제2 등의 용어는 다양한 구성요소들을 설명하는데 사용될 수 있지만, 상기 구성요소들은 상기 용어들에 의해 한정되어서는 안 된다. 상기 용어들은 하나의 구성요소를 다른 구성요소로부터 구별하는 목적으로만 사용된다. 예를 들어, 본 발명의 권리 범위를 벗어나지 않으면서 제1 구성요소는 제2 구성요소로 명명될 수 있고, 유사하게 제2 구성요소도 제1 구성요소로 명명될 수 있다. 한편, 다르게 정의되지 않는 한, 기술적이거나 과학적인 용어를 포함해서 여기서 사용되는 모든 용어들은 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에 의해 일반적으로 이해되는 것과 동일한 의미를 가지고 있다. 일반적으로 사용되는 사전에 정의되어 있는 것과 같은 용어들은 관련 기술의 문맥 상 가지는 의미와 일치하는 의미를 가지는 것으로 해석되어야 하며, 본 출원에서 명백하게 정의하지 않는 한, 이상적이거나 과도하게 형식적인 의미로 해석되지 않는다.Additionally, terms such as first and second may be used to describe various components, but the components should not be limited by the terms. The above terms are used only for the purpose of distinguishing one component from another. For example, a first component may be named a second component, and similarly, the second component may also be named a first component without departing from the scope of the present invention. Meanwhile, unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as generally understood by those skilled in the art to which the present invention pertains. Terms defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the related technology, and unless explicitly defined in the present application, should not be interpreted in an ideal or excessively formal sense. No.
본 발명의 일 실시형태에 따른 액상의 세라믹전구체와 광경화 공법을 이용한 프리프레그는, A prepreg using a liquid ceramic precursor and a photocuring method according to an embodiment of the present invention,
섬유매트 표면에 액상의 세라믹전구체를 도포한 후 광경화시키고, 상기 액상의 세라믹전구체는 폴리카보실란인 것을 포함하는 것을 특징으로 한다. A liquid ceramic precursor is applied to the surface of the fiber mat and then photocured, and the liquid ceramic precursor is characterized in that it contains polycarbosilane.
본 발명의 일 실시형태에 따른 액상의 세라믹전구체와 광경화 공법을 이용한 프리프레그는 섬유매트 표면에 액상의 세라믹전구체를 도포한 후 광경화 함으로써 적층이 가능한 프리프레그를 제공하는 것이다.A prepreg using a liquid ceramic precursor and a photocuring method according to an embodiment of the present invention provides a prepreg that can be laminated by applying a liquid ceramic precursor to the surface of a fiber mat and then photocuring it.
FRP 제조 방법 중 가장 널리 사용되는 방법은 복합소재 성형 중간재인 시트형상의 프리프레그를 이용한 제조 방법이다.The most widely used FRP manufacturing method is a manufacturing method using sheet-shaped prepreg, an intermediate material for forming composite materials.
프리프레그 제조에 사용되는 플라스틱(혹은 레진)은 열가소성의 성질로 용융점도는 높은 것을 사용하는데, 액상의 전구체는 열가소성으로 제조되지는 않는다.The plastic (or resin) used to manufacture prepreg is thermoplastic and has a high melt viscosity, but the liquid precursor is not manufactured as thermoplastic.
도 1은 본 발명에 따른 광경화된 폴리카보실란의 DSC 분석 결과를 나타낸 그래프이다.Figure 1 is a graph showing the results of DSC analysis of photocured polycarbosilane according to the present invention.
폴리카보실란은 광경화가 가능하며, 광경화된 폴리카보실란은 점성과 탄성을 모두 가지고 있으므로 프리프레그 형태로 제공하는 것이 가능하다.Polycarbosilane can be photocured, and since photocured polycarbosilane has both viscosity and elasticity, it is possible to provide it in the form of a prepreg.
이 경우 프리프레그의 적층성형이 가능하며 가장 많이 사용되는 vacuum bag 공정 등에 적용이 가능하므로 별도의 성형장치를 필요로 하지 않는다는 장점이 있다.In this case, lamination molding of prepreg is possible and can be applied to the most widely used vacuum bag process, so there is an advantage of not requiring a separate molding device.
이상으로 본 발명의 특정한 부분을 상세히 기술하였는 바, 본 발명이 속한 기술분야에서 통상의 지식을 가진 자에게 있어서 이러한 구체적인 기술은 단지 바람직한 구현예일 뿐이며, 이에 본 발명의 범위가 제한되는 것이 아님은 명백하다. 본 발명이 속한 기술분야에서 통상의 지식을 가진 자라면 상기 내용을 바탕으로 본 발명의 범주 내에서 다양한 응용 및 변형을 행하는 것이 가능할 것이다.As the specific parts of the present invention have been described in detail above, it is clear to those skilled in the art that these specific techniques are merely preferred embodiments and do not limit the scope of the present invention. do. Anyone skilled in the art to which the present invention pertains will be able to make various applications and modifications within the scope of the present invention based on the above contents.
따라서, 본 발명의 실질적인 범위는 첨부된 특허청구범위와 그의 등가물에 의하여 정의된다고 할 것이다.Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (1)
상기 액상의 세라믹전구체는 폴리카보실란인 것을 포함하는 액상의 세라믹전구체와 광경화 공법을 이용한 프리프레그.Liquid ceramic precursor is applied to the surface of the fiber mat and then photocured.
The liquid ceramic precursor is a prepreg using a liquid ceramic precursor containing polycarbosilane and a photocuring method.
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