KR20030068962A - Method and apparatus for producing molybdenum disilicide powder using self-propagating high-temperature synthesis(SHS) - Google Patents

Method and apparatus for producing molybdenum disilicide powder using self-propagating high-temperature synthesis(SHS) Download PDF

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KR20030068962A
KR20030068962A KR1020020008800A KR20020008800A KR20030068962A KR 20030068962 A KR20030068962 A KR 20030068962A KR 1020020008800 A KR1020020008800 A KR 1020020008800A KR 20020008800 A KR20020008800 A KR 20020008800A KR 20030068962 A KR20030068962 A KR 20030068962A
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powder
molybdenum
mosi
heating element
reaction
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한동빈
이정근
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(주)위너 테크
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/06—Metal silicides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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Abstract

PURPOSE: A method and an apparatus for mass producing high quality molybdenum disilicide (MoSi2) powder by improving conventional self-propagating high-temperature synthesis (SHS) are provided. CONSTITUTION: The method for manufacturing molybdenum disilicide powder comprises steps of milling the mixture by mixing molybdenum (Mo) powder and silicon (Si) powder; synthesizing the mixture into molybdenum disilicide (MoSi2) using self-propagating high-temperature synthesis (SHS) under hydrogen atmosphere; and a powdering the molybdenum disilicide (MoSi2) by milling the synthesized molybdenum disilicide (MoSi2). The apparatus for manufacturing molybdenum disilicide powder comprises a preheating furnace(2); a reaction furnace(1) which is arranged inside the preheating furnace(2), and in which a heating element(8) for initiating reaction of molybdenum (Mo) and silicon (Si) powder is included; a cooling water pipe(4) for surrounding the outer wall of the reaction furnace(1); a preheating unit(3) which is arranged on the inner wall of the preheating furnace(2), and in which a heating element for increasing initial reaction heat is included; a gas pipe for supplying gas into the reaction furnace(1) or discharging gas from the reaction furnace(1); and a power supply unit(5) for supplying current to the heating element(8), wherein the wall of the reaction furnace(1) is made of graphite, wherein vacuum pump(6) and vacuum gauge(7) are arranged on discharge passageway of the gas pipe to control internal pressure of the reaction furnace(1), and wherein the heating element(8) is a coil type or filament type tungsten (W) wire.

Description

자전 고온 합성법(ＳＨＳ)을 이용한 2규화 몰리브덴 분말의 제조방법 및 장치 {Method and apparatus for producing molybdenum disilicide powder using self-propagating high-temperature synthesis(ＳＨＳ)}Method and apparatus for producing molybdenum bisulfide powder by means of rotating high temperature synthesis method (SHS) {Shoss and apparatus for producing molybdenum disilicide powder using self-propagating high-temperature synthesis (SHS)}

본 발명은 2규화 몰리브덴(MoSi2) 분말의 제조방법 및 장치에 관한 것으로,보다 상세하게는 종래의 자전 고온 합성법을 개선하여 양질의 2규화 몰리브덴(MoSi2) 분말을 대량생산하기 위한 제조방법 및 장치에 관한 것이다.The present invention relates to a method and apparatus for producing molybdenum silicide (MoSi 2 ) powder, and more particularly, to a production method for mass production of high quality molybdenum silicide (MoSi 2 ) powder by improving the conventional high-temperature synthesis method. Relates to a device.

2규화 몰리브덴(MoSi2)은 높은 열전도도, 낮은 열팽창계수, 높은 융점(2,030℃) 및 내산화성이 우수하여 전기를 열원으로 하는 각종 전기로의 발열체의 재료로서 광범위하게 사용되고 있다. 또한 가스 터어빈, 노즐 등의 내열구조 재료로서도 응용되고 있다.Molybdenum bisulfide (MoSi 2 ) is widely used as a material for heating elements of various electric furnaces using electricity as a heat source because of its high thermal conductivity, low coefficient of thermal expansion, high melting point (2,030 ° C), and excellent oxidation resistance. It is also applied to heat-resistant structural materials such as gas turbines and nozzles.

이러한 2규화 몰리브덴(MoSi2)을 제조하는 종래의 방법으로 자전 고온 합성법(SHS: Self-propagating High-Temperature Synthesis)이 장치의 소형화 및 순간 작업에 의한 장점 때문에 오래 전부터 이용되어 왔다.Self-propagating High-Temperature Synthesis (SHS) has been used for a long time since the conventional method of manufacturing molybdenum silicide (MoSi 2 ).

그러나, 순간 고온(1800℃)에서 이루어지는 과정으로 분말 용기 자체의 재질문제가 야기되었고, 이를 방지하기 위하여 냉각수를 흘려 냉각시키는 방법을 채택하고 있으나 합성원료의 외부에서 열손실로 인해 고순도의 분말을 얻을 수 없다는 단점이 있었다.However, the process at the instantaneous high temperature (1800 ℃) caused the material problem of the powder container itself, and in order to prevent this, the method of cooling by flowing the coolant is adopted, but high purity powder is obtained due to the heat loss from the outside of the synthetic raw material. There was a disadvantage of not being able to.

본 발명자는 이러한 종래 기술의 문제점을 해결하고자 예의 연구한 결과, 기존의 2규화 몰리브덴(MoSi2) 제조 장치에서 냉각장치를 생략시켜 외벽을 통한 열손실을 줄여 대량생산이 가능하고, 몰리브덴(Mo)과 규소(Si)를 압축시켜 충진율을 향상시킴으로써 고순도의 2규화 몰리브덴(MoSi2) 분말을 제조할 수 있음을 발견하고, 본 발명에 이르렀다.As a result of earnest research to solve the problems of the prior art, the present inventors omit the cooling device from the conventional molybdenum silicide (MoSi 2 ) manufacturing apparatus to reduce heat loss through the outer wall, thereby enabling mass production, and molybdenum (Mo) It was found that high purity molybdenum silicide (MoSi 2 ) powder can be produced by compressing the silicon and Si to improve the filling rate.

따라서, 본 발명의 목적은 고순도의 2규화 몰리브덴(MoSi2) 분말을 제조할 수 있는 방법을 제공하는데 있다.Accordingly, it is an object of the present invention to provide a method for producing high purity molybdenum silicide (MoSi 2 ) powder.

본 발명의 또 다른 목적은 상기 고순도 2규화 몰리브덴(MoSi2) 분말을 제조하는데 사용되는 장치를 제공하는데 있다.Still another object of the present invention is to provide an apparatus used to prepare the high purity molybdenum silicide (MoSi 2 ) powder.

도 1은 본 발명의 자전 고온 합성법(SHS)을 이용하여 2규화 몰리브덴(MoSi2)을 합성할 수 있는 장치의 개략적인 단면도이다.1 is a schematic cross-sectional view of an apparatus capable of synthesizing molybdenum silicide (MoSi 2 ) using the rotating high temperature synthesis method (SHS) of the present invention.

도면의 주요 부호에 대한 간단한 설명Brief description of the main symbols in the drawings

1: 반응로, 2: 예열로, 3: 예열 장치,1: reactor, 2: preheater, 3: preheater,

4: 냉각수 관, 5: 전원 공급부, 6: 진공 펌프,4: coolant tube, 5: power supply, 6: vacuum pump,

7: 진공 게이지, 8: 발열체.7: vacuum gauge, 8: heating element.

본 발명에 따른 고순도 2규화 몰리브덴(MoSi2) 분말의 제조방법은Method for producing high purity molybdenum silicide (MoSi 2 ) powder according to the present invention

1) 몰리브덴(Mo) 분말과 규소(Si) 분말을 혼합하여 분쇄하는 단계,1) mixing and grinding molybdenum (Mo) powder and silicon (Si) powder,

2) 상기 혼합물을 수소(H2) 분위기하에서 자전 고온 합성법을 이용하여 2규화 몰리브덴(MoSi2)을 합성하는 단계, 및2) synthesizing molybdenum silicide (MoSi 2 ) using the mixture at high temperature in a hydrogen (H 2 ) atmosphere, and

3) 합성된 2규화 몰리브덴(MoSi2)을 분쇄하여 분말화하는 단계를 포함한다.3) pulverizing the synthesized molybdenum silicide (MoSi 2 ).

상기 단계 1)에서 몰리브덴(Mo) 분말과 규소(Si) 분말의 혼합과 분쇄는 기계적 혼합이나 볼 밀 등 통상의 방법을 사용하여 실시된다. 이러한 혼합은 원료분말 간에 접촉 면적을 높이기 위한 것으로, 입자의 크기가 작을수록 반응성이 높아져 최종 제조되는 2규화 몰리브덴(MoSi2)의 수득율을 상승시킨다. 이렇게 얻어진 원료분말 혼합물을 압축(pressing)하여 케이크(cake) 형태로 제조한 후, 자전 고온 합성법에 사용한다. 이러한 몰리브덴(Mo)과 규소(Si)의 케이크는 충진율을 향상시켜 고순도 2규화 몰리브덴(MoSi2)의 합성을 유도하며, 합성시 적층하여 2규화 몰리브덴(MoSi2)의 대량 생산을 가능하게 한다.In step 1), the mixing and pulverization of the molybdenum (Mo) powder and the silicon (Si) powder is performed using a conventional method such as mechanical mixing or a ball mill. This mixing is to increase the contact area between the raw material powder, the smaller the particle size, the higher the reactivity, thereby increasing the yield of molybdenum silicide (MoSi 2 ) to be finally produced. The raw powder mixture thus obtained is pressed to prepare a cake, and then used in a rotating high temperature synthesis method. Such a cake of molybdenum (Mo) and silicon (Si) improves the filling rate to induce the synthesis of high-purity molybdenum silicide (MoSi 2 ), it is laminated during synthesis to enable the mass production of molybdenum silicide (MoSi 2 ).

상기 단계 2)에서는, 케이크 형태로 제조된 몰리브덴(Mo) 분말과 규소(Si) 분말 혼합체를 본 발명에 따른 또 다른 요지인 자전 고온 합성로에서 가열시켜 2규화 몰리브덴(MoSi2)을 합성한다.In step 2), molybdenum silicide (MoSi 2 ) is synthesized by heating a molybdenum (Mo) powder and silicon (Si) powder mixture prepared in the form of a cake in a rotating high temperature synthesis furnace according to the present invention.

본 명세서에서 언급되는 "자전 고온 합성법(SHS: Self-propagating High-Temperature Synthesis)"이란, 반응 개시온도까지 온도를 올려주면, 반응물간 반응 생성열이 발생하여 스스로 반응이 진행되어 합성을 유도하는 합성법을 말한다.The term "self-propagating High-Temperature Synthesis" (SHS) referred to in the present specification refers to a synthesis method in which when the temperature is raised to the initiation temperature of the reaction, heat of reaction generation between reactants is generated and the reaction proceeds to induce synthesis. Say.

본 발명에서 몰리브덴(Mo)과 규소(Si)의 반응 개시온도는 약 300∼800℃로 전원 공급부(5)에서 공급되는 전류에 의해 반응로(1)의 발열체(8)를 가열시켜 반응 개시온도까지 온도를 올려주게 된다. 또한 본 발명에서 몰리브덴(Mo)과 규소(Si)의 반응은 수소(H2) 압력 1.5kg/cm3하에서 진행된다.In the present invention, the reaction initiation temperature of molybdenum (Mo) and silicon (Si) is about 300 to 800 ° C. by heating the heating element (8) of the reactor (1) by the current supplied from the power supply unit (5). The temperature is raised to. In the present invention, the reaction of molybdenum (Mo) and silicon (Si) is carried out under hydrogen (H 2 ) pressure 1.5kg / cm 3 .

상기 단계 3)에서, 최종 제조되는 2규화 몰리브덴(MoSi2)을 밀링 공정을 통해 분말화하는데, 분말의 입도는 발열체나 내열재료로의 성형을 위해 2∼20㎛ 범위가 바람직하다.In the step 3), the final molybdenum silicide (MoSi 2 ) to be powdered through a milling process, the particle size of the powder is preferably in the range of 2 to 20㎛ for molding into a heating element or heat-resistant material.

본 발명은 또한 상기 고순도 2규화 몰리브덴(MoSi2) 분말의 제조방법에 직접 사용되는 장치에 관한 것으로, 기존의 자전 고온 합성로에서 외벽을 통해 손실되는열량을 줄여 반응열을 높이기 위해 냉각장치를 생략하고, 초기 반응열을 높이기 위해 예열 장치(3)를 추가된 것을 특징으로 한다.The present invention also relates to a device used directly in the manufacturing method of the high purity molybdenum silicide (MoSi 2 ) powder, omitting the cooling device to increase the heat of reaction by reducing the amount of heat lost through the outer wall in a conventional rotating high-temperature synthesis furnace In addition, the preheating device (3) is added to increase the initial heat of reaction.

이하, 첨부된 도 1을 참조하여, 본 발명에 따른 고순도 2규화 몰리브덴 (MoSi2) 분말을 제조하기 위한 고온 자전 합성로에 대해 설명한다.Hereinafter, with reference to the accompanying Figure 1, a high-temperature rotating synthesis furnace for producing a high-purity molybdenum silicide (MoSi 2 ) powder according to the present invention.

본 발명에 의하면, 예열로(2); 예열로(2) 내 배치되고 몰리브덴(Mo)과 규소(Si) 분말의 반응을 개시하기 위한 발열체(8)를 포함하는 반응로(1); 상기 반응로(1) 외벽을 포위하여 배치된 냉각수 관(4); 상기 예열로(2) 내벽에 배치되어 초기 반응열을 높이기 위한 발열체를 포함하는 예열 장치(3); 상기 반응로(1) 내부에 가스를 공급·배출하기 위한 가스관; 및 상기 발열체(8)에 전류를 공급하기 위한 전원 공급부(5)를 구비한 제조장치가 제공된다.According to the present invention, the preheating furnace (2); A reactor 1 disposed in the preheater 2 and including a heating element 8 for initiating the reaction of molybdenum (Mo) and silicon (Si) powder; Cooling water pipe (4) disposed surrounding the outer wall of the reactor (1); A preheating device (3) disposed on an inner wall of the preheating furnace (2) and including a heating element for increasing initial reaction heat; A gas pipe for supplying and discharging gas into the reactor (1); And a power supply unit 5 for supplying current to the heating element 8.

상기 반응로(1)의 벽은 냉각수에 의한 열손실의 저하를 막고 단열을 위해 흑연(graphite) 재질로 제작된다.The wall of the reactor 1 is made of graphite material to prevent heat loss caused by cooling water and to insulate.

상기 예열로(2) 내벽에 배치되는 예열 장치(3)는 전원 공급부(미도시)에 의해 발열되는 발열체에 의해 300∼800℃까지 예열되는 것을 특징으로 한다.The preheating device 3 disposed on the inner wall of the preheating furnace 2 is preheated to 300 to 800 ° C. by a heating element that is generated by a power supply unit (not shown).

상기 냉각수 관(4)은 설비 내부의 순간적 고온화를 방지하기 위한 설비 보호용으로 설치된다.The cooling water pipe 4 is installed to protect the facility to prevent the instantaneous high temperature inside the facility.

상기 가스관의 배출 통로에는 진공 펌프(6)와 진공 게이지(7)가 위치되어 반응로(1) 내부의 압력을 조절한다.A vacuum pump 6 and a vacuum gauge 7 are positioned in the discharge passage of the gas pipe to adjust the pressure inside the reactor 1.

상기 발열체(8)는 코일형 또는 필라멘트형 텅스텐(W)선인 것이 바람직하다.The heating element 8 is preferably a coiled or filamentary tungsten (W) wire.

이하, 실시예를 들어 본 발명의 고순도 2규화 몰리브덴(MoSi2) 분말의 제조방법을 설명하지만, 본 발명이 실시예에 한정되는 것은 아니다.Hereinafter, the production method of the high-purity molybdenum silicide (MoSi 2 ) powder of the present invention will be described with reference to Examples, but the present invention is not limited to Examples.

실시예Example

몰리브덴(Mo) 분말(입도: 2∼20㎛) 170g과 규소(Si) 분말(입도: 5∼15㎛) 100g을 혼합하여 분쇄한 후, 압축하여 케이크 형태로 제조하였다. 상기 케이크를 본 발명의 자전 고온 합성로 반응로(1)에 넣고 1.5kg/cm3기압의 수소(H2) 분위기를 조성하였다. 이후, 반응로(1)의 예열 장치(3)에 의해 300∼800℃까지 온도를 올린 다음, 반응로(1) 내부의 발열체(8)에 전류를 공급하여 1500 ∼ 2000℃까지 반응을 올려 반응을 개시하여 2규화 몰리브덴(MoSi2)을 합성하였다. 합성된 2규화 몰리브덴 (MoSi2)을 분쇄하여 본 발명의 2규화 몰리브덴(MoSi2) 분말(입도: 2∼20㎛)을 얻었다.170 g of molybdenum (Mo) powder (particle size: 2 to 20 µm) and 100 g of silicon (Si) powder (particle size: 5 to 15 µm) were mixed and pulverized, and then compressed to prepare a cake. The cake was placed in a reactor (1) with a rotating high temperature synthesis furnace of the present invention to create a hydrogen (H 2 ) atmosphere of 1.5 kg / cm 3 atm. Thereafter, the temperature is raised to 300 to 800 ° C by the preheater 3 of the reactor 1, and then a current is supplied to the heating element 8 inside the reactor 1 to raise the reaction to 1500 to 2000 ° C. And molybdenum silicide (MoSi 2 ) were synthesized. The synthesized molybdenum silicide (MoSi 2 ) was ground to obtain a molybdenum silicide (MoSi 2 ) powder (particle size: 2 to 20 μm) of the present invention.

상술한 바와 같이, 자전 고온 합성법을 이용하여 제조된 본 발명의 2규화 몰리브덴(MoSi2) 분말은 원료분말의 충진율을 향상시킴으로써 고순도로 수득된다.As described above, the molybdenum bisulfide (MoSi 2 ) powder of the present invention prepared by using a high-temperature rotating synthesis method is obtained by improving the filling rate of the raw powder.

또한 본 발명의 제조장치(자전 고온 합성로)는 외벽을 통한 열손실을 줄이기 위해 냉각장치를 생략하고, 초기 반응열을 높이기 위한 예열 장치(3)를 추가함으로써 2규화 몰리브덴(MoSi2)의 대량생산이 가능하다.In addition, the manufacturing apparatus (automatic high temperature synthesis furnace) of the present invention omits the cooling device to reduce heat loss through the outer wall, and mass production of molybdenum silicide (MoSi 2 ) by adding a preheating device (3) to increase the initial heat of reaction. This is possible.

Claims (8)

1) 몰리브덴(Mo) 분말과 규소(Si) 분말을 혼합하여 분쇄하는 단계,1) mixing and grinding molybdenum (Mo) powder and silicon (Si) powder, 2) 상기 혼합물을 수소(H2) 분위기하에서 자전 고온 합성법을 이용하여 2규화 몰리브덴(MoSi2)을 합성하는 단계, 및2) synthesizing molybdenum silicide (MoSi 2 ) using the mixture at high temperature in a hydrogen (H 2 ) atmosphere, and 3) 합성된 2규화 몰리브덴(MoSi2)을 분쇄하여 분말화하는 단계를 포함하는 2규화 몰리브덴(MoSi2) 분말의 제조방법.3) the synthesis of molybdenum silicide 2 (molybdenum silicide 2 to pulverized MoSi 2) comprising powdered (MoSi 2) process for producing a powder. 제 1항에 있어서, 상기 단계 1)의 분말 혼합물이 케이크 형태인 것을 특징으로 하는 2규화 몰리브덴(MoSi2) 분말의 제조방법.The method of claim 1, wherein the second molybdenum silicide (MoSi 2) process for producing a powder, characterized in that the powder mixture of the cake form of the step 1). 제 1항에 있어서, 상기 단계 2)에서 자전 고온 합성 반응의 개시온도가 300∼800℃이고, 수소(H2) 압력 1.5kg/cm3하에서 진행되는 것을 특징으로 하는 2규화 몰리브덴(MoSi2) 분말의 제조방법.The molybdenum silicide (MoSi 2 ) of claim 1, wherein the starting temperature of the high-temperature synthesis reaction is 300-800 ° C. and proceeds under hydrogen (H 2 ) pressure of 1.5 kg / cm 3 . Method for preparing the powder. 제 1항에 있어서, 상기 단계 3)의 분말이 입도 범위 2∼20㎛인 것을 특징으로 하는 2규화 몰리브덴(MoSi2) 분말의 제조방법.The method for producing molybdenum silicide (MoSi 2 ) powder according to claim 1, wherein the powder of step 3) has a particle size range of 2 to 20 μm. 예열로(2); 예열로(2) 내 배치되고 몰리브덴(Mo)과 규소(Si) 분말의 반응을 개시하기 위한 발열체(8)를 포함하는 반응로(1); 상기 반응로(1) 외벽을 포위하여 배치된 냉각수 관(4); 상기 예열로(2) 내벽에 배치되어 초기 반응열을 높이기 위한 발열체를 포함하는 예열 장치(3); 상기 반응로(1) 내부에 가스를 공급·배출하기 위한 가스관; 및 상기 발열체(8)에 전류를 공급하기 위한 전원 공급부(5)를 포함하는 2규화(MoSi2) 몰리브덴의 제조장치.Preheating furnace 2; A reactor 1 disposed in the preheater 2 and including a heating element 8 for initiating the reaction of molybdenum (Mo) and silicon (Si) powder; Cooling water pipe (4) disposed surrounding the outer wall of the reactor (1); A preheating device (3) disposed on an inner wall of the preheating furnace (2) and including a heating element for increasing initial reaction heat; A gas pipe for supplying and discharging gas into the reactor (1); And a second silicide (MoSi 2) apparatus for manufacturing a molybdenum containing power supply 5 for supplying a current to the heating element (8). 제 5항에 있어서, 상기 반응로(1)의 벽이 흑연(graphite) 재질인 것을 특징으로 하는 2규화(MoSi2) 몰리브덴의 제조장치.The method of claim 5, wherein the second silicide (MoSi 2) production apparatus of molybdenum, characterized in that the wall of the reactor (1) of graphite (graphite) material. 제 5항에 있어서, 상기 가스관의 배출 통로에 반응로(1) 내부의 압력을 조절하기 위한 진공 펌프(6)와 진공 게이지(7)가 배치된 것을 특징으로 하는 2규화(MoSi2) 몰리브덴의 제조장치.6. The molybdenum bisulfide (MoSi 2 ) molybdenum according to claim 5, characterized in that a vacuum pump 6 and a vacuum gauge 7 are arranged in the discharge passage of the gas pipe to adjust the pressure in the reactor 1. Manufacturing equipment. 제 5항에 있어서, 상기 발열체(8)가 코일형 또는 필라멘트형 텅스텐(W)선인 것을 특징으로 하는 2규화(MoSi2) 몰리브덴의 제조장치.6. An apparatus for producing bisulfide (MoSi 2 ) molybdenum according to claim 5, characterized in that the heating element (8) is a coiled or filamentary tungsten (W) wire.
KR1020020008800A 2002-02-19 2002-02-19 Method and apparatus for producing molybdenum disilicide powder using self-propagating high-temperature synthesis(SHS) KR20030068962A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100491328B1 (en) * 2002-08-27 2005-05-25 한국기계연구원 Porous mosi2 material by self-propagating high temperature synthesis, and manufacturing method thereof
KR100736604B1 (en) * 2005-11-14 2007-07-09 엘지전자 주식회사 Method and apparatus for manufacturing dielectric material powder and the panel using the same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100491328B1 (en) * 2002-08-27 2005-05-25 한국기계연구원 Porous mosi2 material by self-propagating high temperature synthesis, and manufacturing method thereof
KR100736604B1 (en) * 2005-11-14 2007-07-09 엘지전자 주식회사 Method and apparatus for manufacturing dielectric material powder and the panel using the same

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