KR100321294B1 - Preparation of carbide or boride ceramic powder by self-propagation high temparature synthesis - Google Patents
Preparation of carbide or boride ceramic powder by self-propagation high temparature synthesis Download PDFInfo
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- KR100321294B1 KR100321294B1 KR1019990016772A KR19990016772A KR100321294B1 KR 100321294 B1 KR100321294 B1 KR 100321294B1 KR 1019990016772 A KR1019990016772 A KR 1019990016772A KR 19990016772 A KR19990016772 A KR 19990016772A KR 100321294 B1 KR100321294 B1 KR 100321294B1
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- 239000000843 powder Substances 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 title claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000001308 synthesis method Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007858 starting material Substances 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 238000011002 quantification Methods 0.000 claims 2
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000011812 mixed powder Substances 0.000 description 5
- 229910001120 nichrome Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- -1 B 2 O 3 Chemical compound 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
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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
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
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Abstract
본 발명은 자전고온 합성법에 의한 카바이드 또는 보라이드 세라믹 분말 제조방법으로서, 반응기 내부의 압력을 5 내지 15 기압의 고압으로 유지함으로써 자전고온 합성법(self-propagating high-temperature synthesis, SHS)의 문제점인 미완결 반응 문제점을 해결하여 효율적으로 카바이드(carbide) 또는 보라이드(boride) 세라믹 분말을 제조하는 방법에 관한 것이다.The present invention is a carbide or boride ceramic powder manufacturing method by a high-temperature synthesis method, by maintaining the pressure inside the reactor at a high pressure of 5 to 15 atm uncompleted problem of the self-propagating high-temperature synthesis (SHS) The present invention relates to a method of efficiently producing a carbide or boride ceramic powder by solving a reaction problem.
본 발명에 의하면, 반응중 발생하는 산소를 제거하기 위하여 사용되는 금속(Mg 도는 Al)의 휘발을 억제하고, 반응 중에 생기는 압력증가를 억제할 수 있으며, 반응 과정중의 반응기 내의 압력차이를 작게하여 반응이 보다 균일하게 진행되게 할 뿐 아니라, 완전한 반응을 가능하게 한다.According to the present invention, the volatilization of the metal (Mg or Al) used to remove oxygen generated during the reaction can be suppressed, and the pressure increase generated during the reaction can be suppressed, and the pressure difference in the reactor during the reaction process can be reduced. Not only does the reaction proceed more uniformly, but it also enables a complete reaction.
Description
본 발명은 자전고온 합성법에 의한 카바이드 또는 보라이드 세라믹 분말 제조방법으로서, 상세하게는 화학반응열을 이용하여 화합물을 제조하는 방법, 즉, 일단 외부의 점화로 반응이 시작되면 이 때 생성되는 반응열로 인하여 반응이 자발적으로 진행되는 공정을 이용하는 합성법에 있어서, 반응기 내부의 압력을 고압으로 유지함으로써 자전고온 합성법(self-propagating high-temperature synthesis, SHS)의 문제점인 미완결 반응 문제점을 해결하여 효율적으로 카바이드(carbide) 또는 보라이드(boride) 세라믹 분말을 제조하는 방법에 관한 것이다.The present invention is a method for preparing carbide or boride ceramic powder by the autothermal synthesis method, in detail, a method for preparing a compound using the heat of chemical reaction, that is, once the reaction is started by the external ignition due to the reaction heat generated at this time In the synthesis method using a process in which the reaction proceeds spontaneously, by maintaining the pressure inside the reactor at a high pressure, carbides are effectively solved by solving the problem of incomplete reaction which is a problem of self-propagating high-temperature synthesis (SHS). Or a boride ceramic powder.
자전고온 합성법에 의한 카바이드 또는 보라이드 세라믹 분말의 합성은 많이 시도되고 또한 알려져 있다. 이러한 종래의 방법에서는 반응기 내부의 압력을 대기압 또는 진공으로 유지하고 있음으로써 일반적으로 반응이 완전히 진행되지 않고 중간에서 멈추는 문제점을 가지는 한편, 반응속도가 고르게 전파되지 못하여 생성물의 입자분포가 크며, 미완성 반응으로 인하여 반응이 종료된 후에도 출발원료가 남아있는 문제점을 가진다. 또한 반응과정에서 압력의 증가가 크게 일어나기 때문에 대량으로 반응시키는데 한계가 있어서 주로 소량규모로 이루어져 왔다.Synthesis of carbide or boride ceramic powders by autothermal synthesis has been tried and known a lot. In such a conventional method, the pressure inside the reactor is maintained at atmospheric pressure or vacuum, which generally causes a problem that the reaction does not proceed completely but stops in the middle, while the reaction rate does not propagate evenly, resulting in a large particle distribution of the product and an unfinished reaction. Due to the problem that the starting material remains even after the reaction is completed. In addition, since there is a large increase in pressure during the reaction process, there is a limit to the reaction in large quantities, and has been mainly made in a small amount.
본 발명의 목적은 전술한 종래기술의 문제점을 해결하기 위한 것으로, 균일하고 완전한 자전고온 합성법에 의하여 순도 높은 카바이드 또는 보라이드 세라믹 분말을 제조하는 방법을 제공하는 것이다.An object of the present invention is to solve the above-mentioned problems of the prior art, and to provide a method for producing carbide or boride ceramic powder of high purity by a uniform and complete autothermal synthesis method.
본원 발명의 다른 목적은 반응중 발생하는 산소를 제거하기 위하여 사용되는 Mg, 또는 Al금속의 휘발을 줄일 수 있는 카바이드 또는 보라이드 세라믹 분말 제조방법을 제공하는 것이다.Another object of the present invention is to provide a carbide or boride ceramic powder production method that can reduce the volatilization of Mg, or Al metal used to remove oxygen generated during the reaction.
본 발명은 자전고온 합성법에 의한 카바이드 또는 보라이드 세라믹 분말 제조방법으로서, 상기의 목적을 달성하기 위한 본 발명의 특징은 종래의 방법과는 달리, 반응원료의 분말 크기를 한정하고, 자전고온 합성 반응기 내부에 5 내지 15 기압의 압력을 인가한 후에 점화를 개시하는 것을 특징으로 한다. 이러한 방법을 사용하면 산소를 제거하기 위하여 사용되는 금속(Mg 도는 Al)의 휘발을 억제하고, 반응 중에 생기는 압력증가를 억제할 수 있으며, 반응 과정중의 압력차이를 작게하여 반응이 보다 균일하게 진행될 수 있다. 또한, 점화 전에 반응기 안을 아르곤과 같은 불활성 가스로 수 차례 씻어 냄으로써 반응기 안의 공기 잔류량을 적게하는 것을 특징으로 한다.The present invention is a carbide or boride ceramic powder manufacturing method by a high-temperature synthesis method, the characteristics of the present invention for achieving the above object, unlike the conventional method, limits the powder size of the reaction raw material, auto-high temperature synthesis reactor Inside Ignition is started after applying a pressure of 5 to 15 atm. This method can suppress the volatilization of the metal (Mg or Al) used to remove oxygen, suppress the increase in pressure during the reaction, and reduce the pressure difference during the reaction to make the reaction proceed more uniformly. Can be. In addition, by rinsing the inside of the reactor several times with an inert gas such as argon before ignition, it is characterized in that the residual amount of air in the reactor is reduced.
본 발명의 구성을 구체적으로 살펴보면, -50메쉬(300㎛ 이하) 크기의 금속분말과 -100메쉬(150㎛ 이하) 크기를 가지는 반응 정량의 보론(B) 또는 카본(C)분말을 혼합하는 과정과, 혼합된 혼합물을 자전 고온 합성 반응기 내부에 적당히 배치하고 아르곤과 같은 불활성 가스를 반응기 안에 채운후 다시 내보냄으로써 반응기 안의 공기를 제거하는 공정과, 반응기 내부압력이 5 내지 15기압이 되도록 불활성 가스를 인가한 후 점화시키는 공정 및 반응기를 충분하게 냉각한 후 생성물을 분쇄하는 공정으로 이루어지는 것을 특징으로 한다.Looking specifically at the configuration of the present invention, the process of mixing the boron (B) or carbon (C) powder of the reaction quantitative having a -50 mesh (300㎛ or less) size metal powder and -100 mesh (150㎛ or less) size And removing the air in the reactor by appropriately disposing the mixed mixture inside the autoclave high temperature synthesis reactor and filling the reactor with an inert gas such as argon and then sending it out again, and inert gas such that the pressure inside the reactor is 5 to 15 atm. It is characterized by consisting of a process of igniting and then igniting the product and then cooling the reactor sufficiently and then grinding the product.
또한, 본원 발명의 다른 태양으로는, 가격이 비교적 저렴한 B2O3와 같은 보론 산화물을 이용하여 B4C와 같은 세라믹 분말을 합성하기 위한 방법으로서, -60메쉬(270㎛ 이하) 크기의 제 1 산화물 출발원료와 반응 정량의 제 2 원료 및 발생된 산소를 제거하기 위하여 사용되는 -50메쉬(300㎛ 이하) 크기를 가지는 반응 정량의 Mg 또는 Al 분말을 혼합하는 공정과, 혼합된 혼합물을 자전 고온 합성 반응기 내부에 적당히 배치하고 아르곤과 같은 불활성 가스를 반응기 안에 채운후 다시 내보냄으로써 반응기 안의 공기를 제거하는 공정과, 반응기 내부압력이 5 내지 15기압이 되도록 불활성 가스를 인가한 후 점화시켜 자전 고온 합성반응을 일으키는 공정 및 반응기를 충분하게 냉각한 후 생성물을 분쇄하는 공정으로 이루어지는 것을 특징으로 한다. 예컨데, B4C를 제조하기 위해서는 상기 제 1 산화물 출발원료로 B2O3를, 제 2 출발원료로 C를, 산소제거용 금속으로는 Mg 또는 Al을 사용한다.In another aspect of the present invention, a method for synthesizing a ceramic powder such as B 4 C using boron oxide such as B 2 O 3 , which is relatively inexpensive, includes a -60 mesh (270 μm or less) agent. 1 A process of mixing an oxide starting material, a second raw material of the reaction quantity and a reaction quantity of Mg or Al powder having a size of -50 mesh (less than 300 μm) used to remove the generated oxygen, and rotating the mixed mixture It is appropriately placed inside the high temperature synthesis reactor and filled with an inert gas such as argon into the reactor and then sent out again to remove air in the reactor. It is characterized by consisting of a step of pulverizing the product after sufficiently cooling the reactor and the step causing the synthesis reaction. For example, in order to manufacture B 4 C, B 2 O 3 is used as the first oxide starting material, C is used as the second starting material, and Mg or Al is used as the oxygen removal metal.
출발원료들의 혼합을 위하여 30분 내지 1시간에 걸친 건식 지르코니아 볼밀링을 수행할 수 있으나 혼합방법은 이에 제한되지 않는다.Dry zirconia ball milling may be carried out for 30 minutes to 1 hour for mixing the starting materials, but the mixing method is not limited thereto.
아래에 설명되는 본원 발명의 제 1 실시예에서는 금속으로 Ti(티타늄)을 사용하여 TiB2및 TiC를 제조하였으며, 제 2 실시예에서는 제 1 산화물 출발원료로 B2O3를, 제 2 출발원료로 C를, 산소제거용 금속으로는 Mg 또는 Al을 사용함으로써 B4C를 제조하는 방법에 대하여 기술하고 있으나, 본 발명이 이러한 실시예에 한정되는 것은 아니다.In the first embodiment of the present invention described below, TiB 2 and TiC were prepared using Ti (titanium) as the metal, and in the second embodiment, B 2 O 3 was used as the first oxide starting material, and the second starting material. Furnace C is described as a method for producing B 4 C by using Mg or Al as the metal for oxygen removal, but the present invention is not limited to these examples.
[실시예 1]Example 1
-50 메쉬 크기의 Ti분말 0.2몰과, -100메쉬 크기의 B분말 0.4몰을 폴리프로필렌 용기에 넣고, 직경 5mm의 지르크니아 볼을 이용하여 약 30분간 건식 볼밀링한 후, 체를 이용하여 볼을 분리한다. 혼합분말을 흑연 도가니(graphite crucible) 내에 쌓은 후, 도가니를 2리터의 반응기에 넣고 니크롬 코일을 상기 혼합분말 안에 장착시킨 후, 아르곤 가스를 3기압 정도로 채운 후 내보내고, 다시 채운 후 내보내는 과정을 두, 세차례 반복함으로써 반응기 안의 잔류 공기를 제거하고, 반응기 내부의 압력이 10 기압이 되도록 아르곤 가스를 채웠다. 그 후에 니크롬 코일에 전기를 통해 점화시켜 압력계가 약간 증가할 때 전기 스위치를 끈다. 압력계는 약간 더 증가한 후에 떨어지기 시작하였다. 약 20분 정도 기다렸다가 반응기가 식었을 때 반응기를 열고 엉성하고 딱딱해진 한 개의 덩어리를 꺼냈다. 이 덩어리를 바이브레이션 밀을 사용하여 분쇄한 후 XRD(X선 회절)을 측정한 결과 TiB2피크만 나타났다. 이렇게 제조된 분말의 입도분포는 325메쉬 이하였다.0.2 mol of Ti powder of -50 mesh size and 0.4 mol of B powder of -100 mesh size are placed in a polypropylene container, and dry ball milling for about 30 minutes using a zirconia ball having a diameter of 5 mm, and then Remove the ball. After the mixed powder is stacked in a graphite crucible, the crucible is placed in a reactor of 2 liters, a nichrome coil is mounted in the mixed powder, filled with argon gas at about 3 atm, and then discharged, and then discharged again. By repeating three times, residual air in the reactor was removed, and argon gas was charged so that the pressure inside the reactor was 10 atm. Thereafter, the nichrome coil is electrically ignited to turn off the electrical switch when the pressure gauge increases slightly. The pressure gauge started to fall after a slight increase. After waiting for about 20 minutes, when the reactor cooled down, the reactor was opened and one loose, lumpy mass was taken out. The mass was pulverized using a vibration mill and XRD (X-ray diffraction) was measured.2Only peaks appeared. Of the powder so prepared The particle size distribution was less than 325 mesh.
[실시예 2]Example 2
-50메쉬 크기의 Ti분말 1.0몰과 -325메쉬 크기의 C분말 1.0몰을 실시예 1에서와 동일한 방법으로 혼합하고 반응시켜 엉성하고 딱딱해진 하나의 덩어리를 얻었다. XRD 측정결과 TiC 피크만 나타났다. 또한, 혼합된 분말을 지름 20mm 두께 30mm의 디스크로 만들어 실시예 1과 동일한 방법으로 자전고온 반응을 일으켰다. 반응 결과 부피가 약 1.5배 정도 늘어난 타원형 디스크로 변하였다.1.0 mole of -50 mesh Ti powder and 1.0 mole of -325 mesh C powder were mixed and reacted in the same manner as in Example 1 to obtain a coarse, hardened mass. XRD measurements showed only TiC peaks. In addition, the mixed powder was made into a disk having a diameter of 20 mm and a thickness of 30 mm to cause a high-temperature reaction in the same manner as in Example 1. The reaction resulted in an elliptical disc with a volume about 1.5 times greater.
[실시예 3]Example 3
+100메쉬 크기의 B2O3분말 4.0몰과, -50메쉬 크기의 Mg분말 12몰과, -325메쉬 크기의 C 2.0몰을 1리터 용량의 프로필렌통에 넣고, 지름 5mm의 지르코니아 볼을 사용하여 약 1시간동안 건식 볼 밀링하였다. 이렇게 혼합된 분말을 실시예 1에 서술한 방법으로 반원통형 흑연 도가니(graphite crucible)에 가득 채운 후 도가니를 반응기 내부에 넣고 니크롬 코일을 분말 바로 위에 고정시키고, 실시예 2에서와 같이 혼합된 Ti와 C의 혼합분말로 니크롬 코일 주위를 덮었다. 아르곤 가스로 반응기를 약 3기압으로 채운후 내보내는 과정을 두번 반복함으로써 반응기 내부의 공기를 제거하였다. 그 후에 반응기 내부의 압력이 약 10기압이 되도록 아르곤 가스를 채운후 실시예 1에서와 같은 자전고온 합성반응을 일으켰다. 이 때는 반응물의 양이 많아서 약 1시간 정도의 냉각시간을 주었다. 한 덩어리로 된 반응 생성물을 분리한 후 니크롬 코일 부근의 TiC를 긁어서 제거하였다. 이 덩어리를 분쇄한 후 XRD 측정한 결과 출발물질인 B2O3와 Mg는 나타나지 않고 B4C와 MgO 만 나타났다.4.0 moles of +100 mesh B 2 O 3 powder, 12 moles of -50 mesh Mg powder, and 2.0 moles of -325 mesh C are placed in a 1-liter propylene container and 5 mm zirconia balls are used. Dry ball milling for about 1 hour. The mixed powder was filled in a semi-cylindrical graphite crucible by the method described in Example 1, the crucible was placed inside the reactor, and the nichrome coil was fixed directly on the powder. The mixed powder of C was covered around the nichrome coil. After filling the reactor with argon gas at about 3 atm, the air inside the reactor was removed by repeating the process twice. Thereafter, an argon gas was charged so that the pressure inside the reactor was about 10 atm, and the autothermal synthesis reaction as in Example 1 was performed. At this time, a large amount of reactants gave a cooling time of about 1 hour. The mass of reaction product was separated and then TiC near the nichrome coil was scraped off. After the mass was crushed, XRD measurement showed no starting materials B 2 O 3 and Mg but only B 4 C and MgO.
H2SO4를 이용한 산처리로 혼합물로부터 MgO를 MgSO4로 분리하여 제거한 후 최종 물질인 B4C 분말을 얻었다.MgO was removed by MgSO 4 from the mixture by acid treatment with H 2 SO 4, and the final material, B 4 C powder, was obtained.
[실시예 4]Example 4
+100메쉬 크기의 B2O3분말 5.0몰과, -200메쉬 크기의 Al분말 10.0몰과, -325메쉬 크기의 C분말 2.5몰을 실시예 3과 같은 방법으로 혼합하고 자전고온 반응시켰다. 압력은 천천히 증가하여 35기압까지 올라갔다. 초기압력인 10기압까지 떨어졌을 때 아르곤 가스를 빼고 반응기를 열어 한 덩어리의 생성물을 얻었다. 점화제로 쓰인 TiC를 제거한 후 분쇄하여 XRD 측정한 결과 B4C와 Al2O3의 혼합물로 이루어져 있었다. 같은 종류의 반응을 초기 압력 10 기압 대신에 5기압과 15기압에서 시작하였다. 5기압의 경우는 10기압의 경우와 마찬가지로 XRD상 Al2O3와B4C의 피크만 나타났다. 그러나 15기압의 경우 반응 생성물의 안쪽은 반응이 완전히 진행되어 Al2O3와B4C의 피크만 나타났으나, 반응 생성물의 바깥 부분은 Al2O3와B4C외에도 시작물질인 Al과 B2O3피크가 XRD상에 나타나, 바깥 부분은 반응이 완전히 진행되지 못하였였음을 알 수 있었다.5.0 mol of B 2 O 3 powder of +100 mesh size, 10.0 mol of Al powder of -200 mesh size, and 2.5 mol of C powder of -325 mesh size were mixed in the same manner as in Example 3 and subjected to autothermal reaction. The pressure slowly increased to 35 atm. When the initial pressure dropped to 10 atm, argon gas was removed and the reactor was opened to obtain a mass of the product. After removing TiC used as an ignition agent and pulverizing, XRD measurement resulted in a mixture of B 4 C and Al 2 O 3 . The same kind of reaction started at 5 and 15 atm instead of 10 atm. In the case of 5 atm, only peaks of Al 2 O 3 and B 4 C appeared on XRD. However, in the case of 15 atmospheres in the inside of the reaction product is the reaction is completely conducted Al 2 O outside of the 3 and B 4 peaks, only the nateu or, in C the reaction product began in addition to Al 2 O 3 and B 4 C material Al and The B 2 O 3 peak appeared on the XRD, indicating that the outer portion of the reaction did not proceed completely.
자전고온 합성법(self-propagating high-temperature synthesis, SHS)에서 반응기 내부의 압력을 5내지 15 기압의 고압으로 유지함으로써, 반응 중에 생기는 압력증가를 억제할 수 있으며, 반응 과정중의 압력차이를 작게하여 반응이 보다 균일하게 진행되게 할 뿐 아니라, 완전한 반응을 가능하게 하여, 효율적으로 순도 높은 카바이드(carbide) 또는 보라이드(boride) 세라믹 분말을 합성할 수 있다는 장점을 가진다.In the self-propagating high-temperature synthesis (SHS), the pressure inside the reactor is maintained at a high pressure of 5 to 15 atm, thereby suppressing the increase in pressure during the reaction and reducing the pressure difference during the reaction. Not only does the reaction proceed more uniformly, but also enables the complete reaction, which has the advantage of efficiently synthesizing high purity carbide or boride ceramic powder.
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