KR20060093312A - Apparatus and method of tantalum carbide production by external continuous supply process - Google Patents

Apparatus and method of tantalum carbide production by external continuous supply process Download PDF

Info

Publication number
KR20060093312A
KR20060093312A KR1020060068236A KR20060068236A KR20060093312A KR 20060093312 A KR20060093312 A KR 20060093312A KR 1020060068236 A KR1020060068236 A KR 1020060068236A KR 20060068236 A KR20060068236 A KR 20060068236A KR 20060093312 A KR20060093312 A KR 20060093312A
Authority
KR
South Korea
Prior art keywords
raw material
tantalum carbide
diluent
reducing agent
external continuous
Prior art date
Application number
KR1020060068236A
Other languages
Korean (ko)
Inventor
배인성
Original Assignee
배인성
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 배인성 filed Critical 배인성
Priority to KR1020060068236A priority Critical patent/KR20060093312A/en
Publication of KR20060093312A publication Critical patent/KR20060093312A/en

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F21/00—Dissolving
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys

Abstract

개시된 내용은 외부연속공급법에 의해 탄탈륨카바이드를 제조하는 탄탈륨카바이드 제조장치 및 방법에 관한 것이다.Disclosed is a tantalum carbide production apparatus and method for producing tantalum carbide by an external continuous feeding method.

본 발명의 외부연속공급법에 의한 탄탈륨카바이드 제조장치는 원료(오산화탄탈륨, 카본, 마그네슘 등)들이 산소와 결합하여 산화되는 것을 방지하기 위한 진공장치; 희석제와 환원제가 장입된 반응용기를 적정온도로 가열하기 위한 발열장치; 원료(오산화탄탈륨, 카본, 희석제 등)를 외부에서 연속적으로 장입시키 위한 원료외부연속공급장치를 포함하는 외부연속공급법에 의한 탄탈륨카바이드 제조장치로서 달성된다.Tantalum carbide production apparatus according to the external continuous supply method of the present invention is a vacuum device for preventing the raw material (tantalum pentoxide, carbon, magnesium, etc.) to be combined with oxygen and oxidized; A heating device for heating the reaction vessel loaded with the diluent and the reducing agent to an appropriate temperature; It is achieved as a tantalum carbide production apparatus by an external continuous feed method including a raw material external continuous supply device for continuously charging raw materials (tantalum pentoxide, carbon, diluent, etc.) from the outside.

본 발명의 외부연속공급법에 의한 탄탈륨카바이드 제조방법은 반응챔버 내의 잔류산소를 제거하고, 환원제와 일부 희석제를 적정온도로 일정시간 가열하는 하소단계; 상기 하소단계에서 용해된 환원제와 원료와의 반응을 위해 반응용기내에 원료를 일정한 속도로 연속적으로 장입하는 원료공급단계; 상기 원료공급단계에서 환원제와 원료가 반응하여 탄탈륨카바이드를 생성하는 탄탈륨카바이드 생성단계를 포함하는 외부연속공급법에 의한 탄탈륨카바이드 제조방법으로 달성된다.Tantalum carbide production method according to the external continuous supply method of the present invention is a calcination step of removing residual oxygen in the reaction chamber, heating the reducing agent and some diluent to a proper temperature for a predetermined time; A raw material supply step of continuously charging the raw materials into the reaction vessel at a constant rate for reaction between the reducing agent dissolved in the calcination step and the raw materials; In the raw material supply step is achieved with a tantalum carbide production method by an external continuous feed method comprising a tantalum carbide generation step of reacting the reducing agent and the raw material to produce tantalum carbide.

외부연속공급법, 탄탈륨카바이드, 탄탈륨카바이드제조장치, 탄탈륨카바이드제조방법  External continuous supply method, tantalum carbide, tantalum carbide manufacturing apparatus, tantalum carbide manufacturing method

Description

외부연속공급법에 의한 탄탈륨카바이드 제조장치 및 방법{Apparatus and method of tantalum carbide production by external continuous supply process}Apparatus and method of tantalum carbide production by external continuous supply process

도 1은 종래의 탄탈륨카바이드 제조장치 및 방법을 설명하기 위한 구성도1 is a configuration diagram for explaining a conventional tantalum carbide production apparatus and method

도 2는 본 발명에 따른 외부연속공급법에 의한 탄탈륨카바이드 제조장치 및 방법을 설명하기 위한 구성도2 is a block diagram for explaining a tantalum carbide production apparatus and method by an external continuous supply method according to the present invention.

본 발명은 외부연속공급법에 의한 탄탈륨카바이드 제조장치 및 방법에 관한 것으로, 특히 원료외부연속공급장치를 이용하여 진공챔버 내부의 반응용기에 원료(Ta2O5), 온도제어를 위한 희석제(KCl, NaCl 등), 카본(C)을 일정한 속도로 연속적으로 공급할 수 있게 함으로서 반응용기에 용해되어 있는 환원제와 외부에서 공급하는 원료가 반응하여 입자가 작고 균일한 탄탈륨카바이드를 제조하는 탄탈륨카바이드 제조장치 및 방법에 관한 것이다. The present invention relates to a tantalum carbide production apparatus and method by an external continuous supply method, in particular, a raw material (Ta 2 O 5 ), a diluent (KCl) for temperature control in the reaction vessel inside the vacuum chamber using an external continuous supply device. , NaCl, etc.) and the tantalum carbide production apparatus for producing a small and uniform tantalum carbide particles by reacting the reducing agent dissolved in the reaction vessel and the raw material supplied from the outside by allowing the continuous supply of carbon (C) at a constant rate and It is about a method.

일반적으로 탄탈륨카바이드는 초경합금의 내산화성을 향상시킴과 동시에 WC와 TiC의 입자성장을 억제하고, 내마모성과 강도를 향상시키기 위해 첨가제로 사용 되고 있으며, 절삭공구에서부터 내마모, 내충격용 공구, 고온 고압용 부품 및 초내열재료 등 넓은 범위에 사용되고 있다. 그러나 이와 같이 널리 사용되고 있는 탄탈륨카바이드는 그 제조공정에 있어서 온도제어가 어렵기 때문에 입자크기가 불균일하고 불순물이 많이 함유되는 등 고품질의 탄탈륨카바이드를 제조하는데 있어서 문제점이 있었다. 이에 대한 종래의 실시예를 도 1에 나타내었다.Generally, tantalum carbide is used as an additive to improve the oxidation resistance of cemented carbide and to suppress grain growth of WC and TiC, and to improve wear resistance and strength, and to be abrasion resistant, impact resistant tool, and high temperature and high pressure. It is used in a wide range of parts and super heat-resistant materials. However, such a widely used tantalum carbide has a problem in producing high quality tantalum carbide, such as non-uniform particle size and a large amount of impurities because it is difficult to control the temperature in the manufacturing process. A conventional embodiment thereof is shown in FIG. 1.

도 1은 종래의 탄탈륨카바이드 제조장치 및 방법을 설명하기 위한 구성도이다. 종래의 탄탈륨카바이드 제조는 금속열환원법을 이용하였다. 1 is a configuration diagram for explaining a conventional tantalum carbide production apparatus and method. Conventional tantalum carbide production using a metal thermal reduction method.

이에 대한 대략적인 제조공정은 원료로서 오산화탄탈륨(Ta2O5), 환원제로서 마그네슘(Mg), 합성제로서 카본(C)을 일정한 비율로 일정시간 볼밀 등을 이용하여 혼합한 후, 진공챔버(1)내의 반응용기(2)에 장입한다. 그리고 진공펌프(3)로 진공을 유지하고, 가스취입구(4)를 통해 불활성가스를 유입시켜 진공챔버(1) 내부의 산소를 가스배출구(5)를 통하여 배출시키고, 발열체(6)로 600~1200℃로 가열하여 혼합물의 원활한 반응을 위해 교반기(7)를 이용하여 일정한 속도로 교반하면서 환원반응을 실시한 후, 상온까지 충분히 냉각하여 반응용기(2)내에 고착되어 있는 생성물(탄탈륨카바이드+산화마그네슘)을 용해 분리하여 회수하는 방법으로 제조하였다.An approximate manufacturing process for this is a mixture of tantalum pentoxide (Ta 2 O 5 ) as a raw material, magnesium (Mg) as a reducing agent, and carbon (C) as a synthesizing agent at a constant ratio using a ball mill for a predetermined time, and then a vacuum chamber ( Charge into reaction container 2 in 1). Then, the vacuum is maintained by the vacuum pump 3, an inert gas is introduced through the gas inlet 4, and oxygen in the vacuum chamber 1 is discharged through the gas outlet 5, and the heating element 6 is 600. In order to smoothly react the mixture by heating to ˜1200 ° C., the reduction reaction was carried out while stirring at a constant speed using a stirrer (7), and then cooled sufficiently to room temperature to fix the product (tantalum carbide + oxidation). Magnesium) to dissolve and recover.

그러나 이와 같은 탄탈륨카바이드 제조공정은 원료와 환원제 및 카본의 반응으로 인한 큰 발열을 제어하기 못하기 때문에 급격한 반응온도의 상승으로 인해 입자성장이 촉진되어 상대적으로 큰 입자를 가지며, 또한 입자가 불균일한 문제점이 있었다.However, since the tantalum carbide manufacturing process cannot control a large heat generation caused by the reaction between the raw material, the reducing agent, and carbon, particle growth is promoted due to a sudden rise in the reaction temperature, and thus, the particles are relatively large. There was this.

따라서, 본 발명의 목적은 상기에서와 같은 문제점을 해결하기 위해 안출한 것으로, 원료외부연속공급장치를 이용하여 반응챔버 내부의 반응용기에 원료, 온도제어를 위한 희석제, 카본을 일정한 속도로 연속적으로 공급할 수 있게 함으로서 반응용기에 용해되어 있는 환원제와 외부에서 공급하는 원료가 반응하여 입자가 작고 균일한 탄탈륨카바이드를 제조하는데 목적이 있다. Accordingly, an object of the present invention is to solve the problems as described above, by using a continuous feed outside the raw material to continuously feed the raw material, diluent for temperature control, carbon to the reaction vessel inside the reaction chamber at a constant rate It is possible to supply the reducing agent dissolved in the reaction vessel and the raw material supplied from the outside to react to produce a small and uniform tantalum carbide particles.

이와 같은 목적을 달성하기 위한 본 발명에 따른 외부연속공급법에 의한 탄탈륨카바이드 제조장치는 원료(오산화탄탈륨, 카본, 마그네슘 등)들이 산소와 결합하여 산화되는 것을 방지하기 위한 진공장치; 희석제와 환원제가 장입된 반응용기를 적정온도로 가열하기 위한 발열장치; 원료(오산화탄탈륨, 카본, 희석제 등)를 외부에서 연속적으로 장입시키 위한 원료외부연속공급장치를 포함하는 외부연속공급법에 의한 탄탈륨카바이드 제조장치로서 달성된다.An apparatus for manufacturing tantalum carbide by an external continuous supply method according to the present invention for achieving the above object includes a vacuum device for preventing raw materials (tantalum pentoxide, carbon, magnesium, etc.) from being combined with oxygen and oxidized; A heating device for heating the reaction vessel loaded with the diluent and the reducing agent to an appropriate temperature; It is achieved as a tantalum carbide production apparatus by an external continuous feed method including a raw material external continuous supply device for continuously charging raw materials (tantalum pentoxide, carbon, diluent, etc.) from the outside.

이와 같은 목적을 달성하기 위한 본 발명에 따른 외부연속공급법에 의한 탄탈륨카바이드 제조방법은 반응챔버 내의 잔류산소를 제거하고, 환원제와 일부 희석제를 적정온도로 일정시간 가열하는 하소단계; 상기 하소단계에서 용해된 환원제와 원료와의 반응을 위해 반응용기내에 원료를 일정한 속도로 연속적으로 장입하는 원료공급단계; 상기 원료공급단계에서 환원제와 원료가 반응하여 탄탈륨카바이드를 생성하는 탄탈륨카바이드 생성단계를 포함하는 외부연속공급법에 의한 탄탈륨카바이드 제조방법으로 이루어진다.Tantalum carbide production method by an external continuous supply method according to the present invention for achieving the above object is a calcination step of removing residual oxygen in the reaction chamber, heating the reducing agent and some diluent to a proper temperature for a predetermined time; A raw material supply step of continuously charging the raw materials into the reaction vessel at a constant rate for reaction between the reducing agent dissolved in the calcination step and the raw materials; In the raw material supply step is made of a tantalum carbide production method by an external continuous feed method comprising a tantalum carbide generation step of reacting the reducing agent and the raw material to produce tantalum carbide.

이하, 본 발명의 바람직한 실시예를 도면을 통해 상세히 설명한다.Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings.

도 2는 본 발명에 따른 외부연속공급법에 의한 탄탈륨카바이드 제조장치 및 방법을 설명하기 위한 구성도이다.2 is a block diagram for explaining a tantalum carbide production apparatus and method by an external continuous supply method according to the present invention.

상기 도 2에 따른 본 발명에 따른 외부연속공급법에 의한 탄탈륨카바이드 제조장치는 원료(오산화탄탈륨, 카본, 마그네슘 등)들이 산소와 결합하여 산화되는 것을 방지하기 위한 진공장치; 반응챔버(100)내의 희석제와 환원제가 장입된 반응용기(110)를 적정온도로 가열하기 위한 발열장치; 원료(오산화탄탈륨, 카본, 희석제 등)를 외부에서 연속적으로 장입시키 위한 원료외부연속공급장치(120)로 이루어진다.The tantalum carbide production apparatus according to the external continuous supply method according to the present invention according to FIG. 2 includes a vacuum device for preventing raw materials (tantalum pentoxide, carbon, magnesium, etc.) from being combined with oxygen and oxidized; A heating device for heating the reaction vessel 110 in which the diluent and the reducing agent in the reaction chamber 100 are charged to an appropriate temperature; It consists of the raw material external continuous supply apparatus 120 for continuously charging a raw material (tantalum pentoxide, carbon, a diluent, etc.) from the outside.

진공장치는 반응용기(110) 및 반응챔버(100) 내부에 진공압을 발생시키는 진공펌프(130)로 구성되어 있고, 이 반응챔버(100)는 내부에 환원제와 희석제가 장입된 반응용기(110)를 구비하고, 아르곤 가스 등의 불활성 가스를 취입하여 산소를 배출하기 위한 가스취입구(140)와 배출구(150)를 구비하며, 진공압력에 의해 상부가 개폐되는 것을 방지하기 위해 클램프 형식의 잠금장치(160)가 있는 덮개(170)를 구비하고 있으며, 진공펌프(130)의 개/폐를 위해 전기로 하우징(200) 정면에 조절밸브(210)를 구비하고 있다. The vacuum apparatus is composed of a reaction vessel 110 and a vacuum pump 130 for generating a vacuum pressure inside the reaction chamber 100, the reaction chamber 100 is a reaction vessel 110 is charged with a reducing agent and diluent therein And a gas inlet 140 and an outlet 150 for discharging oxygen by injecting an inert gas such as argon gas, and a clamp type lock to prevent the upper part from being opened and closed by vacuum pressure. A cover 170 with the device 160 is provided, and a control valve 210 is provided on the front of the furnace housing 200 for opening / closing the vacuum pump 130.

발열장치는 전기로 하우징(200)과 열선의 저항을 이용하여 열을 발생하는 발열체(220)와 발열체(220)에 의해 발생하는 온도를 조절하는 온도조절장치(230)로 이루어져 있다. 전기로 하우징(200)의 상부에는 반응챔버(102)가 삽입되는 요홈(240)을 구비하고, 이 요홈(240)의 벽부에는 발열체(220)가 있으며, 전기로 하 우징(200) 정면에 온도조절을 위해 온도조절장치(230)를 구비하고 있고, 반응시 전류와 전압을 나타내주는 전류계(250), 전압계(260) 및 전원스위치(270)가 구비되어 있다.The heating device is composed of a heating element 220 for generating heat using the resistance of the electric furnace housing 200 and the heating wire and a temperature control device 230 for controlling the temperature generated by the heating element (220). The upper part of the furnace housing 200 is provided with a recess 240 into which the reaction chamber 102 is inserted, and a wall of the recess 240 has a heating element 220 and a temperature in front of the furnace housing 200. It is provided with a temperature control device 230 for the control, and is provided with an ammeter 250, a voltmeter 260 and a power switch 270 that indicates the current and voltage in the reaction.

원료 외부연속공급장치(120)는 원료(오산화탄탈륨, 희석제, 카본)를 장입시키기 위한 원료챔버(300)와 원료의 공급속도를 조절하기 위한 공급속도조절장치(310) 및 진공유지/배기를 위한 진공장치(320), 가스취입구(330), 배기구(340)를 구비하며, 진공압력에 의해 상부가 개폐되는 것을 방지하기 위해 클램프 형식의 잠금장치(350)가 있는 덮개(360)를 구비하고 있다.The raw material external continuous supply device 120 is a raw material chamber 300 for charging the raw material (tantalum pentoxide, diluent, carbon) and the feed rate control device 310 for adjusting the supply speed of the raw material and for the vacuum holding / exhaust It is provided with a vacuum device 320, gas inlet 330, exhaust port 340, and has a cover 360 with a clamp type locking device 350 to prevent the upper portion is opened and closed by the vacuum pressure have.

또한 탄탈륨카바이드 생성 완료 후, 냉각을 위해 반응챔버 상부 외주면에 냉각장치(400)를 구비하고 있다.In addition, the cooling device 400 is provided on the outer circumferential surface of the reaction chamber for cooling after the tantalum carbide production is completed.

도 3은 본 발명에 따른 외부연속공급법에 의한 탄탈륨카바이드 제조방법을 설명하기 위한 블럭도이다. 3 is a block diagram illustrating a method for manufacturing tantalum carbide by an external continuous supply method according to the present invention.

상기 도면에 따른 본 발명의 외부연속공급법에 의한 탄탈륨카바이드 제조방법은 반응챔버(100)와 원료챔버(300) 내의 산소를 배출하고, 환원제와 일부 희석제를 적정 진공압과 적정온도로 일정시간 가열하는 하소단계(500)와 목적 온도에 도달한 후, 용해된 환원제와 원료를 반응시키기 위해 원료(오산화탄탈륨, 카본, 희석제)를 장입하는 원료공급단계(600), 환원제와 원료가 반응하여 탄탈륨카바이드가 형성되는 탄탈륨카바이드 생성단계(700) 및 생성된 반응물을 냉각하는 냉각단계(710)로 이루어진다.Tantalum carbide manufacturing method according to the external continuous supply method of the present invention according to the drawings to discharge the oxygen in the reaction chamber 100 and the raw material chamber 300, heating the reducing agent and some diluent to a proper vacuum pressure and a suitable temperature for a predetermined time After the calcination step 500 and the target temperature is reached, the raw material supply step 600 of charging the raw material (tantalum pentoxide, carbon, diluent) to react the dissolved reducing agent and the raw material, the reducing agent and the raw material reacts to tantalum carbide Tantalum carbide generation step 700 is formed and a cooling step 710 for cooling the generated reactants.

하소단계(500)는 환원제 및 일부 희석제를 반응용기(110)내에 장입하는 환원 제 및 희석제장입단계(510)와 원료(오산화탄탈륨, 카본, 희석제)를 원료챔버(300)에 장입하는 원료장입단계(520) 및 장입된 환원제, 희석제, 원료 등이 산화되지 않도록 반응챔버(100) 및 원료챔버(300)내의 산소를 제거하기 위해 진공/아르곤퍼징의 일련의 작업을 수회 반복하는 산소배출단계(530)로 이루어진다.In the calcination step 500, a reducing agent and a diluent loading step 510 for charging a reducing agent and some diluents into the reaction vessel 110 and a raw material loading step for charging a raw material (tantalum pentoxide, carbon, and diluent) into the raw material chamber 300. 520 and an oxygen discharge step 530 of repeating a series of operations of vacuum / argon fuzzing to remove oxygen in the reaction chamber 100 and the raw material chamber 300 so that the charged reducing agent, diluent, raw material, etc. are not oxidized. )

원료공급단계(600)는 목적 온도에 도달한 후, 용해된 환원제와 원료를 반응시키기 위해 원료챔버(300)내의 원료(오산화탄탈륨, 카본, 희석제)를 반응용기(110)내에 적정장입속도로 장입함으로서 달성된다. After the raw material supplying step 600 reaches the target temperature, the raw material (tantalum pentoxide, carbon, diluent) in the raw material chamber 300 is charged into the reaction vessel 110 at an appropriate charging speed in order to react the dissolved reducing agent with the raw material. Is achieved.

탄탈륨카바이드 생성단계(700)는 반응용기(110)내에 용해되어 있는 환원제가 원료장입후 원료가 용해되면서 반응이 시작하여 탄탈륨카바이드가 형성됨으로서 달성된다.Tantalum carbide generation step 700 is achieved by the reaction is started as the raw material is dissolved after the raw material is dissolved in the reducing agent dissolved in the reaction vessel 110 is formed of tantalum carbide.

또한 냉각단계(710)는 탄탈륨카바이드 생성 완료 후, 반응물을 냉각시키기 위해 구비하고 있다.In addition, the cooling step 710 is provided to cool the reactants after the tantalum carbide generation is completed.

도 2와 도 3을 참조하여 본 발명의 실시예에 대하여 상세히 설명한다.An embodiment of the present invention will be described in detail with reference to FIGS. 2 and 3.

상온에서 반응용기(110)내에 환원제로서 마그네슘과 희석제로서 염화나트륨, 염화칼륨 등을 장입하고, 원료챔버(300)내에 원료로서 오산화탄탈륨, 카본을 혼합하여 장입한 후, 진공펌프(130)(320)를 이용하여 10- 3토르(torr) 정도의 진공을 형성한 후 아르곤가스를 취입하여 반응챔버(10) 및 원료챔버(300)내의 산소를 배출하는 과정을 수회 반복한다. 온도를 약 300℃로 상승시키고, 아르곤가스를 760토르까지 취입하여 반응챔버(100)내의 잔류산소를 완전히 제거하는 과정을 수회 반복하여 실시한 후, 아르곤가스 분위기 하에서 반응챔버(100)를 600~1200℃로 가열하여 반응용기(110)내의 환원제와 희석제를 완전히 용해시킨다. 원료챔버(300)를 개방하여 반응용기(110)내로 원료를 장입시키면 반응용기(110)내의 환원제와 장입한 원료가 반응하여 탄탈륨카바이드가 생성된다. 이때 반응속도 및 반응온도는 원료장입속도 및 희석제장입속도에 따라 조절할 수 있다. 반응용기(110)내의 반응식은 식 ①로 표현된다.After charging magnesium and diluent sodium chloride and potassium chloride as a reducing agent in the reaction vessel 110 at room temperature, and charging and mixing tantalum pentoxide and carbon as raw materials in the raw material chamber 300, vacuum pumps 130 and 320 are charged. used in 10 - after the formation of 3 Torr (torr) vacuum degree of the process by blowing argon gas exhaust oxygen in the reaction chamber 10 and the material chamber 300 is repeated several times. After the temperature was raised to about 300 ° C. and argon gas was blown to 760 torr to remove residual oxygen in the reaction chamber 100 several times, the reaction chamber 100 was heated to 600 to 1200 under an argon gas atmosphere. Heating to ℃ ℃ completely dissolve the reducing agent and diluent in the reaction vessel (110). When the raw material chamber 300 is opened and the raw material is charged into the reaction vessel 110, the reducing agent and the loaded raw material in the reaction vessel 110 react to generate tantalum carbide. At this time, the reaction rate and the reaction temperature can be adjusted according to the raw material loading rate and diluent loading rate. The reaction formula in the reaction vessel 110 is represented by equation ①.

Ta2O5 + 5Mg + 2C → 2TaC + 5MgO ①Ta 2 O 5 + 5Mg + 2C → 2TaC + 5MgO ①

한편, 소정의 공정이 종료된 후 반응용기(110)내에 생성된 탄탈륨카바이드는 냉각장치(400)를 이용하여 상온까지 충분히 냉각시켜 회수한다.On the other hand, after the predetermined process is completed, the tantalum carbide generated in the reaction vessel 110 is recovered by sufficiently cooling to room temperature using the cooling apparatus 400.

따라서 본 발명은 원료외부연속공급장치를 이용하여 진공챔버 내부의 반응용기에 원료(Ta2O5), 온도제어를 위한 희석제(KCl, KF, NaCl 등), 카본(C)을 일정한 속도로 연속적으로 공급할 수 있게 함으로서 반응속도의 제어가 가능하고, 일정한 반응온도를 유지할 수 있는 장점으로 입자가 작고 균일한 탄탈륨카바이드를 제조할 수 있다. Therefore, the present invention continuously feeds the raw material (Ta 2 O 5 ), the diluent (KCl, KF, NaCl, etc.), carbon (C) to the reaction vessel inside the vacuum chamber by using a continuous feed material outside the raw material at a constant rate It is possible to control the reaction rate by supplying it to be able to supply a small and uniform tantalum carbide particles with the advantage of maintaining a constant reaction temperature.

이상 서술한 바와 같이, 본 발명의 외부연속공급법에 의한 탄탈륨카바이드 제조장치 및 방법은 종래의 제조장치 및 방법을 개선한 것으로 반응속도의 제어가 가능하고, 일정한 반응온도를 유지할 수 있어 입자가 작고 균일한 탄탈륨카바이드를 제조할 수 있는 장점이 있다. As described above, the tantalum carbide production apparatus and method by the external continuous feeding method of the present invention is an improvement of the conventional production apparatus and method, it is possible to control the reaction rate, it is possible to maintain a constant reaction temperature, small particles There is an advantage to produce a uniform tantalum carbide.

Claims (2)

원료(Ta2O5), 희석제(KCl, KF, NaCl 등), 카본(C)이 담긴 원료챔버를 구비하고, 원료 등이 산소와 결합하여 산화되는 것을 방지하기 위한 진공장치를 구비하며, 상기 반응용기에 상기 원료, 희석제, 카본을 일정한 속도로 연속적으로 장입할 수 있는 원료외부연속공급장치를 포함하는 원료외부연속공급법에 의한 탄탈륨카바이드 제조장치.A raw material chamber containing a raw material (Ta 2 O 5 ), a diluent (KCl, KF, NaCl, etc.), carbon (C), and a vacuum apparatus for preventing the raw material, etc. from being combined with oxygen and oxidized. An apparatus for producing tantalum carbide by an external raw material continuous feeding method, comprising a raw material external continuous supply device capable of continuously charging the raw material, the diluent, and carbon at a constant rate to a reaction vessel. 탄탈륨카바이드를 제조하는데 있어서, 반응챔버 및 원료챔버내의 산소를 배출하고, 환원제 및 희석제를 적정 진공압과 적정 온도로 일정시간 가열하는 하소단계, 환원제와 희석제가 용해된 후, 원료챔버내의 원료, 희석제, 카본을 일정한 속도로 반응용기내로 장입하는 원료장입단계 및 상기 원료, 환원제 및 카본이 반응하여 탄탈륨카바이드가 생성되는 탄탈륨카바이드 생성단계를 포함하는 원료외부연속공급법에 의한 탄탈륨카바이드 제조방법.In the preparation of tantalum carbide, the calcination step of discharging oxygen in the reaction chamber and the raw material chamber, heating the reducing agent and the diluent to a proper vacuum pressure and the appropriate temperature for a predetermined time, and after the reducing agent and the diluent are dissolved, the raw material and diluent in the raw material chamber And a raw material charging step of charging carbon into a reaction vessel at a constant rate, and a tantalum carbide production step of reacting the raw material, the reducing agent, and carbon to produce tantalum carbide.
KR1020060068236A 2006-07-21 2006-07-21 Apparatus and method of tantalum carbide production by external continuous supply process KR20060093312A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020060068236A KR20060093312A (en) 2006-07-21 2006-07-21 Apparatus and method of tantalum carbide production by external continuous supply process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020060068236A KR20060093312A (en) 2006-07-21 2006-07-21 Apparatus and method of tantalum carbide production by external continuous supply process

Publications (1)

Publication Number Publication Date
KR20060093312A true KR20060093312A (en) 2006-08-24

Family

ID=37601462

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020060068236A KR20060093312A (en) 2006-07-21 2006-07-21 Apparatus and method of tantalum carbide production by external continuous supply process

Country Status (1)

Country Link
KR (1) KR20060093312A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134073A (en) * 2011-02-28 2011-07-27 长沙伟徽高科技新材料股份有限公司 Preparation method of ultrafine tantalum carbide powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134073A (en) * 2011-02-28 2011-07-27 长沙伟徽高科技新材料股份有限公司 Preparation method of ultrafine tantalum carbide powder
CN102134073B (en) * 2011-02-28 2012-11-14 长沙伟徽高科技新材料股份有限公司 Preparation method of ultrafine tantalum carbide powder

Similar Documents

Publication Publication Date Title
US4008090A (en) Process for the production of tungsten carbide or mixed metal carbides
JP4215911B2 (en) Niobium powder agglomerates
US5958106A (en) Method of making metals and other elements from the halide vapor of the metal
JP6579237B2 (en) Method for producing positive electrode active material for lithium secondary battery
CN103459624B (en) Method for recovering valuable metals
WO2010085006A1 (en) Fabrication method of nano-sized metal carbide powder using self-propagating high-temperature synthesis
KR101774319B1 (en) Manufacturemethod for titanium powder
US20230083267A1 (en) Production method of carbon nanotube assembly
US20150064094A1 (en) Method of preparing titanium carbide powder
KR20060093312A (en) Apparatus and method of tantalum carbide production by external continuous supply process
KR101044723B1 (en) Preparation of Ultra Fine WC Powder by Self-propagating High-Temperature Synthesis induced Molten Slats
US5338523A (en) Method of making transition metal carbide and boride powders
US11713251B2 (en) Method for preparing powdered composite carbide of tungsten and titanium
KR20040074828A (en) Method for manufacturing nanophase tic composite powders by metallothermic reduction
CN1204043C (en) Synthesis method for powder ceramic complexes of refractory metals
KR102376778B1 (en) Smelting equipment for the production of tantalum powder
CN109354020A (en) A method of preparing chromium carbide or chromium nitride
JPS6197110A (en) Manufacture of silicon nitride having high alpha-phase content
US5011798A (en) Chromium additive and method for producing chromium alloy using the same
JPH0288727A (en) Production of metal titanium
KR100384654B1 (en) Apparatus and method of tantalum production by continuous process
KR101405393B1 (en) TiC powder manufacturing reactor
RU2792036C1 (en) METHOD OF OBTAINING VANADIUM-ALUMINUM CARBIDE V2AlC USING SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS
US20240076192A1 (en) Methods and apparatus of producing silicon nanoparticles
KR20090123252A (en) Fabrication method of ultra fine tungsten powders by self-propagating high-temperature synthesis induced molten salts

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E601 Decision to refuse application