KR20080047167A - Method of manufacturing titanium powder using titanium sponge - Google Patents

Method of manufacturing titanium powder using titanium sponge Download PDF

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KR20080047167A
KR20080047167A KR1020060117186A KR20060117186A KR20080047167A KR 20080047167 A KR20080047167 A KR 20080047167A KR 1020060117186 A KR1020060117186 A KR 1020060117186A KR 20060117186 A KR20060117186 A KR 20060117186A KR 20080047167 A KR20080047167 A KR 20080047167A
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titanium
titanium hydride
reactor
hydride
powder
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Korean (ko)
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류기석
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주식회사 마이크로테크
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A method for the preparation of titanium powder is provided to relieve burdens of process conditions and process facilities by obtaining titanium hydride even at low temperatures under atmospheric pressure conditions. A method for the preparation of titanium powder comprises the steps of: steps(10,20) of injecting a titanium sponge or titanium chips into a reactor, and heating the titanium sponge or titanium chips while supplying argon gas into the reactor at a temperature of 150 to 200 deg.C under atmospheric pressure conditions for one hour to one hour and 30 minutes; a step(30) of simultaneously supplying hydrogen into the reactor and heating the reactant at a temperature of 150 to 500 deg.C under atmospheric pressure conditions for 10 minutes to one hour and 30 minutes to form titanium hydride; a step(40) of cooling the titanium hydride; and a step(50) of milling the titanium hydride by a milling machine while supplying argon gas into the titanium hydride to produce a titanium hydride power. The method further comprises a step(60) of injecting the titanium hydride power into a reactor and heating the titanium hydride power to a temperature of 600 to 800 deg.C to subject the titanium hydride power to dehydrogenation.

Description

티타늄 분말 제조방법{method of manufacturing titanium powder using titanium sponge}Method of manufacturing titanium powder using titanium sponge

도 1은 본 발명에 따른 티타늄 분말 제조공정을 나타내 보인 공정도이다.1 is a process chart showing a titanium powder manufacturing process according to the present invention.

본 발명은 티타늄 스폰지 또는 티타늄 칩을 이용한 티타늄 분말 제조방법에 관한 것으로서, 상세하게는 저온에서도 수소화반응이 이루어질 수 있도록 처리하는 티타늄 분말 제조방법에 관한 것이다.The present invention relates to a titanium powder manufacturing method using a titanium sponge or a titanium chip, and more particularly, to a titanium powder manufacturing method for treating so that a hydrogenation reaction can be performed even at a low temperature.

티타늄 및 티타늄 합금은 강도 및 밀도 비가 높고 내열성, 내부식성, 피로강도가 높아 항공, 우주, 해양 및 화학 장치용 소재로서 많이 이용되고 있고, 최근에는 가볍고 강한 소재의 특성을 이용하기 위해 자동차 부품, 골프채 등 이용분야가 다양한 산업분야로 확대되고 있다.Titanium and titanium alloys are widely used as materials for aviation, aerospace, marine and chemical devices because of their high strength and density ratio, high heat resistance, corrosion resistance and fatigue strength. The usage field is expanding to various industrial fields.

그런데, 티타늄은 철, 구리 및 알루미늄과 같은 금속에 비해 높은 녹는점과 강도를 갖고 있어 일반적인 용해 및 주조가 불가능하고, 주조한 잉곳도 단조, 압연 및 절삭 가공이 어려운 문제점 있다.However, since titanium has a higher melting point and strength than metals such as iron, copper, and aluminum, general melting and casting are impossible, and casting ingots are also difficult to forge, roll, and cut.

최근에는 이러한 가공상의 어려움을 개선코자 티타늄 또는 티타늄 합금분말 을 이용하여 성형하는 분말 야금법이 널리 이용되고 있다.Recently, powder metallurgy, which uses titanium or titanium alloy powder, is widely used to improve such processing difficulties.

분말 야금법에 이용되는 티타늄 분말은 산화티타늄을 크롤법(kroll)법에 의해 제조된 티타늄 스폰지를 이용하여 티타늄 수소화물로 만들고, 티타늄 수소화물을 분쇄하여 사용하거나, 고온으로 가열하여 탈수소화 처리한 것이 이용된다. 국내 공개 특허 제1994-0003644호에는 이러한 티타늄 미분말을 제조하는 방법이 개시되어 있다.Titanium powder used in powder metallurgy is made of titanium hydride using titanium sponge prepared by kroll method, and used by pulverizing titanium hydride or dehydrogenation by heating to high temperature. Is used. Korean Unexamined Patent Publication No. 194-0003644 discloses a method for producing such a fine titanium powder.

그런데, 상기 방법은 티타늄 수소화물을 얻기 위해 700 내지 850℃의 고온에서 진공상태로 수행해야만 하기 때문에 공정 조건이 복잡하고, 진공펌프 등 요구되기 때문에 공정 설비가 증가 되는 단점이 있다.However, the method has a disadvantage in that the process conditions are complicated because the process must be performed at a high temperature of 700 to 850 ° C. in order to obtain titanium hydride, and the process equipment is increased because a vacuum pump is required.

본 발명은 상기와 같은 문제점을 개선하기 위하여 창안된 것으로서, 저온 및 대기압하에서도 티타늄 수소화물을 얻을 수 있도록 하여 공정조건 및 공정설비 부담을 완화시킬 수 있는 티타늄 분말 제조 방법을 제공하는데 그 목적이 있다.The present invention was devised to improve the above problems, and an object of the present invention is to provide a titanium powder manufacturing method which can reduce the process conditions and the process equipment burden by obtaining titanium hydride even at low temperature and atmospheric pressure. .

상기의 목적을 달성하기 위하여 본 발명에 따른 티타늄 분말 제조방법은 가. 반응기 내에 티타늄 스폰지 또는 티타늄 칩을 넣고, 아르곤가스를 상기 반응기 내에 공급하면서 가열하는 단계와; 나. 상기 반응기 내에 수소를 공급하면서 가열하여 티타늄 수소화물을 형성하는 단계와; 다. 상기 티타늄 수소화물을 냉각하는 단계와; 라. 상기 티타늄 수소화물을 분쇄기로 분쇄하여 분말화 하는 단계;를 포함한다.Titanium powder production method according to the present invention to achieve the above object is a. Putting a titanium sponge or a titanium chip into the reactor and heating the argon gas while supplying it into the reactor; I. Heating to supply hydrogen in the reactor to form titanium hydride; All. Cooling the titanium hydride; la. And pulverizing the titanium hydride with a grinder.

바람직하게는 상기 가 단계는 대기압상태에서 150 내지 200℃의 온도로 1시간 내지 1시간 30분 동안 수행하고, 상기 나 단계는 대기압 상태에서 150 내지 500℃온도로 10분 내지 1시간 30분 동안 수행한다.Preferably, the addition step is carried out for 1 hour to 1 hour 30 minutes at a temperature of 150 to 200 ℃ at atmospheric pressure, the step B is performed for 10 minutes to 1 hour 30 minutes at a temperature of 150 to 500 ℃ at atmospheric pressure do.

또한, 상기 분말화 단계에서 상기 티타늄 수소화물에 아르곤 가스를 공급하면서 분쇄하는 것이 바람직하다.In addition, it is preferable to grind while supplying argon gas to the titanium hydride in the powdering step.

상기 분말화 단계를 거친 티타늄 수소화물 분말을 반응기 내에 넣고 600 내지 800℃로 가열하여 탈수소 처리하는 단계;를 더 포함할 수 있다.Putting the titanium hydride powder subjected to the powdering step into the reactor and heating to 600 to 800 ℃ dehydrogenation; may further include a.

이하, 본 발명에 따른 티타늄 분말 제조공정을 나타내 보인 도 1을 참조하면서 본 발명의 바람직한 실시 예에 따른 티타늄 분말 제조방법을 더욱 상세하게 설명한다.Hereinafter, with reference to Figure 1 showing a titanium powder manufacturing process according to the present invention will be described in more detail a titanium powder manufacturing method according to a preferred embodiment of the present invention.

먼저, 반응기 내에 티타늄소재를 장입한다(단계 10).First, a titanium material is charged into a reactor (step 10).

여기서 반응기는 전기로가 적용될 수 있다.Here, the reactor may be applied with an electric furnace.

티타늄 소재는 티타늄 스폰지 또는 티타늄 판재를 가공하는 과정에서 부스러기 형태로 분리되는 스크랩(이하 칩이라 한다)을 재활용하기 위해 적용될 수 있다.Titanium material may be applied to recycle scrap (hereinafter referred to as chips) that is separated into chips in the process of processing titanium sponge or titanium sheet.

다음은 아르곤 가스분위기에서 반응기를 가열한다(단계 20). 단계 20은 반응기 내에 아르곤 가스(Ar)를 공급하면서 대기압 상태에서 150 내지 200℃의 온도로 1시간 내지 1시간 30분 동안 수행하는 것이 바람직하다.The reactor is then heated in an argon gas atmosphere (step 20). Step 20 is preferably performed for 1 hour to 1 hour 30 minutes at a temperature of 150 to 200 ℃ at atmospheric pressure while supplying argon gas (Ar) into the reactor.

이러한 아르곤 가스에 의한 티타늄 소재의 열처리는 티타늄 수소화물을 얻기 위한 후속 공정에서 수소와의 반응을 위해 요구되는 가열온도를 낮출 수 있다.Such heat treatment of the titanium material with argon gas may lower the heating temperature required for reaction with hydrogen in a subsequent process to obtain titanium hydride.

다음은 아르곤 가스 공급을 차단하고, 수소를 반응기 내에 공급하면서 가열 한다(단계 30). 바람직하게는 단계 30에서는 대기압 상태에서 150 내지 500℃ 온도로 10분 내지 1시간 30분 동안 수행한다. 단계 30을 거치면 티타늄 소재는 수소와 반응하여 티타늄 수소화물(TiHx, 0<x≤2)로 형성된다.The argon gas supply is then cut off and heated while feeding hydrogen into the reactor (step 30). Preferably in step 30 it is carried out at 150 to 500 ℃ temperature for 10 minutes to 1 hour 30 minutes at atmospheric pressure. After step 30, the titanium material reacts with hydrogen to form titanium hydride (TiHx, 0 <x≤2).

단계 30 이후에는 반응기 내에서 티타늄 수소화물을 100℃까지 자연 냉각시킨다(단계 40).After step 30 the titanium hydride is naturally cooled to 100 ° C. in the reactor (step 40).

이후 티타늄 수소화물을 분쇄기로 분쇄하여 분말화한다(단계 50). 분쇄기는 티타늄 볼 밀이 적용될 수 있다.The titanium hydride is then pulverized with a grinder to powderize (step 50). The mill can be applied with a titanium ball mill.

단계 50에서 분쇄에 의해 형성되는 분말의 입경은 목적하는 용도에 맞게 적용하면 되고, 일 예로서, 수백 마이크로미터 이하 예를 들면, 10 내지 100마이크로미터 또는 수 나노미터의 입경을 갖도록 분쇄한다.The particle size of the powder formed by the pulverization in step 50 may be applied according to the intended use. For example, the particle is pulverized to have a particle size of several hundred micrometers or less, for example, 10 to 100 micrometers or several nanometers.

더욱 바람직하게는 분쇄과정에서 아르곤 가스를 티타늄 수소화물에 2atm압력으로 잠입시켜 티타늄 수소화물을 분쇄한다.More preferably, argon gas is immersed in titanium hydride at 2 atm pressure to pulverize titanium hydride in the pulverization process.

단계 50을 거쳐 분말화된 티타늄 수소화분말은 그대로 사용할 수도 있다.The titanium hydrogenated powder powdered through step 50 may be used as it is.

한편, 탈수소처리하고자 할 경우 티타늄 수소화분말을 반응기에 넣고 600 내지 800℃로 가열하여 탈수소화 처리하면 된다(단계 60).On the other hand, if you want to dehydrogenation, the titanium hydrogenated powder is put in a reactor and heated to 600 to 800 ℃ dehydrogenation treatment (step 60).

지금까지 설명된 바와 같이 본 발명에 따른 티타늄 분말 제조방법에 의하면, 티타늄 수소화물을 생성하기 위해 요구되는 가열온도를 낮출 수 있고, 대기압하에서도 가능함으로써 제조공정이 단순화되고 공정설비를 단순화할 수 있는 장점을 제공한다.According to the titanium powder manufacturing method according to the present invention as described so far, it is possible to lower the heating temperature required to produce titanium hydride, and even under atmospheric pressure, which can simplify the manufacturing process and simplify the process equipment. Provide advantages.

Claims (4)

가. 반응기 내에 티타늄 스폰지 또는 티타늄 칩을 넣고, 아르곤가스를 상기 반응기 내에 공급하면서 가열하는 단계와;end. Putting a titanium sponge or a titanium chip into the reactor and heating the argon gas while supplying the argon gas into the reactor; 나. 상기 반응기 내에 수소를 공급하면서 가열하여 티타늄 수소화물을 형성하는 단계와;I. Heating to supply hydrogen in the reactor to form titanium hydride; 다. 상기 티타늄 수소화물을 냉각하는 단계와;All. Cooling the titanium hydride; 라. 상기 티타늄 수소화물을 분쇄기로 분쇄하여 분말화 하는 단계;를 포함하는 것을 특징으로 하는 티타늄 분말 제조방법.la. And pulverizing the titanium hydride with a grinder to powder the titanium hydride. 제1항에 있어서, 상기 가 단계는 대기압상태에서 150 내지 200℃의 온도로 1시간 내지 1시간 30분 동안 수행하고,The method of claim 1, wherein the adding step is performed for 1 hour to 1 hour 30 minutes at a temperature of 150 to 200 ℃ at atmospheric pressure, 상기 나 단계는 대기압 상태에서 150 내지 500℃온도로 10분 내지 1시간 30분 동안 수행하는 것을 특징으로 하는 티타늄 분말 제조방법.The b step is titanium powder production method characterized in that performed for 10 minutes to 1 hour 30 minutes at 150 to 500 ℃ temperature at atmospheric pressure. 제2항에 있어서, 상기 분말화 단계에서 상기 티타늄 수소화물에 아르곤 가스를 공급하면서 분쇄하는 것을 특징으로 하는 티타늄 분말 제조방법.3. The method of claim 2, wherein in the powdering step, the titanium powder is pulverized while supplying argon gas to the titanium hydride. 제3항에 있어서, 상기 분말화 단계를 거쳐 생성된 상기 티타늄 수소화물 분말을 반응기 내에 넣고 600 내지 800℃로 가열하여 탈수소 처리하는 단계;를 더 포 함하는 것을 특징으로 하는 티타늄 분말 제조방법.The method of claim 3, further comprising the step of putting the titanium hydride powder produced through the powdering step into a reactor and heating to 600 to 800 ° C for dehydrogenation.
KR1020060117186A 2006-11-24 2006-11-24 Method of manufacturing titanium powder using titanium sponge KR20080047167A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101259434B1 (en) * 2012-07-27 2013-04-30 한국지질자원연구원 Method of manufacturing titanium alloy powder with low oxygen concentration from titanum alloy scraps
RU2631692C1 (en) * 2016-10-27 2017-09-26 Акционерное общество "Государственный научно-исследовательский и проектный институт редкометаллической промышленности АО "Гиредмет" Method for production of fine-dispersed spherical titanium-containing powders
KR20190044233A (en) * 2017-10-20 2019-04-30 한국생산기술연구원 Method for producing high purity metal powder by repeated hydrogenation-dehydrogenation
CN111069613A (en) * 2019-11-29 2020-04-28 丹阳汇鑫复合材料科技有限公司 Method for preparing nano titanium powder from hydrogen-embrittlement metal titanium
KR20200065836A (en) * 2018-11-30 2020-06-09 한국생산기술연구원 High Purity titanium powder Manufacturing Method Using Dehydrogenation
US11077497B2 (en) 2017-06-07 2021-08-03 Global Titanium Inc. Deoxidation of metal powders

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101259434B1 (en) * 2012-07-27 2013-04-30 한국지질자원연구원 Method of manufacturing titanium alloy powder with low oxygen concentration from titanum alloy scraps
RU2631692C1 (en) * 2016-10-27 2017-09-26 Акционерное общество "Государственный научно-исследовательский и проектный институт редкометаллической промышленности АО "Гиредмет" Method for production of fine-dispersed spherical titanium-containing powders
US11077497B2 (en) 2017-06-07 2021-08-03 Global Titanium Inc. Deoxidation of metal powders
KR20190044233A (en) * 2017-10-20 2019-04-30 한국생산기술연구원 Method for producing high purity metal powder by repeated hydrogenation-dehydrogenation
KR20200065836A (en) * 2018-11-30 2020-06-09 한국생산기술연구원 High Purity titanium powder Manufacturing Method Using Dehydrogenation
CN111069613A (en) * 2019-11-29 2020-04-28 丹阳汇鑫复合材料科技有限公司 Method for preparing nano titanium powder from hydrogen-embrittlement metal titanium

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