KR20070032416A - Method of producing metal powder - Google Patents
Method of producing metal powder Download PDFInfo
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- KR20070032416A KR20070032416A KR20050086594A KR20050086594A KR20070032416A KR 20070032416 A KR20070032416 A KR 20070032416A KR 20050086594 A KR20050086594 A KR 20050086594A KR 20050086594 A KR20050086594 A KR 20050086594A KR 20070032416 A KR20070032416 A KR 20070032416A
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- 239000000843 powder Substances 0.000 title claims abstract description 73
- 239000002184 metal Substances 0.000 title claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims description 44
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 239000008187 granular material Substances 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 6
- 239000010959 steel Substances 0.000 claims abstract description 6
- 239000006227 byproduct Substances 0.000 claims abstract description 5
- 238000005097 cold rolling Methods 0.000 claims abstract description 5
- 238000005098 hot rolling Methods 0.000 claims abstract description 5
- 235000013980 iron oxide Nutrition 0.000 claims description 54
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 38
- 238000005469 granulation Methods 0.000 claims description 14
- 230000003179 granulation Effects 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims 1
- 230000001965 increasing effect Effects 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 238000005245 sintering Methods 0.000 abstract description 5
- 150000007513 acids Chemical class 0.000 abstract description 3
- 238000007865 diluting Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- 239000007921 spray Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- YNVZDODIHZTHOZ-UHFFFAOYSA-K 2-hydroxypropanoate;iron(3+) Chemical compound [Fe+3].CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O YNVZDODIHZTHOZ-UHFFFAOYSA-K 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910000805 Pig iron Inorganic materials 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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Classifications
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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
- B22F8/00—Manufacture of articles from scrap or waste metal particles
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
본 발명은 제철소의 열간 압연과 냉간 압연의 공정 중에 부산물로 발생하는 산화철을 환원하여 금속 분말을 제조하는 방법에 관한 것으로, 본 발명의 목적은 미세한 산화철 분말을 유기 결합제를 사용하여 과립을 함으로써 산화철 분말의 외형적인 크기가 커져서 산화철 분말의 흩날림이 방지되고, 가사 밀도가 1.0 ~ 1.6 gr/cm3로 높아지게 되어 환원 장비에 많은 양의 산화철을 장입할 수 있도록 하고, 이의 환원에 의한 금속 분말의 제조방법을 제공함에 있다.The present invention relates to a method for producing a metal powder by reducing the iron oxide generated as a by-product during the hot rolling and cold rolling of the steel mill, the object of the present invention is to fine iron oxide powder granules using an organic binder to iron oxide powder The apparent size of the iron oxide powder is prevented from being scattered, and the pot density is increased to 1.0 to 1.6 gr / cm 3 so that a large amount of iron oxide can be charged into the reduction equipment, and the method for producing the metal powder by reduction thereof In providing.
특히, 상기 유기 결합제로써 황산, 질산, 염산 등의 강산을 소정 농도로 희석하여 사용함으로써 미세한 산화철 입자 간의 화학적인 결합을 유도하여 환원 시 소결 현상을 용이하게 하여 금속 분말의 평균 입경, 가사 밀도 및 흐름성 등의 특성을 개선시킬 수 있도록 한 것이다.In particular, by diluting strong acids such as sulfuric acid, nitric acid, and hydrochloric acid to a predetermined concentration as the organic binder, chemical bonds between fine iron oxide particles are induced to facilitate sintering during reduction, so that the average particle diameter, pot density and flow of the metal powder are reduced. It is to improve the characteristics such as sex.
Description
도 1은 본 발명의 실시예에 따른 금속 분말의 제조방법을 개략적으로 나타낸 흐름도.1 is a flow chart schematically showing a method for producing a metal powder according to an embodiment of the present invention.
본 발명은 제철소의 열간 압연과 냉간 압연의 공정 중에서 부산물로 발생하는 산화철을 환원하여 금속 분말을 제조하는 방법에 관한 것으로, 보다 상세하게는 미세한 분말인 산화철을 양호한 특성의 과립 상태로 만들어 처리함으로써 취급하기가 용이하고, 환원 설비에 산화철 장입 시 밀도를 높여 공정 비용을 줄일 수 있으며, 제조되는 금속 분말의 특성을 기술적으로 제어할 수 있도록 한 금속 분말의 제조방법에 관한 것이다.The present invention relates to a method for producing metal powder by reducing iron oxide generated as a by-product during the hot rolling and cold rolling processes of steel mills, and more particularly, by treating iron oxide, which is a fine powder, in a granular state with good properties and treated. The present invention relates to a method for preparing a metal powder, which is easy to do, to increase the density when charging iron oxide into a reduction facility, and to reduce the process cost, and to technically control the characteristics of the metal powder to be produced.
일반적으로 금속(철) 분말을 제조하는 종래의 기술에는 산화철(FeO, Fe2O3, Fe3O4)을 환원하는 방법, 용융 철을 분무하는 Atomizing 방법, 카보닐 철(Fe(CO)5)을 열분해하여 철 분말을 제조하는 방법, 철을 함유한 유산철(FeSO4) 또는 염화철(FeCl2, FeCl3) 등의 수용액에서 철을 전해 채취하는 방법 등이 알려져 있다.In general, conventional techniques for producing metal (iron) powder include a method for reducing iron oxides (FeO, Fe 2 O 3 , Fe 3 O 4 ), Atomizing method for spraying molten iron, carbonyl iron (Fe (CO) 5 ), A method of producing iron powder by pyrolysis, a method of electrolytically collecting iron from an aqueous solution such as iron-containing iron lactate (FeSO 4 ) or iron chloride (FeCl 2 , FeCl 3 ) and the like are known.
상기 방법들에 의해 제조된 금속 분말은 각기 장점 및 단점을 갖고 있는데, 특히, 상기 산화철을 환원하는 방법으로 제조된 환원철은 연성이 높아 기계 가공성이 좋으며 압축 성형성이 좋은 장점이 있는 반면에, 비표면적이 커서 소결 시 수축율이 크기 때문에 부품 크기 불량의 가능성이 높은 문제 등의 단점을 갖는다.The metal powders produced by the above methods have advantages and disadvantages, respectively. In particular, the reduced iron produced by the method of reducing the iron oxide has high ductility and good machinability and good compression moldability. Since the surface area is large, the shrinkage rate during sintering is high, which causes disadvantages such as a high possibility of defective part size.
그러나, 상기와 같은 단점에도 불구하고 상기 산화철을 환원하는 방법으로 제조된 환원철은 다른 제조 방법에 의해 제조되는 금속 분말에 비해 가격이 저렴하고 분말의 특성이 양호하기 때문에 일반 기계부품, 자동차용 기어, 자성용 코어 등에 다량으로 사용되고 있다.However, in spite of the above disadvantages, the reduced iron produced by the method of reducing the iron oxide is cheaper than the metal powder produced by the other production method and the characteristics of the powder are good, so that general mechanical parts, automotive gears, It is used in a large amount in magnetic cores.
한편, 산화철의 환원은 제철소에서 철광석을 환원하여 선철을 제조하는 것에 주로 이용되고 있으나, 근래 들어 철 분말의 용도가 많이 개발되었기 때문에 제철소의 열간 압연과 냉간 압연 공정의 부산물로 발생하는 산화철을 수소 가스로 환원하여 환원철 분말을 제조하여 각종 분야의 부품 등에 활용되고 있다.On the other hand, the reduction of iron oxide is mainly used for producing pig iron by reducing iron ore in steel mills, but iron oxides, which are generated as by-products of hot rolling and cold rolling processes of steel mills, have been used since iron powders have been developed in recent years. Reduced to produce reduced iron powder has been utilized in parts of various fields.
그러나, 제철소의 열간 압연 및 냉간 압연 공정 중 부산물로 발생하는 산화철의 수소 가스에 의한 환원으로 제조되는 금속 분말은 입자 크기와 분말의 밀도 및 분말의 흐름성을 제어하기가 어렵고, 산화철은 미세 분말이 포함되어 있으므로 취급이 어려우며, 또한, 가사 밀도가 낮은 산화철을 환원 장비에 장입 시 장입 밀도가 낮아서 공정 비용이 많이 들게 되는 문제점이 있었다.However, it is difficult to control the particle size, the density of the powder and the flowability of the powder in the metal powder produced by the reduction by the hydrogen gas of iron oxide generated as a by-product during the hot rolling and cold rolling process of steel mills, iron oxide is fine powder Since it is difficult to handle, and also, when loading the iron oxide having a low house density into the reduction equipment, there was a problem that the process cost is high because the charge density is low.
즉, 제철 공정에서 발생하는 산화철은 FeO, Fe2O3, Fe3O4 등의 화학식을 갖는 분말로써 그 크기가 sub micro-meter ~ centi-meter로 그 분포가 매우 넓은데, 그 중 sub micro-meter ~ 10 micro-meter 크기의 산화철은 너무 미세하기 때문에 분말의 흩날림, 정밀 설비로의 침투, 일단 부착되면 잘 제거되지 않는 등의 취급이 곤란한 문제가 발생하게 되고, 또한, 산화철 미세 분말의 가사밀도가 약 0.4 gr/cm3 정도로 매우 낮아서 공정 설비에 많이 장입을 할 수 없기 때문에 설비를 크게 제작해야 되는 등 산화철 처리에 필요한 공정 비용이 증대되는 문제점이 있는 것이다.In other words, the iron oxide produced in the iron making process is a powder having a chemical formula such as FeO, Fe 2 O 3 , Fe 3 O 4 , the size of the sub micro-meter ~ centi-meter is very wide distribution, among which sub micro Iron oxides of -meter to 10 micrometers are so fine that problems such as scattering of powders, penetration into precision equipment, and poor removal once adhered to them can occur. Since the density is very low, about 0.4 gr / cm 3 , it is not possible to charge a lot into the process equipment, so the process cost required for iron oxide treatment is increased, such as the need to manufacture a large equipment.
따라서 본 발명은 상기와 같은 문제점을 해결하기 위해 안출된 것으로, 본 발명의 목적은 미세한 산화철 분말을 유기 결합제를 사용하여 과립을 함으로써 산화철 분말의 외형적인 크기가 커져서 산화철 분말의 흩날림이 방지되고, 가사 밀도가 1.0 ~ 1.6 gr/cm3로 높아지게 되어 환원 장비에 많은 양의 산화철을 장입할 수 있도록 하고, 이의 환원에 의한 금속 분말의 제조방법을 제공함에 있다.Therefore, the present invention has been made to solve the above problems, an object of the present invention is to granulate the fine iron oxide powder using an organic binder to increase the external size of the iron oxide powder to prevent scattering of iron oxide powder, housework The density is increased to 1.0 ~ 1.6 gr / cm 3 to be able to load a large amount of iron oxide in the reduction equipment, and to provide a method for producing a metal powder by the reduction thereof.
특히, 상기 유기 결합제로써 황산, 질산, 염산 등의 강산을 소정 농도로 희석하여 사용함으로써 미세한 산화철 입자 간의 화학적인 결합을 유도하여 환원 시 소결 현상을 용이하게 하여 금속 분말의 평균 입경, 가사 밀도 및 흐름성 등의 특성을 개선시킬 수 있도록 한 금속 분말의 제조방법을 제공함에 있다.In particular, by diluting strong acids such as sulfuric acid, nitric acid, and hydrochloric acid to a predetermined concentration as the organic binder, chemical bonds between fine iron oxide particles are induced to facilitate sintering during reduction, so that the average particle diameter, pot density and flow of the metal powder are reduced. It is to provide a method for producing a metal powder to improve the properties such as sex.
상기 목적을 달성하기 위한 본 발명에 따른 금속 분말의 제조 방법은 도 1에 도시된 바와 같이, 미세 산화철 분말을 유기 결합제를 사용하여 소정 크기로 응집시키는 과립 단계와, 상기 유기 결합제를 제거하기 위한 건조 단계와, 건조된 산화 철을 가열하여 환원철을 생성하는 환원 단계와, 환원된 철 분말의 분쇄 단계와, 분쇄된 철 분말의 분급 단계 및 포장 단계를 포함하여 이루어지는 것을 특징으로 한다.Method for producing a metal powder according to the present invention for achieving the above object is a granulation step of agglomerated fine iron oxide powder to a predetermined size using an organic binder, as shown in Figure 1, and drying to remove the organic binder And a reduction step of heating the dried iron oxide to produce reduced iron, a grinding step of the reduced iron powder, a classification step and a packing step of the crushed iron powder.
상기와 같은 금속 분말의 제조방법에 있어서, 유기 결합제를 투입한 미세 산화철 분말을 스프레이 드라이어(Spray Dryer), 버티컬 그래뉼레이터(Vertical Granulator), 게이지 그래뉼레이터(Gauge Granulator), 바이브레이션 밀(Vibration Mill) 등의 설비를 이용하여 과립하게 되며, 이러한 과립자는 1 ~ 5 mm 크기로 만들어지게 된다.In the method of manufacturing the metal powder as described above, the fine iron oxide powder in which the organic binder is added is spray dryer (Verray Dryer), Vertical Granulator (Vertical Granulator), Gauge Granulator (Vibration Mill), etc. It is granulated using the equipment of these granules are made to 1 ~ 5 mm in size.
특히, 본 발명에 따른 금속 분말의 제조 방법에서는 산화철 분말의 과립 공정에서 사용되는 결합제로써 종래에 일반적으로 사용되었던 물 대신에 질산, 염산, 황산 등의 강산을 사용함으로써 입자간의 화학적 결합을 유도하였다.In particular, in the method for producing a metal powder according to the present invention, chemical bonding between particles is induced by using strong acids such as nitric acid, hydrochloric acid, sulfuric acid, etc. instead of water, which is generally used as a binder used in the granulation process of iron oxide powder.
즉, 종래에 과립 공정에서 물을 결합제로 사용하여 제조된 금속 분말의 경우에는 고객의 요구 품질과 다소 차이가 있었으나, 본 발명의 과립 공정에서 물 대신에 강산을 소정 농도만큼 희석시켜 사용하게 되면 과립된 산화철 분말의 외형적인 크기가 커지게 되며, 이로 인하여 흩날림이 방지되고, 가사 밀도가 1.0 ~ 1.6 gr/cm3로 크게 되어 환원 장비에 많은 양의 산화철을 장입할 수 있게 되고, 미세한 산화철 입자간의 화학적인 결합을 유도하여 환원 시 소결 현상을 용이하게 하여 환원 처리된 금속 분말의 평균 입경 및 가사 밀도, 흐름성 등의 특성을 고객이 요구하는 수준으로 개선시킬 수 있게 된다.That is, in the case of the metal powder manufactured by using water as a binder in the granulation process in the prior art, there was a little difference from the quality required by the customer. The apparent size of the iron oxide powder is increased, thereby preventing scattering and increasing the house density to 1.0 to 1.6 gr / cm 3 , so that a large amount of iron oxide can be charged into the reduction equipment, and fine iron oxide particles By inducing chemical bonds to facilitate the sintering phenomenon during reduction, it is possible to improve the characteristics such as the average particle diameter, pot life density, flowability of the reduced metal powder to the level required by the customer.
이 때, 상기 강산 중에 질산은 5 ~ 35%, 염산은 5 ~ 18%, 황산은 5 ~ 50%의 농도로 희석하여 사용하게 된다.At this time, the nitric acid is 5 to 35% in the strong acid, 5 to 18% hydrochloric acid, sulfuric acid is diluted to a concentration of 5 to 50%.
한편, 본 발명에 따른 금속 분말의 제조방법에 있어서, 상기 건조 단계는 과립 공정을 거친 과립 산화철 중에서 과립할 때 사용된 결합제 및 산화철 자체에 포함된 유기물질을 제거하기 위해 드라이 오븐(Dry Oven)을 사용하여 150℃에서 2시간 동안 대기의 분위기에서 건조시키는 것이다.On the other hand, in the manufacturing method of the metal powder according to the present invention, the drying step is to dry the oven (Dry Oven) to remove the organic material contained in the binder and iron oxide itself used when granulating in the granulated iron oxide after the granulation process It is used to dry in the atmosphere of air for 2 hours at 150 ℃.
또한, 상기 환원 단계에서는 건조가 완료된 과립 산화철을 수소가스 분위기의 전기로(Static or Dynamic Electric Furnace)를 사용하여 환원 온도 700 ~ 1100℃에서 2 ~ 8시간 동안 열처리하게 되면 은회색이며 재료에 작은 기공이 많은 Sponge Type의 금속(환원철) 분말이 제조된다. In addition, in the reduction step, when the dried granulated iron oxide is heat treated at a reduction temperature of 700 to 1100 ° C. for 2 to 8 hours using a hydrogen gas atmosphere (Static or Dynamic Electric Furnace), silver gray and small pores are formed in the material. Many sponge type metal (reduced iron) powders are produced.
상기 분쇄 단계에서는 환원된 금속 분말을 바이브레이션 밀 등의 분쇄 장비를 이용하여 10 ~ 30분 동안 분쇄하게 되고, 상기 단계에서 분쇄된 금속 분말은 다시 180 ㎛(80 Mesh)의 스크린(Screen)을 사용하여 분급하게 되는 분급 단계를 거쳐 포장이 되면 최종적으로 금속 분말의 제조가 완료되는 것이다.In the pulverizing step, the reduced metal powder is pulverized for 10 to 30 minutes using a pulverizing equipment such as a vibration mill, and the pulverized metal powder is again used using a screen of 180 μm (80 Mesh). When the packaging is subjected to the classification step to be classified, the manufacture of the metal powder is finally completed.
이하 본 발명의 제조방법을 각 실시예에 의하여 상세히 설명하면 다음과 같다.Hereinafter, the manufacturing method of the present invention will be described in detail with reference to the following examples.
[실시예 1]Example 1
실시예 1에서는 미세한 산화철 분말을 스프레이 드라이어(Spray Dryer), 게이지 그래뉼레이터(Gauge Granulator), 바이브레이션 밀(Vibration Mill) 등 여러 종류의 설비를 사용하여 과립을 하였으며, 상기 각 설비에 의해 과립된 과립자의 명칭을 Spary Dryer, Gauge Granulator #10, VM 30으로 표1에 표시하였다.In Example 1, the fine iron oxide powder was granulated using various kinds of equipment, such as a spray dryer, a gauge granulator, and a vibration mill. The names are given in Table 1 as Spary Dryer, Gauge Granulator # 10, and VM 30.
우선, 스프레이 드라이어에 의한 과립자는 물을 사용하여 농도 55%의 산화철 슬러리(Slurry) 용액을 제조하였으며, 이 용액을 온도 약 700℃의 챔버(Chamber) 내에서 9000rpm으로 회전하는 판(Plate)에 분무 및 건조시켜 과립자로 만들었다.First, the granules by the spray drier prepared a slurry solution of iron oxide having a concentration of 55% using water, and sprayed the solution on a plate rotating at 9000 rpm in a chamber at a temperature of about 700 ° C. And dried to granules.
또한, 게이지 그래뉼레이터 과립자(Gauge Granulator #10)는 결합제로써 물을 산화철의 중량 대비 약 17%를 투입하여 버티컬 그래뉼레이터로 1차 과립을 한 이후에 게이지 그래뉼레이터 10 Mesh의 망을 통과시켜 2차로 과립을 하였다.In addition, Gauge Granulator # 10 is water as a binder by adding about 17% water by weight of iron oxide, and after the first granules with a vertical granulator, through the mesh of the gauge granulator 10 mesh 2 Granulated with tea.
또한, 바이브레이션 밀 과립자는(VM 30) 바이브레이션 밀을 사용하여 30분간 Milling을 하여 과립을 하였으며, 이 때 결합제는 사용하지 않았다.In addition, the vibration mill granulator (VM 30) using a vibration mill for 30 minutes to mill the granules, at this time did not use a binder.
표 1에 나타낸 바와 같이 상기 각 과립 설비를 사용하여 과립을 한 결과의 특성은 다음과 같다.As shown in Table 1, the characteristics of the resultant granules using the respective granulation facilities are as follows.
과립 공정이 완료된 과립자의 크기는 과립하기 전의 미세한 산화철보다 40 ~ 1000배로 매우 커져 분말 취급이 용이하게 된다.After the granulation process is completed, the size of the granules is 40 to 1000 times larger than the fine iron oxide before granulation, thereby facilitating powder handling.
또한, 과립자의 가사 밀도는 과립하기 전의 미세한 산화철보다 약 1.5 ~ 3.5배 높아져서 설비에 장입하는 밀도를 높일 수 있기 때문에 환원철 제조 비용을 절감할 수 있다.In addition, the pot density of the granules may be about 1.5 to 3.5 times higher than the fine iron oxide before granulation, thereby increasing the density of charging the equipment, thereby reducing the reduced iron manufacturing cost.
그러나, 과립자의 비표면적은 과립하기 전의 미세한 산화철과 비교하여 변화는 거의 없어서 과립 산화철의 환원 활성도는 비슷할 것으로 판단되며, 과립을 하여 건조한 이후의 수분은 원래의 산화철과 비슷한 값을 가지고 있었다.However, the specific surface area of the granules was almost unchanged compared to the fine iron oxide before granulation, so that the reduction activity of the granular iron oxide was similar, and the moisture after drying was similar to the original iron oxide.
표 1Table 1
한편, 표 1에 나타낸 과립 산화철의 특성 중 평균 입경은 주사 전자 현미경으로 촬영한 결과로부터 구하였고, 가사 밀도는 진동형 겉보기 밀도 측정기로 측정하였으며, 비표면적은 질소 가스를 흡착하는 Brunauer, Emmett, Teller가 도출한 BET법으로 측정하였으며, 수분은 105℃에서 60분 가열하여 무게 감량으로 구하였다.On the other hand, the average particle diameter of the characteristics of the granulated iron oxide shown in Table 1 was obtained from the results of scanning electron microscopy, and the pot density was measured with a vibratory apparent density meter, and the specific surface area was measured by Brunauer, Emmett, and Teller, which adsorb nitrogen gas. It was measured by the derived BET method, and the moisture was heated at 105 ° C. for 60 minutes to obtain weight loss.
표 1의 과립을 한 산화철을 1100℃에서 2시간 동안 수소 분위기에서 환원하여 분쇄하고 분급한 결과의 금속 분말의 특성을 표 2를 참조하여 상세히 설명하면 다음과 같다.The characteristics of the metal powder obtained by reducing and pulverizing and classifying the iron oxide with the granules of Table 1 in a hydrogen atmosphere at 1100 ° C. for 2 hours will be described in detail with reference to Table 2 as follows.
표 2에 나타낸 바와 같이 상기 세 가지 과립 방법에 따른 과립 산화철을 환원한 결과, 평균 입경이 84 ~ 90 ㎛, 가사 밀도가 2.39 ~ 2.46 gr/cm3, 흐름성을 나타내는 hall 통과 시간은 45 ~ 49 sec/50 gr 정도로써 세 가지 과립 방법에 상관없이 그 특성이 서로 유사하고 차이점이 거의 없었다.As shown in Table 2, as a result of reducing the granulated iron oxides according to the three granulation methods, the average particle diameter was 84 to 90 µm, the house density was 2.39 to 2.46 gr / cm 3 , and the hall passing time was 45 to 49. As for sec / 50 gr, the characteristics of the three granules were similar to each other and showed little difference.
표 2TABLE 2
또한, 표 2에 나타낸 금속 분말의 특성인 평균 입경은 입도 분포 측정기에 의한 입도 분포로부터 누적 50%가 되는 크기로 결정하였고, 가사 밀도는 KSD ISO 3923-1(깔때기법)의 기준으로 측정하였으며, 흐름성은 ISO 4490(Hall Flow-meter Method)의 기준으로 환원철 50 gr이 hall을 통과하는 시간을 측정하였다.In addition, the average particle diameter, which is a characteristic of the metal powder shown in Table 2, was determined to be 50% cumulative from the particle size distribution by the particle size distribution meter, and the pot density was measured based on KSD ISO 3923-1 (funnel method). The flowability measured the time that 50 gr of reduced iron passed through the hall according to the ISO 4490 (Hall Flow-meter Method).
[실시예 2]Example 2
실시예 2에서는 질산(HNO3)을 물로 희석하여 5 ~ 35%의 농도로 제조하고 이를 산화철 무게 대비 약 17%를 산화철에 투입하여 버티컬 그래뉼레이터로 1차 과립하고, 다시 10 Mesh의 망을 사용한 게이지 그래뉼레이터로 2차 과립을 한 후에 건조하여 과립자 시료를 준비하였다.In Example 2, nitric acid (HNO 3 ) was diluted with water to prepare a concentration of 5 to 35%, and about 17% of the iron oxide weight was added to iron oxide, and granulated first with a vertical granulator, and again, a mesh of 10 mesh was used. Granule samples were prepared by drying the secondary granules with a gauge granulator and drying them.
상기와 같이 준비된 과립자 시료를 1100℃에서 2시간 동안 수소 분위기에서 환원하여 분쇄하고 분급한 결과의 금속 분말의 특성은 표 3과 같다.The granular sample prepared as described above is pulverized and reduced in a hydrogen atmosphere at 1100 ° C. for 2 hours.
표 3에 나타낸 바와 같이 질산의 농도가 높아질수록 금속 분말의 평균 입경은 84㎛에서 최대 100㎛로 커졌고, 가사 밀도는 2.40 gr/cm3에서 최대 3.05 gr/cm3로 높아졌으며, 흐름성을 나타내는 hall 통과시간은 45 sec/50 gr에서 34 sec/50 gr로 짧아졌다.As shown in Table 3, as the concentration of nitric acid increased, the average particle diameter of the metal powder increased from 84 µm to 100 µm, and the pot density increased from 2.40 gr / cm 3 to 3.05 gr / cm 3 , indicating flowability. Hall passing time was shortened from 45 sec / 50 gr to 34 sec / 50 gr.
즉, 상기와 같은 결과는 질산 농도가 높은 용액을 결합제로 사용하여 과립을 한 후에 얻어지게 되는 금속 분말은 물 만을 결합제로 사용하는 경우보다 평균 입경, 가사 밀도, 흐름성 등의 금속분말 특성이 개선되는 것을 의미한다.That is, the above results indicate that the metal powders obtained after granulation using a solution having a high nitric acid concentration are improved in terms of metal powder characteristics such as average particle diameter, pot density, and flowability, compared to the case where only water is used as the binder. It means to be.
표 3TABLE 3
이상에서 설명한 것은 본 발명에 따른 금속 분말의 제조방법을 실시하기 위한 실시예에 불과한 것으로서, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 여러 가지 치환 및 변형, 변경이 가능하므로 전술한 실시예 및 첨부도면에 한정되는 것이 아니다.What has been described above is only an embodiment for carrying out the method of manufacturing the metal powder according to the present invention, various substitutions, modifications, and changes can be made within the scope without departing from the technical spirit of the present invention, the above-described embodiment and the accompanying It is not limited to the drawing.
상술한 바와 같은 본 발명은, 미세한 산화철 분말을 유기 결합제를 사용하여 과립을 함으로써 산화철의 입자가 커지게 되어 취급이 용이해지며, 또한, 가사 밀도가 높아져서 환원 장치에 산화철을 많이 장입할 수 있어 소요 비용을 절감할 수 있는 이점을 가진다.According to the present invention as described above, the fine iron oxide powder is granulated using an organic binder, so that the particles of iron oxide become large and easy to handle, and the pot density is high, so that a large amount of iron oxide can be charged into the reduction apparatus. It has the advantage of reducing costs.
특히, 상기 유기 결합제로써 물 대신 강산을 사용하여 산화철 분말을 과립함으로써 산화철 1차 입자간의 화학적 결합을 유도하고, 고온 환원에 의한 입자간의 소결 현상이 용이하게 하여 제조되는 금속 분말의 요구 특성인 평균 입경, 가사 밀도 및 흐름성의 제어가 가능해지는 효과가 있다.In particular, by incorporating a strong acid instead of water as the organic binder to granulate the iron oxide powder to induce chemical bonding between the iron oxide primary particles, the sintering phenomenon between particles by high temperature reduction facilitates the average particle size, which is a required characteristic of the metal powder produced In addition, it is possible to control the house density and flowability.
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