US20050109159A1 - Method of manufacturing Fe nanopowders by chemical vapor condensation - Google Patents
Method of manufacturing Fe nanopowders by chemical vapor condensation Download PDFInfo
- Publication number
- US20050109159A1 US20050109159A1 US10/974,125 US97412504A US2005109159A1 US 20050109159 A1 US20050109159 A1 US 20050109159A1 US 97412504 A US97412504 A US 97412504A US 2005109159 A1 US2005109159 A1 US 2005109159A1
- Authority
- US
- United States
- Prior art keywords
- powders
- gas
- nanopowders
- iron
- chemical vapor
- Prior art date
- Legal status (The legal status 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 status listed.)
- Abandoned
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Classifications
-
- 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
- B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous 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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/712—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the surface treatment or coating of magnetic 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
Definitions
- the present invention relates to a manufacturing method of iron nanopowders, and more specifically, to a method of manufacturing nano-sized iron powders by means of chemical vapor condensation.
- Fine powders having magnetic properties that is, fine magnetic powders, have various applications, for example, contrast media for magnetic resonators, recording media for magnetic tapes, magnetic fluid materials, etc.
- the magnetic powders presently commercially available, are exemplified by oxide-based powders, such as Fe 2 O 3 , Fe 3 O 4 , Fe-ferrite and Co-ferrite.
- the magnetic powders have been mainly manufactured by a liquid reaction process, such as metal hydroxide reduction or metal salt reduction.
- the contrast medium having high quality and the magnetic fluid for sealing materials are possible to be manufactured by use of only material powders exhibiting superparamagnetic properties, which are fined to have a particle size not larger than a single magnetic domain. Accordingly, there required methods of synthesizing finer magnetic metal powders having further decreased particle sizes while improving magnetic properties thereof.
- an object of the present invention is to alleviate the problems encountered in the related art and to provide a method of synthesizing metal iron powders having sizes of tens of nm, by vaporizing an iron atom-containing liquid material having a low melting point at high temperatures and then condensing iron atoms in decomposed Fe and CO gas by chemical vapor condensation.
- the prevent invention provides a method of manufacturing Fe nanopowders by chemical vapor condensation, including: vaporizing a Fe-containing liquid precursor to gas, to obtain a vaporized gas; decomposing the vaporized gas to Fe while being introduced with an inert gas, to obtain decomposed Fe; and condensing the decomposed Fe, to obtain Fe nanopowders.
- FIG. 1 is a schematic view of a chemical vapor condensation device used in the present invention
- FIG. 2 is electron micrographs of Fe nanopowders manufactured at different reaction temperatures
- FIG. 3 is an X-ray diffraction spectrum for the Fe nanopowders of FIG. 2 ;
- FIG. 4 is enlarged electron micrographs of parts of the Fe nanopowders, in the Fe nanopowders of FIG. 2 .
- a pure iron material has a magnetization value two or three times higher than that of oxide materials, and also, has low anisotropic properties, thus having a lower coercive force. Further, as a particle size of iron decreases, the magnetization value is constantly reduced while the coercive force is increased, whereby iron is possible to be used as a magnetic recording medium. Moreover, iron having a very small particle size comes to be a superparamagnetic material, and hence, is usable as a magnetic fluid.
- the device ( 1 ) includes a ceramic bubbler ( 3 ), a reactor ( 6 ), and a chamber ( 7 ).
- a liquid precursor containing Fe is vaporized to gas by means of the ceramic bubbler ( 3 ). That is, the liquid precursor in a storage bath ( 2 ) is fed through a feeding pipe ( 5 ) and a feeder ( 4 ), and then is vaporized while passing through the ceramic bubbler ( 3 ) that is maintained at predetermined temperatures.
- the Fe-containing liquid precursor is exemplified by iron pentacarbonyl (Fe(CO) 5 ), or iron acetate ((CH 3 CHO 2 ) 2 Fe), in which iron pentacarbonyl having a vaporization point of about 103° C. is easily vaporized at 150-220° C.
- the gas vaporized by use of the ceramic bubbler ( 3 ) is not decomposed to Fe and CO gas in the above temperature ranges. Therefore, while the vaporized gas is introduced with an inert gas, it passes through the reactor ( 6 ) which is maintained at high temperatures, whereby Fe is decomposed from the vaporized gas.
- the reactor ( 6 ) is in the temperature range of 400 to 1000° C., and preferably, 400 to 800° C. If the temperature of the reactor ( 6 ) is higher than 1000° C., large quantities of ⁇ -Fe phase are obtained, together with ⁇ -Fe. In such cases, the ⁇ -Fe phase as a non-magnetic material negatively affects requirement properties of synthetic powders, which is unfavorable.
- the decomposed Fe gas transferred to the reactor ( 6 ) along with the inert gas is condensed to the size of tens of nm therein, and is formed to be crystalline Fe powders, which are then sprayed into the chamber ( 7 ).
- the crystalline Fe gas is floated for several hours and then is attached to an inner wall or a bottom surface of the chamber ( 7 ). Even after the precursor solution is completely fed, the floating of the Fe powders is continued for several hours in the chamber ( 7 ).
- the inert gas is continuously introduced into the chamber ( 7 ) until all the synthesized Fe powders are stably settled down, whereby the inside of the chamber ( 7 ) is maintained in a non-oxidative protection atmosphere and the CO gas remaining in a very small amount in the chamber ( 7 ) is discharged out of the chamber ( 7 ).
- the chamber ( 7 ) when the chamber ( 7 ) is opened as soon as the synthesized Fe powders are collected therein, it may be exploded. Hence, before the chamber ( 7 ) is opened, a small amount of oxygen is fed into the chamber ( 7 ) through an inlet ( 8 ) thereof, and thus, the iron nanopowders are coated with an oxide layer. Like this, it is preferred that the iron nanopowders are subjected to passivation treatment to be stably handled under atmosphere.
- Iron pentacarbonyl as a liquid precursor was fed into a chemical vapor condensation device of FIG. 1 , thus manufacturing Fe powders.
- a ceramic bubbler ( 3 ) of the above device was maintained in a range of 150-200° C., and the liquid precursor was fed at 0.30 g/min.
- Ar gas was introduced at 2000 cc/min into the ceramic bubbler ( 3 )
- the vaporized gas passed through a reactor ( 6 ) and then was sprayed into a chamber ( 7 ).
- the reactor was formed with a virtually pure alumina tube having an inner diameter of 5 mm and a length of 300 mm, and was in the temperature range of 400 to 1000° C.
- the manufactured Fe powders were observed by means of an electron microscope. The results are depicted in FIG. 2 .
- the Fe powders have an average particle size of 8, 17 and 68 nm when the synthesizing temperatures are 400° C. (inventive example 1), 600° C. (inventive example 2) and 800° C. (inventive example 4).
- the average particle size of the Fe powders increases to 96 nm.
- the particle sizes of the powders synthesized at 400 and 600° C. are very fine to the extent of 20 nm or less, such powders may be agglomerated together. In this case, the agglomerated powders may be separated by use of energy sources, such as ultrasonic waves and microwaves.
- FIG. 3 shows analytic results of X-ray diffraction patterns of Fe powders according to reaction temperatures.
- the Fe powders synthesized at 400° C. and 600° C., respectively have an amorphous type peak of Fe 3 O 4 .
- the Fe powders synthesized at 800° C. and 1000° C., respectively have such an oxide, they have no X-ray diffraction peak. This is because the above oxide has a very small volume compared to the increased particle size of iron.
- large quantities of ⁇ -Fe which have a bad effect on the properties of the synthesized powders, are present, together with ⁇ -Fe.
- FIG. 4 shows enlarged micrographs of the Fe powders synthesized at 600° C. and 800° C. among the Fe powders of FIG. 2 , to observe the oxide coating layer on the respective Fe powders.
- the Fe powders synthesized at 600° C. and 800° C., respectively have the oxide layer which is 3-4 nm thick. That is, even though the surface oxide layer is slightly thicker according to the increase of the reaction temperature, it is hardly affected by the reaction temperature.
- Fe powders were synthesized in the same manner as in Example 1, with the exception that the liquid precursor was fed at 0.15 g/min and reacted at 600° C. (inventive example 3).
- the Fe powders had an average particle size of 16 nm. From this, it can be found that a slow feeding rate of the precursor solution does not greatly affect the fineness of Fe powders.
- the maximum magnetization value may decrease even to about 50% or less of a maximum value of a bulk material. For example, a theoretical maximum magnetization value of bulk pure iron amounts to 225 emu/g, while the maximum magnetization value of iron of the present invention decreases from about 200 emu/g to about 120 emu/g by particle fineness.
- the present invention provides a method of manufacturing Fe nanopowders by chemical vapor condensation, characterized in that sizes, phases and magnetic properties of the synthesized Fe nanopowders can be controlled according to reaction temperatures.
- the Fe nanopowders of the present invention is applicable as a magnetic recording medium. Further, through process improvement, such as decrease of the reaction temperatures, the Fe powders can be further fined, whereby they can be used as a magnetic fluid.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
- Soft Magnetic Materials (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2003-0077589 | 2003-11-04 | ||
KR1020030077589A KR100572244B1 (ko) | 2003-11-04 | 2003-11-04 | 화학기상응축법에 의한 나노 철분말의 제조방법 |
Publications (1)
Publication Number | Publication Date |
---|---|
US20050109159A1 true US20050109159A1 (en) | 2005-05-26 |
Family
ID=34587868
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US10/974,125 Abandoned US20050109159A1 (en) | 2003-11-04 | 2004-10-26 | Method of manufacturing Fe nanopowders by chemical vapor condensation |
Country Status (3)
Country | Link |
---|---|
US (1) | US20050109159A1 (ja) |
JP (1) | JP2005139555A (ja) |
KR (1) | KR100572244B1 (ja) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050150329A1 (en) * | 2003-11-05 | 2005-07-14 | Kim Byung K. | Method of producing nano-sized Fe powder having polymer coated layer |
US7601324B1 (en) | 2008-07-11 | 2009-10-13 | King Fahd University Of Petroleum And Minerals | Method for synthesizing metal oxide |
CN104985177A (zh) * | 2015-06-18 | 2015-10-21 | 南开大学 | 一种表面钝化的纳米锗颗粒的制备方法 |
JP2016510300A (ja) * | 2013-01-22 | 2016-04-07 | エムセデ テクノロジーズ ソシエテ ア レスポンサビリテ リミティー | カーボンナノ構造を生成する方法および装置 |
JP2019006674A (ja) * | 2018-08-23 | 2019-01-17 | エムセデ テクノロジーズ ソシエテ ア レスポンサビリテ リミティー | カーボンナノ構造を生成する方法および装置 |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100801114B1 (ko) | 2006-08-01 | 2008-02-05 | 한국원자력연구원 | 나노분말 제조장치 및 그 제조방법 |
JP7236063B1 (ja) | 2021-11-10 | 2023-03-09 | コリア インスティチュート オブ インダストリアル テクノロジー | 無機粉末の製造装置及び製造方法 |
KR102572729B1 (ko) * | 2021-11-10 | 2023-08-31 | 한국생산기술연구원 | 무기분말의 제조장치 및 제조방법 |
KR102564634B1 (ko) * | 2021-11-10 | 2023-08-08 | 한국생산기술연구원 | 무기분말의 제조장치 및 제조방법 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5766306A (en) * | 1996-06-04 | 1998-06-16 | The Boeing Company | Continuous process for making nanoscale amorphous magnetic metals |
US6033624A (en) * | 1995-02-15 | 2000-03-07 | The University Of Conneticut | Methods for the manufacturing of nanostructured metals, metal carbides, and metal alloys |
-
2003
- 2003-11-04 KR KR1020030077589A patent/KR100572244B1/ko not_active IP Right Cessation
-
2004
- 2004-10-26 US US10/974,125 patent/US20050109159A1/en not_active Abandoned
- 2004-11-04 JP JP2004320990A patent/JP2005139555A/ja active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6033624A (en) * | 1995-02-15 | 2000-03-07 | The University Of Conneticut | Methods for the manufacturing of nanostructured metals, metal carbides, and metal alloys |
US5766306A (en) * | 1996-06-04 | 1998-06-16 | The Boeing Company | Continuous process for making nanoscale amorphous magnetic metals |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050150329A1 (en) * | 2003-11-05 | 2005-07-14 | Kim Byung K. | Method of producing nano-sized Fe powder having polymer coated layer |
US7396502B2 (en) | 2003-11-05 | 2008-07-08 | Korea Institute Of Machinery And Materials | Method of producing nano-sized Fe powder having polymer coated layer |
US7601324B1 (en) | 2008-07-11 | 2009-10-13 | King Fahd University Of Petroleum And Minerals | Method for synthesizing metal oxide |
JP2016510300A (ja) * | 2013-01-22 | 2016-04-07 | エムセデ テクノロジーズ ソシエテ ア レスポンサビリテ リミティー | カーボンナノ構造を生成する方法および装置 |
CN104985177A (zh) * | 2015-06-18 | 2015-10-21 | 南开大学 | 一种表面钝化的纳米锗颗粒的制备方法 |
JP2019006674A (ja) * | 2018-08-23 | 2019-01-17 | エムセデ テクノロジーズ ソシエテ ア レスポンサビリテ リミティー | カーボンナノ構造を生成する方法および装置 |
Also Published As
Publication number | Publication date |
---|---|
KR20050042929A (ko) | 2005-05-11 |
JP2005139555A (ja) | 2005-06-02 |
KR100572244B1 (ko) | 2006-04-19 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
AS | Assignment |
Owner name: KOREA INSTITUTE OF MACHINERY AND MATERIALS, KOREA, Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:KIM, BYUNG KEE;LEE, DONG WON;CHOI, CHUL JIN;REEL/FRAME:015936/0361;SIGNING DATES FROM 20041015 TO 20041017 |
|
STCB | Information on status: application discontinuation |
Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION |