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WO2006009409A1 - Procede de preparation d'une matiere de base de poudre metallique de taille nanometrique et procede de production d'un corps fritte au moyen de ladite matiere de base - Google Patents

Procede de preparation d'une matiere de base de poudre metallique de taille nanometrique et procede de production d'un corps fritte au moyen de ladite matiere de base Download PDF

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Publication number
WO2006009409A1
WO2006009409A1 PCT/KR2005/002378 KR2005002378W WO2006009409A1 WO 2006009409 A1 WO2006009409 A1 WO 2006009409A1 KR 2005002378 W KR2005002378 W KR 2005002378W WO 2006009409 A1 WO2006009409 A1 WO 2006009409A1
Authority
WO
WIPO (PCT)
Prior art keywords
metal powder
nano
sized metal
feedstock
sintered body
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.)
Ceased
Application number
PCT/KR2005/002378
Other languages
English (en)
Inventor
Jai-Sung Lee
Yun-Sung Kang
Bum-Ha Cha
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Industry University Cooperation Foundation IUCF HYU
Industry University Cooperation Foundation of Sogang University
Original Assignee
Industry University Cooperation Foundation IUCF HYU
Industry University Cooperation Foundation of Sogang University
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 Industry University Cooperation Foundation IUCF HYU, Industry University Cooperation Foundation of Sogang University filed Critical Industry University Cooperation Foundation IUCF HYU
Priority to US11/658,283 priority Critical patent/US20080286141A1/en
Priority to JP2007522431A priority patent/JP2008507623A/ja
Publication of WO2006009409A1 publication Critical patent/WO2006009409A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/148—Agglomerating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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

Definitions

  • the present invention relates to a method for preparing a nano-sized metal powder feedstock. More particularly, the present invention relates to a method for preparing a feedstock suitable for the production of a sintered body of a nano-sized metal powder that can be completely compacted without deformation, such as twists and cracks, and a method for producing a sintered body using the feedstock.
  • the problems en ⁇ countered with the process are that large particles are grown and thus undesirable mod ⁇ ifications to characteristics of the raw materials are involved, deteriorating the physical properties of the sintered body.
  • additional processing steps e.g., addition of a small amount of an alloy element, pressurization during sintering, and remolding, have been employed.
  • nano-sized metal powders have superior sinterability, they can be uniformly shrunken and completely compacted by low-temperature/atmospheric pressure sintering techniques.
  • nano-sized metal powders have highly uniform and fine crystalline structures, product char ⁇ acteristics are improved. Under these circumstances, application of nano-sized metal powders to metal injection molding techniques is actively under study.
  • Korean Patent No. 0366773 (Title: A method for producing a nano-sized metal powder feedstock for metal injection molding, patentee: Hanyang Educational Institute) suggests a method for producing a feedstock for metal injection molding by which explosive oxidation of the nano-sized metal powder can be controlled and complete compaction of a product can be achieved while maintaining the shape of the product during production. According to this method, the coating of a binder to the nano-sized metal powder inhibits explosive oxidation of the nano-sized metal powder and improves complete compaction of the product.
  • the method is limited tothe production of a feedstock of the nano-sized metal powder, and fails to sufficiently consider the applicability to a near-net product.
  • the nano-sized powder since the nano-sized powder has a large interfacial energy, non-uniform pore distribution may arise inside the molded body after debinding. In addition, pores remain even after low-temperature/atmospheric pressure sintering, thus deteriorating the mechanical properties of a sintered body. Accordingly, the nano-sized powder should undergo high-temperature sintering at above l,000°C.
  • the present invention has been made in view of the above problems of the prior art, and it is an object of the present invention to provide a method for preparing a nano-sized metal powder feedstock suitable for the production of a sintered body that can be completely compacted by preventing the occurrence of coarse pores during subsequent debinding through the structural control of the nano-sized metal powder.
  • a method for preparing a nano-sized metal powder feedstock comprising the steps of preparing a nano-sized metal powder, mixing the metal powder with a solution of an organic binder in a solvent, and wet-milling the mixture so that aggregates of the metal powder are uniformly formed.
  • the mixing step and the wet-milling step are simultaneously carried out to simplify the procedure of the method.
  • pores can be uniformly distributed during the subsequent formation of a molded body, desired debinding can be carried out without deformation of the molded body, despite mixing of only one or two organic binders with the metal powder.
  • the organic binder is a water-soluble binder and the solvent is distilled water or alcohol.
  • the water-soluble organic binder may be stearic acid.
  • the viscosity of the binder solution is preferably 2
  • a binder solution having a viscosity of 0.002 PaDs there can be preferably used.
  • the nano-sized metal powder is an Fe-based alloy powder and contains at least one metal selected from the group consisting of Ni, Cu, Mo and W.
  • a representative nano- sized metal powder is an Fe-Ni powder whose Ni content is 2 ⁇ 80 wt%.
  • the mixing step may further include the sub-step of adding a surfactant to the mixture.
  • the surfactant is preferably added in an amount not exceeding 2 wt%.
  • the mixing step and the wet-milling step are preferably carried out in a state where atmospheric air is blocked. Specifically, the steps can be carried out in an inert gasor protective gas atmosphere.
  • a method for producing a sintered body using a nano-sized metal powder comprises the steps of preparing the nano-sized metal powder feedstock, molding the nano-sized metal powder feedstock into a desired shape, debinding the molded body, and sintering the debound body.
  • the molding step can be carried out by injection molding or extrusion molding.
  • the debinding step is carried out by heating the molded body to about 300°C to about 500°C at a rate 3 ⁇ 10 °C/min., thus shortening the debinding time to about 2 hours.
  • the sintering step can be carried out by rapidly heating the debound body to about
  • the sintering step is carried out consecutively after the debinding step.
  • the sintered body thus produced has a grain size of 200 D or less and a degree of compaction of 95% or higher.
  • the present invention is characterized in that the size of the aggregates of the nano- sized metal powder is uniformly controlled so that the aggregates can be applied to low-temperature/atmospheric pressure sintering.
  • the nano-sized metal powder is mixed with the organic binder in a solution state and is wet-milled, thereby maintaining the size of the aggregates at a uniform level.
  • the use of the binder solution allows the binder to be more effectively coated on the surface of the powder particles so that oxidation of the particles is prevented. Ac ⁇ cordingly, even when a small amount of the binder is added during molding, the viscosity of the binder solution is lowered for sufficient coating, thus providing a nano- sized metal powder feedstock that can be stored in air for a prolonged period of time without oxidative contamination.
  • the binder is commonly mixed in an amount of from about 2% to about 50%.
  • the binder is added in a relatively small amount, e.g., in bi-directional compression molding, sufficient coating effects cannot be attained by the method disclosed in Korean Patent No. 0366773.
  • the use of the binder solution and wet-milling process in the present invention ensures uniform distribution of the aggregates and more effective coating of the binder.
  • the solvent used to form the binder solution is not especially limited to distilled water or alcohol. Any solvent can be used so long as it forms a binder solution having a sufficiently low viscosity. Various known solvents can be used depending on the particular kind of the binder. At this time, the binder solution preferably has a viscosity not higher than about 2 PaDs at from about 100°C to 200°C. [29] In the method for preparing a feedstock of the present invention, the step of mixing the nano-sized metal powder and the binder solution and the wet-milling step for uniform size control of the aggregates can be simultaneously carried out to simplify the procedure of the method.
  • the binder solution and the nano-sized metal powder are charged into a milling machine and the mixture is milled.
  • Mixing and grinding in the milling machine enables both the coating of the binder solution and size control of the aggregates.
  • These processing steps are preferably carried out in a state where atmospheric air is blocked. More specifically, it is preferred that the processing steps are carried out in clean equipment filled with an inert or protective gas.
  • a small amount of a surfactant can be optionally used as a dispersant.
  • the surfactant is preferably added in an amount not exceeding 2 wt%, based on the weight of the mixture, so as not to deteriorate the characteristics of the sintered body.
  • the nano-sized metal feedstock is used to produce a sintered body
  • aggregates are uniformly distributed in the feedstock and thus occurrence of coarse pores is prevented. Accordingly, deformation arising from separation of the binder can be minimized during the subsequent debinding. Accordingly, unlike in conventional methods (where five or more binders are used depending on temperature gradients), one or two binders can be used in the present invention, thus simplifying the procedure of the method.
  • the debinding is conducted by heating the molded body to 300 ⁇ 500°C at a rate 3 ⁇ 10 °C/min., thus shortening the debinding time to about 2 hours.
  • the debound body has a uniform particle size without occurrence of coarse pores, low-temperature/atmospheric pressure sintering at a temperature range of 500—1, 000°C can be applied to the debound body to manufacture a nano-sized metal product having a grain size of 200 D or less and a degree of compaction of 95% or higher.
  • Fig. 1 is a scanning electron micrograph (SEM) of a nano-sized Fe-Ni alloy powder that can be used in the present invention.
  • Fig. 2 is a graph showing the results of the particle size analysis of a nano-sized Fe-
  • FIGs. 3 and 4 are scanning electron micrographs of the broken side of a debound body of a nano-sized Fe-Ni alloy powder obtained in Example 2 of the present invention at different magnifications (20Ox and 20,00Ox, respectively).
  • FIG. 5 shows photographs of a molded body and a sintered body of a nano-sized Fe-
  • Fig. 6 is an optical micrograph (20Ox) of a sintered body of a nano-sized Fe-Ni alloy powder produced in Example 2 of the present invention.
  • Fig. 7 is a scanning electron micrograph of an overetched surface of the sintered body shown in Fig. 6. Mode for the Invention
  • a nano-sized Fe-Ni alloy powder was prepared as a nano-sized metal powder in accordance with the following procedure. Specifically, an Fe oxide and an Ni oxide, each of which had an average particle size of 1 m, were mixed together to have a weight ratio of 92 : 8, and were then subjected to high-energy ball milling in a steel attritor for 10 hours to finely pulverize the mixture to a size of 10—20 D.
  • the pulverized mixture was dried and reduced under a hydrogen atmosphere at 450°C for 40 minutes to prepare a nano-sized Fe-8wt% Ni alloy powder.
  • particles having a size of about 70 D gathered to form aggregates having a size of about 5 m to tens of micrometers.
  • a binder solution and a surfactant were added to the nano-sized Fe-8wt% Ni alloy powder.
  • the binder solution was prepared by mixing 5g of stearic acid (CH (CH )COOH) and 35 ml of ethanol as a solvent.
  • As the surfactant 0.5 mol of octanol (C H O) was used.
  • the mixing was conducted together with wet-milling using a three- dimensional mixer. Specifically, the milling was conducted using 4Og of steel balls at 60 rpm for 9 hours. The milled mixture was dried until the loading rate of the nano- sized Fe-8wt% Ni alloy powder reached 50%, to prepare a nano-sized metal powder feedstock.
  • Fig. 2 is a graph showing the results of the particle size analysis of the nano-sized
  • the nano-sized Fe-Ni alloy powder feedstock using a laser particle size analyzer (LPA).
  • LPA laser particle size analyzer
  • the nano-sized Fe-Ni alloy powder feedstock was prepared by adding 0.5 mol of octanol as a surfactant to the Fe-8wt% Ni nano-sized metal powder in 35 ml of ethyl alcohol, and wet-milling the mixture using 40 g of steel balls for 9 hours.
  • the laser particle size analysis indicates that the powder particles with a size of tens of mi ⁇ crometers were efficiently pulverized and dispersed by wet-milling to form aggregates with an average size of 700 D.
  • a cylindrical sintered body was produced using a nano-sized metal powder feedstock.
  • the nano-sized metal powder feedstock prepared in Example 1 was injected into a cylindrical mold under 100 MPa at 100°C to produce a cylindrical molded body.
  • the cylindrical molded body thus produced was compacted to about 52% (see the left hand side of Fig. 5).
  • Fig. 3 is a scanning electron micrograph (20Ox) of the broken side of the sample obtained after debinding
  • Fig. 4 is a scanning electron micrograph (20,00Ox) of the broken side of the debound body.
  • no coarse pores (micrometer-scale pores) adversely affecting the subsequent sintering process were observed, and instead, a fine structure consisting of uniform particles with a size not larger than 100 D was observed. This is because the aggregates wet-milled in Example 1 were uniformly filled into pores between unpulverized aggregates.
  • Fig. 6 is an optical micrograph (20Ox) showing the fine structure of the cylindrical
  • Fig. 6 is a scanning electron micrograph (5,000x) showing the grain of the cylindrical Fe-8wt% Ni sintered body after overetching. As shown in Fig. 7, the sintered body has a fine structure wherein the grains having a size of about 300 D are uniformly distributed.
  • the sintered bodies (MIM-2200, MIM-2700 and MIM-4605) according to the standard specification adopted by the Metal Powder Industry Federation (MPIF) have a Vickers hardness of 85—130.
  • the injection molded metal powder sintered bodies according to the Japanese standard specification were subjected to car- burization and annealing in order to improve the mechanical properties of the injection molded Fe-Ni powders, they have a high Vickers hardness of 300 (in the case of 2 wt% Ni) and 340 (in the case of 8 wt% Ni).
  • the Fe-8wt% Ni sintered body produced in the present invention has a Vickers hardness of 298, which is greater than two times that specified in the U. S standard specification.
  • the Vickers hardness of the Fe- 8wt% Ni sintered body produced in the present invention is comparable to that specified in Japanese standard specification without involving additional carburization and annealing for improving the mechanical properties of the sintered body.
  • the application of wet-milling in the presence of the binder solution allows the binder to be more effectively coated on the surface of the powder particles and enables uniform control of the size of the aggregates. Since the nano-sized metal powder feedstock prepared by the methods of the present invention can maintain the internal structure of the molded body uniform and fine, completely compacted near-net nanos- grappltured products can be manufactured without deformation, such as twists and cracks, even after sintering using the nano-sized metal powder feedstock. Therefore, according to the method of the present invention, simplification of the production procedure and reduction in production costs can be expected.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention concerne un procédé de préparation d'une matière de base de poudre métallique de taille nanométrique. Ce procédé consiste à préparer une poudre métallique de taille nanométrique, à mélanger la poudre métallique avec une solution d'un liant organique dans un solvant, et à réaliser un concassage humide du mélange, de telle manière que des agrégats de poudre métallique sont formés uniformément. Cette invention a aussi trait à un procédé de production d'un corps fritté au moyen de la matière de base.
PCT/KR2005/002378 2004-07-23 2005-07-22 Procede de preparation d'une matiere de base de poudre metallique de taille nanometrique et procede de production d'un corps fritte au moyen de ladite matiere de base Ceased WO2006009409A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US11/658,283 US20080286141A1 (en) 2004-07-23 2005-07-22 Method for Preparing Nano-Sized Metal Powder Feedstock and Method for Producing Sintered Body Using the Feedstock
JP2007522431A JP2008507623A (ja) 2004-07-23 2005-07-22 ナノ寸法の金属粉末のフィードストックを調製する方法及び該フィードストックを用いた焼結体を製造する方法。

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020040057701A KR20060008046A (ko) 2004-07-23 2004-07-23 나노크기의 금속분말 피드스톡 제조방법 및 이를 이용한소결체 제조방법
KR10-2004-0057701 2004-07-23

Publications (1)

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WO2006009409A1 true WO2006009409A1 (fr) 2006-01-26

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PCT/KR2005/002378 Ceased WO2006009409A1 (fr) 2004-07-23 2005-07-22 Procede de preparation d'une matiere de base de poudre metallique de taille nanometrique et procede de production d'un corps fritte au moyen de ladite matiere de base

Country Status (4)

Country Link
US (1) US20080286141A1 (fr)
JP (1) JP2008507623A (fr)
KR (1) KR20060008046A (fr)
WO (1) WO2006009409A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
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CN107815592A (zh) * 2017-10-26 2018-03-20 北京科技大学 一种发动机燃油喷嘴电磁阀磁芯的制备方法
CN109822090A (zh) * 2017-11-23 2019-05-31 中国科学院化学研究所 一种原位包覆有机物的纳米铜粉的制备方法
WO2020198658A1 (fr) * 2019-03-28 2020-10-01 Veloxint Corporation Systèmes et procédés de moulage par injection de poudres métalliques nanocristallines

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KR100796150B1 (ko) * 2006-08-30 2008-01-21 한국피아이엠(주) 고형상비를 가지는 자동차 브레이크용 솔레노이드밸브 시트하우징의 제조방법
CN101462163A (zh) * 2009-01-16 2009-06-24 江西稀有稀土金属钨业集团有限公司 硬质合金混合料制备的球磨工艺
CN102312132B (zh) * 2011-09-15 2013-01-02 西安理工大学 一种真空烧结制备Ni-W合金的方法
KR20160069447A (ko) * 2014-12-05 2016-06-16 한양대학교 에리카산학협력단 금속 분말, 그 제조 방법, 및 이를 이용한 성형품의 제조 방법
JP6994638B2 (ja) * 2015-10-09 2022-02-21 パーティクル３ディー アプス ３ｄ印刷用供給原料およびその使用
CN107857594A (zh) * 2017-11-29 2018-03-30 北京科技大学 一种氮化铝陶瓷异型件及其制备方法
RU2718946C1 (ru) * 2019-06-17 2020-04-15 Федеральное государственное бюджетное учреждение науки Институт физики прочности и материаловедения Сибирского отделения Российской академии наук (ИФПМ СО РАН) Способ получения гранулированной металлопорошковой композиции (фидстока) и композиция, полученная данным способом

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107815592A (zh) * 2017-10-26 2018-03-20 北京科技大学 一种发动机燃油喷嘴电磁阀磁芯的制备方法
CN109822090A (zh) * 2017-11-23 2019-05-31 中国科学院化学研究所 一种原位包覆有机物的纳米铜粉的制备方法
WO2020198658A1 (fr) * 2019-03-28 2020-10-01 Veloxint Corporation Systèmes et procédés de moulage par injection de poudres métalliques nanocristallines

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KR20060008046A (ko) 2006-01-26
US20080286141A1 (en) 2008-11-20

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