US3748118A - Process for preparing finely particled metallic nickel powder having a spheroidal form - Google Patents

Process for preparing finely particled metallic nickel powder having a spheroidal form Download PDF

Info

Publication number
US3748118A
US3748118A US00210608A US3748118DA US3748118A US 3748118 A US3748118 A US 3748118A US 00210608 A US00210608 A US 00210608A US 3748118D A US3748118D A US 3748118DA US 3748118 A US3748118 A US 3748118A
Authority
US
United States
Prior art keywords
nickel
process according
acrylonitrile
nickel powder
powder
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.)
Expired - Lifetime
Application number
US00210608A
Other languages
English (en)
Inventor
F Montino
F Guerriere
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.)
MONTICATINI EDISON SpA
MONTICATINI EDISON SpA IT
Original Assignee
MONTICATINI EDISON SpA
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 MONTICATINI EDISON SpA filed Critical MONTICATINI EDISON SpA
Application granted granted Critical
Publication of US3748118A publication Critical patent/US3748118A/en
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • 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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors

Definitions

  • ABSTRACT A process for preparing finely divided, homogeneous, metallic nickel powder with a very narrow granulometric spectrum having a spheroidal form and with a granulometric range between 0.07 and 2 microns, characterized in that a hydroalcoholic suspension of a nickel compound selected from the class consisting of the hydroxide, the formate and the acetylacetonate is treated with hydrogen at temperatures ranging from 160 to 250 C and at hydrogen partial pressures ranging from 25 to 100 am, in the presence of one or more additives selected from the class consisting of acrylonitrile, pyridine, and complexes of zerovalent nickel.
  • the present invention relates to a process for preparing powder of metallic nickel. More particularly, it relatesto aproxiess for preparing finely divided, homogeneous,;., metallic'nickel powder having a changeable granulometrydep'ending on the operational conditions and varying frorrt'0.07 to 2 microns and a spheroidal form. i f
  • Finely divided nickel powders having a spheroidal form, with a diameter between 0.1 and 2 microns, are used more and more in powder metallurgy.
  • Thewer'y' -fin'e nickel powders may be also used to manufacture the socalled dispersion strengthened alloys" consisting oi fine mixtures of a dispersoid (oxide,
  • boride, carbide the metallic nickel body.
  • These alloys have an excellent heat-resistance (l,000-l,300 C), higherthan that of several superalloys and competing with'the molybdenum alloys.
  • lnthese alloys there is an optimum relation between the radius of the dis persoid'atld'th'at of the body; for instance for a radius of 0.0l'-0-.'l imicron of the dispersoid, the radius of the body should be of the order of 0.05 0.5 micron.
  • the finely particled nickel powders are used, moreover, either for making different types of sintered alloys (Ni, Cr, Co, Ni-W, Ni-Cu), or for makingalloys based on Fe-Ni used as magnetic materials, or for making self-lubricating porous gears, or for making electrodes for alkalinebatteries and for fuel cells.
  • Ni nickel powders are used for making porous barriers based on Ni, for the separation in gaseous phase of uranium isotopes.
  • the object of the present invention is therefore to provide a simple and economic process for preparing very fine nickel powder having a controllable diameter, a spheroidal form and a homogeneous granulometry.
  • finely particled and homogeneous metallic nickel powder in the granulometric range between 0.07 and 2 microns with a spheroidal form and with a very narrow granulometric spectrum is obtained by treating with hydrogen a hydro-alcoholic suspension of a nickel compound selected from the hydrate, formate and acetylacetonate, at temperatures ranging from 160 to 250 C and at hydrogen partial pressures ranging from 25 to 100 atm in the presence of one or-more'additives selected from the class consisting of acrylonitrile, pyridine and zerovalent nickel complexes.
  • the hydrogen pressure between 25 and 100 atm.
  • the reaction is completed in a few minutes and with practically quantitative yields.
  • the Ni powder thus obtained is washed with water and methanol, then dried in a nitrogen stream and under vacuum.
  • the Ni powder product may contain as impurities C from 0.1 to 1 percent and H and N from 0.05 to 0.2 percent. These impurities can be completely eliminated by heating in a hydrogen atmosphere.
  • the powders so obtained are characterized by a very narrow granulometry spectrum: of the' granules being within a maximum difference of i 15 20% with respect to the average diameter of the granules.
  • the nickel compounds suitable for use in the process according to the present invention are nickel compounds such as, for instance, nickel hydroxide, and salts such as nickel formate, and nickel acetylacetonate.
  • the nickel compound is used in concentrations between 10 and g/ 1; and preferably around 60 g/l.
  • water-soluble alcohols or glycols may be used; preferably methyl alcohol and monoethylene glycol.
  • the mixture of alcohol-water is used in a ratio comprised between 10:1 and 1:10 the ratio alcohol/wa ter controls, under otherwise the same conditions, the diameter of the obtained particles. High ratios give products of smaller diameter.
  • Additives capable of giving the spheroidal form to the particles are compounds, such as acrylonitrile and pyridine, added in quantities ranging from 1 to 50 g/l. Without the addition of these additives the powder does not have a spheroidal form and is more aggregated.
  • the quantity of bis-acrylonitrile-nickel or of other nickel zero-valent compounds, added to obtain a control of the particle size in the range of from 0.7 0.07 microns, can vary between 1 and 50 g/l.
  • the greater concentrations give rise to smallerdiameters.
  • EXAMPLE 1 143 g of a 33% Ni(OH) obtained by precipitation with NaOl-l of NiCl, (equal to 47 g of dry Ni(OH) and 96 g H O) were suspended in a solution of 540 cc of monoethylene glycol and 24 cc of H in order to have a glycol/water ratio equal to 4.5/1. 26 cc of acrylonitrile, 14 cc of pyridine and 50 mg of Ni powder were added thereto. The mixture thus obtained was poured into a 2-liter stainless steel autoclave provided with a blade stirrer and resistance heating. After having eliminated the air by purging with N the temperature was brought to 200 C and 50 atm of H were charged thereto.
  • the nickel powder thus obtained was repeatedly washed with methanol and dried in a nitrogen stream and then under vacuum. 29 g. of nickel powders are obtained.
  • Theaverage diameter of the granules was 1.2 microns. More than 80 percent of the granules had a diameter ranging from 1 to 1.4 microns.
  • the following test was carried out by varying the glycol/water ratio. The test was conducted as above described, by using 47 g of Ni(OH), (32 percent) suspended in 550 cc of glycol and 10 cc of H 0 (ratio glycol/H O 5:1). 23 cc of acrylonitrile, 14 cc of pyridine and 50 mg of very fine nickel were added to the mixture. 29 g. of powders were obtained. The nickel granules thus obtained had an average diameter of 0.8 microns and a spheroidal shape. 83 percent of the granules had a diameter ranging from 0.68 to 0.92 micron.
  • EXAMPLE 2 143 g of Ni(Ol-D at 31.4% (equal to 45 g of dry Ni(OH and 98 cc H O) were suspended in 500 cc of ethylene glycol plus 152 cc of R 0 to obtain 750 cc of a mixture having a ratio glycol/H O 2/1. 21 cc of acrylonitrile, 9 cc of pyridine and 1.5 g of bisacrylonitrile-nickel were added thereto. Reduction, washing and drying were carried out as described in Example 1. 28 g of powders were obtained. Granules having an average diameter of 0. l 7 microns were obtained. 90 percent of the granules had a diameter ranging from 0.14 to 0.20 micron.
  • EXAMPLE 3 136 g of Ni(OH) at 33 percent (equal to 45 g of dry Ni(OH and 91 g of 11 0) were suspended in 240 cc of methanol and 389 cc of H 0 in order to have a ratio methanol/H O 1/2. 5.8 g of bisacrylonitrile-nickel, 15 cc of acrylonitrile, and 5 cc of pyridine were added thereto. Reduction, washing and drying were carried out as described in Example 1. g of powders were obtained. The average diameter of the granules was 0.09 microns and their shape was spheroidal. 85 percent of the granules had a diameter ranging from 0.07 to 0.11 micron.
  • EXAMPLE 4 40 g of Ni-actylacetonate were suspended in 720 cc of a mixture of glycol/H O having a ratio of 1:2. 1.2 g of bisacrylonitrile-nickel, 5 cc of acrylonitrile and 5 cc of pyridine were added thereto. Reduction, washing and drying were carried out as in Example 1. 9.1 g of powders were obtained. The average diameter of the granules was 0.1 microns and the shape was spheroidal.
  • a process for preparing finely divided, homogeneous, metallic nickel powder with a very narrow granulometric spectrum having a spheroidal form and with a granulometric range between 0.07 and 2 microns characterized in that a hydroalcoholic suspension of a nickel compound selected from the class consisting of the hydroxide, the formate and the acetylacetonate is treated with hydrogen at temperatures ranging from 160 to 250 C and at hydrogen partial pressures ranging from 25 to atm, in the presence of one or more additives selected from the class consisting of acrylonitrile, pyridine and complexes of zerovalent nickel.
  • hydroalcoholic component comprises a lower alcohol or a glycol.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Catalysts (AREA)
US00210608A 1970-12-24 1971-12-21 Process for preparing finely particled metallic nickel powder having a spheroidal form Expired - Lifetime US3748118A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
IT3353070 1970-12-24

Publications (1)

Publication Number Publication Date
US3748118A true US3748118A (en) 1973-07-24

Family

ID=11237761

Family Applications (1)

Application Number Title Priority Date Filing Date
US00210608A Expired - Lifetime US3748118A (en) 1970-12-24 1971-12-21 Process for preparing finely particled metallic nickel powder having a spheroidal form

Country Status (8)

Country Link
US (1) US3748118A (enrdf_load_stackoverflow)
JP (1) JPS5523881B1 (enrdf_load_stackoverflow)
BE (1) BE777278A (enrdf_load_stackoverflow)
CA (1) CA944158A (enrdf_load_stackoverflow)
DE (1) DE2163866C3 (enrdf_load_stackoverflow)
FR (1) FR2118996B1 (enrdf_load_stackoverflow)
GB (1) GB1321180A (enrdf_load_stackoverflow)
NL (1) NL7117454A (enrdf_load_stackoverflow)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3850612A (en) * 1972-09-25 1974-11-26 Montedison Spa Process for preparing finely particled nickel powders having a spheroidal form
US6316100B1 (en) 1997-02-24 2001-11-13 Superior Micropowders Llc Nickel powders, methods for producing powders and devices fabricated from same
US6406513B2 (en) * 2000-02-03 2002-06-18 Mitsui Mining And Smelting Co., Ltd. Nickel powder and conductive paste
US6454830B1 (en) * 1999-08-31 2002-09-24 Toho Titanium Co., Ltd. Nickel powder for multilayer ceramic capacitors
RU2233730C1 (ru) * 2003-02-20 2004-08-10 Институт химии твердого тела и механохимии СО РАН, НИУ Способ получения субмикронного порошка никеля
US20050097987A1 (en) * 1998-02-24 2005-05-12 Cabot Corporation Coated copper-containing powders, methods and apparatus for producing such powders, and copper-containing devices fabricated from same
US20050262966A1 (en) * 1997-02-24 2005-12-01 Chandler Clive D Nickel powders, methods for producing powders and devices fabricated from same
US20060090597A1 (en) * 2004-10-29 2006-05-04 Goia Dan V Polyol-based method for producing ultra-fine metal powders
US7083747B2 (en) 1997-02-24 2006-08-01 Cabot Corporation Aerosol method and apparatus, coated particulate products, and electronic devices made therefrom
DE102015006727A1 (de) 2015-05-30 2016-12-01 Rainer Pommersheim Verfahren und technischer Prozess zur Herstellung von Mikro- und Nanopartikeln unterschiedlicher Größe

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0456679A1 (en) * 1989-02-02 1991-11-21 Btg International Limited Forming a metal coating

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2651105A (en) * 1942-04-07 1953-09-08 Electro Chimie Metal Manufacture of permanent magnets
US2726151A (en) * 1949-07-12 1955-12-06 Schweiz Sprengstoff Fabrik A G Producing and reactivating a carrierless nickel catalyst
US2730441A (en) * 1953-02-02 1956-01-10 Republic Steel Corp Process of reducing iron formate
US2733142A (en) * 1956-01-31 Purification of nickel powder
US2807532A (en) * 1954-12-30 1957-09-24 Monsanto Chemicals Method of preparing nickel catalyst
US2827473A (en) * 1955-03-31 1958-03-18 Alan D Franklin Process for producing granular materials for magnets

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2733142A (en) * 1956-01-31 Purification of nickel powder
US2651105A (en) * 1942-04-07 1953-09-08 Electro Chimie Metal Manufacture of permanent magnets
US2726151A (en) * 1949-07-12 1955-12-06 Schweiz Sprengstoff Fabrik A G Producing and reactivating a carrierless nickel catalyst
US2730441A (en) * 1953-02-02 1956-01-10 Republic Steel Corp Process of reducing iron formate
US2807532A (en) * 1954-12-30 1957-09-24 Monsanto Chemicals Method of preparing nickel catalyst
US2827473A (en) * 1955-03-31 1958-03-18 Alan D Franklin Process for producing granular materials for magnets

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3850612A (en) * 1972-09-25 1974-11-26 Montedison Spa Process for preparing finely particled nickel powders having a spheroidal form
US7083747B2 (en) 1997-02-24 2006-08-01 Cabot Corporation Aerosol method and apparatus, coated particulate products, and electronic devices made therefrom
US6316100B1 (en) 1997-02-24 2001-11-13 Superior Micropowders Llc Nickel powders, methods for producing powders and devices fabricated from same
US7384447B2 (en) 1997-02-24 2008-06-10 Cabot Corporation Coated nickel-containing powders, methods and apparatus for producing such powders and devices fabricated from same
US7354471B2 (en) 1997-02-24 2008-04-08 Cabot Corporation Coated silver-containing particles, method and apparatus of manufacture, and silver-containing devices made therefrom
US7097686B2 (en) 1997-02-24 2006-08-29 Cabot Corporation Nickel powders, methods for producing powders and devices fabricated from same
US20040231758A1 (en) * 1997-02-24 2004-11-25 Hampden-Smith Mark J. Silver-containing particles, method and apparatus of manufacture, silver-containing devices made therefrom
US20050061107A1 (en) * 1997-02-24 2005-03-24 Hampden-Smith Mark J. Coated silver-containing particles, method and apparatus of manufacture, and silver-containing devices made therefrom
US20050097988A1 (en) * 1997-02-24 2005-05-12 Cabot Corporation Coated nickel-containing powders, methods and apparatus for producing such powders and devices fabricated from same
US20050262966A1 (en) * 1997-02-24 2005-12-01 Chandler Clive D Nickel powders, methods for producing powders and devices fabricated from same
US7004994B2 (en) 1997-02-24 2006-02-28 Cabot Corporation Method for making a film from silver-containing particles
US7087198B2 (en) 1997-02-24 2006-08-08 Cabot Corporation Aerosol method and apparatus, particulate products, and electronic devices made therefrom
US20050097987A1 (en) * 1998-02-24 2005-05-12 Cabot Corporation Coated copper-containing powders, methods and apparatus for producing such powders, and copper-containing devices fabricated from same
US6454830B1 (en) * 1999-08-31 2002-09-24 Toho Titanium Co., Ltd. Nickel powder for multilayer ceramic capacitors
US6406513B2 (en) * 2000-02-03 2002-06-18 Mitsui Mining And Smelting Co., Ltd. Nickel powder and conductive paste
RU2233730C1 (ru) * 2003-02-20 2004-08-10 Институт химии твердого тела и механохимии СО РАН, НИУ Способ получения субмикронного порошка никеля
US20060090597A1 (en) * 2004-10-29 2006-05-04 Goia Dan V Polyol-based method for producing ultra-fine metal powders
DE102015006727A1 (de) 2015-05-30 2016-12-01 Rainer Pommersheim Verfahren und technischer Prozess zur Herstellung von Mikro- und Nanopartikeln unterschiedlicher Größe
WO2016193087A1 (de) 2015-05-30 2016-12-08 Tuliport S.À.R.L. Verfahren und technischer prozess zur herstellung von mikro- und nanopartikeln unterschiedlicher grösse

Also Published As

Publication number Publication date
NL7117454A (enrdf_load_stackoverflow) 1972-06-27
DE2163866C3 (de) 1980-12-18
GB1321180A (en) 1973-06-20
FR2118996B1 (enrdf_load_stackoverflow) 1974-06-07
CA944158A (en) 1974-03-26
JPS5523881B1 (enrdf_load_stackoverflow) 1980-06-25
FR2118996A1 (enrdf_load_stackoverflow) 1972-08-04
DE2163866A1 (de) 1972-07-20
BE777278A (fr) 1972-06-26
DE2163866B2 (de) 1980-04-30

Similar Documents

Publication Publication Date Title
US3748118A (en) Process for preparing finely particled metallic nickel powder having a spheroidal form
US3850612A (en) Process for preparing finely particled nickel powders having a spheroidal form
CN101642818A (zh) 一种制备镍纳米颗粒的方法
CN104475126A (zh) 燃料电池用碳载核壳型铂钴-铂催化剂及其制备方法
CN113422073A (zh) 钴修饰的碳载超细铂纳米合金催化剂的制备方法
CN108213456B (zh) 一种立方体纳米铜粉的制备方法
US4089676A (en) Method for producing nickel metal powder
JPH10509213A (ja) ミクロンサイズのニッケル金属粉末およびその製造方法
KR20180133043A (ko) 은 입자 및 이의 제조방법
CN116351477A (zh) 一种除甲醛负载型Pt6团簇催化剂及其制备方法
CN117226089A (zh) 一种MOFs衍生高熵合金/碳复合吸波材料及其制备方法
JPS6155562B2 (enrdf_load_stackoverflow)
CN114011412B (zh) 一种氧化钴多孔纳米片及其制备方法与应用
CN115881980B (zh) 一种燃料电池用Pt合金电催化剂及共还原制备方法
US3711274A (en) Process for preparing finely particled nickel powder
CN107126960A (zh) 一种高分散负载型贵金属纳米粒子及其制备方法
CN113346094A (zh) 一种负载型高分散、小尺寸铂基有序合金电催化剂的宏量制备方法
US2699458A (en) Porous sintered metal bodies for a storage battery
US5925166A (en) Process for obtaining iron or iron-based powders by organic liquid phase precipitation
JPH11505884A (ja) コバルト金属集塊体、その製法及びその使用法
US3925114A (en) Process for preparation of magnetic alloy powder
CN117680155A (zh) 基于表面合金化的非贵金属催化剂及其制备方法与应用
CN117773096A (zh) 一种高纯度球形镍粉及其制备方法与用途
CN116899605A (zh) 一种Co@NCNTs催化剂的制备方法及其在酚类加氢中的应用
US2646457A (en) Electrode for alkaline batteries