EP0080641B1 - Procédé de fabrication de pièces en matériaux composés d'argent et d'oxyde métallique sans cadmium pour contacts électriques - Google Patents
Procédé de fabrication de pièces en matériaux composés d'argent et d'oxyde métallique sans cadmium pour contacts électriques Download PDFInfo
- Publication number
- EP0080641B1 EP0080641B1 EP82110530A EP82110530A EP0080641B1 EP 0080641 B1 EP0080641 B1 EP 0080641B1 EP 82110530 A EP82110530 A EP 82110530A EP 82110530 A EP82110530 A EP 82110530A EP 0080641 B1 EP0080641 B1 EP 0080641B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- powder
- sintering
- cadmium
- oxide
- metal oxide
- 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
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
- H01H1/02372—Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
Definitions
- the invention relates to a method for producing molded parts from cadmium-free silver-metal oxide composite materials with at least two metal oxide components for electrical contact pieces with a solderable or weldable second layer, in which pressure-atomized and then internally oxidized silver alloy powder (AgMe, Me? ) with Me, from zinc (Zn) or tin (Sn) in an amount of 12 to 25 vol .-% oxide and Me 2 from at least one of the metals bismuth (Bi), lead (Pb), copper (Cu), indium (In) in an amount of 0.1 to 2 vol .-% oxide pressed to form parts and these are compressed by sintering in air or a neutral atmosphere and by re-pressing.
- pressure-atomized and then internally oxidized silver alloy powder AgMe, Me?
- Me zinc
- Sn tin
- Me 2 from at least one of the metals bismuth (Bi), lead (Pb), copper (Cu), indium (In) in an amount of 0.1
- Molded parts made of silver-metal oxide composites are generally classified according to the manufacturing technologies: They can be manufactured using powder metallurgy, e.g. B. by sintering and extruding silver-metal oxide powder mixtures or by sintering and compacting such silver alloy powders, which are first subjected to an internal oxidation in a separate process step to produce an internally oxidized silver alloy powder (IOLP).
- powder metallurgy e.g. B. by sintering and extruding silver-metal oxide powder mixtures or by sintering and compacting such silver alloy powders, which are first subjected to an internal oxidation in a separate process step to produce an internally oxidized silver alloy powder (IOLP).
- the first method is described, for example, in EP-A-0 024 349, while the use of internally oxidized alloy powders for the production of the composite materials can be found especially in AT-B-331 529.
- an internal oxidation of the silver-metal alloys in compact form by solid-state diffusion of oxygen can also take place, which is described in detail in DE-A-2428 146 and also in DE-A-2 428 147.
- a blank of the alloy is forged and / or rolled into a metal sheet. transferred, which is then exposed to an oxygen atmosphere for longer periods.
- a silver alloy powder with at least one base metal of a coarse particle size class is converted into an IOLP by internal oxidation, which is then comminuted by grinding into a composite powder of finer particle size class, and then the further process steps for the production of molded part -Contact pieces is subjected.
- Cadmium is consistently used as the base metal due to the favorable sound properties, but according to today's assessment the cadmium oxide is to be rated as toxic.
- cadmium-free silver metal oxide contact materials cannot yet meet all the property requirements that larger contactors have to meet.
- Contact materials e.g. B. from AgSnO z in an extruded version z. B. parallel to the extrusion direction too high heating and disruptive material migration. While the excessive heating can be reduced by adding tungsten oxide (W0 3 ), the disruptive material migration still occurs with large contactors. Only one AgSn0 2 contact material, used perpendicular to the extrusion direction, showed no material migration; however, with this quality, the secure connection technology with the carrier has not yet been solved.
- the object of the invention is therefore to provide a method by which it is possible to produce cadmium oxide-free AgSnOr or AgZnO contact materials as molded parts with a solderable or weldable second layer.
- this object is achieved in that a) the pressure-atomized silver alloy powder is ground dry or wet in a mill in order to produce platelet-shaped particles from the round alloy powder particles, b) the internal oxidation is carried out in two stages, b1) in one first temperature range between 673 K and 773 K for 2 to 6 hours and b2) in a second temperature range between 873 K and 1 073 K for 0.5 to 2 hours, and c) in a temperature range between 973 K and 1 173.
- the degree of reshaping depends on the mill used, the grinding time and, in the case of wet grinding, also somewhat on the grinding liquid. Isopropanol has proven particularly suitable for wet grinding. The degree of deformation can be described microscopically by the change in the particle shape.
- the AgMe alloy powders used usually show a rounded shape after production before grinding.
- the mean diameter 12 of the roundish particle 11 before grinding is approximately half the diameter 22 corresponding to the thickness of the platelet-shaped part formed chens 21 reduced after grinding.
- the main criterion in the grinding process is the shaping, ie the change in the particle shape, during the grinding.
- the reduction in the average particle diameter is of minor importance.
- the fill and tap densities also change during the milling treatment.
- the desired reshaping of the powder particles was achieved with a ball mill in dry grinding and with an agitator ball mill in wet grinding.
- a melt of the composition 91.8% by mass of Ag, 6% by mass of Zn and 2.2% by mass of Bi was produced from the metals silver, zinc and bismuth.
- the homogenized alloy was ground in metal powder by pressure atomization with water.
- the AgZn-Bi alloy powder of particle size ⁇ 0.2 mm was milled under propanol in a stirred ball mill with steel balls for 15 minutes.
- the powder properties change as follows: bulk density from 3.33 g / cm 3 to 2.78 g / cm 3 and the tap density from 4.17 g / cm 3 to 3.85 g / cm 3 ; -The flow time in the 60 ° funnel with a 4 mm nozzle diameter changes from 20 s / 100 g to 27 s / 100 g.
- the particle shape has changed as a result of shaping in the manner shown schematically in FIGS. 1 and 2.
- the powder is dried.
- the internal oxidation was carried out by heating in air. First at 673 K for 2 hours and then at 873 K for 1 hour.
- the completeness of the internal oxidation of the alloy powder to the AgZnOBi 2 0 3 composite powder was determined by increasing the weight and the oxide particles which had separated out in the powder particles were assessed in cross section. Complete internal oxidation was achieved.
- the precipitates of the oxide particles are in part in the particle size range ⁇ 0.5 ⁇ m and in part in particle sizes 0.5-2 ⁇ m.
- the internally oxidized composite powder is mixed with 0.2% stearic acid ester as a pressure-relieving additive.
- the ready-to-press powder was pressed on an automatic press to give two-layer molded contact pieces with a contact layer of 2.4 mm and a silver layer of about 0.3 mm thickness with a pressure of 600 MPa.
- the size of the molded contact pieces was 15 x 16 x 2.5 mm 3 .
- the compacts were sintered at 1,023 K for 1 hour in air.
- the contact pieces were compacted by cold pressing at 800 MPa. During a second sintering at 1 123 K in air for 1 hour, the strength was further increased and the final shape of the contact pieces was obtained by a further cold pressing, the porosity being ⁇ 2%.
- the bending strength of the contact pieces was> 1 400 N.
- the structure of this contact material shows a clear orientation in the cross section, which is not present in the same production of the contact piece from unground powder. By increasing the sintering temperature and time, the degree of alignment can be reduced.
- the bending strength of a contact piece e.g. B. the size 15 x 16 x 2.5 mm 3 , this is placed on round rods of 4 mm diameter, which are set at a distance of 12 mm, and loaded in the middle with a bending punch with a radius of 2 mm until it breaks.
- the silver layer is on the pressure side.
- the sintering conditions are chosen so that a minimum breaking strength is achieved.
- the bending strength can be increased by increasing the sintering temperature and extending the sintering time.
- the contact properties of the material were measured on a test switch under conditions as described in «Zf Maschinenstofftechnik / J. of Materials Technology 7, 381 to 389 (1976) on page 382 in the right column of Table 1.
- the burnup value of 20 mm 3 is about 30% cheaper than that of the contact material of the same composition made from unground powder.
- Example 1 An AgSnBiCu alloy was processed into alloy powder in the same manner as described in Example 1. After wet grinding as in Example 1, the internal oxidation was carried out at 673 K for 6 hours and then at 873 K for 2 hours in air, a composite powder of the composition AgSnO 2 8.76 Bi 2 O 3 3.57 CuO 0.98 was obtained. The production data as given in Example 1 could also be used here.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Switches (AREA)
- Contacts (AREA)
Claims (3)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3146972 | 1981-11-26 | ||
DE19813146972 DE3146972A1 (de) | 1981-11-26 | 1981-11-26 | Verfahren zum herstellen von formteilen aus cadmiumfreien silber-metalloxid-verbundwerkstoffen fuer elektrische kontaktstuecke |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0080641A1 EP0080641A1 (fr) | 1983-06-08 |
EP0080641B1 true EP0080641B1 (fr) | 1985-08-28 |
Family
ID=6147294
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP82110530A Expired EP0080641B1 (fr) | 1981-11-26 | 1982-11-15 | Procédé de fabrication de pièces en matériaux composés d'argent et d'oxyde métallique sans cadmium pour contacts électriques |
Country Status (5)
Country | Link |
---|---|
US (1) | US4609525A (fr) |
EP (1) | EP0080641B1 (fr) |
JP (1) | JPS5896801A (fr) |
BR (1) | BR8206819A (fr) |
DE (2) | DE3146972A1 (fr) |
Families Citing this family (22)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3304637A1 (de) * | 1983-02-10 | 1984-08-16 | Siemens AG, 1000 Berlin und 8000 München | Sinterkontaktwerkstoff fuer niederspannungsschaltgeraete |
EP0152606B1 (fr) * | 1984-01-30 | 1987-09-09 | Siemens Aktiengesellschaft | Matériau de contact et procédé de préparation de pièces de contact |
DE3405218A1 (de) * | 1984-02-14 | 1985-09-05 | Siemens AG, 1000 Berlin und 8000 München | Sinterkontaktwerkstoff und verfahren zu dessen herstellung |
US4680162A (en) * | 1984-12-11 | 1987-07-14 | Chugai Denki Kogyo K.K. | Method for preparing Ag-SnO system alloy electrical contact material |
JPS63425A (ja) * | 1986-06-20 | 1988-01-05 | Tanaka Kikinzoku Kogyo Kk | 電気接点材料の製造方法 |
JPH06104873B2 (ja) * | 1986-07-08 | 1994-12-21 | 富士電機株式会社 | 銀―金属酸化物系接点用材料及びその製造方法 |
DE3909384A1 (de) * | 1988-03-26 | 1989-10-19 | Duerrwaechter E Dr Doduco | Halbzeug fuer elektrische kontakte aus einem verbundwerkstoff auf silber-zinnoxid-basis und pulvermetallurgisches verfahren zu seiner herstellung |
US5134039A (en) * | 1988-04-11 | 1992-07-28 | Leach & Garner Company | Metal articles having a plurality of ultrafine particles dispersed therein |
EP0369283B1 (fr) * | 1988-11-17 | 1994-09-14 | Siemens Aktiengesellschaft | Matériau de contact fritté pour appareillages interrupteurs à basse tension de la technique de l'énergie, spécialement pour des contacteurs |
DE4142374A1 (de) * | 1991-12-20 | 1993-06-24 | Siemens Ag | Verfahren zum vorbeloten von kontaktstuecken fuer elektrische schaltgeraete |
US5296189A (en) * | 1992-04-28 | 1994-03-22 | International Business Machines Corporation | Method for producing metal powder with a uniform distribution of dispersants, method of uses thereof and structures fabricated therewith |
ES2091633T5 (es) * | 1992-09-16 | 2003-09-01 | Ami Doduco Gmbh | Material para contactos electricos a base de plata-oxido de estaño o de plata-oxido zinc y procedimiento para su fabricacion. |
US5292477A (en) * | 1992-10-22 | 1994-03-08 | International Business Machines Corporation | Supersaturation method for producing metal powder with a uniform distribution of dispersants method of uses thereof and structures fabricated therewith |
DE4344322A1 (de) * | 1993-12-23 | 1995-06-29 | Siemens Ag | Sinterkontaktwerkstoff |
DE19503182C1 (de) * | 1995-02-01 | 1996-05-15 | Degussa | Sinterwerkstoff auf der Basis Silber-Zinnoxid für elektrische Kontakte und Verfahren zu dessen Herstellung |
TW517095B (en) * | 1999-04-23 | 2003-01-11 | Tanaka Precious Metal Ind Co L | Method for producing Ag-ZnO electric contact material and electric contact material produced thereby |
WO2003009323A1 (fr) * | 2001-07-18 | 2003-01-30 | Nec Schott Components Corporation | Fusible thermique |
WO2011023584A2 (fr) | 2009-08-27 | 2011-03-03 | Polymers Crc Ltd. | Composition d'oxyde de zinc-argent de taille nanométrique |
CN102074278B (zh) * | 2010-12-09 | 2011-12-28 | 温州宏丰电工合金股份有限公司 | 颗粒定向排列增强银基电触头材料的制备方法 |
CN102142325B (zh) * | 2010-12-30 | 2013-04-03 | 温州宏丰电工合金股份有限公司 | 颗粒定向排列增强银基氧化物电触头材料及其制备方法 |
US9028586B2 (en) * | 2011-12-29 | 2015-05-12 | Umicore | Oxidation method |
CN117107100B (zh) * | 2023-08-28 | 2024-01-30 | 昆明理工大学 | 一种核壳结构金属氧化物增强银基材料的方法 |
Family Cites Families (33)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2425053A (en) * | 1944-06-23 | 1947-08-05 | Cutler Hammer Inc | Silver-backed nonwelding contact and method of making the same |
DE1303549B (de) * | 1965-06-30 | 1972-03-23 | Siemens Ag | Verfahren zum Herstellen eines Sinter Verbundstoffes fur hochbelastbare elektri sehe Kontakte |
US3578443A (en) * | 1969-01-21 | 1971-05-11 | Massachusetts Inst Technology | Method of producing oxide-dispersion-strengthened alloys |
US3649242A (en) * | 1969-11-26 | 1972-03-14 | Nasa | Method for producing dispersion-strengthened alloys by converting metal to a halide, comminuting, reducing the metal halide to the metal and sintering |
CA909036A (en) * | 1970-01-27 | 1972-09-05 | A. W. Fustukian David | Metal dispersoid powder compositions |
US3709667A (en) * | 1971-01-19 | 1973-01-09 | Johnson Matthey Co Ltd | Dispersion strengthening of platinum group metals and alloys |
GB1397319A (en) * | 1972-08-25 | 1975-06-11 | Square D Co | Electrically conductive materials |
CH588152A5 (fr) * | 1972-12-11 | 1977-05-31 | Siemens Ag | |
US3859087A (en) * | 1973-02-01 | 1975-01-07 | Gte Sylvania Inc | Manufacture of electrical contact materials |
US3874941A (en) * | 1973-03-22 | 1975-04-01 | Chugai Electric Ind Co Ltd | Silver-metal oxide contact materials |
US3933485A (en) * | 1973-07-20 | 1976-01-20 | Chugai Denki Kogyo Kabushiki-Kaisha | Electrical contact material |
US3933486A (en) * | 1974-02-12 | 1976-01-20 | Chugai Denki Kogyo Kabushiki-Kaisha | Silver-metal oxide composite and method of manufacturing the same |
GB1444199A (en) * | 1974-06-14 | 1976-07-28 | Square D Co | Method of producing a silver cadmium oxide electrically conductive composite material |
US3976482A (en) * | 1975-01-31 | 1976-08-24 | The International Nickel Company, Inc. | Method of making prealloyed thermoplastic powder and consolidated article |
JPS523193A (en) * | 1975-06-24 | 1977-01-11 | Sumitomo Electric Ind Ltd | Electric contact material |
JPS5351128A (en) * | 1976-10-21 | 1978-05-10 | Nat Res Inst Metals | Electric contact materials |
US4141727A (en) * | 1976-12-03 | 1979-02-27 | Matsushita Electric Industrial Co., Ltd. | Electrical contact material and method of making the same |
JPS6018734B2 (ja) * | 1977-04-14 | 1985-05-11 | 松下電器産業株式会社 | 電気接点材料 |
JPS6018735B2 (ja) * | 1977-12-15 | 1985-05-11 | 松下電器産業株式会社 | 電気接点材料 |
US4150982A (en) * | 1978-03-13 | 1979-04-24 | Chugai Denki Kogyo Kabushiki-Kaisha | AG-Metal oxides electrical contact materials containing internally oxidized indium oxides and/or tin oxides |
US4161403A (en) * | 1978-03-22 | 1979-07-17 | Chugai Denki Kogyo Kabushiki-Kaisha | Composite electrical contact material of Ag-alloy matrix and internally oxidized dispersed phase |
DE2824117A1 (de) * | 1978-06-01 | 1979-12-06 | Siemens Ag | Verfahren zum herstellen eines anisotropen sinterverbundwerkstoffes mit richtgefuege |
JPS6013051B2 (ja) * | 1978-08-11 | 1985-04-04 | 中外電気工業株式会社 | 銀↓−錫↓−ビスマス系合金を内部酸化した電気接点材料の改良 |
JPS5543775A (en) * | 1978-09-21 | 1980-03-27 | Sumitomo Electric Industries | Electric contact material and method of fabricating same |
US4243413A (en) * | 1979-02-26 | 1981-01-06 | Chugai Denki Kogyo Kabushiki-Kaisha | Integrated Ag-SnO alloy electrical contact materials |
US4274873A (en) * | 1979-04-09 | 1981-06-23 | Scm Corporation | Dispersion strengthened metals |
DE2933338C3 (de) * | 1979-08-17 | 1983-04-28 | Degussa Ag, 6000 Frankfurt | Werkstoff für elektrische Kontakte und Verfahren zu seiner Herstellung |
JPS5687641A (en) * | 1979-12-19 | 1981-07-16 | Fuji Electric Co Ltd | Manufacture of silver-tin oxide electrical contact |
JPS5690941A (en) * | 1979-12-25 | 1981-07-23 | Tanaka Kikinzoku Kogyo Kk | Composite electrical contact material |
JPS5690940A (en) * | 1979-12-25 | 1981-07-23 | Tanaka Kikinzoku Kogyo Kk | Composite electrical contact material |
JPS56102536A (en) * | 1980-01-18 | 1981-08-17 | Tanaka Kikinzoku Kogyo Kk | Composite electrical contact material |
DE3017424A1 (de) * | 1980-05-07 | 1981-11-12 | Degussa Ag, 6000 Frankfurt | Werkstoff fuer elektrische kontakte |
DE3204794A1 (de) * | 1981-02-12 | 1982-09-16 | Chugai Denki Kogyo K.K., Tokyo | Innen oxidierte silber-zinn-wismut-verbindung fuer elektrische kontaktmaterialien |
-
1981
- 1981-11-26 DE DE19813146972 patent/DE3146972A1/de not_active Withdrawn
-
1982
- 1982-11-15 DE DE8282110530T patent/DE3265890D1/de not_active Expired
- 1982-11-15 EP EP82110530A patent/EP0080641B1/fr not_active Expired
- 1982-11-25 JP JP57206830A patent/JPS5896801A/ja active Granted
- 1982-11-25 BR BR8206819A patent/BR8206819A/pt unknown
-
1985
- 1985-11-15 US US06/799,183 patent/US4609525A/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JPS646259B2 (fr) | 1989-02-02 |
DE3146972A1 (de) | 1983-06-01 |
DE3265890D1 (en) | 1985-10-03 |
EP0080641A1 (fr) | 1983-06-08 |
US4609525A (en) | 1986-09-02 |
BR8206819A (pt) | 1983-10-04 |
JPS5896801A (ja) | 1983-06-09 |
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