CN1587426A - Process for preparing gold-germanium, gold-germanium-antimony alloy material - Google Patents
Process for preparing gold-germanium, gold-germanium-antimony alloy material Download PDFInfo
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- CN1587426A CN1587426A CN 200410070605 CN200410070605A CN1587426A CN 1587426 A CN1587426 A CN 1587426A CN 200410070605 CN200410070605 CN 200410070605 CN 200410070605 A CN200410070605 A CN 200410070605A CN 1587426 A CN1587426 A CN 1587426A
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Abstract
The present invention relates to the preparation process Ag-Ge and Ag-Ge-Sb alloy material, and especially the preparation process Ag-Ge and Ag-Ge-Sb alloy material under the protective argon. The alloy components are determined, and during the preparation, argon pressure is 0.01-0.1 MPa and argon flow rate is 3.0-8.0 L/min. A two-stage smelting mode is adopted, and the present invention has the features of being simple, convenient and favorable to mass production.
Description
Technical field
The present invention relates to the preparation method of gold-germanium, gold-germanium-antimony alloy material, specifically relate to a kind of new gold-germanium, the preparation method of gold-germanium-antimony alloy material, this product belongs to the precious metal material field.Product can be widely used in instrument, instrument, electronic temperature measurement, vacuum plating, accurate contact, electronic devices and components, semi-conductor, semiconductor integrated circuit etc.
Background technology
The preparation method of existing gold-germanium, gold-germanium-antimony alloy material, adopt the conventional vacuum melting method, owing in fusion process, constantly vacuumize, the elements germanium of adding, the metal vapors of antimony constantly are drawn out of, finally cause gold-germanium, the imbalance of gold-germanium-antimony alloy material alloy ratio.Product rejection when serious.This has become a technical barrier of gold-germanium, gold-germanium-antimony alloy material preparation.
Along with science and technology development, also more and more higher to the requirement of various instruments, instrument, communications facility, military equipment.The application of gold on various accurate self-reacting devices also more and more occupies critical positions.
Be extensive use of the coiling with pulse modified line displacement and angular travel on industrial measurement and the operating device, potentiometer occupies critical positions, and the current potential quality is the determinative of Measurement and Control System operating accuracy.For this reason, often require the long term operation under the differing temps of various industrial atmospheres of this equipment.This is to adopt the reason of au-alloy as the precision potentiometer critical material.
Some part material of the precision potentiometer of using in measuring technology has very high ratio resistance, and little of the temperature coefficient of resistance that approaches zero, so that resistance is constant (difficulty of maintenance constant is very big) when work.Measure temperature and often adopt thermopair and resistance thermometer.Thermopair is made up of the wire of two kinds of different components, because the temperature head between the cold junction of measurement point causes the thermoelectric force that can measure with millivoltmeter, temperature is measured in the variation that is based on the thermoelectric force of temperature, and it is very strict therefore the thermostability of material being required.Gold-germanium alloy, gold-germanium-antimony alloy, decapacitation are satisfied outside the above-mentioned requirements, have reached level preferably at everyways such as the mechanical property of processing, thermostabilitys.
In modern communication system, Controlling System and computery, though its compact construction, device miniatureization, the possibility that still should guarantee to carry out necessary inspection.Taking individual part and element demountable structure in this respect, is rational technically.To reliability and the higher requirement of proposition in work-ing life, the necessity and the importance of research novel contact is proposed naturally.Because arrangement of parts is compact and the margin of energy of unit volume increases, in communication system, improve the validity of system, when the development contact material, must consider some factors relevant with surrounding environment, as good electric conductivity, stable resistance and good solidity to corrosion, workability, thermostability etc.Because the alloy of gold has above-mentioned advantageous property, be widely used in electricity in the making of industrial contact.In secular use,, also can guarantee when faint current conversion and very little contact pressure, to have good contact reliability even in changeable environment.
Au-alloy is used in the kind of electric contact material and also is being on the increase.Be multiple layer as rivet type composite electric contact material (according to GB11096-89) with precious metal and alloy, copper is the bimetal composite contact that basic material is made; At low-voltage apparatus, be used as the switch of small-sized load in the products such as instrument, the electrical contact of rly. etc.; The signal equipment contact material " according to Japanese JISC2509-1965]; Gold and silver nickelalloy contact material (according to U.S. ASTM B477-92) is as the slip electrical contact, and kind has thin plate, band, bar and silk material; Palau material (according to U.S. A5YMB540-91) comprises band, bar and silk material; Au-alloy contact material (pasting the 41-sun according to U.S. AsTN) generally is made into band, bar and silk material.
Because platability, high-ductility and the good processing properties of au-alloy, can adopt methods such as compacting, plating, cladding, galvanic deposit to make various dissimilar, different purposes electrical contacts, as can make communication equipment contact, slide contact of gold-platinum, gold-germanium, gold-germanium-antimony; With the telephone relay contact that gold-germanium is made, wear-resisting and can guarantee the transmission of signal: as to make high strength, anti-corrosion electric contact with gold-germanium;
Gold-germanium, gold-germanium-antimony alloy material etc. are used as conductor material and are widely used in electronics, semi-conductor equipment and the microcircuit and do conductor material.Making as semiconductor integrated circuit.Make unicircuit early stage the processing procedure wafer production be unable to do without gold-germanium, gold-germanium-antimony alloy material.This class alloy material is evaporated to above 6 cun-12 cun semi-conductors circle crystalline substances by vacuum coating technology, not only improved wafer oxidation-resistance, but also increase its heat-sinking capability.The semi-conductor circle is brilliant just can make semiconductor integrated circuit through operations such as (plated thickness is not less than 1 micron), the chip of packing into, bonding wire, encapsulation behind vacuum metallizing-germanium or the gold-germanium-antimony alloy material.Therefore gold-germanium, gold-germanium-antimony alloy are indispensable process materials on production of integrated circuits.
Gold-germanium, gold-germanium-antimony alloy material have the character of many preciousnesses when being used as the auri scolder, the development of new texture material development work such as the jet engine of using along with electronic industry, vacuum technique, atomic energy apparatus, aircraft and rocket, aerospace device, the range of application of gold-germanium, gold-germanium-antimony alloy material auri scolder becomes more broad.
It mainly is intensity, thermotolerance, solidity to corrosion, sputter and the processing performance of wet performance, welding that the character of the auri scolder that gold-germanium, gold-germanium-antimony alloy material are made requires.Be used to weld waveguide, unicircuit, semiconductor electronic pipe, wireless apparatus, vacuum instrumentation.Gold-germanium, gold-germanium-antimony alloy material congruent melting type alloy flowability are good, and the ability of filling small gap is strong, and metals such as copper, iron, nickel, aluminium, manganese, tungsten and alloy are all had good wetting property.With the low-keyed mutual chemical action of welding metal, do not destroy the size of weld seam, do not cause the weldment strength degradation.When welding vacuum weld seam, gold-copper brazing alloy any problem can not occur under subatmospheric.In electronic industry under a lot of situations, use during the soldering component congruent melting or near gold-germanium, the gold-germanium-antimony alloy material scolder of congruent melting, has blocky weld seam and creep resisting stability, chromatize has oxidation-resistance, be widely used in aviation and the rocketry, at high temperature require to have high-intensity welding.
In the semiconductor integrated circuit assembling, extensively adopt gold-germanium, gold-germanium-antimony alloy material auri scolder to do soldering.In order to improve the heat conduction of semi-conductor instrument, it is installed on the metal base plate.Because semiconductor material has the conductivity of consolidated form (n type P type), then scolder also must have the conductivity of same form, and the welding with p type is to adopt gold-element Ge preparation.Scolder with n type then adopts VA family element to prepare, as gold-arsenic, gold-germanium-antimony etc.Also adopt conductive scolder with meltable eutectic.Auri scolder with specific conductivity has good electrical contact between semi-conductor, and low melting point has guaranteed its processing performance in brazing process.
Because existing technology can't security deposit-germanium, the high precision of gold-germanium-antimony alloy material product ratio, therefore is restricted in many precise electronic product manufacture crafts.Therefore, provide the gold-germanium of high degree of accuracy, gold-germanium-antimony alloy material process for producing very urgent.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, and provide a kind of high degree of accuracy to prepare easy, effective gold-germanium, the preparation method of gold-germanium-antimony alloy material.
The object of the invention can realize that preparation gold-germanium, gold-germanium-antimony alloy material are that two steps of branch are carried out in the following order by following measure fork-like farm tool used in ancient China:
The first step: batching
Getting Gold Content is: high-purity bronze of 99.999% according to germanium, the following weight ratio alloyage material of antimony: 1, gold: the germanium weight ratio is: Au88.000 gram: Ge12.000 gram-Au93.000 gram: Ge7.000 gram 2, gold: germanium: the antimony weight ratio is: the Au88.000 gram: the Ge11.98 gram: Sb0.120 restrains
Au93.000 gram: Ge6.900 gram: Sb0.100 gram
Take by weighing germanium, antimony material earlier and put into that (German Indutherm production model is: CC-400) high-temperature electric resistance furnace adds the High Purity Gold powder material then with its surface coverage.Seal, cover tight electric stove hearth.
Second step: melting
With 0.01-0.1Mpa pressure, it is 99.99% high-purity argon gas that the flow that per minute 3.0-8.0 rises charges into content, drives net air 10-20 minute with argon gas in stove.Little by little heat up then, the fs is warming up to 700 and kept 5 minutes when spending.
Stop inflation, close the air intake valve and the valve of giving vent to anger, keep furnace chamber to contain argon gas, subordinate phase news speed is warming up to 1250 and keeps 10 minutes time of fusion when spending, and this moment, gold-germanium, gold-germanium-antimony alloy material fusion were finished.Close furnace power, open inflation and give vent to anger valve still according to above-mentioned argon gas gas-filled protective condition continue inflation cold really to the stove temperature be 700 degree.Mode ingot casting to cast down continuously obtains gold-germanium, gold-germanium-antimony alloy material.
Product of the present invention is that gold-germanium, the gold-germanium-antimony alloy material physico-chemical property of Dark grey is as follows:
1, chemical molecular formula: Au-Ge, Au-Ge-Sb
2, Gold Content: 88.000%-93.000%
3, color: Dark grey
4, state: metal alloy
5, density: 16.81-18.53 gram/cubic centimetre
6, fusing point: 390 ℃-450 ℃
The present invention has following advantage compared to existing technology: technological process of the present invention is simple, flow process is reasonable, product precision height, and cost is low, and the user is easy to use, helps the characteristics of suitability for industrialized production.The present invention adopts the preparation method of one group of gold-germanium, gold-germanium-antimony alloy material.Having obtained can be for highly dense precision gold-germanium, the gold-germanium-antimony alloy material of industrial utilization.
Embodiment
Enumerate two embodiment below, the present invention is further specified, but the invention is not restricted to these embodiment.
Major equipment of the present invention
1, CC-400 electric furnace: German Indutherm produces
2, electronic balance: German Sa Duoli scholar produces
Embodiment 1
The first step: batching
Take by weighing monocrystalline germanium 120 gram put into (German Indutherm production model is: CC400) high-temperature electric resistance furnace, add high-purity bronze 880.00 grams of 99.999%, add the High Purity Gold powder material then with its surface coverage.Seal, cover tight electric stove hearth.
Second step: melting
With 0.03Mpa pressure, it is 99.99% high-purity argon gas that the flow that per minute is 5.0 liters charges into content in stove, drives net air 15 minutes with argon gas.Little by little heat up then, the fs is warming up to 700 and kept 5 minutes when spending.
Stop inflation, close the air intake valve and the valve of giving vent to anger, keep furnace chamber to contain argon gas, subordinate phase news speed is warming up to 1250 and keeps 10 minutes time of fusion when spending, and this moment, gold-germanium, gold-germanium-antimony alloy material fusion were finished.Close furnace power, open inflation and give vent to anger valve still according to above-mentioned argon gas gas-filled protective condition continue inflation cold really to the stove temperature be 700 degree.With the mode ingot casting of casting down continuously, obtain High Purity Gold-Ge alloy material 1000 grams.Contain gold: 88.00%, germanic: 12.00%.
Embodiment 2
The first step: batching
Take by weighing monocrystalline germanium 70 gram put into (German Indutherm production model is: CC-400) high-temperature electric resistance furnace, add high-purity bronze 930.00 grams of 99.999%, add the High Purity Gold powder material then with its surface coverage.Seal, cover tight electric stove hearth.
Second step: melting
With 0.08Mpa pressure, it is 99.99% high-purity argon gas that the flow that per minute is 8.0 liters charges into content in stove, drives net air 20 minutes with argon gas.Little by little heat up then, the fs is warming up to 700 and kept 5 minutes when spending.
Stop inflation, close the air intake valve and the valve of giving vent to anger, keep furnace chamber to contain argon gas, subordinate phase news speed is warming up to 1250 and keeps 10 minutes time of fusion when spending, and the fusion of gold-Ge alloy material this moment is finished.Close furnace power then, open the inflation and the valve of giving vent to anger, still continue inflation according to above-mentioned argon gas gas-filled protective condition.Cold really to the stove temperature be 700 degree.With the mode ingot casting of casting down continuously, obtain High Purity Gold-Ge alloy material 1000 grams.Contain gold: 93.00%, germanic: 7.00%.
Embodiment 3
The first step: batching
Take by weighing monocrystalline germanium 119.800 gram, high purity antimony 1.200 grams put into (German Indutherm production model is: CC-400) high-temperature electric resistance furnace, add high-purity bronze 880.00 grams of 99.999%, add the High Purity Gold powder material then with its surface coverage.Seal, cover tight electric stove hearth.
Second step: melting
With 0.03Mpa pressure, it is 99.99% high-purity argon gas that the flow that per minute is 5.0 liters charges into content in stove, drives net air 15 minutes with argon gas.Little by little heat up then, the fs is warming up to 700 and kept 5 minutes when spending.
Stop inflation, close the air intake valve and the valve of giving vent to anger, keep furnace chamber to contain argon gas, subordinate phase news speed is warming up to 1250 and keeps 10 minutes time of fusion when spending, and the fusion of gold-germanium-antimony alloy material this moment is finished.Close furnace power, open inflation and give vent to anger valve still according to above-mentioned argon gas gas-filled protective condition continue inflation cold really to the stove temperature be 700 degree.With the mode ingot casting of casting down continuously, obtain High Purity Gold-Ge alloy material 1000 grams.Contain gold: 88.00%, germanic: 11.98%, contain antimony: 0.120%.
Embodiment 4
The first step: batching
Take by weighing monocrystalline germanium 119.800 gram, high purity antimony 1.200 grams put into (German Indutherm production model is: CC-400) high-temperature electric resistance furnace, add high-purity bronze 880.00 grams of 99.999%, add the High Purity Gold powder material then with its surface coverage.Seal, cover tight electric stove hearth.
Second step: melting
With 0.08Mpa pressure, it is 99.99% high-purity argon gas that the flow that per minute is 8.0 liters charges into content in stove, drives net air 20 minutes with argon gas.Little by little heat up then, the fs is warming up to 700 and kept 5 minutes when spending.
Stop inflation, close the air intake valve and the valve of giving vent to anger, keep furnace chamber to contain argon gas, subordinate phase news speed is warming up to 1250 and keeps 10 minutes time of fusion when spending, and the fusion of gold-germanium-antimony alloy material this moment is finished.Close furnace power, open inflation and give vent to anger valve still according to above-mentioned argon gas gas-filled protective condition continue inflation cold really to the stove temperature be 700 degree.With the mode ingot casting of casting down continuously, obtain High Purity Gold-Ge alloy material 1000 grams.Contain gold: 88.00%, germanic: 11.98%, contain antimony: 0.120%.
Claims (4)
1, the preparation method of a kind of gold-germanium, gold-germanium-antimony alloy material; That concrete is the preparation method of gold-germanium, gold-germanium-antimony alloy material under the rare gas element argon shield.
2, according to the method for claim 1, the condition that feeds argon gas is:
1) pressure: 0.01-0.1Mpa
2) flow: per minute 3.0-8.0 liter.
3, according to the method for claim 1, the material weight that participates in the preparation alloy is such as following:
Gold: the germanium weight ratio is:
1) Au88.000 gram: Ge12.000 gram----Au93.000 gram: Ge7.000 restrains gold: germanium: the antimony weight ratio is:
2) Au88.000 gram: Ge11.98 gram: Sb0.120 gram----Au93.000 gram: Ge6.900 gram: Sb0.100 gram
4, according to the method for claim 1, fusion process fs that time-division in two stages carry out of heating up is that 700 degree, subordinate phase are 1250 degree.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100706054A CN100427624C (en) | 2004-07-23 | 2004-07-23 | Process for preparing gold-germanium, gold-germanium-antimony alloy material |
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| CNB2004100706054A CN100427624C (en) | 2004-07-23 | 2004-07-23 | Process for preparing gold-germanium, gold-germanium-antimony alloy material |
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| CN1587426A true CN1587426A (en) | 2005-03-02 |
| CN100427624C CN100427624C (en) | 2008-10-22 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251147A (en) * | 2011-07-21 | 2011-11-23 | 云南天浩稀贵金属股份有限公司 | Germanium ornament alloy |
| CN104561639A (en) * | 2014-12-26 | 2015-04-29 | 北京有色金属与稀土应用研究所 | Gold alloy target and preparation method thereof |
| CN105132873A (en) * | 2015-09-08 | 2015-12-09 | 有研亿金新材料有限公司 | Au-Sn alloy sputtering target material and preparation method thereof |
| CN106119589A (en) * | 2015-04-09 | 2016-11-16 | 韩国电子通信研究院 | For the precious metal material of 3 D-printing, its preparation method and the 3 D-printing method using it |
| CN106636721A (en) * | 2015-10-30 | 2017-05-10 | 深圳市周大福珠宝制造有限公司 | Gold alloy |
| CN107151748A (en) * | 2016-03-02 | 2017-09-12 | 广州先艺电子科技有限公司 | A kind of method of smelting of gold-germanium alloy solder |
| CN109207752A (en) * | 2018-09-26 | 2019-01-15 | 云南大学 | A kind of AuGe Modeling on Solidificated Structure of Eutectic Alloys regulation method and the alloy material |
| US10612112B2 (en) | 2015-04-09 | 2020-04-07 | Electronics And Telecommunications Research Institute | Noble metal material for 3-dimensional printing, method for manufacturing the same, and method for 3-dimensional printing using the same |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3317434B2 (en) * | 1995-12-01 | 2002-08-26 | 住友金属鉱山株式会社 | Gold alloy and method for producing the same |
-
2004
- 2004-07-23 CN CNB2004100706054A patent/CN100427624C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251147A (en) * | 2011-07-21 | 2011-11-23 | 云南天浩稀贵金属股份有限公司 | Germanium ornament alloy |
| CN104561639A (en) * | 2014-12-26 | 2015-04-29 | 北京有色金属与稀土应用研究所 | Gold alloy target and preparation method thereof |
| CN104561639B (en) * | 2014-12-26 | 2017-01-18 | 北京有色金属与稀土应用研究所 | Gold alloy target and preparation method thereof |
| CN106119589A (en) * | 2015-04-09 | 2016-11-16 | 韩国电子通信研究院 | For the precious metal material of 3 D-printing, its preparation method and the 3 D-printing method using it |
| US10612112B2 (en) | 2015-04-09 | 2020-04-07 | Electronics And Telecommunications Research Institute | Noble metal material for 3-dimensional printing, method for manufacturing the same, and method for 3-dimensional printing using the same |
| CN105132873A (en) * | 2015-09-08 | 2015-12-09 | 有研亿金新材料有限公司 | Au-Sn alloy sputtering target material and preparation method thereof |
| CN105132873B (en) * | 2015-09-08 | 2018-04-10 | 有研亿金新材料有限公司 | Gold-germanium alloy sputtering target material and preparation method thereof |
| CN106636721A (en) * | 2015-10-30 | 2017-05-10 | 深圳市周大福珠宝制造有限公司 | Gold alloy |
| CN107151748A (en) * | 2016-03-02 | 2017-09-12 | 广州先艺电子科技有限公司 | A kind of method of smelting of gold-germanium alloy solder |
| CN107151748B (en) * | 2016-03-02 | 2019-08-06 | 广州先艺电子科技有限公司 | A kind of method of smelting of gold-germanium alloy solder |
| CN109207752A (en) * | 2018-09-26 | 2019-01-15 | 云南大学 | A kind of AuGe Modeling on Solidificated Structure of Eutectic Alloys regulation method and the alloy material |
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| Publication number | Publication date |
|---|---|
| CN100427624C (en) | 2008-10-22 |
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