CN109175784A - A kind of novel oxidation-resistant quaternary alloy solder - Google Patents
A kind of novel oxidation-resistant quaternary alloy solder Download PDFInfo
- Publication number
- CN109175784A CN109175784A CN201811285346.5A CN201811285346A CN109175784A CN 109175784 A CN109175784 A CN 109175784A CN 201811285346 A CN201811285346 A CN 201811285346A CN 109175784 A CN109175784 A CN 109175784A
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- Prior art keywords
- solder
- temperature
- alloy
- novel oxidation
- quaternary alloy
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0233—Sheets, foils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a kind of novel oxidation-resistant quaternary alloy solder, the solder is made of the element of following weight percent: Ag 45~50%, Cu 48.6~52.2%, Ge 1~2%, Si 0.4~0.8%.Oxidation resistant low-silver solder alloy processability of the present invention is good, and solder wetting is good, and sealing-in strength of joint is high, and antioxygenic property is good；Alternative now widely used Ag72Cu28 solder, the sealing-in especially suitable for ceramics and metal in electron tube.
Description
Technical field
The invention belongs to welding fields, are related to a kind of silver-base solder that silver content is low, ceramic suitable for electron tube
With the sealing-in of metal.
Background technique
Silver-base solder properties are excellent (such as mechanical property, electric conductivity, corrosion resistance, connector air-tightness), wide
It is general to be used as vacuum seal solder.Ag72Cu28 alloy has eutectic alloy institutional framework, and eutectic melting point is 779 DEG C, sealing temperature
About 830 DEG C, to the wetability and good fluidity of metal and ceramics, the shapes such as in blocks, silk are easily worked, are free of Volatile Elements,
Meet the requirement of electron tube.However, the silver content of Ag72Cu28 solder is up to 72%, have the following problems: first is that silver dollar
Element belongs to precious metal element, and price is higher, and the solder of high silver content considerably increases the cost of solder；Second is that silver element belongs to ground
Shell rare metal, excessive exploitation lead to the waste of resource.Therefore, in craftsmanship, processability and the sealing-in for guaranteeing original solder
Under the premise of temperature-resistant, the silver content how reduced in silver-base solder becomes electrovacuum industry urgent problem to be solved.Retrieval
Current published low silver alloy solder patent, although discovery partial monopoly silver content is minimized, the mechanical property of solder and
Welding temperature is essentially identical to the performance of Ag72Cu28 solder, but the antioxygenic property of solder is difficult to ensure always, is largely effected on
The sealing-in of solder uses.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, this application provides a kind of novel oxidation-resistant quaternary alloy solders.This
Invention oxidation resistant low-silver solder alloy silver content is low, and sealing temperature is suitable with Ag72Cu28, and solder processability is good, solder wetting
Good, sealing-in strength of joint is high, and antioxygenic property is good；Alternative now widely used Ag72Cu28 solder, especially suitable for electricity
The sealing-in of ceramics and metal in vacuum device.
Technical scheme is as follows:
A kind of novel oxidation-resistant quaternary alloy solder, the solder are made of the element of following weight percent:
Ge and Si weight ratio Ge:Si >=2.5.
A kind of preparation method of the novel oxidation-resistant quaternary alloy solder, the preparation method include the following steps:
(1) Ag, Cu, Ge, Si of purity 99.9% are mixed by each element component ratio；
(2) it is put into vacuum induction melting furnace, vacuum degree reaches 4 × 10 in furnace-1~4 × 10-2It is begun to warm up after Pa, it will
Furnace temperature is increased to 1200~1300 DEG C, keeps the temperature 30~50 minutes；
(3) after alloy all melts, it is filled with nitrogen, about 1000 DEG C is cooled to, then pours into molten metal in mold,
Obtain brazing filler metal alloy ingot casting；
(4) peeling is carried out to ingot casting, removes oxide, then carries out cold rolling, rolled to 1~2mm thickness；
(5) it anneals at a temperature of 650 DEG C, is then cold rolled to the foil of 0.05~0.1mm thickness.
The present invention is beneficial to be had the technical effect that
1, silver-based alloy solder brazing temperature of the invention and Ag72Cu28 are suitable, and about 830~850 DEG C.
2, in silver-based alloy solder of the present invention Ge element, Si element and the two weight ratio control, ensure that solder sealing-in
Simultaneously, inoxidizability is greatly improved tensile strength afterwards.
3, silver solder silver content of the invention is substantially less than Ag72Cu28 solder.
Specific embodiment
Below with reference to embodiment, the present invention is specifically described.Each embodiment is prepared according to following preparation method:
Embodiment 1
A kind of preparation method of the novel oxidation-resistant quaternary alloy solder, the preparation method include the following steps:
(1) Ag, Cu, Ge, Si of purity 99.9% are mixed into (each element dosage is referring to table 1) by each element component ratio；
(2) it is put into vacuum induction melting furnace, vacuum degree is begun to warm up after reaching 0.04Pa in furnace, and furnace temperature is increased to
1200 DEG C, keep the temperature 30 minutes；
(3) after alloy all melts, it is filled with nitrogen, about 1000 DEG C is cooled to, then pours into molten metal in mold,
Obtain brazing filler metal alloy ingot casting；
(4) peeling is carried out to ingot casting, removes oxide, then carries out cold rolling, roll 1mm thickness；
(5) it anneals at a temperature of 650 DEG C, is then cold rolled to the foil of 0.05mm thickness.
Embodiment 2
A kind of preparation method of the novel oxidation-resistant quaternary alloy solder, the preparation method include the following steps:
(1) Ag, Cu, Ge, Si of purity 99.9% are mixed into (each element dosage is referring to table 1) by each element component ratio；
(2) it is put into vacuum induction melting furnace, vacuum degree is begun to warm up after reaching 0.2Pa in furnace, and furnace temperature is increased to
1250 DEG C, keep the temperature 40 minutes；
(3) after alloy all melts, it is filled with nitrogen, about 1000 DEG C is cooled to, then pours into molten metal in mold,
Obtain brazing filler metal alloy ingot casting；
(4) peeling is carried out to ingot casting, removes oxide, then carries out cold rolling, roll 1.5mm thickness；
(5) it anneals at a temperature of 650 DEG C, is then cold rolled to the foil of 0.07mm thickness.
Embodiment 3
A kind of preparation method of the novel oxidation-resistant quaternary alloy solder, the preparation method include the following steps:
(1) Ag, Cu, Ge, Si of purity 99.9% are mixed into (each element dosage is referring to table 1) by each element component ratio；
(2) it is put into vacuum induction melting furnace, vacuum degree is begun to warm up after reaching 0.4Pa in furnace, and furnace temperature is increased to
1300 DEG C, keep the temperature 50 minutes；
(3) after alloy all melts, it is filled with nitrogen, about 1000 DEG C is cooled to, then pours into molten metal in mold,
Obtain brazing filler metal alloy ingot casting；
(4) peeling is carried out to ingot casting, removes oxide, then carries out cold rolling, roll 2mm thickness；
(5) it anneals at a temperature of 650 DEG C, is then cold rolled to the foil of 0.1mm thickness.
Table 1 (unit: weight %)
| Embodiment | Ag | Cu | Ge | Si |
| 1 | 45 | 52.2 | 2 | 0.8 |
| 2 | 48 | 50 | 1.5 | 0.5 |
| 3 | 50 | 48.6 | 1 | 0.4 |
Solder obtained by Examples 1 to 3 is tested for the property with Ag72Cu28 solder, the results are shown in Table 2.
Ceramic and metal jointing strength of joint (being indicated with connector carrying pulling force) refers to that aluminium oxide ceramics and kovar alloy seal
Banjo fixing butt jointing after connecing carries pulling force, and can cut down pipe diameter is 14mm, and with a thickness of 0.5mm, magnetron connects ceramics with that can cut down sealing-in
The carrying pulling tension requirements of head must not be lower than 3.5KN.
Table 2
| Brazing temperature (DEG C) | Ceramic and metal jointing strength of joint (KN) | |
| Embodiment 1 | 830~850 | 5.2 |
| Embodiment 2 | 830~850 | 5.5 |
| Embodiment 3 | 830~850 | 5.3 |
| Ag72Cu28 | 830~850 | 5.0 |
The solder and Ag72Cu28 solder that Examples 1 to 3 obtains carry out Oxidation Resistance Test, and 4 samples are individually placed to humidify
In insulating box, temperature sets 250 DEG C, and humidity 80%, amount of oxygen 30%, standing time 30 days, the surface oxidation quantity of slag was more, then resisted
Oxidisability is weaker, and the results are shown in Table 3.
Table 3
| Sample | It aoxidizes the quantity of slag (g) |
| Embodiment 1 | 0.62 |
| Embodiment 2 | 0.55 |
| Embodiment 3 | 0.60 |
| Ag72Cu28 | 0.65 |
Claims (3)
1. a kind of novel oxidation-resistant quaternary alloy solder, it is characterised in that: the solder by following weight percent element group
At:
2. novel oxidation-resistant quaternary alloy solder according to claim 1, it is characterised in that: Ge and Si weight ratio Ge:Si
≥2.5。
3. the preparation method of novel oxidation-resistant quaternary alloy solder described in a kind of claim 1, which is characterized in that the preparation side
Method includes the following steps:
(1) Ag, Cu, Ge, Si of purity 99.9% are mixed by each element component ratio；
(2) it is put into vacuum induction melting furnace, vacuum degree reaches 4 × 10 in furnace-1~4 × 10-2It is begun to warm up after Pa, by furnace temperature liter
Height keeps the temperature 30~50 minutes to 1200~1300 DEG C；
(3) after alloy all melts, it is filled with nitrogen, about 1000 DEG C is cooled to, then molten metal is poured into mold, is obtained
Brazing filler metal alloy ingot casting；
(4) peeling is carried out to ingot casting, removes oxide, then carries out cold rolling, rolled to 1~2mm thickness；
(5) it anneals at a temperature of 650 DEG C, is then cold rolled to the foil of 0.05~0.1mm thickness.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811285346.5A CN109175784A (en) | 2018-10-31 | 2018-10-31 | A kind of novel oxidation-resistant quaternary alloy solder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811285346.5A CN109175784A (en) | 2018-10-31 | 2018-10-31 | A kind of novel oxidation-resistant quaternary alloy solder |
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| Publication Number | Publication Date |
|---|---|
| CN109175784A true CN109175784A (en) | 2019-01-11 |
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ID=64940898
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811285346.5A Pending CN109175784A (en) | 2018-10-31 | 2018-10-31 | A kind of novel oxidation-resistant quaternary alloy solder |
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| CN (1) | CN109175784A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114193026A (en) * | 2021-12-30 | 2022-03-18 | 郑州机械研究所有限公司 | High-silver brazing filler metal for welding pure silver jewelry and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57187195A (en) * | 1981-05-13 | 1982-11-17 | Tokuriki Honten Co Ltd | Silver solder material |
| JPS61242787A (en) * | 1985-04-22 | 1986-10-29 | Tokuriki Honten Co Ltd | Silver brazing filler metal |
| DE19725956A1 (en) * | 1996-07-20 | 1998-01-22 | Degussa | Manganese-containing copper-zinc-silver brazing alloy for highly stressed steel pipe |
| GB2355990A (en) * | 1999-11-05 | 2001-05-09 | Peter Gamon Johns | A silver/copper/germanium alloy composition |
| CN101007376A (en) * | 2007-01-24 | 2007-08-01 | 秦国义 | Silver based electric vacuum solder |
| CN104411450A (en) * | 2013-01-18 | 2015-03-11 | 优美科股份公司及两合公司 | Alloys |
| CN107617831A (en) * | 2017-10-17 | 2018-01-23 | 无锡日月合金材料有限公司 | A kind of ceramic and metal jointing oxidation resistant low-silver solder |
| CN107838575A (en) * | 2017-10-17 | 2018-03-27 | 无锡日月合金材料有限公司 | A kind of ceramic and metal jointing low silver content silver solder |
-
2018
- 2018-10-31 CN CN201811285346.5A patent/CN109175784A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57187195A (en) * | 1981-05-13 | 1982-11-17 | Tokuriki Honten Co Ltd | Silver solder material |
| JPS61242787A (en) * | 1985-04-22 | 1986-10-29 | Tokuriki Honten Co Ltd | Silver brazing filler metal |
| DE19725956A1 (en) * | 1996-07-20 | 1998-01-22 | Degussa | Manganese-containing copper-zinc-silver brazing alloy for highly stressed steel pipe |
| GB2355990A (en) * | 1999-11-05 | 2001-05-09 | Peter Gamon Johns | A silver/copper/germanium alloy composition |
| CN101007376A (en) * | 2007-01-24 | 2007-08-01 | 秦国义 | Silver based electric vacuum solder |
| CN104411450A (en) * | 2013-01-18 | 2015-03-11 | 优美科股份公司及两合公司 | Alloys |
| CN107617831A (en) * | 2017-10-17 | 2018-01-23 | 无锡日月合金材料有限公司 | A kind of ceramic and metal jointing oxidation resistant low-silver solder |
| CN107838575A (en) * | 2017-10-17 | 2018-03-27 | 无锡日月合金材料有限公司 | A kind of ceramic and metal jointing low silver content silver solder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114193026A (en) * | 2021-12-30 | 2022-03-18 | 郑州机械研究所有限公司 | High-silver brazing filler metal for welding pure silver jewelry and preparation method thereof |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190111 |
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| RJ01 | Rejection of invention patent application after publication |