CN107760911A - A kind of copper-based anti-oxidant sealing alloy solder and preparation method thereof - Google Patents
A kind of copper-based anti-oxidant sealing alloy solder and preparation method thereof Download PDFInfo
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- CN107760911A CN107760911A CN201711013393.XA CN201711013393A CN107760911A CN 107760911 A CN107760911 A CN 107760911A CN 201711013393 A CN201711013393 A CN 201711013393A CN 107760911 A CN107760911 A CN 107760911A
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- solder
- ingot casting
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- 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
- B23K35/302—Cu as the principal constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a kind of copper-based anti-oxidant sealing alloy solder, the mass percent of its component and each component is：Ge：11~13%；Si：1~5%；Ni：0.3~0.4%；Co：0.1~0.2%；Ce：0.1~0.2%；B：0.1~0.15%；Nd：0.1~0.15%；Surplus is Cu.The present invention is directed to the defects of acid bronze alloy antioxidant is weak, further improves the antioxygenic property of copper-base alloy tin solder.
Description
Technical field
The present invention relates to the seal, sealing materials technical field of radio tube in vacuum electronic industry, more particularly, to a kind of copper
Anti-oxidant multicomponent alloy seal, sealing materials of base and preparation method thereof.
Background technology
With the critical role that encapsulation technology occupies in modernization vacuum electronic field, excellent seal, sealing materials are selected
It is more aobvious most important.In electrovacuum sealing-in field, the connecting material being related to includes metal and metal, metal and ceramics etc..Pass
The seal, sealing materials silver-based solder of system has the wetting property and decay resistance that mechanical property is good, high because of it, in radio tube
It is widely used in sealing-in industry.As the demand to silver-base solder is increasing, silver is used as precious metal material, and price is swift and violent
Increase, the cost for directly resulting in solder greatly increases.Therefore, it is a kind of comprehensive in radio tube industry increasingly with keen competition
Conjunction performance is good, the low active demand for having become existing market without silver-colored sealing-in solder of cost.
Acid bronze alloy steam forces down, and elevated temperature strength is good, and the wetability between various metals is good, can be used as various metals connection
Material.Copper germanium alloy is because it has high-melting-point feature, by high-temperature stage welding of the more use in sublevel welding.Due to
Copper germanium alloy is easy to the characteristics of oxidation, can not can not meet current requirement.
The content of the invention
In view of the above-mentioned problems existing in the prior art, this application provides a kind of copper-based anti-oxidant sealing alloy solder and its
Preparation method.The present invention is directed to the defects of acid bronze alloy antioxidant is weak, further improves the inoxidizability of copper-base alloy tin solder
Energy.Technical scheme is as follows：
The mass percent of a kind of copper-based anti-oxidant sealing alloy solder, its component and each component is：Ge：11~13%；
Si：1~5%；Ni：0.3~0.4%；Co：0.1~0.2%；Ce：0.1~0.2%；B：0.1~0.15%；Nd：0.1~
0.15%；Surplus is Cu.
The preparation method of described copper-based anti-oxidant sealing alloy solder, specific preparation process are as follows：
(1) Ge, Co, Ni raw material are put into melting in vacuum melting furnace and prepare germanium cobalt nickel intermediate alloy；
(2) intermediate alloy prepared in step (1) and Cu, Si, Ce, B, Nd raw material are together put into smelting furnace and melted
Refining；
(3) after vacuum reaches 0.06~0.2Pa in smelting furnace, then 1200~1350 DEG C will be heated in stove, be incubated
20~25 minutes, it is completely melt after forming alloy molten liquid, fused solution is cast in shaper, circulating water temperature to room
Wen Hou, shaper is gone to take out out of vacuum drying oven, obtains processing the ingot casting needed for this welding material；
(4) the ingot casting solution treatment at 550~650 DEG C that will be obtained in step (3), 45~50 minutes are incubated, rapid water
It is cooled to room temperature, then Ageing Treatment 30~35 minutes at 400~450 DEG C again；
(5) the advanced driving of the ingot casting obtained in step (4) is shelled, to ream the dirty and oxide layer on ingot casting surface, then
Cold rolling is carried out, controlled rolling passage is at 30~35 times, and when reaching 3~5mm to thickness, clot is put into annealing furnace, temperature
450~550 DEG C are arranged on, 30~40 minutes is incubated, then naturally cools to room temperature；
(6) band obtained in step (5) is continued into cold rolling, controlled rolling passage is rolled down to thickness as 1.2 at 6~8 times
After~1.8mm, clot is put into annealing furnace, and temperature setting is incubated 20~30 minutes, then natural cooling at 450~520 DEG C
To room temperature；
(7) after being 0.08~0.15mm by the band obtained in step (6) continuation finish rolling to thickness, punching press after sub-cut band
Go out required solder products with varying degrees.
The present invention is beneficial to be had technical effect that：
The present invention is equipped with suitable refining, casting, deformation technique, obtained copper-based solder by the optimization to each element
Weld strength more improve, and there is excellent inoxidizability.Inoxidizability height can greatly improve the shelf-life of solder, and
And solder is set to preserve higher sealing property in sealing-in.
Embodiment
With reference to embodiment, the present invention is specifically described.The quality of each raw material components used in embodiment 1~3
As shown in table 1, unit kg.
Table 1
Embodiment 1
The preparation method for the copper-based anti-oxidant sealing alloy solder that the applicant provides is as follows：
(1) Ge, Co, Ni raw material are put into melting in vacuum melting furnace and prepare germanium cobalt nickel intermediate alloy；
(2) intermediate alloy prepared in step (1) and Cu, Si, Ce, B, Nd raw material are together put into smelting furnace and melted
Refining；
(3) after vacuum reaches 0.06Pa in smelting furnace, then 1200 DEG C will be heated in stove, be incubated 20 minutes, completely
After fusing forms alloy molten liquid, fused solution is cast in shaper, after circulating water temperature to room temperature, by shaper
Go to take out out of vacuum drying oven, obtain processing the ingot casting needed for this welding material；
(4) the ingot casting solution treatment at 550 DEG C that will be obtained in step (3), 50 minutes being incubated, rapid water is cooled to room temperature,
Then Ageing Treatment 35 minutes at 400 DEG C again；
(5) the advanced driving of the ingot casting obtained in step (4) is shelled, to ream the dirty and oxide layer on ingot casting surface, then
Cold rolling is carried out, controlled rolling passage is at 30 times, and when reaching 5mm to thickness, clot is put into annealing furnace, and temperature setting exists
450 DEG C, 40 minutes are incubated, then naturally cools to room temperature；
(6) band obtained in step (5) is continued into cold rolling, for controlled rolling passage at 6 times, it is 1.8mm to be rolled down to thickness
Afterwards, clot is put into annealing furnace, and temperature setting is incubated 30 minutes, then naturally cools to room temperature at 450 DEG C；
(7) after being 0.08mm by the band obtained in step (6) continuation finish rolling to thickness, stamp out after sub-cut band required
Solder products with varying degrees.
Embodiment 2
The preparation method for the copper-based anti-oxidant sealing alloy solder that the applicant provides is as follows：
(1) Ge, Co, Ni raw material are put into melting in vacuum melting furnace and prepare germanium cobalt nickel intermediate alloy；
(2) intermediate alloy prepared in step (1) and Cu, Si, Ce, B, Nd raw material are together put into smelting furnace and melted
Refining；
(3) after vacuum reaches 0.1Pa in smelting furnace, then 1300 DEG C will be heated in stove, be incubated 22 minutes, it is completely molten
Change form alloy molten liquid after, by fused solution cast shaper in, after circulating water temperature to room temperature, by shaper from
Go to take out in vacuum drying oven, obtain processing the ingot casting needed for this welding material；
(4) the ingot casting solution treatment at 600 DEG C that will be obtained in step (3), 48 minutes being incubated, rapid water is cooled to room temperature,
Then Ageing Treatment 32 minutes at 420 DEG C again；
(5) the advanced driving of the ingot casting obtained in step (4) is shelled, to ream the dirty and oxide layer on ingot casting surface, then
Cold rolling is carried out, controlled rolling passage is at 33 times, and when reaching 4mm to thickness, clot is put into annealing furnace, and temperature setting exists
500 DEG C, 35 minutes are incubated, then naturally cools to room temperature；
(6) band obtained in step (5) is continued into cold rolling, for controlled rolling passage at 7 times, it is 1.4mm to be rolled down to thickness
Afterwards, clot is put into annealing furnace, and temperature setting is incubated 25 minutes, then naturally cools to room temperature at 500 DEG C；
(7) after being 0.1mm by the band obtained in step (6) continuation finish rolling to thickness, stamp out after sub-cut band required
Solder products with varying degrees.
Embodiment 3
The preparation method for the copper-based anti-oxidant sealing alloy solder that the applicant provides is as follows：
(1) Ge, Co, Ni raw material are put into melting in vacuum melting furnace and prepare germanium cobalt nickel intermediate alloy；
(2) intermediate alloy prepared in step (1) and Cu, Si, Ce, B, Nd raw material are together put into smelting furnace and melted
Refining；
(3) after vacuum reaches 0.2Pa in smelting furnace, then 1350 DEG C will be heated in stove, be incubated 25 minutes, it is completely molten
Change form alloy molten liquid after, by fused solution cast shaper in, after circulating water temperature to room temperature, by shaper from
Go to take out in vacuum drying oven, obtain processing the ingot casting needed for this welding material；
(4) the ingot casting solution treatment at 650 DEG C that will be obtained in step (3), 45 minutes being incubated, rapid water is cooled to room temperature,
Then Ageing Treatment 30 minutes at 450 DEG C again；
(5) the advanced driving of the ingot casting obtained in step (4) is shelled, to ream the dirty and oxide layer on ingot casting surface, then
Cold rolling is carried out, controlled rolling passage is at 35 times, and when reaching 3mm to thickness, clot is put into annealing furnace, and temperature setting exists
550 DEG C, 30 minutes are incubated, then naturally cools to room temperature；
(6) band obtained in step (5) is continued into cold rolling, for controlled rolling passage at 8 times, it is 1.2mm to be rolled down to thickness
Afterwards, clot is put into annealing furnace, and temperature setting is incubated 20 minutes, then naturally cools to room temperature at 520 DEG C；
(7) after being 0.15mm by the band obtained in step (6) continuation finish rolling to thickness, stamp out after sub-cut band required
Solder products with varying degrees.
Test case：
The solder test data that embodiment 1~3 is prepared is as shown in table 2, table 3；By the three of CN201610874171.6
Individual embodiment contrasts respectively as comparative example 1~3.
(1) sealing temperature and weld strength of solder, as shown in table 2.
Table 2
| Performance | Sealing temperature (DEG C) | Weld strength (KN/cm2) |
| Embodiment 1 | 770~800 | 6.8 |
| Embodiment 2 | 780~800 | 6.6 |
| Embodiment 3 | 790~810 | 7.1 |
| Comparative example 1 | 820~930 | 5.8 |
| Comparative example 2 | 850~930 | 5.6 |
| Comparative example 3 | 870~900 | 5.1 |
(2) by solder natural exposing 90 days in air, by observing solder surface color, judge that alloy welds
The inoxidizability of material, as a result as shown in table 3.
Table 3
| Performance | Sealing temperature |
| Embodiment 1 | It is non-discolouring |
| Embodiment 2 | It is non-discolouring |
| Embodiment 3 | It is non-discolouring |
| Comparative example 1 | Black |
| Comparative example 2 | Black |
| Comparative example 3 | Black |
Claims (2)
1. a kind of copper-based anti-oxidant sealing alloy solder, it is characterised in that its component and the mass percent of each component are：Ge：11
~13%；Si：1~5%；Ni：0.3~0.4%；Co：0.1~0.2%；Ce：0.1~0.2%；B：0.1~0.15%；Nd：
0.1~0.15%；Surplus is Cu.
2. the preparation method of the copper-based anti-oxidant sealing alloy solder described in a kind of claim 1, it is characterised in that specific to prepare
Step is as follows：
(1) Ge, Co, Ni raw material are put into melting in vacuum melting furnace and prepare germanium cobalt nickel intermediate alloy；
(2) intermediate alloy prepared in step (1) and Cu, Si, Ce, B, Nd raw material are together put into melting in smelting furnace；
(3) after vacuum reaches 0.06~0.2Pa in smelting furnace, then 1200~1350 DEG C will be heated in stove, insulation 20~
25 minutes, it is completely melt after forming alloy molten liquid, fused solution is cast in shaper, circulating water temperature to room temperature
Afterwards, shaper is gone to take out out of vacuum drying oven, obtains processing the ingot casting needed for this welding material；
(4) the ingot casting solution treatment at 550~650 DEG C that will be obtained in step (3), 45~50 minutes are incubated, rapid water is cooled to
Room temperature, then Ageing Treatment 30~35 minutes at 400~450 DEG C again；
(5) the advanced driving of the ingot casting obtained in step (4) is shelled, to ream the dirty and oxide layer on ingot casting surface, then carried out
Cold rolling, controlled rolling passage is at 30~35 times, and when reaching 3~5mm to thickness, clot is put into annealing furnace, temperature setting
At 450~550 DEG C, 30~40 minutes are incubated, then naturally cools to room temperature；
(6) band obtained in step (5) is continued into cold rolling, controlled rolling passage at 6~8 times, be rolled down to thickness for 1.2~
After 1.8mm, clot is put into annealing furnace, and temperature setting is incubated 20~30 minutes, then naturally cooled at 450~520 DEG C
Room temperature；
(7) after being 0.08~0.15mm by the band obtained in step (6) continuation finish rolling to thickness, institute is stamped out after sub-cut band
The solder products with varying degrees needed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711013393.XA CN107760911A (en) | 2017-10-26 | 2017-10-26 | A kind of copper-based anti-oxidant sealing alloy solder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711013393.XA CN107760911A (en) | 2017-10-26 | 2017-10-26 | A kind of copper-based anti-oxidant sealing alloy solder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107760911A true CN107760911A (en) | 2018-03-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711013393.XA Pending CN107760911A (en) | 2017-10-26 | 2017-10-26 | A kind of copper-based anti-oxidant sealing alloy solder and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109175785A (en) * | 2018-10-31 | 2019-01-11 | 无锡日月合金材料有限公司 | A kind of vacuum seal solder alloy |
| CN109175783A (en) * | 2018-10-31 | 2019-01-11 | 无锡日月合金材料有限公司 | A kind of quaternary alloy solder |
| CN111299901A (en) * | 2019-12-12 | 2020-06-19 | 郑州机械研究所有限公司 | Brazing alloy, brazing filler metal, preparation method and application of brazing filler metal and prepared brazing product |
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| CN106222478A (en) * | 2016-08-23 | 2016-12-14 | 无锡日月合金材料有限公司 | A kind of ternary-alloy sealing material and preparation method thereof |
| CN106381415A (en) * | 2016-09-30 | 2017-02-08 | 无锡日月合金材料有限公司 | Copper-based silver-free sealing alloy material and preparation method thereof |
| CN106435325A (en) * | 2016-10-10 | 2017-02-22 | 无锡日月合金材料有限公司 | Multielement alloy sealing material and preparation method thereof |
| CN106467941A (en) * | 2016-09-30 | 2017-03-01 | 无锡日月合金材料有限公司 | A kind of radio tube sealing-in low silver multicomponent alloy material and preparation method thereof |
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2017
- 2017-10-26 CN CN201711013393.XA patent/CN107760911A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106222478A (en) * | 2016-08-23 | 2016-12-14 | 无锡日月合金材料有限公司 | A kind of ternary-alloy sealing material and preparation method thereof |
| CN106381415A (en) * | 2016-09-30 | 2017-02-08 | 无锡日月合金材料有限公司 | Copper-based silver-free sealing alloy material and preparation method thereof |
| CN106467941A (en) * | 2016-09-30 | 2017-03-01 | 无锡日月合金材料有限公司 | A kind of radio tube sealing-in low silver multicomponent alloy material and preparation method thereof |
| CN106435325A (en) * | 2016-10-10 | 2017-02-22 | 无锡日月合金材料有限公司 | Multielement alloy sealing material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109175785A (en) * | 2018-10-31 | 2019-01-11 | 无锡日月合金材料有限公司 | A kind of vacuum seal solder alloy |
| CN109175783A (en) * | 2018-10-31 | 2019-01-11 | 无锡日月合金材料有限公司 | A kind of quaternary alloy solder |
| CN111299901A (en) * | 2019-12-12 | 2020-06-19 | 郑州机械研究所有限公司 | Brazing alloy, brazing filler metal, preparation method and application of brazing filler metal and prepared brazing product |
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Application publication date: 20180306 |