CN114393345A - Low-silver vacuum solder with small temperature difference of melting point and flow point - Google Patents
Low-silver vacuum solder with small temperature difference of melting point and flow point Download PDFInfo
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- CN114393345A CN114393345A CN202111656522.3A CN202111656522A CN114393345A CN 114393345 A CN114393345 A CN 114393345A CN 202111656522 A CN202111656522 A CN 202111656522A CN 114393345 A CN114393345 A CN 114393345A
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- 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
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Abstract
The invention discloses a low-silver vacuum solder with small temperature difference of melting point and flow point. The low-silver vacuum solder comprises the following chemical components in percentage by mass: ag 53-60%, In2.0-6.6%, Ge0.1-1.5%, Ni0.1-2%, and the balance of Cu. The solder prepared by the invention has lower melting point and flow point, small temperature difference between the melting point and the flow point, high product strength, and better wettability, ductility, abrasion resistance and corrosion resistance.
Description
Technical Field
The invention relates to the technical field of welding materials, in particular to a low-silver vacuum solder with small temperature difference of melting point and flow point.
Background
The silver-copper alloy refers to a silver alloy with copper as a main alloying element. Silver and copper are eutectic alloys with a solid solution boundary to each other. Copper can strengthen silver and significantly reduce melting point and thermal conductivity. Generally speaking, the alloy has the advantages of fine crystallization, no brittleness, good wear resistance, strong sulfide resistance, good mechanical property and fusion welding resistance, high hardness, good electric conduction and heat conduction performance. Therefore, the contact material made of silver-copper alloy has been widely used in practice. Another major application of silver-copper alloys is their use as brazing solders. Such as AgCu25, AgCu28, AgCu55 and the like, which are the most widely used brazing filler metals at present, have moderate melting point, good electrical conductivity, higher plasticity, high welding strength, high thermal conductivity, high softening temperature and better corrosion resistance in various media. Silver-based solders are widely used in device soldering, especially in the temperature range of 600-.
The most commonly used silver-based solder is the eutectic Ag72Cu28 alloy solder. The high-strength high-conductivity high-strength high-ductility high-wettability brazing alloy has excellent technological properties such as proper melting point, good ductility, good wettability, high caulking capacity, consistent melting point and flow point (780 ℃) and the like, has high welding quality, and can form a high-strength, high-conductivity and corrosion-resistant brazing joint. And thus is widely used for soldering of electric vacuum devices and the like.
On the other hand, in vacuum devices such as vacuum arc-extinguishing chambers, stainless steel materials are widely used because they have excellent oxidation resistance, low cost, and high packaging efficiency. In order to improve the product performance, the silver-copper alloy AgCu28 can be considered to be used for soldering in the vacuum device.
However, it has been found that brazing with the silver-copper alloy AgCu28 has a disadvantage in that it is not capable of direct wet brazing on stainless steel workpieces. It is necessary to consider adding other metal elements to improve wettability. In addition, the cost of the silver-based material is high, and in order to reduce the cost of the solder, the content of silver needs to be reduced, and the content of other metal elements needs to be increased. However, the addition of other metal elements causes large difference of melting point and flow point of the solder, uneven melting of the solder, poor flowing property and unsatisfactory wetting property, and finally causes large difference of welding result of workpieces, poor welding and defects and hidden troubles of workpiece welding. From the above analysis, in order to reduce the product cost and improve the performance, a low-silver vacuum solder with small melting point and flow point temperature difference and good wettability should be developed to meet the market demand.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the low-silver vacuum solder with smaller melting point and flow point temperature difference. The low-silver vacuum solder is formed by taking silver-copper alloy Ag72Cu28 as a base and adding trace elements (Ge, Ni and the like), and has small melting point and flow point temperature difference. The solder prepared by the invention has lower melting point and flow point, small temperature difference between the melting point and the flow point, high product strength, and better product wettability, ductility, abrasion resistance and corrosion resistance.
The technical scheme of the invention is as follows:
a low-silver vacuum solder with small melting point and flow point temperature difference comprises the following chemical components in percentage by mass: ag 53-60%, In2.0-6.6%, Ge0.1-1.5%, Ni0.1-2%, and the balance of Cu.
Further, the low-silver vacuum solder comprises the following chemical components in percentage by mass: 55% of Ag, 3% of In, 0.6% of Ge, 0.9% of Ni and the balance of Cu.
Further, the low-silver vacuum solder comprises the following chemical components in percentage by mass: 56% of Ag, 4% of In, 0.9% of Ge, 0.6% of Ni and the balance of Cu.
A preparation method of the low-silver vacuum solder with small melting point and flow point temperature difference comprises the following steps:
(1) ag powder, Cu powder, In powder, Ge powder and Ni powder are mixed according to the mass percentage: ag 53-60%, In2.0-6.6%, Ge0.1-1.5%, Ni0.1-2%, and the balance of Cu, and mixing;
(2) placing the prepared material in a vacuum induction furnace for heating, smelting and cooling to finally form a brazing filler metal alloy cast ingot with the thickness of 20 mm;
(3) homogenizing the solder alloy cast ingot, peeling to remove an oxide layer, cold rolling for 2-3 times, and annealing to obtain a solder semi-finished product;
(4) and (3) repeating cold rolling and annealing processes of the semi-finished brazing filler metal for 2-8 times, and then rolling to a strip with the thickness of 0.1mm to obtain the low-silver vacuum brazing filler metal with small melting point and flow point temperature difference.
Further, in the step (2), the heating and melting process comprises the following specific steps: keeping the vacuum degree in the vacuum induction furnace at 0.1Pa, when the temperature rises to 900 ℃, filling argon, and preserving the temperature for 20-30 min.
Further, in the step (2), the cooling temperature is 780-820 ℃.
Further, in steps (3) and (4), the annealing temperature is 650 ℃.
The beneficial technical effects of the invention are as follows:
(1) the content of silver used in the invention is greatly reduced (more than or equal to 10%) compared with AgCu28, the raw material cost can be effectively reduced (the overall cost is close to the cost of AgCu28Ni materials), and meanwhile, the welding strength is also improved.
(2) According to the invention, because the content of silver is reduced, the content of copper is correspondingly increased, the melting point of the material is improved, and the melting point of indium is 156.61 ℃, so that the melting point can be effectively reduced by adding indium, and the problem of melting point increase caused by copper increase is solved; meanwhile, the strength of the product is enhanced, the ductility, wear resistance and corrosion resistance of the product are improved, and the welding performance is improved.
(3) Ge and Ni are added, and the addition of the germanium improves the wettability and the ductility of the alloy and improves the wear resistance and the corrosion resistance of the alloy; the addition of nickel effectively reduces the segregation of the alloy, enhances the corrosion resistance and the wear resistance, and achieves higher strength when the stainless steel is welded.
(4) The formula formed by the five elements is scientific and reasonable, and the material has lower melting point and flow point, small temperature difference of the melting point and the flow point, high product strength, and better wettability, ductility, abrasion resistance and corrosion resistance of the product due to the integral synergistic effect.
Drawings
FIG. 1 shows the results of DSC tests of example 4 of the present invention.
Fig. 2 is a graph comparing the melting effect of the solder prepared in example 4 of the present invention and the commercial AgCu28Ni material.
In the figure: a. melting effect of commercial AgCu28Ni2 material; b. example 4 of the present invention is the effect of melting solder.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1:
the low-silver vacuum solder with small melting point and flow point temperature difference is characterized by comprising the following chemical components in percentage by mass: ag 55%, In 3%, Ge0.6%, Ni0.9% and the balance of Cu.
The preparation method of the low-silver vacuum solder comprises the following steps:
(1) proportioning five elements of Ag, Cu, In, Ge and Ni according to the mass percentage;
(2) heating and smelting the prepared material in a vacuum induction furnace, wherein the vacuum degree in the vacuum induction furnace is 0.1 Pa; when the temperature is heated to 900 ℃, argon is filled, and the temperature is kept for 20min under the protection of argon; then cooling to 800 ℃, pouring into a mould, and cooling to form a solder alloy cast ingot with the thickness of 20 mm.
(3) Homogenizing the solder alloy cast ingot, peeling to remove an oxide layer, cold rolling for three times, and annealing in a nitrogen furnace at 650 ℃ to obtain a solder semi-finished product
(4) Then, the cold rolling is repeated for three times, the annealing process is repeated for 5 times, and the low-silver vacuum solder with smaller melting point and flow point temperature difference is obtained after the strip with the thickness of 0.1mm is rolled.
Example 2:
the low-silver vacuum solder with small melting point and flow point temperature difference is characterized by comprising the following chemical components in percentage by mass: ag 57%, In2.5%, Ge0.5%, Ni 1% and the balance of Cu.
The preparation method of the low-silver vacuum solder comprises the following steps:
(1) proportioning five elements of Ag, Cu, In, Ge and Ni according to the mass percentage;
(2) heating and smelting the prepared material in a vacuum induction furnace, wherein the vacuum degree in the vacuum induction furnace is 0.1 Pa; when the temperature is heated to 900 ℃, argon is filled, and the temperature is kept for 25min under the protection of argon; then cooling to 800 ℃, pouring into a mould, and cooling to form a solder alloy cast ingot with the thickness of 20 mm.
(3) Homogenizing the solder alloy cast ingot, peeling to remove oxide layer, cold rolling for 2 times, and annealing in a nitrogen furnace at 650 deg.C to obtain solder semi-finished product
(4) Then cold rolling is repeated for 2 times, the annealing process is repeated for 5 times, and the low-silver vacuum solder with smaller melting point and flow point temperature difference is obtained after the low-silver vacuum solder is rolled to a strip with the thickness of 0.1 mm.
Example 3:
the low-silver vacuum solder with small melting point and flow point temperature difference is characterized by comprising the following chemical components in percentage by mass: ag 58%, In3.5%, Ge0.8%, Ni1.5%, and the balance of Cu.
The preparation method of the low-silver vacuum solder comprises the following steps:
(1) proportioning five elements of Ag, Cu, In, Ge and Ni according to the mass percentage;
(2) heating and smelting the prepared material in a vacuum induction furnace, wherein the vacuum degree in the vacuum induction furnace is 0.1 Pa; when the temperature is heated to 900 ℃, argon is filled, and the temperature is kept for 20min under the protection of argon; then cooling to 800 ℃, pouring into a mould, and cooling to form a solder alloy cast ingot with the thickness of 20 mm.
(3) Homogenizing the solder alloy cast ingot, peeling to remove oxide layer, cold rolling for 2 times, and annealing in a nitrogen furnace at 650 deg.C to obtain solder semi-finished product
(4) Then cold rolling is repeated for 2 times, the annealing process is repeated for 6 times, and the low-silver vacuum solder with smaller melting point and flow point temperature difference is obtained after the low-silver vacuum solder is rolled to a strip with the thickness of 0.1 mm.
Example 4:
the low-silver vacuum solder with small melting point and flow point temperature difference is characterized by comprising the following chemical components in percentage by mass: ag 56%, In 4%, Ge0.9%, Ni0.6% and the balance of Cu.
The preparation method of the low-silver vacuum solder comprises the following steps:
(1) proportioning five elements of Ag, Cu, In, Ge and Ni according to the mass percentage;
(2) heating and smelting the prepared material in a vacuum induction furnace, wherein the vacuum degree in the vacuum induction furnace is 0.1 Pa; when the temperature is heated to 900 ℃, argon is filled, and the temperature is kept for 30min under the protection of argon; then cooling to 800 ℃, pouring into a mould, and cooling to form a solder alloy cast ingot with the thickness of 20 mm.
(3) Homogenizing the solder alloy cast ingot, peeling to remove an oxide layer, cold rolling for three times, and annealing in a nitrogen furnace at 650 ℃ to obtain a solder semi-finished product
(4) Then, the cold rolling is repeated for three times, the annealing process is repeated for 8 times, and the low-silver vacuum solder with smaller melting point and flow point temperature difference is obtained after the strip with the thickness of 0.1mm is rolled.
Example 5:
the low-silver vacuum solder with small melting point and flow point temperature difference is characterized by comprising the following chemical components in percentage by mass: ag 53%, In6.6%, Ge0.1%, Ni 2% and the balance of Cu.
The preparation method of the low-silver vacuum solder comprises the following steps:
(1) proportioning five elements of Ag, Cu, In, Ge and Ni according to the mass percentage;
(2) heating and smelting the prepared material in a vacuum induction furnace, wherein the vacuum degree in the vacuum induction furnace is 0.1 Pa; when the temperature is heated to 900 ℃, argon is filled, and the temperature is kept for 30min under the protection of argon; then cooled to 780 ℃, poured into a mold and cooled to form a solder alloy cast ingot with the thickness of 20 mm.
(3) Homogenizing the solder alloy cast ingot, peeling to remove an oxide layer, cold rolling for three times, and annealing in a nitrogen furnace at 650 ℃ to obtain a solder semi-finished product
(4) Then, the cold rolling is repeated for three times, the annealing process is repeated for 3 times, and the low-silver vacuum solder with smaller melting point and flow point temperature difference is obtained after the strip with the thickness of 0.1mm is rolled.
Comparative example 1:
the comparative example is the same as the example 4, except that the low-silver vacuum solder comprises the following chemical components in percentage by mass: ag 56%, In 4%, Ge0.9% and the balance of Cu.
Comparative example 2:
the comparative example is the same as the example 4, and is different from the low-silver vacuum solder in that the low-silver vacuum solder comprises the following chemical components in percentage by mass: ag 56%, In 1.5%, Ge 0.9%, Ni 2.2%, and the balance of Cu.
Test example:
the solder prepared in example 4 was measured using a DSC tester, and the test results are shown in fig. 1. As can be seen from FIG. 1, the melting point and the flow point of the material prepared in example 4 are 780.1 ℃ and 785 ℃, respectively, and the melting point and the flow point are small, and the temperature difference between the melting point and the flow point is small (4.9 ℃). The material prepared in example 4 was high in strength as measured by a tensile tester. A material melting comparison test is carried out on a stainless steel plate (as shown in figure 2, a is a standard commercial AgCu28Ni2 material, and b is the solder prepared in the embodiment 4 of the invention), and the fact that the material in the b picture has the fluidity and the wettability close to those of the a is found, but the melting point, the flow point and the mechanical property of the solder prepared in the embodiment 4 of the invention are better, so that the material prepared by the formula and the method provided by the invention has good performance comprehensively and meets the actual requirements of the electro-vacuum industry.
As can be seen from comparative example 1, when only indium and germanium were added to the solder, and no nickel was added, the prepared solder had large differences in melting point and flow point, the solder melted unevenly, and the fluidity and wettability were not satisfactory. As can be seen from comparative example 2, when the Ni content In the brazing filler metal is more than 2% and the In content is less than 2%, the prepared brazing filler metal has large difference of melting point and flow point, non-ideal wetting property and insufficient strength, and the performance of the brazing filler metal cannot meet the requirements of customers.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (7)
1. The low-silver vacuum solder with small melting point and flow point temperature difference is characterized by comprising the following chemical components in percentage by mass: ag 53-60%, In2.0-6.6%, Ge0.1-1.5%, Ni0.1-2%, and the balance of Cu.
2. The low-silver vacuum solder as claimed in claim 1, wherein the low-silver vacuum solder comprises the following chemical components in percentage by mass: 55% of Ag, 3% of In, 0.6% of Ge, 0.9% of Ni and the balance of Cu.
3. The low-silver vacuum solder as claimed in claim 1, wherein the low-silver vacuum solder comprises the following chemical components in percentage by mass: 56% of Ag, 4% of In, 0.9% of Ge, 0.6% of Ni and the balance of Cu.
4. A method for preparing a low-silver vacuum solder with small melting point and flow point temperature difference according to any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) ag powder, Cu powder, In powder, Ge powder and Ni powder are mixed according to the mass percentage: ag 53-60%, In2.0-6.6%, Ge0.1-1.5%, Ni0.1-2%, and the balance of Cu, and mixing;
(2) placing the prepared material in a vacuum induction furnace for heating, smelting and cooling to finally form a brazing filler metal alloy cast ingot with the thickness of 20 mm;
(3) homogenizing the solder alloy cast ingot, peeling to remove an oxide layer, cold rolling, and annealing to obtain a solder semi-finished product;
(4) and (3) repeating cold rolling and annealing processes of the semi-finished brazing filler metal for 2-8 times, and then rolling to a strip with the thickness of 0.1mm to obtain the low-silver vacuum brazing filler metal with small melting point and flow point temperature difference.
5. The preparation method according to claim 4, wherein in the step (2), the heating smelting is carried out by the following specific processes: keeping the vacuum degree in the vacuum induction furnace at 0.1Pa, when the temperature rises to 900 ℃, filling argon, and preserving the temperature for 20-30 min.
6. The method as claimed in claim 4, wherein the cooling temperature in step (2) is 780-820 ℃.
7. The method according to claim 4, wherein the annealing is performed at 650 ℃ in each of the steps (3) and (4).
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| CN202111656522.3A CN114393345A (en) | 2021-12-30 | 2021-12-30 | Low-silver vacuum solder with small temperature difference of melting point and flow point |
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| CN202111656522.3A CN114393345A (en) | 2021-12-30 | 2021-12-30 | Low-silver vacuum solder with small temperature difference of melting point and flow point |
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| JPS57149092A (en) * | 1981-03-11 | 1982-09-14 | Tokuriki Honten Co Ltd | Silver solder material |
| JPS61242787A (en) * | 1985-04-22 | 1986-10-29 | Tokuriki Honten Co Ltd | Silver brazing filler metal |
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| CN101007376A (en) * | 2007-01-24 | 2007-08-01 | 秦国义 | Silver based electric vacuum solder |
| JP4093322B1 (en) * | 2007-09-06 | 2008-06-04 | 株式会社新潟Ｔｌｏ | Low melting point silver brazing material |
| CN101337309A (en) * | 2007-07-05 | 2009-01-07 | 哈尔滨理工大学 | Tin-silver-cuprum-germanium leadless solder . |
| CN103170760A (en) * | 2011-12-20 | 2013-06-26 | 北京有色金属与稀土应用研究所 | Electric vacuum brazing filler and preparation method thereof |
| CN104526181A (en) * | 2014-12-03 | 2015-04-22 | 浙江亚通焊材有限公司 | Electric vacuum silver base alloy solder for vacuum electronic device brazing sealing and preparation method thereof |
| CN104646846A (en) * | 2013-11-21 | 2015-05-27 | 北京有色金属与稀土应用研究所 | Silver, copper, palladium and gold alloy brazing wire and preparation method thereof |
| CN105177342A (en) * | 2015-09-24 | 2015-12-23 | 无锡日月合金材料有限公司 | Preparation method of ternary alloy sealing material |
| CN108161274A (en) * | 2017-11-24 | 2018-06-15 | 北京有色金属与稀土应用研究所 | It is a kind of for sealing-in solder of electron tube and preparation method thereof |
| CN110238559A (en) * | 2019-06-17 | 2019-09-17 | 无锡日月合金材料有限公司 | A kind of novel quaternary alloy solder and preparation method thereof |
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2021
- 2021-12-30 CN CN202111656522.3A patent/CN114393345A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57149092A (en) * | 1981-03-11 | 1982-09-14 | Tokuriki Honten Co Ltd | Silver solder material |
| JPS61242787A (en) * | 1985-04-22 | 1986-10-29 | Tokuriki Honten Co Ltd | Silver brazing filler metal |
| GB9926313D0 (en) * | 1999-11-05 | 2000-01-12 | Johns Peter G | A silver/copper/germanium alloy composition |
| CN101007376A (en) * | 2007-01-24 | 2007-08-01 | 秦国义 | Silver based electric vacuum solder |
| CN101337309A (en) * | 2007-07-05 | 2009-01-07 | 哈尔滨理工大学 | Tin-silver-cuprum-germanium leadless solder . |
| JP4093322B1 (en) * | 2007-09-06 | 2008-06-04 | 株式会社新潟Ｔｌｏ | Low melting point silver brazing material |
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| CN104646846A (en) * | 2013-11-21 | 2015-05-27 | 北京有色金属与稀土应用研究所 | Silver, copper, palladium and gold alloy brazing wire and preparation method thereof |
| CN104526181A (en) * | 2014-12-03 | 2015-04-22 | 浙江亚通焊材有限公司 | Electric vacuum silver base alloy solder for vacuum electronic device brazing sealing and preparation method thereof |
| CN105177342A (en) * | 2015-09-24 | 2015-12-23 | 无锡日月合金材料有限公司 | Preparation method of ternary alloy sealing material |
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| CN110238559A (en) * | 2019-06-17 | 2019-09-17 | 无锡日月合金材料有限公司 | A kind of novel quaternary alloy solder and preparation method thereof |
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