CN112518169A - Low-melting-point high-strength low-silver cadmium-free manganese-free multi-element silver solder and preparation method thereof - Google Patents
Low-melting-point high-strength low-silver cadmium-free manganese-free multi-element silver solder and preparation method thereof Download PDFInfo
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- CN112518169A CN112518169A CN202011397957.6A CN202011397957A CN112518169A CN 112518169 A CN112518169 A CN 112518169A CN 202011397957 A CN202011397957 A CN 202011397957A CN 112518169 A CN112518169 A CN 112518169A
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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
- B23K35/28—Selection of soldering or welding materials proper with the principal constituent melting at less than 950 degrees C
- B23K35/282—Zn 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
- B23K35/40—Making wire or rods for soldering or welding
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/06—Alloys containing less than 50% by weight of each constituent containing zinc
-
- 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
- C22C9/04—Alloys based on copper with zinc as the next major constituent
Abstract
The application relates to a low-silver cadmium-free manganese-free multi-element silver solder with low melting point and high strength and a preparation method thereof, wherein the multi-element silver solder is composed of 19-23% of silver, 32-35% of zinc, 1.0-3.0% of tin, 0-2.0% of nickel, 0-3.0% of indium, 0.01-1.0% of alloy elements and the balance of copper, wherein the alloy elements are one or more of phosphorus, lanthanum and cerium. The alloy elements comprise, by mass, 0.2-1% of phosphorus, 0-0.02% of lanthanum and 0-0.01% of cerium. The preparation method of the multi-element silver solder comprises the following steps: s1: heating copper in the Cu-X alloy in a crucible of an intermediate frequency smelting furnace to be completely melted, and adding alloy metal X until the Cu-X alloy is completely melted; s2: adding silver, zinc, tin, nickel and indium with the purity of at least 99.99 percent and the rest part except copper in the Cu-X alloy into a crucible of a medium-frequency smelting furnace containing the melted Cu-X alloy according to the component proportion of the low-silver cadmium-free manganese-free multi-element silver brazing filler metal for smelting and casting; s3: and (5) carrying out subsequent treatment. The solder is simple to prepare, contains no cadmium and manganese, has low total content of silver and indium, and has appropriate solidus and liquidus temperatures, welding performance and good processability.
Description
Technical Field
The application relates to a low-silver cadmium-free manganese-free multi-element silver solder with low melting point and high strength and a preparation method thereof.
Background
The silver-based brazing filler metal is a medium-temperature brazing filler metal widely applied to various alloys such as low-carbon steel, stainless steel, copper alloy and the like, and has excellent technological properties, proper melting temperature, good gap filling capacity and wettability. With the increase of silver price, the cost of the silver-based solder is high, and the low-silver solder with high performance is always the target pursued by enterprises. The performance with cadmium-containing silver solder is most outstanding among the low silver solder of tradition, mainly because along with silver content reduction in the solder, its melting temperature can constantly rise, and spreadability also can drop, the melting temperature scope that can effectively reduce the solder of the joining of cadmium element this moment reduces the brittle phase in the solder, increases the wetting ability of spreading, has promoted the solderability by a wide margin. However, the cadmium element has great harm to the health of welding operators and the surrounding environment, and the production and use of the solder containing cadmium are gradually forbidden by relevant environmental regulations at home and abroad based on the environmental protection requirement, so that the cadmium-free low-silver solder is actively popularized.
The existing mature cadmium-free low-melting-point silver solder mainly comprises 30-45 wt.% silver-copper-zinc ternary solder and 25-34 wt.% silver-copper-zinc (tin or indium) quaternary solder, such as the classic BAg45CuZn (solidus 665 ℃, liquidus 745 ℃), BAg30CuZnSn (solidus 665 ℃, liquidus 755 ℃) and BAg30CuZnIn (solidus 640 ℃, liquidus 755 ℃) recommended in GB/T10046 silver solder) are used for replacing BAg45CuZn, so as to reduce the silver content and the production cost. If the silver content is reduced by another 5wt.%, its melting temperature will rise by about 15-40 ℃ as in the BAg25CuZn solders listed in the standard (solidus 700 ℃, liquidus 790 ℃) and BAg25CuZnSn solders (solidus 680 ℃, liquidus 760 ℃). For this reason, researchers and solder manufacturers have been working on developing new low silver cadmium-free solders.
The applicant has conducted relevant literature search for low silver cadmium-free solders. In published documents, CN 110280924A discloses a low-silver cadmium-free silver solder, the Ag content is only 11.0-13.0%, the solidus temperature is no more than 765 ℃, and the liquidus temperature is no more than 795 ℃; CN101524793A adopts cadmium-free low-silver solder containing trace lithium and niobium to purify the structure, improves the spreading wettability of the solder, and has higher solidus (725 ℃ -735 ℃) and liquidus (760 ℃ -770 ℃) temperatures because the silver content is lower than 19 wt.%; CN106077995A discloses a cadmium-free low-silver brazing filler metal containing manganese and tin, wherein the Ag content is in the range of 13-19%, the solidus temperature is 685 ℃, and the liquidus temperature is 765 ℃. The silver content of the brazing filler metal related to the three patent documents is less than 20 wt.%, but the welding temperature is higher, and the brazing filler metal cannot replace mature low-silver brazing filler metal products such as BAg25CuZnSn and BAg26 CuZnSnIn. CN10494247B recommends a cadmium-free silver solder containing Sn, Si, Zn and Pr and its preparation method, the silver content is 30 wt.%, the solidus temperature is 670 deg.C, the liquidus temperature is 765 deg.C, the main advantage of this patent lies in that after adding rare earth element Pr, the spreading performance and the tensile strength of soldered joint are effectively improved, it can be used to replace BAg45CuZn with high silver content, the soldered brass joint can reach 320 MPa-370 MPa range, but the silver content is relatively high, its cost is still high. CN103418933A discloses a cadmium-free silver solder for connecting brass and stainless steel, wherein the silver content is 18-22 wt%, the solder is alloyed by mixed rare earth elements of In, Sn, Ni and lanthanum and cerium, the solder has good wettability with brass and stainless steel, and is used for replacing silver-copper-zinc solder with the silver content of 25 wt% or more, but In the embodiment, the solidus line of only two examples is lower than 680 ℃, the liquidus line is lower than 790 ℃, the proportion of silver and indium In the component formula is about 25-26 wt%, and considering that the price of indium is equivalent to or even higher than that of silver, the solder can not be used for replacing the solder with the silver content of 25-26 wt% to reduce the cost.
Therefore, among the silver-copper-zinc based solders disclosed in the literature, a green low-silver solder which has a silver content of about 20 wt.%, a soldering temperature range close to that of the BAg26 cuznsinn solder, good formability and soldering performance and can be compared with the BAg26 cuznsinn solder is still a blank.
Disclosure of Invention
The technical problem solved by the application is to overcome the defects in the prior art, and provide a low-melting-point cadmium-free manganese-free low-silver solder for connecting copper alloy and carbon steel and a preparation method thereof, wherein the solder does not contain toxic element cadmium and volatile element manganese, has lower total content of silver and indium than BAg26CuZnSnIn, low cost, solidus and liquidus temperature equivalent to BAg26CuZnSnIn, welding process performance indexes and excellent processability.
The technical scheme adopted by the application for solving the technical problems comprises the following steps: a low-silver cadmium-free manganese-free multi-element silver solder with low melting point and high strength is composed of the following raw materials in percentage by mass:
Ag 19%~23%
Zn 32%~35%
Sn 1.0%~3.0%
Ni 0~2.0%
In 0~3.0%
alloy element X0.01% -1.0% (X is one or more of phosphorus, lanthanum and cerium)
The balance being Cu.
The alloy element X consists of 0.2-1% of P, 0-0.02% of La and 0-0.01% of Ce in percentage by mass.
The technical scheme that this application solved above-mentioned technical problem and adopted still includes:
the preparation method of the low-silver cadmium-free manganese-free multi-element silver solder with low melting point and high strength comprises the following steps:
s1: pre-smelting a small amount of copper (copper in the Cu-X alloy) and trace alloy element X into a Cu-X alloy, heating the Cu of the Cu-X in a crucible of a medium-frequency smelting furnace to be completely molten, and adding alloy metal X until the Cu-X alloy is completely molten (normally, the molten Cu-X alloy is transparent and green);
s2: silver, zinc, tin, nickel and indium with the purity of at least 99.99 percent and the rest part of copper in the Cu-X alloy are removed, the silver, the zinc, the tin, the nickel and the indium are added into a crucible of a medium-frequency smelting furnace containing the melted Cu-X alloy according to the component proportion of the low-silver cadmium-free manganese-free multi-element silver brazing filler metal, and smelting and casting are carried out by adopting a medium-frequency smelting process;
s3: the required brazing filler metal in strip, wire or ribbon form is obtained by the subsequent treatment of the prior art, such as extrusion, drawing or rolling.
The Cu-X alloy usually contains 0.01-10 g of copper.
Compared with the prior art, the application has the following advantages and effects: the preparation method is simple, the brazing filler metal does not contain toxic elements of cadmium and volatile elements of manganese, the total content of silver and indium is lower than that of BAg26CuZnSnIn, the cost is low, and the brazing filler metal has solidus line and liquidus line temperature equivalent to those of BAg26CuZnSnIn, welding process performance indexes and excellent processability.
Detailed Description
The present application is explained in further detail below, and the following examples are illustrative of the present application and the present application is not limited to the following examples.
Example 1: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
Ag：21.0%、Zn：34.5%，Sn：1.5%、In: 1.0%, X: 0.2% and the balance of Cu, wherein the alloy element X in the example is P: 0.195%, Ce: 0.005 percent. The solidus temperature is 636 ℃, the liquidus temperature is 783 ℃, and the unit spread area on pure copper (red copper) is 3.50 mm2The tensile strength of the joint for 45# steel was 377 MPa, the tensile strength of the joint for H62 brass was 342 MPa, and the microhardness of the braze was 215 HV 0.2.
Example 2: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 22.0%, Zn: 34.5%, Sn: 1.0%, X: 0.5%, and the balance being Cu, the alloying elements X in this example being P: 0.49%, La: 0.01 percent. The solidus temperature was 613 ℃ and the liquidus temperature was 772 ℃ and the unit spread area on pure copper was 3.80 mm2The tensile strength of the joint for 45# steel is 380 MPa, the tensile strength of the joint for H62 brass is 337 MPa, and the microhardness of the brazing filler metal is 215 HV 0.2.
Example 3: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 23.0%, Zn: 34.4%, Sn: 1.5%, X: 0.8 percent, and the balance of Cu, wherein the alloy element X in the example is P: 0.785%, La: 0.01%, Ce: 0.005 percent. The solidus temperature was 584 ℃ and the liquidus temperature was 762 ℃ and the unit spread area on pure copper was 5.03 mm2The tensile strength of the joint for 45# steel was 392 MPa, the tensile strength of the joint for H62 brass was 357 MPa, and the microhardness of the solder was 244 HV 0.2.
Example 4: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 21.0%, Zn: 33.3%, Sn: 1.5%, Ni: 1.0%, In: 2.5%, X: 0.2% and the balance of Cu, wherein the alloy element X in the example is P: 0.195%, Ce: 0.005 percent. The solidus temperature is 600 ℃, the liquidus temperature is 771 ℃, and the unit spreading area on pure copper is 4.63 mm2The tensile strength of the joint for 45# steel is 356 MPa, the tensile strength of the joint for H62 brass is 346 MPa, and the microhardness of the brazing filler metal is 202 HV 0.2.
Example 5: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 20.0%, Zn: 33%, Sn: 2.0%, Ni: 2.0%, In: 1.0%, X: 0.5%, and the balance being Cu, the alloying elements X in this example being P: 0.49%, La: 0.01 percent. The solidus temperature is 668 ℃, the liquidus temperature is 773 ℃, and the unit spread area on pure copper is 4.50 mm2Per gram, the joint tensile strength for 45# steel was 399 MPa, the joint tensile strength for H62 brass was 359 MPa, and the braze microhardness was 197 HV 0.2.
Example 6: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 20.0%, Zn: 33.3%, Sn: 1.0%, Ni: 1.0%, In: 2.5%, X: 1.0 percent and the balance of Cu, wherein the alloy element X in the example is P: 0.985%, La: 0.01%, Ce: 0.005 percent. The solidus temperature is 687 ℃, the liquidus temperature is 771 ℃, and the unit spreading area on pure copper is 4.76 mm2The tensile strength of the joint for 45# steel is 352 MPa, the tensile strength of the joint for H62 brass is 321 MPa, and the microhardness of the brazing filler metal is 162 HV 0.2.
Example 7: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 19.0%, Zn: 32.3%, Sn: 3.0%, Ni: 1.5%, In: 2.0%, X: 0.2% and the balance of Cu, wherein the alloy element X in the example is P: 0.195%, Ce: 0.005 percent. The solidus temperature is 690 ℃, the liquidus temperature is 774 ℃, and the unit spread area on pure copper is 4.17 mm2The tensile strength of the joint for 45# steel is 385 MPa, the tensile strength of the joint for H62 brass is 340 MPa, and the microhardness of the brazing filler metal is 220 HV 0.2.
Example 8: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 21.0%, Zn: 33.3%, Sn: 1.5%, Ni: 1.0%, In: 2.5%, X: 0.3%, and the balance being Cu, wherein the alloy element X in the example is P: 0.29%, La: 0.01 percent. The solidus temperature was 646 ℃ and the liquidus temperature was 780 ℃ and the unit spread area on pure copper was 3.62 mm2The tensile strength of the joint for 45# steel is 372 MPa, the tensile strength of the joint for H62 brass is 345 MPa, and the microhardness of the brazing filler metal is 167 HV 0.2.
Example 9: according to the mass percentage, the components of the low-melting-point cadmium-free manganese-free low-silver solder alloy are selected as follows:
ag: 21.0%, Zn: 33.3%, Sn: 2.5%, Ni: 1.5%, In: 2.0%, X: 0.3%, and the balance being Cu, wherein the alloy element X in the example is P: 0.285%, La: 0.01%, Ce: 0.005 percent. The solidus temperature was 634 ℃ and the liquidus temperature was 776 ℃ and the area of spread was 4.81 mm in units on pure copper2The tensile strength of the joint for 45# steel is 390 MPa, the tensile strength of the joint for H62 brass is 356 MPa, and the microhardness of the brazing filler metal is 230 HV 0.2.
Comparative example 1:
the brazing filler metal alloy comprises the following components in percentage by mass:
ag: 26.0%, Zn: 33%, Sn: 1.5%, In: 2.5 percent and the balance of Cu, wherein the solidus temperature is 662 ℃, the liquidus temperature is 767 ℃, and the unit spreading area on the pure copper is 4.97 mm2The tensile strength of the joint for 45# steel is 396 MPa, the tensile strength of the joint for H62 brass is 351 MPa, and the microhardness of the brazing filler metal is 194 HV 0.2.
Compared with the comparative example, the examples have the ingredient formula with lower material cost, and each performance index is close to or even superior to the comparative example. As In example 3, the total content of Ag, Ni and In, which are noble metals, is 23%, the comparative example is 28.5%, and after 0.8% of the alloy element combination X is added, the solidus and liquidus temperatures are lower than those of the comparative example, the spreading performance and microhardness are better than those of the comparative example, and the joint strength is similar.
Compared with the existing BAg26CuZnSnIn silver solder, the silver solder has the advantages that the silver solder does not contain toxic element cadmium, the content of noble metal silver (indium) is reduced, the melting temperature range, the wetting spreading performance and the brazing seam mechanical property which are similar to those of the BAg26CuZnSnIn solder are obtained, in the actual production, the solder can be used for obtaining a welding wire with the diameter of 0.8mm through a drawing process, a welding ring is easy to manufacture, the BAg26CuZnSnIn solder is expected to be replaced, and the production cost is reduced by 10-20%, so that the technical scheme of the application has advancement.
The following are specific data in the examples of the present application:
note: 1. the melting temperature of the brazing filler metal is measured according to GB/T1425-1996 'test method for measuring the melting temperature range of the precious metal and the alloy thereof by thermal analysis';
2. the spreading experiment is carried out according to GB/T11363-: keeping the temperature for 10 s after the brazing filler metal is melted at 850 ℃;
3. the base materials of 45# -45# steel and H62-H62 brass are used for oxygen-acetylene flame brazing, the joint tensile strength test is carried out according to the regulations of GB/T11363-. The sample of the 45# steel is broken at the joint position after being stretched, and the sample of the H62 brass is broken at the base material position after being stretched.
4. The hardness test is carried out according to the regulations of GB/T27552-.
All simple variations and combinations of the technical features and technical solutions of the present application are considered to fall within the scope of the present application. .
Claims (4)
1. The low-silver cadmium-free manganese-free multi-element silver solder with low melting point and high strength is characterized by comprising 19-23% of silver, 32-35% of zinc, 1.0-3.0% of tin, 0-2.0% of nickel, 0-3.0% of indium, 0.01-1.0% of alloy elements and the balance of copper, wherein the alloy elements contain one or more of phosphorus, lanthanum and cerium.
2. The low melting point, high strength, low silver, cadmium-free, manganese-free silver brazing filler metal of claim 1, wherein: the alloy elements comprise, by mass, 0.2-1% of phosphorus, 0-0.02% of lanthanum and 0-0.01% of cerium.
3. A preparation method of low-silver cadmium-free manganese-free multi-element silver solder with low melting point and high strength is characterized by comprising the following steps:
s1: heating copper in the Cu-X alloy in a crucible of an intermediate frequency smelting furnace to be completely melted, and adding alloy metal X until the Cu-X alloy is completely melted;
s2: adding silver, zinc, tin, nickel and indium with the purity of at least 99.99 percent and the rest part except copper in the Cu-X alloy into a crucible of a medium-frequency smelting furnace containing the melted Cu-X alloy according to the component proportion of the low-silver cadmium-free manganese-free multi-element silver brazing filler metal for smelting and casting;
s3: and (5) carrying out subsequent treatment.
4. The method for preparing the low-melting-point high-strength low-silver cadmium-free manganese-free multi-element silver solder as claimed in claim 3, which is characterized in that: the copper in the Cu-X is 0.01-10 g.
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Cited By (3)
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|---|---|---|---|---|
| CN113843546A (en) * | 2021-09-23 | 2021-12-28 | 金华市金钟焊接材料有限公司 | CuPSnAg Ni-Re ultra-silver solder, preparation method and application |
| CN114473292A (en) * | 2021-12-30 | 2022-05-13 | 郑州机械研究所有限公司 | Low-silver brazing filler metal for welding pure-silver jewelry and preparation method thereof |
| CN114850729A (en) * | 2022-03-25 | 2022-08-05 | 郑州机械研究所有限公司 | Cadmium-free silver brazing material |
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| CN106181123A (en) * | 2016-08-19 | 2016-12-07 | 佛山晓世科技服务有限公司 | A kind of low silver middle temperature brazing material |
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