CN101693325A - High-toughness cadmium-free silver solder and preparation method thereof - Google Patents
High-toughness cadmium-free silver solder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-toughness cadmium-free silver solder and a preparation method thereof. The solder comprises the following materials by weight percent: 22-58 percent of Ag, 15-35 percent of Cu, 13-38 percent of Zn, 4-8 percent of Mn, 1.5-5 percent of Ni, 0.8-3 percent of Co, 0.01-0.45 percent of B, 0-1.5 percent of V, 0-1.5 percent of Nb, 0.005-0.9 percent of Ce, 0.005-0.9 percent of La and 0-0.5 percent of Sr. The preparation method comprises the following steps of smelting the metal with high-melting point and partial copper into a preliminary alloy A, smelting oxidized metal and partial copper in a vacuum furnace into a preliminary alloy B, smelting silver and the remained copper in an intermediate-frequency furnace and then adding the preliminary alloy A, adding metals of manganese and zinc and then adding the preliminary alloy B after complete fusion, fusing completely again and standing for 60 minutes, and casting to form a silver alloy ingot, performing even annealing and scaling on the alloy ingot, extruding the alloy into a stripe shape or a bar shape by an isothermal extrusion method, and then rolling into a band or drawing and reducing to a filament.
Description
Technical field
The present invention relates to a kind of welding material, relate to a kind of high-toughness cadmium-free silver solder that diamond compact (PDC) and cubic boron nitride composite sheet (PCBN) are welded and preparation method thereof that is specially adapted to specifically.
Background technology
Diamond compact (PDC) and the application of cubic boron nitride composite sheet (PCBN) in industrial production and social life are increasingly extensive, because its hardness height, wearability are good, thermal conductivity and mar proof are good, PDC and the PCBN important function in the modern industry material is irreplaceable.At aspects such as oil drilling, geologic prospect, coal digging, machining, automobile preparation, manufacture of cement, aluminium alloy processing, electronic chip, rubber plastic engineering, daily necessitiess, in order to reduce cost, to improve effect, strengthening safety, PDC and PCBN superhard material have been obtained gratifying achievements.
The extensive use of PDC and PCBN depends on the development of soldering tech to a great extent.The welding of PDC and PCBN is difficulty relatively, is difficult to be welded on the application that has limited PDC and PCBN to a certain extent.Soldering processes are generally adopted in the welding of PDC and PCBN, the extremely individual laser braze welding technology that else adopts.The subject matter that exists in PDC and the PCBN soldering is because the high-wearing feature of PDC and PCBN, extra long life and middle low temperature brazing high temperature use a series of contradictions of bringing.PDC and PCBN are difficult to wetting, must keep relative low temperature again during soldering, weld seam must have high-temp and high-strength, high temperature high tenacity and good anti-fatigue performance, brazed seam ratio of brazing area height, brazed seam inside must not have be mingled with pore, brazed seam surface must not wrinkle skin, defective such as band sand holes.
For elevated temperature strength, high temperature toughness and the anti-fatigue performance that improves brazed seam, adopting the solder that contains a large amount of nickel, manganese element is the key of resolving contradiction.Prepare company and developed several typical special-purpose solders for solving the top solder in this difficult problem whole world.4900 compositions of the Degussa company exploitation of Germany are Ag49Cu16Zn23Ni4.5Mn7.5, the Handy﹠amp of the U.S.; The composition of the Braze495 of Harman company exploitation is close with it, the composition of the Safety-silv60T that the Harris company of the U.S. produces is Ag60Cu29Ni3Mn6, the BAg24 composition that the Belgian Umicore of international non-ferrous metal big fish company promotes mainly is Ag50Cu20Zn28Ni2, and the composition of the main product 1245 of U.S.'s lucky star (Fusion) company is Ag50Cu15.5Zn15.5Cd16Ni3.Above-mentioned solder all is to add nickel manganese cadmium etc. on the Ag-Cu-Zn basis.These solders have can solve the brazed seam strength problem but toughness and fatigue strength are low, but what have can solve brazed seam intensity, toughness, fatigue problem brazing temperature height, and can solve intensity, toughness, fatigue and the brazing temperature problem that have still contain the harmful element cadmium comprehensively.
Summary of the invention
Purpose of the present invention provides a kind of PDC and PCBN weld strength, toughness, fatigue and brazing temperature problem of can comprehensively solving at existing weak point in the above-mentioned prior art just, does not contain high-toughness cadmium-free silver solder of harmful element cadmium and preparation method thereof again.
Purpose of the present invention can realize by following technique measures:
High-toughness cadmium-free silver solder of the present invention comprises following weight percentages: silver-colored Ag:22～58%; Copper Cu:15～35%; Zinc Zn:13～38%; Manganese Mn:4～8%. Nickel: 1.5～5%; Cobalt Co:0.8～3%; Boron: 0.01～0.45%; Vanadium V:0～1.5%; Niobium Nb:0～1.5%; Cerium Ce:0.005～0.9%; Lanthanum La:0.005～0.9%; Strontium Sr:0～0.5%.
Preparation method of the present invention comprises the steps:
A, refractory metal nickel, cobalt Co, vanadium V, niobium Nb are smelted into intermediate alloy A1, A2, A3, A4 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A3 is by the Cu97 of weight ratio: V3 forms; Described intermediate alloy A4 is by the Cu98 of weight ratio: Nb2 forms;
B, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms;
C, the silver and the copper of surplus are melted in intermediate frequency furnace, temperature reaches and adds any or all of among intermediate alloy A1, A2, A3 or the A4 behind 1350K～1500k, fully merge the complex salt covering of back with dewatering borax and boric anhydride, add manganese metal, zinc again after the molten metal temperature dropped to 1250K～1400K, stop heating, when treating that metal fully merges back molten metal temperature and drops to 1150～1300K, add any or all of among intermediate alloy B1, B2, the B3; Wherein the weight ratio of dewatering borax and boric anhydride is 7: 3;
D, fully merge once more and left standstill 60 minutes, casting forms the silver alloy ingot casting, and cooldown rate is greater than 100K/S during the casting ingot casting; Alloy cast ingot homogenizing annealing 8 hours between 900K～1000K is taken crust off; Between 800K～873K, solder is squeezed into banded or bar-shaped with the isothermal extrusion; Banded alloy is through the rolling strip that is prepared into repeatedly, and the rolling pass working modulus is between 30～40%; Bar-shaped alloy becomes filament through rolling, drawing tube reducing, and the drawing passes working modulus is between 8～10%.
The present invention introduces Co on the alloy system basis of Ag, Cu, Zn, Ni, Mn, Co is the most excellent in all metals to the wetability of carbide alloy, and the elevated temperature strength of Co descends extremely slow, seldom add in the solder mainly is that interpolation difficulty, manufacturing technology are difficult to break through, solve similar problem in the past and often selected Pd for use, but the price of Pd is too high, generally only is used for military industrial technology, aerospace field or nuclear industry.And preparation method of the present invention can the alloy system that adds Ag, Cu, Zn, Ni, Mn to the Co success in, make the solder of acquisition have elevated temperature strength height, high temperature toughness height, feature that anti-fatigue performance is good.
For further improving the mechanical behavior under high temperature of high-toughness cadmium-free silver solder, micro-V, Nb have been added in the solder; For institutional framework, its crystal grain of refinement of improving high-toughness cadmium-free silver solder, purify its crystal boundary, reach the purpose that improves fatigue strength, also added trace elements such as B, Ce, La, Sr in the solder.
The existing beneficial effect fruit of serviceability of the present invention is as follows:
A, when high-toughness cadmium-free silver solder of the present invention is used for soldering PDC or PCBN, easy to operate, soldering efficient height, brazed seam intensity height, toughness height are arranged, characteristics such as fatigability is good, brazing temperature is low, the feature of environmental protection is good.When high-toughness cadmium-free silver solder is made the arrowband and is used for automatic induction brazing, can enhance productivity greatly.The combination property that this solder is used for soldering PDC or PCBN is better than domestic and international various solders at present.
B, high-toughness cadmium-free silver solder of the present invention also can be used for the soldering carbide alloy, compare with silver solder of the same type, and solder brazing efficient height, brazed seam intensity height, toughness height, fatigability is good, brazing temperature is low, the feature of environmental protection is good.But compare with copper base solder, brazing cost is higher, but compares high many of its soldering efficient with copper base solder, has that pore is few, slag inclusion is few, the weld seam high reliability features simultaneously again.
C, high-toughness cadmium-free silver solder of the present invention also can be used for the soldering steel or stainless steel, compare the still old soldering efficient of solder height, brazed seam intensity height, toughness height, distinguishing feature such as fatigability is good, brazing temperature is low, the feature of environmental protection is good with the silver solder with content.But the brazing cost of this class solder is higher, and this mainly is that conventional silver-base solder contains cadmium, thereby has improved brazing manufacturability.And cadmium is disabled in the electrical engineering and electric apparatus field in the whole world, and along with sustainable development and green manufacturing are paid attention to by people, containing the cadmium solder will be forbidden by large tracts of land gradually.
The specific embodiment
Embodiment 1
A, get by weight percentage: Ag:25%; Cu:32%; Zn:35%; Ni:2%; Co:1%; Mn:4.75%; B:0.01%; Nb:0.01%; V:0.01%; Ce:0.06%; La:0.09%; Sr:0.07%;
B, refractory metal nickel, cobalt Co, vanadium V, niobium Nb are smelted into intermediate alloy A1, A2, A3, A4 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A3 is by the Cu97 of weight ratio: V3 forms; Described intermediate alloy A4 is by the Cu98 of weight ratio: Nb2 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms;
D, silver and remaining copper are melted in intermediate frequency furnace, temperature adds intermediate alloy A after reaching 1350K～1500k, fully merge the complex salt covering of back with dewatering borax and boric anhydride, add manganese metal Mn, zinc Zn again after the molten metal temperature dropped to 1250K～1400K, stop heating, treat that metal fully merges when afterwards the molten metal temperature drops to 1150～1300K, adds intermediate alloy B; Wherein the weight ratio of dewatering borax and boric anhydride is 7: 3;
E, fully merge once more and left standstill 60 minutes, casting forms the silver alloy ingot casting, and cooldown rate is greater than 100K/S during the casting ingot casting; Alloy cast ingot homogenizing annealing 8 hours between 900K～1000K is taken crust off; Between 800K～873K, solder is squeezed into banded or bar-shaped with the isothermal extrusion; Banded alloy is through the rolling strip that is prepared into repeatedly, and the rolling pass working modulus is between 30～40%; Bar-shaped alloy becomes filament through rolling, drawing tube reducing, and the drawing passes working modulus is between 8～10%.
In following examples (2-8) except that step a, b, c and embodiment 1 have part different, all the other steps are all identical with embodiment 1.
Embodiment 2
A, get by weight percentage: Ag:30%; Cu:26%; Zn:34%; Ni:2%; Co:2%; Mn:5.8%; B:0.01%; V:0.01%; Sr:0.08%; Ce:0.04%; La:0.06%;
B, refractory metal nickel, cobalt Co, vanadium V are smelted into intermediate alloy A1, A2, A3 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A3 is by the Cu97 of weight ratio: V3 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms.
Embodiment 3
Get by weight percentage: Ag:35%; Cu:22%; Zn:32.5%; Ni:1.5%; Co:2%; Mn:6.74%; B:0.01%; Nb:0.01%; Ce:0.06%; La:0.09%; Sr:0.09%;
B, refractory metal nickel, cobalt Co, niobium Nb and copper Cu are smelted into intermediate alloy, refractory metal nickel, cobalt Co, niobium Nb are smelted into intermediate alloy A1, A2, A4 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A4 is by the Cu98 of weight ratio: Nb2 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms.
Embodiment 4
A, get by weight percentage: Ag:40%; Cu:21%; Zn:31%; Ni:1%; Co:1%; Mn:5.7%; B:0.01%; V:0.04%; Ce; 0.06%; La:0.09%; Sr:0.1%;
B, refractory metal nickel, cobalt Co, vanadium V are smelted into intermediate alloy A1, A2, A3 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A3 is by the Cu97 of weight ratio: V3 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms.
Embodiment 5
A, get by weight percentage: Ag:45%; Cu:22%; Zn:23%; Ni:2%; Co:2%; Mn:5.70%; B:0.01%; Ce:0.06%; La:0.09%; Sr:0.14%;
B, refractory metal nickel, cobalt Co are smelted into intermediate alloy A1, A2 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms.
Embodiment 6
A, get by weight percentage: Ag:49%; Cu:17%; Zn:23%; Ni:3%; Co:1.5%; Mn:6.35%; B:0.01%; Sr:0.14%;
B, refractory metal nickel, cobalt Co are smelted into intermediate alloy A1, A2 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms;
C, easy oxidation metal boron, strontium Sr are smelted into intermediate alloy B1, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms.
Embodiment 7
A, get by weight percentage: Ag:50%; Cu:17%; Zn:22%; Ni:2.5%; Co:2%; Mn:6.34%; B:0.01%; V:0.05%; Ce:0.04%; La:0.06%;
B, refractory metal nickel, cobalt Co, vanadium V are smelted into intermediate alloy A1, A2, A3 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A3 is by the Cu97 of weight ratio: V3 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La are smelted into intermediate alloy B1, B2 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms.
Embodiment 8
A, get by weight percentage: Ag:55%; Cu:21%; Zn:15%; Ni:2%; Co:2%; Mn:4.88%; B:0.02%; Ce:0.04%; La:0.06%;
B, refractory metal nickel, cobalt Co are smelted into intermediate alloy A1, A2 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms;
C, easy oxidation metal boron, cerium Ce and lanthanum La are smelted into intermediate alloy B1, B2 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms.
Claims (2)
1. high-toughness cadmium-free silver solder, it is characterized in that: described solder comprises following weight percentages: silver-colored Ag:22～58%; Copper Cu:15～35%; Zinc Zn:13～38%; Manganese Mn:4～8%; Nickel: 1.5～5%; Cobalt Co:0.8～3%; Boron: 0.01～0.45%; Vanadium V:0～1.5%; Niobium Nb:0～1.5%; Cerium Ce:0.005～0.9%; Lanthanum La:0.005～0.9%; Strontium Sr:0～0.5%.
2. preparation method who is used for the described solder of claim 1, it is characterized in that: described preparation method comprises the steps:
A, refractory metal nickel, cobalt Co, vanadium V, niobium Nb are smelted into intermediate alloy A1, A2, A3, A4 with copper Cu respectively; Described intermediate alloy A1 is by the Cu50 of weight ratio: Ni50 forms; Described intermediate alloy A2 is by the Cu70 of weight ratio: Co30 forms; Described intermediate alloy A3 is by the Cu97 of weight ratio: V3 forms; Described intermediate alloy A4 is by the Cu98 of weight ratio: Nb2 forms;
B, easy oxidation metal boron, cerium Ce and lanthanum La, strontium Sr are smelted into intermediate alloy B1, B2, B3 with copper Cu respectively in vacuum drying oven; Described intermediate alloy B1 is by the Cu86 of weight ratio: B14 forms; Described intermediate alloy B2 is by the Cu80 of weight ratio: La12+Ce8 forms; Described intermediate alloy B3 is by the Cu80 of weight ratio: Sr20 forms;
C, the silver and the copper of surplus are melted in intermediate frequency furnace, temperature reaches and adds any or all of among intermediate alloy A1, A2, A3 or the A4 behind 1350K～1500k, fully merge the complex salt covering of back with dewatering borax and boric anhydride, add manganese metal, zinc again after the molten metal temperature dropped to 1250K～1400K, stop heating, when treating that metal fully merges back molten metal temperature and drops to 1150～1300K, add any or all of among intermediate alloy B1, B2, the B3; Wherein the weight ratio of dewatering borax and boric anhydride is 7: 3;
D, fully merge once more and left standstill 60 minutes, casting forms the silver alloy ingot casting, and cooldown rate is greater than 100K/S during the casting ingot casting; Alloy cast ingot homogenizing annealing 8 hours between 900K～1000K is taken crust off; Between 800K～873K, solder is squeezed into banded or bar-shaped with the isothermal extrusion; Banded alloy is through the rolling strip that is prepared into repeatedly, and the rolling pass working modulus is between 30～40%; Bar-shaped alloy becomes filament through rolling, drawing tube reducing, and the drawing passes working modulus is between 8～10%.
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