CN102554509B - Vacuum brazing solder and process of Mo-Cu alloy and stainless steel - Google Patents
Vacuum brazing solder and process of Mo-Cu alloy and stainless steel Download PDFInfo
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- CN102554509B CN102554509B CN 201210043379 CN201210043379A CN102554509B CN 102554509 B CN102554509 B CN 102554509B CN 201210043379 CN201210043379 CN 201210043379 CN 201210043379 A CN201210043379 A CN 201210043379A CN 102554509 B CN102554509 B CN 102554509B
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Abstract
The invention relates to a vacuum brazing solder and a process of Mo-Cu alloy and stainless steel. The process comprises the steps of placing BNi2 amorphous alloy solder between preprocessed Mo-Cu alloy and surface to be brazed of austenitic stainless steel, controlling the joint gap between 40-80mum, gently placing the assembled Mo-Cu alloy and the stainless steel at a uniform temperature zone in a vacuum brazing furnace, vacuumizing and brazing, wherein the BNi2 amorphous alloy solder comprises the components in percentage by mass: 6.5-7.5% of Cr, 3.0-5.0% of Si, 2.7-3.5% of B, 2.5-3.5% of Fe, less than or equal to 0.02% of C and the balance of Ni. The Mo-Cu alloy and stainless steel joint obtained by the process disclosed by the invention have the advantages of little impurity, high density, strong high temperature resisting ability and the like and can be used for manufacturing instrument and meter elements, electronic packaging and high temperature resisting devices.
Description
Technical field
The present invention relates to a kind of molybdenum-copper and stainless soldering processes, particularly a kind of method that adopts amorphous filler metal molybdenum-copper and stainless steel to be carried out vacuum brazing belongs to the foreign material welding technology field.
Background technology
Molybdenum-copper has higher thermal conductivity factor and lower thermal coefficient of expansion reaches preferably heat resistance, therefore is of use in many ways.Its high thermal conductivity factor has preferably future as high-power electronic device and radiating element; The low seal, sealing materials that can be used as of its coefficient of expansion; Its good heat resistance can be used as high-temperature component etc.But when molybdenum-copper and stainless steel welding, because between the two thermal coefficient of expansion and the capacity of heat transmission differ larger, the joint easily produces very large stress, increases the crackle tendency.And molybdenum-copper is responsive to gaseous impurity, and the joint easily produces pore, seam organization thick (200～500 μ m), and when joint cooled off fast, interstitial impurity also can form segregation at crystal boundary.Therefore, the pollution of gaseous impurity and seam organization alligatoring are the subject matter that molybdenum-copper and austenitic stainless steel welding face.
At present, welding in vacuum or protective atmosphere is to suppress molybdenum-copper to be polluted preferably approach by gaseous impurity.Adopt molybdenum manganese metal method for brazing to Mo-Cu composite and Al such as Beijing vacuum electronic technical research institute
2O
3Pottery carries out sealing-in, and the joint performance of acquisition meets the instructions for use of HIGH-POWERED MICROWAVES component vacuum tubulation; University of Science ﹠ Technology, Beijing adopts the Ag-Cu-Ti solder that Mo-Cu composite and AlN pottery are carried out brazing in controlled atmosphere, and solder and mother metal have preferably wetability; Shandong University adopts the tungsten argon arc soldering method that molybdenum-copper and austenitic stainless steel are welded.These methods can suppress the pollution of external gaseous impurity, obtain the higher seam organization of purity.But in order to obtain the welding point of high-compactness, utilize that amorphous filler metals fusion temperature scope is extremely narrow, fusing time is extremely short, have the characteristics of good moment flowability, molybdenum-copper and stainless steel are carried out vacuum brazing, can obtain fine and close high-strength joint.The patent No. is that 2010105280034 Chinese patent discloses and a kind ofly carries out molybdenum-copper and stainless vacuum brazing technique with the Cu-Mn-Co brazing filler metal, compare with amorphous filler metals, Cu-Mn-Co brazing filler metal fusion temperature wider range, the temperature retention time that needs is longer, is unfavorable for improving welding production efficiency.
Summary of the invention
The objective of the invention is for the deficiencies in the prior art, and provide a kind of molybdenum-copper and stainless vacuum brazing solder and technique, this kind process using amorphous filler metals is carried out vacuum brazing with molybdenum-copper and austenitic stainless steel and is connected, not only avoid the processing procedure of the molybdenum-copper nickel preplating that relates in other soldering processes, need not again to add brazing flux.Therefore, these soldering processes have the characteristics such as flexible operation is simple, cost is low, easy to utilize, are particularly useful for the welding of molybdenum-copper and austenitic stainless steel, also can be used for the welding of molybdenum-copper and other low-alloy steel, heat resisting steel.
A kind of molybdenum-copper and stainless vacuum brazing solder, its mass percent consists of: Cr 6.5～7.5%, and Si 3.0～5.0%, and B 2.7～3.5%, and Fe 2.5～3.5%, C≤0.02%, Ni surplus.
A kind of molybdenum-copper and stainless vacuum brazing technique may further comprise the steps:
(1) molybdenum-copper and stainless steel are carried out surface treatment, remove oxide-film and foreign matter;
(2) be that the foil-like BNi2 amorphous filler metals of 50～80 μ m places between pretreated molybdenum-copper and the austenitic stainless steel welding surface with thickness, then assemble, the control play movement is between 40～80 μ m, the mass percent of BNi2 amorphous filler metals consists of: Cr 6.5～7.5%, Si 3.0～5.0%, and B 2.7～3.5%, and Fe 2.5～3.5%, C≤0.02%, the Ni surplus;
(3) place gently the uniform temperature zone in the vacuum brazing furnace to vacuumize soldering molybdenum-copper and the stainless steel that assembles.
Molybdenum-copper and stainless steel carried out surface treatment step be described in the above-mentioned steps (1): first molybdenum-copper and stainless steel surfaces are adopted the SiC coated abrasive working of 800#, remove the oxide-film on surface; Then molybdenum-copper and stainless steel part are placed on respectively ultrasonic cleaning 20～30min in the acetone, hot-air seasoning.
The soldering that vacuumizes described in the above-mentioned steps (3) places uniform temperature zone in the vacuum brazing furnace gently for molybdenum-copper that will assemble and stainless steel, shuts the vacuum brazing stove evacuation, reaches 1.33 * 10 to vacuum
-4～1.33 * 10
-3Heat during Pa, then preferably follow these steps to soldering:
1) makes the vacuum drying oven linear temperature increase, make furnace temperature at the uniform velocity be raised to 850 ℃ with 50min;
2) carry out phase I insulation 20min, the deflation course of workpiece mother metal and solder can fully be carried out, the hot stage soldering oven can be kept higher vacuum after being convenient to;
3) the phase I insulation is rapidly heated after finishing, and in 20min furnace temperature at the uniform velocity is raised to 1030 ℃ from 850 ℃;
4) after furnace temperature reaches 1030 ℃, carry out second stage insulation 15min, in order to avoid excessive thermal inertia, guarantee temperature-controlled precision;
5) after the second stage insulation finishes, in 15min, furnace temperature is at the uniform velocity risen to 1090 ℃ ± 10 ℃ from 1030 ℃;
6) when furnace temperature reaches 1090 ℃ ± 10 ℃, carry out phase III insulation 10min, in order to guarantee the solder diffusion fully, and take into account the difference of Heating Zone Temperature;
7) after the phase III, insulation finished, the vacuum brazing furnace stopped heating cooled off naturally with stove;
When 8) treating that the vacuum chamber temperature is cooled to below 100 ℃, take out weldment.
The present invention adopts the direct rapid melting of BNi2 amorphous filler metals and wetting realization molybdenum-copper and stainless vacuum brazing.Its soldering operation principle is: the BNi2 amorphous filler metals of utilizing flash set technology preparation (rapid solidification preparation method is existing mature technology), have very large degree of supercooling and solid liquid interface fltting speed, enlarged solid solubility limit, suppress the formation of equilibrium phase, make the solder chemical composition even, segregation significantly reduces, and because the fusion temperature scope extremely narrow (970 ℃～1000 ℃) of BNi2 amorphous filler metals, fusing time is extremely short, thereby it is mobile to have good moment, the capillary absorption function can be given full play to, thereby fine and close molybdenum-copper and stainless steel high-strength joint can be obtained.In addition, the Ni element can be dissolved in Cu, can be dissolved in Mo again, and can increase the solubility of solid-state molybdenum in liquid copper, therefore can improve preferably the wetability between liquid phase copper and the Mo in brazing process, increases the combination at molybdenum-copper and stainless steel braze welding interface.
Compare with fusion welding method, adopt soldering processes of the present invention, not only can reduce cooling velocity, reduce the generation tendency of compound between brittle metal; And welding is to carry out in a vacuum, can reduce the pollution of gaseous impurity, improves the degree of purity of weld seam; Simultaneously, adopt the uniform BNi2 amorphous filler metals of chemical composition, can improve the density of soldering interface.The shear strength that obtains molybdenum-copper and stainless steel adapting piece reaches 200～230MPa.
Compare with the Cu-Mn-Co brazing filler metal, adopt soldering processes of the present invention, can reduce the high temperature retention time, be conducive to improve welding efficiency, and the strength of joint that obtains is also higher.
The vacuum brazing temperature curve that the present invention adopts arranges three insulation platforms, and its effect is respectively: the one, and the deflation course of workpiece mother metal and solder can fully be carried out, be convenient to the hot stage soldering oven and can keep higher vacuum; The 2nd, make uniformity of temperature profile in the soldering oven, to guarantee accurately to control temperature; The 3rd, promote abundant fusing and the diffusion of solder, improve strength of joint.
Adopt technique of the present invention, the molybdenum-copper of acquisition and stainless joint have the advantages such as impurity is few, density is high, heat-resisting ability is strong, can be used for the manufacturing of Instrument Elements, Electronic Packaging, high temperature resistant device.
Description of drawings
Fig. 1 is molybdenum-copper of the present invention and stainless vacuum brazing technique temperature profile;
1. be warming up to 850 ℃; 2. be incubated 20min; 3. be warming up to 1030 ℃; 4. be incubated 15min; 5. be warming up to 1090 ℃ ± 10 ℃; 6. be incubated 10min; 7. cool off with stove.
The specific embodiment
Further specify below in conjunction with embodiment.
Embodiment 1:
The vacuum brazing of molybdenum-copper plate and 1Cr8Ni9Ti austenitic stainless steel banjo fixing butt jointing, molybdenum-copper consist of Mo60%-Cu40% (mass fraction), are of a size of 30mm * 8mm, and thickness is 2.5mm; Austenitic stainless steel is the 1Cr8Ni9Ti stainless steel, is of a size of 30mm * 10mm, and thickness is 3.0mm.
The first step, the stainless surface treatment of molybdenum-copper and 1Cr8Ni9Ti:
With the SiC coated abrasive working of molybdenum-copper and 1Cr8Ni9Ti stainless steel surfaces employing 800#, remove the oxide-film on surface first;
Then put into acetone, ultrasonic cleaning 30min, the taking-up oven dry is stand-by.
Second step, the stainless assembling of molybdenum-copper and 1Cr8Ni9Ti:
Be that (chemical composition is: Cr 6.5% for the foil-like BNi2 amorphous filler metals of 50 μ m with thickness, Si 5.0%, B 2.7%, Fe 3.5%, C≤0.02%, the Ni surplus places between pretreated molybdenum-copper and the 1Cr8Ni9Ti stainless steel welding surface by percentage to the quality), then assemble control play movement 40～60 μ m.
In the 3rd step, the molybdenum-copper that assembles and stainless steel are put into vacuum brazing furnace carry out soldering.Body of heater adopts tungsten bar to heat, and the working vacuum degree is 1.33 * 10
-5Pa, uniform temperature zone are of a size of 305mm * 305mm * 457mm, adopt heating in the Digital Program Control stove, insulation and temperature-fall period.
Assembly parts are placed uniform temperature zone in the vacuum brazing furnace gently, shut the vacuum brazing stove evacuation, reach 1.33 * 10 to vacuum
-3Heat during Pa.Carry out soldering according to the brazing process temperature curve of setting, its process is as follows:
1) makes the vacuum drying oven linear temperature increase, make furnace temperature at the uniform velocity be raised to 850 ℃ with 50min;
2) carry out phase I insulation 20min, the deflation course of workpiece mother metal and solder can fully be carried out, the hot stage soldering oven can be kept higher vacuum after being convenient to;
3) the phase I insulation is rapidly heated after finishing, and in 20min furnace temperature at the uniform velocity is raised to 1030 ℃ from 850 ℃;
4) after furnace temperature reaches 1030 ℃, carry out second stage insulation 15min, in order to avoid excessive thermal inertia, guarantee temperature-controlled precision;
5) after the second stage insulation finishes, in 15min, furnace temperature is at the uniform velocity risen to 1100 ℃ from 1030 ℃;
6) when furnace temperature reaches 1100 ℃, carry out phase III insulation 10min, in order to guarantee the solder diffusion fully, and take into account the difference of Heating Zone Temperature;
7) after the phase III, insulation finished, the vacuum brazing furnace stopped heating cooled off naturally with stove;
When 8) treating that the vacuum chamber temperature is cooled to below 100 ℃, take out weldment.
The molybdenum-copper and the 1Cr8Ni9Ti stainless steel butt braze appearance of weld that obtain are attractive in appearance, and solder is good to molybdenum-copper and 1Cr8Ni9Ti stainless steel surfaces wetability.Do not find microfissure, the defective such as be mingled with through the metallography microscope sem observation, the brazing area interface is in conjunction with good, and shearing strength of joint reaches 210MPa.
Embodiment 2
The vacuum brazing of molybdenum-copper plate and corrosion resistant plate lap joint, molybdenum-copper consist of Mo50%-Cu50% (mass fraction), are of a size of 30mm * 8mm, and thickness is 2.5mm; Austenitic stainless steel is the 1Cr8Ni9Ti stainless steel, is of a size of 30mm * 10mm, and thickness is 3.0mm.
The first step, molybdenum-copper and stainless surface treatment:
With the SiC coated abrasive working of molybdenum-copper and 1Cr8Ni9Ti stainless steel surfaces employing 800#, remove the oxide-film on surface first;
Then put into acetone ultrasonic cleaning 25min, hot-air seasoning.
Second step, molybdenum-copper and stainless assembling:
Be that (chemical composition is: Cr 7.5% for the foil-like BNi2 amorphous filler metals of 70 μ m with thickness, Si 3.0%, B 3.5%, Fe 2.5%, C≤0.02%, the Ni surplus places between pretreated molybdenum-copper and the 1Cr8Ni9Ti stainless steel welding surface by percentage to the quality), then assemble control play movement 40～60 μ m.
In the 3rd step, the molybdenum-copper that assembles and stainless steel are put into vacuum brazing furnace carry out soldering.Body of heater adopts tungsten bar to heat, and the working vacuum degree is 1.33 * 10
-5Pa, uniform temperature zone are of a size of 305mm * 305mm * 457mm, adopt heating in the Digital Program Control stove, insulation and temperature-fall period.
Assembly parts are placed uniform temperature zone in the vacuum brazing furnace gently, shut the vacuum brazing stove evacuation, reach 1.33 * 10 to vacuum
-3Heat during Pa.Carry out soldering according to the brazing process temperature curve of setting, its process is as follows:
1) makes the vacuum drying oven linear temperature increase, make furnace temperature at the uniform velocity be raised to 850 ℃ with 50min;
2) carry out phase I insulation 20min, the deflation course of workpiece mother metal and solder can fully be carried out, the hot stage soldering oven can be kept higher vacuum after being convenient to;
3) the phase I insulation is rapidly heated after finishing, and in 20min furnace temperature at the uniform velocity is raised to 1030 ℃ from 850 ℃;
4) after furnace temperature reaches 1030 ℃, carry out second stage insulation 15min, in order to avoid excessive thermal inertia, guarantee temperature-controlled precision;
5) after the second stage insulation finishes, in 15min, furnace temperature is at the uniform velocity risen to 1090 ℃ from 1030 ℃;
6) when furnace temperature reaches 1090 ℃, carry out phase III insulation 10min, in order to guarantee the solder diffusion fully, and take into account the difference of Heating Zone Temperature;
7) after the phase III, insulation finished, the vacuum brazing furnace stopped heating cooled off naturally with stove;
When 8) treating that the vacuum chamber temperature is cooled to below 100 ℃, take out weldment.
The molybdenum-copper and the 1Cr8Ni9Ti stainless steel butt braze appearance of weld that obtain are attractive in appearance, and solder is good to molybdenum-copper and 1Cr8Ni9Ti stainless steel surfaces wetability.Do not find microfissure, the defective such as be mingled with through the metallography microscope sem observation, the brazing area interface is in conjunction with good, and shearing strength of joint reaches 230MPa.
Embodiment 3
Step is with embodiment 1, and the mass percent of BNi2 amorphous filler metals that different is consists of: Cr 6.8%, and Si 3.8%, and B 2.9%, and Fe 3.1%, C≤0.02%, Ni surplus.
The molybdenum-copper and the 1Cr8Ni9Ti stainless steel butt braze appearance of weld that obtain are attractive in appearance, and solder is good to molybdenum-copper and 1Cr8Ni9Ti stainless steel surfaces wetability.Do not find microfissure, the defective such as be mingled with through the metallography microscope sem observation, the brazing area interface is in conjunction with good, and shearing strength of joint reaches 225MPa.
Claims (2)
1. a molybdenum-copper and stainless vacuum brazing technique is characterized in that, may further comprise the steps:
(1) molybdenum-copper and stainless steel are carried out surface treatment, remove oxide-film and foreign matter;
(2) be that the foil-like BNi2 amorphous filler metals of 50～80 μ m places between pretreated molybdenum-copper and the austenitic stainless steel welding surface with thickness, then assemble, the control play movement is between 40～80 μ m, the mass percent of BNi2 amorphous filler metals consists of: Cr6.5～7.5%, Si3.0～5.0%, B2.7～3.5%, Fe2.5～3.5%, C≤0.02%, the Ni surplus;
(3) place gently the uniform temperature zone in the vacuum brazing furnace to vacuumize soldering molybdenum-copper and the stainless steel that assembles; Describedly vacuumize soldering and place gently uniform temperature zone in the vacuum brazing furnace for molybdenum-copper that will assemble and stainless steel, shut the vacuum brazing stove evacuation, reach 1.33 * 10 to vacuum
-4～1.33 * 10
-3Heat during Pa, then follow these steps to soldering:
1) makes the vacuum drying oven linear temperature increase, make furnace temperature at the uniform velocity be raised to 850 ℃ with 50min;
2) carry out phase I insulation 20min, the deflation course of workpiece mother metal and solder can fully be carried out, the hot stage soldering oven can be kept higher vacuum after being convenient to;
3) the phase I insulation is rapidly heated after finishing, and in 20min furnace temperature at the uniform velocity is raised to 1030 ℃ from 850 ℃;
4) after furnace temperature reaches 1030 ℃, carry out second stage insulation 15min, in order to avoid excessive thermal inertia, guarantee temperature-controlled precision;
5) after the second stage insulation finishes, in 15min, furnace temperature is at the uniform velocity risen to 1090 ℃ ± 10 ℃ from 1030 ℃;
6) when furnace temperature reaches 1090 ℃ ± 10 ℃, carry out phase III insulation 10min, in order to guarantee the solder diffusion fully, and take into account the difference of Heating Zone Temperature;
7) after the phase III, insulation finished, the vacuum brazing furnace stopped heating cooled off naturally with stove;
When 8) treating that the vacuum chamber temperature is cooled to below 100 ℃, take out weldment.
2. a kind of molybdenum-copper according to claim 1 and stainless vacuum brazing technique, it is characterized in that, molybdenum-copper and stainless steel carried out surface treatment step be described in the step (1): first molybdenum-copper and stainless steel surfaces are adopted the SiC coated abrasive working of 800#, remove the oxide-film on surface; Then molybdenum-copper and stainless steel part are placed on respectively ultrasonic cleaning 20～30min in the acetone, hot-air seasoning.
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