CN101704160B - Heterogeneous metal connecting method for tungsten, copper and alloy thereof - Google Patents

Heterogeneous metal connecting method for tungsten, copper and alloy thereof Download PDF

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Publication number
CN101704160B
CN101704160B CN2009102192984A CN200910219298A CN101704160B CN 101704160 B CN101704160 B CN 101704160B CN 2009102192984 A CN2009102192984 A CN 2009102192984A CN 200910219298 A CN200910219298 A CN 200910219298A CN 101704160 B CN101704160 B CN 101704160B
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tungsten
minutes
vacuum chamber
vacuum
copper
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CN101704160A (en
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杨建锋
李军
陈俊凌
乔冠军
鲍崇高
李春芳
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

The invention discloses a heterogeneous metal connecting method for tungsten, copper and alloy thereof, which comprises the following steps: firstly, processing the surface of tungsten metal and performing surface treatment; plating nickel to the tungsten metal, processing the surface of the tungsten metal, and cleaning the tungsten metal; then, processing and cleaning the copper alloy; and finally, overlapping and assembling the tungsten and the copper alloy to form weldment, and connecting the weldments in a vacuum chamber through pressure diffusion welding to form a connecting piece. The method has the remarkable characteristics that before vacuum diffusion welding connection for the tungsten and the copper, a layer of thin nickel is firstly electroplated on the surface of the tungsten metal, and then is subjected to vacuum diffusion welding with the copper alloy so as to implement diffusion connection of tungsten-copper heterogeneous metals. The method has the advantages of simple and convenient process operation, low cost and good connecting effect, and develops a new path for the connection of the tungsten-copper heterogeneous metals; and the shearing strength can reach 50 to 80 percent of a tungsten base material.

Description

A kind of tungsten and copper and diverse metal alloy method of attachment thereof
Technical field
The present invention relates to the method for attachment between dissimilar metal in the materials processing technology field, particularly a kind of tungsten and copper and diverse metal alloy method of attachment thereof.
Background technology
Tungsten (W) is exotic material because of advantage such as fusing point height, corrosion resistance be good and often be elected to be; As heat proof material, tungsten has special application in fields such as Aero-Space, the energy and electronics, as the lining of fuel nozzle, vacuum electron device anode etc.; Cu and alloy thereof be because of high heat conductance (400W/mK) characteristics, and often elect heat sink material as.Be connected with tungsten and can reach the reinforcement thermolysis.For this reason, the connector of tungsten and copper and alloy thereof is the first-selected composite structural member towards the plasma element.Because tungsten and the copper difference aspect mechanics and physical property, particularly difference of thermal expansion coefficients (α Cu=4 α w), will directly cause producing great residual stress in the joint, cause the fracture of joint in temperature-fall period.Tungsten and copper fusing point are widely different on the other hand, can not directly form metallurgical binding, thereby also are difficult to directly adopt the method for diffusion to connect.
Because the high residual stress that the tungsten copper connection procedure produces can influence the quality of joint, therefore,, improve the joint serviceability in order effectively to alleviate residual stress, tungsten copper often needs the intermediate layer when connecting.At present, W and the method for attachment of Cu alloy mainly are that soft metal Ni, Ti or the cupromanganese good with plasticity, that yield strength is lower carries out diffusion welding (DW) or active soldering as the intermediate layer.Its mechanism is to add the intermediate layer in the connection procedure and plastic deformation and creep by this intermediate layer come relieve stresses in diffusion.But, can't freely control owing to increase intermediate layer thickness, or interlayer surfaces deals with improperly, can cause can not realizing that with metal surface to be connected effective the diffusion is connected, form hidden defective, finally reduce the intensity of joint.In addition, also have a kind of intermediate layer to adopt tungsten copper FGM material (FGM), promptly adopt powder to mix the method that superposes with layering, make the linear expansion coefficient in intermediate layer carry out the transition to opposite side, thereby coupling is connected material by a side.Yet tungsten copper FGM material preparation process relative complex is used still very limited.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of tungsten and copper and diverse metal alloy method of attachment thereof, realize the connection of tungsten copper dissimilar metal,, have the advantage easy to operate, that cost is low, easy to utilize to obtain good tungsten copper diffusion jointing.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of tungsten and copper and diverse metal alloy method of attachment thereof may further comprise the steps:
One, polished to 1000~1500# with abrasive paper for metallograph in tungsten metal surface to be connected, be that 5%~10% hydrofluoric acid, weight concentration are that 5%~10% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic cleaning frequency is 20~30KHz, each cleaned 10~20 minutes, dried up, standby;
Two, the tungsten metal after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is at 3~10A/dm 2In the scope, electroplating time 20~40 minutes, thickness of coating is controlled at 10~30 μ m, and bath temperature remains on 50~70 ℃;
Three, to the tungsten metal surface after electroplating with the abrasive paper for metallograph polishing to 1000~1500#, be 5%~10% acetone ultrasonic cleaning 10~20 minutes with weight concentration afterwards, dry up, standby;
Four, copper metal surface to be connected being milled to 1000~1500# with sand paper, is 5%~10% acetone ultrasonic cleaning 10~20 minutes with weight concentration then, dries up, standby;
Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last.
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 100-170g/l; Magnesium sulfate 21-30g/l; Boric acid 14-30g/l; Sodium chloride 4-12g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and preferred water bath heating temperature is 50~70 ℃ during plating.
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 5Pa~0.3Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 3 * 10 -2Pa~3 * 10 -3Begin heating behind the Pa again, heating rate is 100~250 ℃/h, when treating that the vacuum chamber temperature is heated to 400~480 ℃, begins to be pressurized to 1~1.5MPa, continue to heat up when reaching 880~950 ℃, increase connection pressure to being 3~12MPa, relatively preferably connecting pressure is 5~10Mpa, temperature retention time 45~90 minutes, after temperature retention time finishes, workpiece slowly cools off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
At tungsten metal surface plating one deck nickel, THICKNESS CONTROL is at 10~30 μ m before diffusion connects in the present invention, and nickel has formed stronger adhesion in the tungsten metal surface, and then carries out vacuum with copper alloy and spread and be connected.The process characteristic of this connection: the one, tungsten plating nickel on surface layer plays the effect of transition zone in tungsten copper vacuum diffusion connection procedure, effectively alleviate residual stress, has improved the joint serviceability; The 2nd, galvanizer's artistic skill is effectively controlled the thickness of nickel coating, guarantees suitable transition zone, alleviates internal stress to greatest extent; The 3rd, before connecting, diffusion formed stronger adhesion between nickel and the tungsten metal, will in connecting, more can promote fully diffusion between the tungsten nickel metal with the final vacuum diffusion.
Electronickelling thickness and compactness are crucial.Therefore, under the condition that guarantees current density, the nickel plating time is long more, and nickel coating is even more, and thickness is big more; But in order to guarantee that the nickel coating THICKNESS CONTROL is between 10~30 μ m with diffusion fully between the metal level in the final vacuum diffusion connection procedure.If nickel plating thickness is too big, the intermetallic compound that generates fragility can too much can reduce the intensity of diffusion jointing on the contrary.
The characteristics that the present invention gives prominence to are: before tungsten copper vacuum diffusion connects, at first at the thin nickel of surface electroplating of metallic tungsten one deck, carry out the diffusion that vacuum diffusion welding realizes the tungsten copper dissimilar metal with copper alloy more subsequently and be connected.This method technological operation is easy, cost is low, good connecting effect, and shear strength can reach the 50-80% of tungsten mother metal, for tungsten is connected the new approach of having started with copper heterogenous metal.
The specific embodiment
Embodiment one
Present embodiment may further comprise the steps:
One, polish to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that will be of a size of 15mm * 7mm * 3mm, be that 5% hydrofluoric acid and weight concentration are that 5% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 20KHz, each cleaned 10 minutes, dried up, standby;
Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 5A/dm 2, electroplating time 30 minutes, thickness of coating is controlled at 22 μ m, and bath temperature remains on 60 ℃;
Three, polished to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, afterwards with being 5% acetone ultrasonic cleaning 15 minutes with weight concentration, dry up, standby;
Four, the CuCrZr alloy surface to be connected that will be of a size of 7mm * 6.5mm * 3mm is milled to 1200# with sand paper, then with being 5% acetone ultrasonic cleaning 15 minutes with weight concentration, dries up, standby;
Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 160g/l; Magnesium sulfate 26g/l; Boric acid 16g/l; Sodium chloride 10g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 60 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 5Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 3 * 10 -2Begin heating behind the Pa again, heating rate is 100 ℃/h, when treating that the vacuum chamber temperature is heated to 480 ℃, begin to be pressurized to 1MPa, continue to heat up when reaching 920 ℃, increase and connect pressure to 5MPa, be incubated 50 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
The connector that present embodiment makes, jointing can reach 166MPa through shearing test intensity, connects respond well.
Embodiment two
Present embodiment may further comprise the steps:
One, polish to 1000# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that will be of a size of 15mm * 6.5mm * 3mm, be that 10% hydrofluoric acid, weight concentration are that 10% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 25KHz, each cleaned 20 minutes, dried up, standby;
Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 8A/dm 2, electroplating time 25 minutes, thickness of coating is controlled at 15 μ m, and bath temperature remains on 65 ℃;
Three, polished to 1000# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, used the acetone ultrasonic cleaning afterwards 12 minutes, dry up, standby;
Four, the CuCrZr alloy surface to be connected that will be of a size of 6.5mm * 6.5mm * 3mm is milled to 1000# with sand paper, uses the acetone ultrasonic cleaning then 15 minutes, dries up, standby;
Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 110g/l; Magnesium sulfate 25g/l; Boric acid 20g/l; Sodium chloride 5g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 50 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 4 * 10 -1Pa starts diffusion pump then and makes the vacuum of vacuum chamber reach 1 * 10 -2Begin heating behind the Pa again, heating rate is 150 ℃/h, when treating that the vacuum chamber temperature is heated to 440 ℃, begin to be pressurized to 1.2MPa, continue to heat up when reaching 900 ℃, increase and connect pressure to 10MPa, be incubated 70 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
The connector that present embodiment makes, jointing can reach 173MPa through shearing test intensity, connects respond well.
Embodiment three
Present embodiment may further comprise the steps:
One, polish to 1500# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that will be of a size of φ 10mm * 3mm, be that 8% hydrofluoric acid, weight concentration are that 8% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 30KHz, and each cleaned 15 minutes, dries up, standby;
Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 5A/dm 2, electroplating time 25 minutes, thickness of coating is controlled at 18 μ m, and bath temperature remains on 70 ℃;
Three, being polished to 1500# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, is 8% acetone ultrasonic cleaning 10 minutes with weight concentration afterwards, dries up, standby;
Four, the CuCrZr alloy surface to be connected that will be of a size of φ 5mm * 3mm is milled to 1500# with sand paper, is 8% acetone ultrasonic cleaning 20 minutes with weight concentration then, dries up, standby;
Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 140g/l; Magnesium sulfate 30g/l; Boric acid 25g/l; Sodium chloride 8g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 55 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 1Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 7 * 10 -3Begin heating behind the Pa again, heating rate is 250 ℃/h, when treating that the vacuum chamber temperature is heated to 460 ℃, begin to be pressurized to 1.5MPa, continue to heat up when reaching 920 ℃, increase and connect pressure to 8MPa, temperature retention time 60 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
The connector that present embodiment makes, jointing can reach 187MPa through shearing test intensity, connects respond well.
Embodiment four
Present embodiment may further comprise the steps:
One, polish to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that will be of a size of φ 12mm * 3.5mm, be that 6% hydrofluoric acid, weight concentration are that 6% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 28KHz, and each cleaned 12 minutes, dries up, standby;
Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 10A/dm 2, electroplating time 20 minutes, thickness of coating is controlled at 12 μ m, and bath temperature remains on 55 ℃;
Three, polished to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, used the acetone ultrasonic cleaning afterwards 20 minutes, dry up, standby;
Four, the CuZn alloy surface to be connected that will be of a size of φ 6mm * 3.5mm is milled to 1200# with sand paper, is 6% acetone ultrasonic cleaning 15 minutes with weight concentration then, dries up, standby;
Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 170g/l; Magnesium sulfate 21g/l; Boric acid 18g/l; Sodium chloride 12g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 70 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 3Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 5 * 10 -3Begin heating behind the Pa again, heating rate is 200 ℃/h, when treating that the vacuum chamber temperature is heated to 440 ℃, begin to be pressurized to 1.3MPa, continue to heat up when reaching 880 ℃, increase and connect pressure to 12MPa, temperature retention time 45 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
The connector that present embodiment makes, jointing can reach 155MPa through shearing test intensity, connects respond well.
Embodiment five
Present embodiment may further comprise the steps:
One, polish to 1300# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that will be of a size of φ 12mm * 4mm, be that 9% hydrofluoric acid, weight concentration are that 9% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 22KHz, and each cleaned 15 minutes, dries up, standby;
Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 3A/dm 2, electroplating time 40 minutes, thickness of coating is controlled at 28 μ m, and bath temperature remains on 50 ℃;
Three, polished to 1300# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, used the acetone ultrasonic cleaning afterwards 12 minutes, dry up, standby;
Four, the QCr0.5 chromium-bronze alloy surface to be connected that will be of a size of φ 5mm * 3mm is milled to 1300# with sand paper, is 9% acetone ultrasonic cleaning 12 minutes with weight concentration then, dries up, standby;
Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 130g/l; Magnesium sulfate 28g/l; Boric acid 30g/l; Sodium chloride 4g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and preferred water bath heating temperature is 65 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 6 * 10 -1Pa starts diffusion pump then and makes the vacuum of vacuum chamber reach 3 * 10 -3Begin heating behind the Pa again, heating rate is 180 ℃/h, when treating that the vacuum chamber temperature is heated to 400 ℃, begin to be pressurized to 1~1.5MPa, continue to heat up when reaching 950 ℃, increase and connect pressure to 3MPa, temperature retention time 90 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
The connector that present embodiment makes, jointing can reach 168MPa through shearing test intensity, connects respond well.

Claims (8)

1. a tungsten and copper and diverse metal alloy method of attachment thereof, it is characterized in that, may further comprise the steps: one, polished to 1000~1500# with abrasive paper for metallograph in tungsten metal surface to be connected, be that 5%~10% hydrofluoric acid, weight concentration are that 5%~10% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 20~30KHz, each cleaned 10~20 minutes, dried up, standby; Two, the tungsten metal after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is at 3~10A/dm 2In the scope, electroplating time 20~40 minutes, thickness of coating is controlled at 10~30 μ m, and bath temperature remains on 50~70 ℃, and the prescription of described electroplate liquid is as follows: nickelous sulfate 100-170g/l, magnesium sulfate 21 1 30g/l, boric acid 14-30g/l, sodium chloride 4-12g/l; Three, to the tungsten metal surface after electroplating with the abrasive paper for metallograph polishing to 1000~1500#, be 5%~10% acetone ultrasonic cleaning 10~20 minutes with weight concentration afterwards, dry up, standby; Four, copper metal surface to be connected being milled to 1000~1500# with sand paper, is 5%~10% acetone ultrasonic cleaning 10~20 minutes with weight concentration then, dries up, standby; Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper, place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, described vacuum diffusion welding is: start mechanical pump earlier vacuum chamber is evacuated to 5Pa~0.3Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 3 * 10 -2Pa~3 * 10 -3Begin heating behind the Pa again, heating rate is 100~250 ℃/h, when treating that the vacuum chamber temperature is heated to 400~480 ℃, begin to be pressurized to 1~1.5MPa, continue to heat up when reaching 880~950 ℃, increase and connect pressure to 3~12MPa, temperature retention time 45~90 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
2. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof is characterized in that, electroplate liquid described in the step 2 is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 50~70 ℃ during plating.
3. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof is characterized in that, continue described in the step 5 to heat up when reaching 880~950 ℃, increase to connect pressure to 5~10MPa.
4. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof, it is characterized in that, may further comprise the steps: polish to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that, will be of a size of 15mm * 7mm * 3mm, be that 5% hydrofluoric acid and weight concentration are that 5% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 20KHz, each cleaned 10 minutes, dried up, standby; Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 5A/dm 2, electroplating time 30 minutes, thickness of coating is controlled at 22 μ m, and bath temperature remains on 60 ℃; Three, being polished to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, is 5% acetone ultrasonic cleaning 15 minutes with weight concentration afterwards, dries up, standby; Four, the CuCrZr alloy surface to be connected that will be of a size of 7mm * 6.5mm * 3mm is milled to 1200# with sand paper, is 5% acetone ultrasonic cleaning 15 minutes with weight concentration then, dries up, standby; Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 160g/l; Magnesium sulfate 26g/l; Boric acid 16g/l; Sodium chloride 10g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 60 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 5Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 3 * 10 -2Begin heating behind the Pa again, heating rate is 100 ℃/h, when treating that the vacuum chamber temperature is heated to 480 ℃, begin to be pressurized to 1MPa, continue to heat up when reaching 920 ℃, increase and connect pressure to 5MPa, be incubated 50 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
5. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof, it is characterized in that, may further comprise the steps: polish to 1000# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that, will be of a size of 15mm * 6.5mm * 3mm, be that 10% hydrofluoric acid and weight concentration are that 10% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 25KHz, each cleaned 20 minutes, dried up, standby; Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 8A/dm 2, electroplating time 25 minutes, thickness of coating is controlled at 15 μ m, and bath temperature remains on 65 ℃; Three, polished to 1000# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, used the acetone ultrasonic cleaning afterwards 12 minutes, dry up, standby; Four, the CuCrZr alloy surface to be connected that will be of a size of 6.5mm * 6.5mm * 3mm is milled to 1000# with sand paper, uses the acetone ultrasonic cleaning then 15 minutes, dries up, standby; Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 110g/l; Magnesium sulfate 25g/l; Boric acid 20g/l; Sodium chloride 5g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 50 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 4 * 10 -1Pa starts diffusion pump then and makes the vacuum of vacuum chamber reach 1 * 10 -2Begin heating behind the Pa again, heating rate is 150 ℃/h, when treating that the vacuum chamber temperature is heated to 440 ℃, begin to be pressurized to 1.2MPa, continue to heat up when reaching 900 ℃, increase and connect pressure to 10MPa, be incubated 70 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
6. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof, it is characterized in that, may further comprise the steps: polish to 1500# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that, will be of a size of φ 10mm * 3mm, be that 8% hydrofluoric acid and weight concentration are that 8% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 30KHz, each cleaned 15 minutes, dried up, standby; Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 5A/dm 2, electroplating time 25 minutes, thickness of coating is controlled at 18 μ m, and bath temperature remains on 70 ℃; Three, being polished to 1500# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, is 8% acetone ultrasonic cleaning 10 minutes with weight concentration afterwards, dries up, standby; Four, the CuCrZr alloy surface to be connected that will be of a size of φ 5mm * 3mm is milled to 1500# with sand paper, is 8% acetone ultrasonic cleaning 20 minutes with weight concentration then, dries up, standby; Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 140g/l; Magnesium sulfate 30g/l; Boric acid 25g/l; Sodium chloride 8g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 55 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 1Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 7 * 10 -3Begin heating behind the Pa again, heating rate is 250 ℃/h, when treating that the vacuum chamber temperature is heated to 460 ℃, begin to be pressurized to 1.5MPa, continue to heat up when reaching 920 ℃, increase and connect pressure to 8MPa, temperature retention time 60 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
7. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof, it is characterized in that, may further comprise the steps: polish to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that, will be of a size of φ 12mm * 3.5mm, be that 6% hydrofluoric acid and weight concentration are that 6% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 28KHz, each cleaned 12 minutes, dried up, standby; Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 10A/dm 2, electroplating time 20 minutes, thickness of coating is controlled at 12 μ m, and bath temperature remains on 55 ℃; Three, polished to 1200# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, used the acetone ultrasonic cleaning afterwards 20 minutes, dry up, standby; Four, the CuZn alloy surface to be connected that will be of a size of φ 6mm * 3.5mm is milled to 1200# with sand paper, is 6% acetone ultrasonic cleaning 15 minutes with weight concentration then, dries up, standby; Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 170g/l; Magnesium sulfate 21g/l; Boric acid 18g/l; Sodium chloride 12g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 70 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 3Pa, start diffusion pump then and make the vacuum of vacuum chamber reach 5 * 10 -3Begin heating behind the Pa again, heating rate is 200 ℃/h, when treating that the vacuum chamber temperature is heated to 440 ℃, begin to be pressurized to 1.3MPa, continue to heat up when reaching 880 ℃, increase and connect pressure to 12MPa, temperature retention time 45 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
8. a kind of tungsten according to claim 1 and copper and diverse metal alloy method of attachment thereof, it is characterized in that, may further comprise the steps: polish to 1300# with abrasive paper for metallograph in the industrial pure tungsten surface to be connected that, will be of a size of φ 12mm * 4mm, be that 9% hydrofluoric acid and weight concentration are that 9% acetone carries out ultrasonic cleaning successively then with weight concentration, the ultrasonic wave cleaning frequency is 22KHz, each cleaned 15 minutes, dried up, standby; Two, the industrial pure tungsten after polishing is cleaned in the step 1 is put into electroplate liquid, regulate current/voltage and electroplate, current density is 3A/dm 2, electroplating time 40 minutes, thickness of coating is controlled at 28 μ m, and bath temperature remains on 50 ℃; Three, polished to 1300# with abrasive paper for metallograph in the industrial pure tungsten surface after electroplating, used the acetone ultrasonic cleaning afterwards 12 minutes, dry up, standby; Four, the QCr0.5 chromium-bronze alloy surface to be connected that will be of a size of φ 5mm * 3mm is milled to 1300# with sand paper, is 9% acetone ultrasonic cleaning 12 minutes with weight concentration then, dries up, standby; Five, the tungsten after step 3 and step 4 are handled, to be connected the relative weldment that is superimposed as of copper alloy place the diffusion furnace vacuum chamber, carry out vacuum diffusion welding, obtain connector at last;
The prescription of electroplate liquid described in the step 2 is as follows: nickelous sulfate 130g/l; Magnesium sulfate 28g/l; Boric acid 30g/l; Sodium chloride 4g/l; Electroplate liquid is in the plating bath container, and the plating bath container places water-bath to heat, and water bath heating temperature is 65 ℃ during plating;
Vacuum diffusion welding described in the step 5 is: start mechanical pump earlier vacuum chamber is evacuated to 6 * 10 -1Pa starts diffusion pump then and makes the vacuum of vacuum chamber reach 3 * 10 -3Begin heating behind the Pa again, heating rate is 180 ℃/h, when treating that the vacuum chamber temperature is heated to 400 ℃, begin to be pressurized to 1~1.5MPa, continue to heat up when reaching 950 ℃, increase and connect pressure to 3MPa, temperature retention time 90 minutes, after temperature retention time finished, workpiece slowly cooled off with stove, when treating that the vacuum chamber temperature is cooled to below 100 ℃, can blow-on take out connector.
CN2009102192984A 2009-12-03 2009-12-03 Heterogeneous metal connecting method for tungsten, copper and alloy thereof Expired - Fee Related CN101704160B (en)

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