CN106517828B - It is a kind of that molybdenum group glass/kovar alloy laser soldering method is connected by addition Mo-Mn-Ni metal intermediate layer - Google Patents
It is a kind of that molybdenum group glass/kovar alloy laser soldering method is connected by addition Mo-Mn-Ni metal intermediate layer Download PDFInfo
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- CN106517828B CN106517828B CN201610951616.6A CN201610951616A CN106517828B CN 106517828 B CN106517828 B CN 106517828B CN 201610951616 A CN201610951616 A CN 201610951616A CN 106517828 B CN106517828 B CN 106517828B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/04—Joining glass to metal by means of an interlayer
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Abstract
It is a kind of that molybdenum group glass/kovar alloy laser soldering method is connected by addition Mo-Mn-Ni metal intermediate layer, belong to nonmetallic and metal material interconnection technique field.Include the following steps: glass purified treatment removing kovar alloy surface film oxide, carries out degreasing and go oil processing;Kovar alloy produces oxidation film in oxidation furnace;Mo-Mn-Ni metallic intermediate layer powder bed is produced by tablet press machine;Using " sandwich " welding structure, bottom glass, centre is Mo-Mn-Ni metallic intermediate layer powder, and top layer is kovar alloy, and three is put into furnace after being in close contact and preheats;Laser beam is radiated at kovar alloy surface, carries out laser welding;After welding, weldment is moved to rapidly and carries out stress relief annealing in heating furnace, cools to room temperature with the furnace.Present invention facilitates boundary moistures, reduce post-weld stress, improve strength of joint, while reducing production cost, improve the service life of product.
Description
Technical field
Molybdenum group glass/kovar alloy Laser Welding side is connected by addition Mo-Mn-Ni middle layer the present invention relates to a kind of
Method belongs to nonmetallic and metal material interconnection technique field.
Background technique
Glass material has the characteristics that high intensity, high hardness and corrosion resistance, excellent insulation performance, but the low of glass itself is prolonged
Malleability and poor impact flexibility limit its application in engineering.Thus the glass-of glass and metal excellent performance is combined
Metal composite structure is applied and gives birth to, and be widely used in microelectronics Packaging, battery, instrument, solar vacuum heat-collecting pipe etc.
Field.
Glass and metal welding are widely used in microelectronics Packaging, relay, solar vacuum heat-collecting pipe etc. and have vacuum gas
The occasion that close property requires.But strength of joint is low, and brittleness is big, is very limited in practical applications.Metal material and glass connect
The main problem connect is: (1) thermal expansion coefficient differs greatly, and stress is concentrated, and a large amount of micro-cracks occurs in postwelding, and joint performance is poor;(2)
Glass material is covalent bond mainly in combination with mode, and metal material is ionic bond and metallic bond mainly in combination with mode, and wetability is very
Difference, interface cohesion are difficult;(3) nonmetallic materials poor toughness is easy to happen fracture.Dissimilar material associative key difference leads to material machine
There are larger differences, such as metal material to have good plasticity and toughness and machinability for tool performance and physical property, and nonmetallic
Material fragility is larger, formd with nonmetallic materials it is complementary, therefore to developing a kind of reliable glass and metal joining techniques
Propose an urgent demand.
Glass and the traditional connection method of metal have anode linkage, soldering, friction welding (FW), electron beam welding, explosion weldering etc..But this
There is the defects of being easy aging, accuracy is low, intensity is low and stomata is more in a little methods.Relative to other welding methods, laser beam control
System is simple, it is easy to accomplish automation, Laser Welding can be with strict control heat input, and thermal deformation is smaller, and heat affected area is small, accuracy
Height, forming are fast;Solderable material category is wide and melt back does not occur, and postwelding weld grain is tiny, and weldquality is high;Relative to electricity
Beamlet welding, is not required to vacuum, is not required to X-ray protection, small to human body injury, and local lap adds in laser beam welding
Hot and cold but remains balance, and molten bath is highly stable.
Kovar alloy, also referred to as Fe-Co-Ni alloy, the alloy within the scope of 20-450 DEG C coefficient of linear thermal expansion be 5.1~
5.5×10-6K-1, molybdenum group glass DM308 is that coefficient of linear thermal expansion is 4.9~10 × 10 within the scope of 20-300 DEG C in temperature-6K-1,
The two similar thermal expansion coefficient at room temperature, can be effectively reduced post-weld stress, obtain good welding point.Suitable for microelectronics
Encapsulation, production relay, solar vacuum heat-collecting pipe etc..
Summary of the invention
It is an object of the present invention to provide one kind to connect molybdenum group glass/can cut down conjunction by addition Mo-Mn-Ni metal powder intermediate layer
The laser soldering method of gold.
The technical problems to be solved by the invention are realized using following technical scheme, specifically includes the following steps:
(1) it purifies sample: glass surface is subjected to purified treatment;Kovar alloy surface oxidation is removed with water resistance sand paper
Film is polishing to 1200 mesh from 400 mesh, is polished, and finally carries out degreasing and goes oil processing;
(2) produce oxidation film: by step (1) by surface treatment after kovar alloy in the equipment vacuumized always into
Row processing, is then placed in oxidation furnace and prepares oxidation film, obtains oxidation film by control oxidization time and oxidizing temperature;
(3) prepare transition zone: selection tri- kinds of mixed-powders of Mo, Mn, Ni do transition zone, the composition of mass percent: Mo
10%-15% is accounted for, Ni accounts for 50%-60%, and Mn accounts for 28%-33%, and additive accounts for 0.1%-0.5%, and microelement C accounts for 0.5-
1.5%, SiO20.5-1.5% is accounted for, the additive is PVA, then prepares transition zone using tablet press machine;
(4) weld preheating: welding " sandwich " formula structure, bottom is glass, and centre is transition zone, and top layer is that can cut down conjunction
Gold is in close contact between three, then " sandwich " formula structure of close contact is put into 350-450 DEG C of heating furnace and is carried out
Preheating, preheating time 20-40min;
(5) glass, middle layer and kovar alloy " sandwich " formula structure after preheating laser welding: are placed on fixture
On, laser beam vertical irradiation is welded on kovar alloy surface;
(6) post weld heat treatment: after welding, weldment is moved to rapidly to progress destressing in 350-450 DEG C of heating furnace and is moved back
Then fire cools to room temperature with the furnace, the weldment of reliable glass and kovar alloy can be obtained.
In above-mentioned technical proposal, in the step (1), kovar alloy carries out surface polishing first, then carries out degreasing and goes
Oil processing, then vacuum purification is handled, and finally carries out oxidation processes.
In above-mentioned technical proposal, in the step (2), the vacuum purification time is 10-30min, is vacuumized
Degree is 10-2~10-1MPa, oxidizing temperature control the oxidization time 10-20min between 700-850 DEG C.
In above-mentioned technical proposal, in the step (3), by adjusting powder quality, apply pressure and pressing time control
Transition region thickness;Transition region thickness is 80-100 μm.
In above-mentioned technical proposal, in the step (4) (6), used heating furnace is pillar resistance furnace.
In above-mentioned technical proposal, in the step (5), laser is Nd:YAG laser, Laser Welding ginseng when laser welding
Number is as follows: laser power 550-850W, speed of welding 2.5-8.5mm/s, and defocusing amount is ± 4mm, scanning times 1-3
Road.The present invention selects suitable defocusing amount, obtains good weldment.
In above-mentioned technical proposal, in the step (5), protective gas is argon gas when laser welding, and gas flow is preferably
10-25L/min。
The present invention has a significant advantage that compared with prior art
1. the present invention has developed the laser connection method of a kind of new glass and kovar alloy, by using with kovar alloy
Molybdenum group glass similar in coefficient of linear thermal expansion reduces postwelding thermal stress to the greatest extent.Middle layer selects Mo element that can put down
Weigh coefficient of linear thermal expansion, reduces welding stress, and addition Ni element can be improved wetability, promote boundary moisture, adds Mn element
Strength of joint is improved, micro C element and SiO are added2The reaction interval with kovar alloy oxide on surface can be improved in oxide
Degree enhances shearing strength of joint to preferably promote interface cohesion.
2., such as laser power, speed of welding, defocusing amount, it is defeated can accurately to control heat by optimization laser welding process parameter
Phenomena such as entering, avoiding as compared with cracking caused by high heat-input and fusing.Using weld preheating and post weld heat treatment measure, keep away
Exempt from as rapidly heating up and cracking caused by rapid cooling.
3. method for laser welding of the invention is at low cost, high-efficient, welding quality is good, is more suitable batch micro operations.
Detailed description of the invention
Fig. 1 Laser Welding knot schematic device.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
(1) kovar alloy is polishing to 1200 mesh from 400 mesh, then in acetone soln progress ultrasonic cleaning, cleaning
Between 20min;
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
To aoxidize 10min in 800 DEG C of furnaces;
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), centre addition is intermediate
Layer, is then placed on fixture;
(4) preheating temperature is 300 DEG C, preheating time 20min;
(5) middle layer mass percent is selected are as follows: Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2: 1.0%,
PVA additive accounts for 0.3%, and intermediate layer thickness is 80 μm;
(6) laser model are as follows: YLS-3000-SM, laser parameter are as follows: laser power 700W, speed of welding 4.5mm/
S, gas flow 15L/min;
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling;
Intensity experiment test, after the method welding of this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 9.6MPa.
Embodiment 2
(1) kovar alloy is polishing to 1200 mesh from 400 mesh, then in acetone soln progress ultrasonic cleaning, cleaning
Between 20min;
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
To aoxidize 10min in 800 DEG C of furnaces;
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), centre addition is intermediate
Layer, is then placed on fixture;
(4) preheating temperature is 300 DEG C, preheating time 20min;
(5) middle layer mass percent is selected are as follows: Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additive accounts for 0.3%, and 90 μm of intermediate layer thickness;
(6) laser model are as follows: YLS-3000-SM, laser parameter are as follows: laser power 700W, speed of welding 4.5mm/
S, gas flow 15L/min;
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling;
Intensity experiment test, after the method welding of this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 8.9MPa.
Embodiment 3
(1) kovar alloy is polishing to 1200 mesh from 400 mesh, then in acetone soln progress ultrasonic cleaning, cleaning
Between 20min;
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
It is 800 DEG C, 10min is aoxidized in furnace;
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), centre addition is intermediate
Layer, is then placed on fixture;
(4) preheating temperature is 300 DEG C, preheating time 20min;
(5) middle layer mass percent is selected are as follows: Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additive accounts for 0.3%, and 100 μm of intermediate layer thickness;
(6) laser model are as follows: YLS-3000-SM, laser parameter are as follows: laser power 700W, speed of welding 4.5mm/
S, gas flow 15L/min;
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling;
Intensity experiment test, after the method welding of this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 7.8MPa.
Embodiment 4
(1) kovar alloy is polishing to 1200 mesh from 400 mesh, is then cleaned with ultrasound machine acetone soln, clearly
Wash time 20min;
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
It is 800 DEG C, 10min is aoxidized in furnace;
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), centre addition is intermediate
Layer, is then placed on fixture;
(4) preheating temperature is 300 DEG C, preheating time 20min;
(5) middle layer mass percent is selected are as follows: Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additive accounts for 0.3%, and 80 μm of intermediate layer thickness;
(6) laser model are as follows: YLS-3000-SM, laser parameter are as follows: laser power 750W, speed of welding 4.5mm/
S, gas flow 15L/min;
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling;
Intensity experiment test, after the method welding of this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 9.8MPa.
Embodiment 5
(1) kovar alloy is polishing to 1200 mesh from 400 mesh, is then cleaned with ultrasound machine acetone soln, clearly
Wash time 20min;
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
It is 800 DEG C, 10min is aoxidized in furnace;
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), centre addition is intermediate
Layer, is then placed on fixture;
(4) preheating temperature is 300 DEG C, preheating time 20min;
(5) middle layer mass percent is selected are as follows: Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additive accounts for 0.3%, and 80 μm of intermediate layer thickness;
(6) laser model are as follows: YLS-3000-SM, laser parameter are as follows: laser power 750W, speed of welding 5mm/s,
Gas flow is 15L/min;
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling;
Intensity experiment test, after the method welding of this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 10.96MPa.
Embodiment 6
(1) kovar alloy is polishing to 1200 mesh from 400 mesh, is then cleaned with ultrasound machine acetone soln, clearly
Wash time 20min;
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
It is 800 DEG C, 10min is aoxidized in furnace;
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), centre addition is intermediate
Layer, is then placed on fixture;
(5) preheating temperature is 300 DEG C, preheating time 20min;
(5) middle layer mass percent is selected are as follows: Mo:12%, Ni:55%, Mn:31%, C:0.6%, SiO2:1.2%,
PVA additive accounts for 0.2%, and intermediate layer thickness is 80 μm;
(6) laser model are as follows: YLS-3000-SM, laser parameter are as follows: laser power 750W, speed of welding 4.5mm/
S, gas flow 15L/min;
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling;
Intensity experiment test, after the method welding of this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 9.5MPa.
1 summary sheet of table
Note: ◎ indicates excellent, and zero indicates good, and △ indicates general, × indicate unqualified.
Claims (7)
1. a kind of connect molybdenum group glass/kovar alloy laser soldering method, feature by addition Mo-Mn-Ni metal intermediate layer
It is, comprising the following steps:
(1) it purifies sample: glass surface is subjected to purified treatment;Kovar alloy surface film oxide is removed with water resistance sand paper, from
400 mesh are polishing to 1200 mesh, are polished, and finally carry out degreasing and go oil processing;
(2) produce oxidation film: by step (1) by surface treatment after kovar alloy in the equipment vacuumized always
Reason, is then placed in oxidation furnace and prepares oxidation film, obtains oxidation film by control oxidization time and oxidizing temperature;
(3) prepare transition zone: selection tri- kinds of mixed-powders of Mo, Mn, Ni do transition zone, and the composition of mass percent: Mo is accounted for
10%-15%, Ni account for 50%-60%, and Mn accounts for 28%-33%, and additive accounts for 0.1%-0.5%, and microelement C accounts for 0.5-1.5%, SiO2It accounts for
0.5-1.5%, the additive are PVA, then prepare transition zone using tablet press machine;
(4) weld preheating: welding " sandwich " formula structure, bottom is glass, and centre is transition zone, and top layer is kovar alloy, three
It is in close contact between person, then " sandwich " formula structure of close contact is put into 350-450 DEG C of heating furnace and is preheated,
Preheating time is 20-40min;
(5) laser welding: glass, middle layer and kovar alloy " sandwich " formula structure after preheating are placed on fixture, are swashed
Beam orthogonal is radiated at kovar alloy surface, is welded;
(6) post weld heat treatment: after welding, weldment is moved to rapidly and carries out stress relief annealing in 350-450 DEG C of heating furnace, so
After cool to room temperature with the furnace, the weldment of reliable glass and kovar alloy can be obtained.
2. described in accordance with the claim 1 a kind of by adding Mo-Mn-Ni metal intermediate layer connection molybdenum group glass/kovar alloy
Laser soldering method, which is characterized in that in the step (2), the vacuum purification time be 10-30 min, suction 10-2~
10-1 MPa。
3. described in accordance with the claim 1 a kind of by adding Mo-Mn-Ni metal intermediate layer connection molybdenum group glass/kovar alloy
Laser soldering method, which is characterized in that in the step (2), oxidizing temperature control between 700-850 DEG C, oxidization time is
10-20 min。
4. described in accordance with the claim 1 a kind of by adding Mo-Mn-Ni metal intermediate layer connection molybdenum group glass/kovar alloy
Laser soldering method, which is characterized in that in the step (3), transition region thickness be 80-100 μm.
5. described in accordance with the claim 1 a kind of by adding Mo-Mn-Ni metal intermediate layer connection molybdenum group glass/kovar alloy
Laser soldering method, which is characterized in that in step (4) (6), used heating furnace be pillar resistance furnace.
6. described in accordance with the claim 1 a kind of by adding Mo-Mn-Ni metal intermediate layer connection molybdenum group glass/kovar alloy
Laser soldering method, which is characterized in that in step (5), laser is Nd:YAG laser, Laser Welding parameter when laser welding
As follows: laser power is 550-850 W, and speed of welding is 2.5-8.5 mm/s, and defocusing amount is ± 4 mm, scanning times 1-3
Road.
7. described in accordance with the claim 1 a kind of by adding Mo-Mn-Ni metal intermediate layer connection molybdenum group glass/kovar alloy
Laser soldering method, which is characterized in that in the step (5), protective gas is argon gas, gas flow 10- when laser welding
25 L/min。
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