CN106517828A - Laser welding method for connecting molybdenum-group glass/kovar alloy by adding Mo-Mn-Ni metal interlayer - Google Patents
Laser welding method for connecting molybdenum-group glass/kovar alloy by adding Mo-Mn-Ni metal interlayer Download PDFInfo
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- CN106517828A CN106517828A CN201610951616.6A CN201610951616A CN106517828A CN 106517828 A CN106517828 A CN 106517828A CN 201610951616 A CN201610951616 A CN 201610951616A CN 106517828 A CN106517828 A CN 106517828A
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- kovar alloy
- glass
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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
Abstract
The invention relates to a laser welding method for connecting molybdenum-group glass/kovar alloy by adding a Mo-Mn-Ni metal interlayer, and belongs to the technical field of connection of non-metal and metal materials. The method comprises the following steps: cleaning glass, removing a surface oxidation film from kovar alloy, and performing degreasing and deoiling treatment; preparing an oxidation film on the kovar alloy in an oxidizing furnace; preparing a Mo-Mn-Ni interlayer metal powder layer through a tabletting machine; arranging the glass at the bottom layer, the Mo-Mn-Ni interlayer metal powder at the middle layer and the kovar alloy at the top layer to form a sandwich welded structure, enabling the three to be in close contact, putting into a furnace, and preheating; radiating a laser beam onto the surface of the kovar alloy to perform laser welding; and after the welding is finished, quickly transferring the weldment into the heating furnace, performing stress-relief annealing, and cooling to room temperature in the furnace. The method provided by the invention promotes interface wetting, reduces postwelding stress, improves joint strength, lowers production cost and prolongs product service life.
Description
Technical field
The present invention relates to a kind of Laser Welding side for connecting molybdenum group glass/kovar alloy by adding Mo-Mn-Ni intermediate layers
Method, belongs to nonmetallic and metal material interconnection technique field.
Background technology
The features such as glass material has high intensity, high rigidity, corrosion-resistant, excellent insulation performance, but the low of glass itself prolong
Malleability and poor impact flexibility limit its application in engineering.Thus combine the glass of glass and metal premium properties-
Metal composite structure application and give birth to, and be widely used in microelectronics Packaging, battery, instrument, solar vacuum heat-collecting pipe etc.
Field.
Glass is widely used in microelectronics Packaging, relay, solar vacuum heat-collecting pipe etc. with metal welding vacuum gas
The occasion that close property is required.But strength of joint is low, fragility is big, is very limited in actual applications.Metal material is connected with glass
The subject matter for connecing is：(1) thermal coefficient of expansion differs greatly, stress concentration, 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 wettability is very
Difference, interface cohesion are difficult；(3) nonmetallic materials poor toughness, is susceptible to fracture.Foreign material associative key difference causes material machine
There is larger difference in tool performance and physical property, such as metal material has good plasticity and toughness and machinability, and nonmetallic
Material fragility is larger, defines complementation with nonmetallic materials, therefore to developing a kind of reliable glass and metal joining techniques
Propose an urgent demand.
Glass has anode linkage, soldering, friction welding (FW), electron beam weldering, blast weldering etc. with the traditional method of attachment of metal.But this
There is the defects such as low easily aging, degree of accuracy, low intensity and pore be more in a little methods.Relative to other welding methods, laser beam control
System is simple, it is easy to accomplish automatization, Laser Welding can strictly control heat input, and thermal deformation is less, and heat affected area is little, degree of accuracy
Height, shaping 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 is welded, and is not required to vacuum, is not required to X-ray protection, injures little to the person, 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 alloys, alloy coefficient of linear thermal expansion in the range of 20-450 DEG C is 5.1～
5.5×10-6K-1, molybdenum group glass DM308 is that coefficient of linear thermal expansion is 4.9～10 × 10 in the range of 20-300 DEG C in temperature-6K-1,
The two similar thermal expansion coefficient at room temperature, can effectively reduce post-weld stress, obtain good welding point.Suitable for microelectronics
Encapsulation, production relay, solar vacuum heat-collecting pipe etc..
The content of the invention
It is an object of the present invention to provide a kind of connect molybdenum group glass/can cut down conjunction by adding Mo Mn Ni metal powder intermediate layers
The laser soldering method of gold.
The technical problem to be solved employs the following technical solutions to realize, specifically includes following steps：
(1) purify sample：Glass surface is carried out into purified treatment；Kovar alloy surface oxidation is removed with resistance to water sand paper
Film, is polishing to 1200 mesh from 400 mesh, is polished, and finally carries out defat and goes oil processing；
(2) produce oxide-film：Kovar alloy of the step (1) after surface treatment is entered in the equipment of evacuation always
Row is processed, and prepares oxide-film in being then placed within oxidation furnace, obtains oxide-film by controlling oxidization time and oxidizing temperature；
(3) prepare transition zone：Tri- kinds of mixed-powders of Mo, Mn, Ni are selected to do transition zone, the composition of its 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 trace element C accounts for 0.5-
1.5%, SiO20.5-1.5% is accounted for, and the additive is PVA, then transition zone is prepared using tablet machine；
(4) weld preheating：Welding " sandwich " formula structure, bottom is glass, and middle is transition zone, and top layer is to cut down conjunction
Gold, is in close contact between three, and then " sandwich " the formula structure being in close contact is put in 350-450 DEG C of heating furnace is carried out
Preheating, preheating time is 20-40min；
(5) laser welding：Glass after preheating, intermediate layer and kovar alloy " sandwich " formula structure are placed on into fixture
On, laser beam vertical irradiation is welded on kovar alloy surface；
(6) post weld heat treatment：After welding terminates, destressing is carried out during weldment to be moved to rapidly 350-450 DEG C of heating furnace and moved back
Fire, then cools to room temperature with the furnace, and the weldment of reliable glass and kovar alloy is obtained.
In above-mentioned technical proposal, in the step (1), kovar alloy carries out surface polishing first, then carries out defat and goes
Oil processing, then vacuum purification are processed, and finally carry out oxidation processes.
In above-mentioned technical proposal, in the step (2), the vacuum purification time be 10-30min, evacuation
Spend for 10-2～10-1MPa, between 700-850 DEG C, oxidization time is 10-20min for oxidizing temperature control.
In above-mentioned technical proposal, in the step (3), by adjusting powder quality, applying pressure and press time control
Transition region thickness；Transition region thickness is 80-100 μm.
In above-mentioned technical proposal, in the step (4) (6), the heating furnace for being used is pillar resistance furnace.
In above-mentioned technical proposal, in the step (5), during laser welding, laser instrument is Nd:YAG laser, Laser Welding ginseng
Number is as follows：Laser power is 550-850W, and speed of welding is 2.5-8.5mm/s, and defocusing amount is ± 4mm, and scanning times are 1-3
Road.The present invention selects suitable defocusing amount, obtains good weldment.
In above-mentioned technical proposal, in the step (5), during laser welding, protective gas is argon, and gas flow is preferably
10-25L/min。
The present invention has remarkable advantage compared with prior art：
1. the present invention have developed the laser method of attachment of a kind of new glass and kovar alloy, by employing and kovar alloy
The close molybdenum group glass of coefficient of linear thermal expansion, farthest reduces postwelding thermal stress.Can be put down from Mo elements in intermediate layer
Weighing apparatus coefficient of linear thermal expansion, reduces welding stress, and addition Ni elements can improve wettability, promote boundary moisture, add Mn elements
Strength of joint is improved, adds micro C element and SiO2Oxide can improve the reaction interval with kovar alloy oxide on surface
Degree, so as to preferably promote interface cohesion, strengthens shearing strength of joint.
2., by optimizing laser welding process parameter, such as laser power, speed of welding, defocusing amount can be defeated with precise control heat
Enter, it is to avoid due to phenomenons such as the cracking that causes compared with high heat-input and fusing.Using weld preheating and post weld heat treatment measure, keep away
Exempt from as rapidly liter gently rapidly cools down the cracking for causing.
3. the method for laser welding low cost of the present invention, efficiency high, welding quality are good, are more suitable for batch micro operations.
Description of the drawings
Fig. 1 Laser Welding ties schematic device.
Specific embodiment
The present invention is further illustrated with reference to embodiment, but the present invention is not limited to following examples.
Embodiment 1
(1) kovar alloy is polishing to into 1200 mesh from 400 mesh, then ultrasound wave cleaning is carried out in acetone soln, during 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 stoves；
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), in the middle of middle addition
Layer, is then placed on fixture；
(4) preheating temperature be 300 DEG C, preheating time 20min；
(5) from intermediate layer mass percent it is：Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additives account for 0.3%, and intermediate layer thickness is 80 μm；
(6) laser instrument model：YLS-3000-SM, laser parameter is：Laser power 700W, speed of welding are 4.5mm/
S, gas flow are 15L/min；
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling；
Intensity experiment is tested, and after being welded using the method for 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 into 1200 mesh from 400 mesh, then ultrasound wave cleaning is carried out in acetone soln, during 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 stoves；
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), in the middle of middle addition
Layer, is then placed on fixture；
(4) preheating temperature be 300 DEG C, preheating time 20min；
(5) from intermediate layer mass percent it is：Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additives account for 0.3%, 90 μm of intermediate layer thickness；
(6) laser instrument model：YLS-3000-SM, laser parameter is：Laser power 700W, speed of welding are 4.5mm/
S, gas flow are 15L/min；
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling；
Intensity experiment is tested, and after being welded using the method for 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 into 1200 mesh from 400 mesh, then ultrasound wave cleaning is carried out in acetone soln, during cleaning
Between 20min；
The kovar alloy of (2) 40 × 20 × 1.1mm is 10 in suction-1MPa environmental treatment 20min, then in temperature
For 800 DEG C, 10min in stove, is aoxidized；
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), in the middle of middle addition
Layer, is then placed on fixture；
(4) preheating temperature be 300 DEG C, preheating time 20min；
(5) from intermediate layer mass percent it is：Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additives account for 0.3%, 100 μm of intermediate layer thickness；
(6) laser instrument model：YLS-3000-SM, laser parameter is：Laser power 700W, speed of welding are 4.5mm/
S, gas flow are 15L/min；
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling；
Intensity experiment is tested, and after being welded using the method for 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 into 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
For 800 DEG C, 10min in stove, is aoxidized；
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), in the middle of middle addition
Layer, is then placed on fixture；
(4) preheating temperature be 300 DEG C, preheating time 20min；
(5) from intermediate layer mass percent it is：Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additives account for 0.3%, 80 μm of intermediate layer thickness；
(6) laser instrument model：YLS-3000-SM, laser parameter is：Laser power 750W, speed of welding are 4.5mm/
S, gas flow are 15L/min；
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling；
Intensity experiment is tested, and after being welded using the method for 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 into 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
For 800 DEG C, 10min in stove, is aoxidized；
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), in the middle of middle addition
Layer, is then placed on fixture；
(4) preheating temperature be 300 DEG C, preheating time 20min；
(5) from intermediate layer mass percent it is：Mo:15%, Ni:54%, Mn:29%, C:0.7%, SiO2:1.0%,
PVA additives account for 0.3%, 80 μm of intermediate layer thickness；
(6) laser instrument model：YLS-3000-SM, laser parameter is：Laser power 750W, speed of welding are 5mm/s,
Gas flow is 15L/min；
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling；
Intensity experiment is tested, and after being welded using the method for 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 into 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
For 800 DEG C, 10min in stove, is aoxidized；
(3) the kovar alloy sample after oxidation is placed on molybdenum group glass sample (20 × 15 × 3mm), in the middle of middle addition
Layer, is then placed on fixture；
(5) preheating temperature be 300 DEG C, preheating time 20min；
(5) from intermediate layer mass percent it is：Mo:12%, Ni:55%, Mn:31%, C:0.6%, SiO2:1.2%,
PVA additives account for 0.2%, and intermediate layer thickness is 80 μm；
(6) laser instrument model：YLS-3000-SM, laser parameter is：Laser power 750W, speed of welding are 4.5mm/
S, gas flow are 15L/min；
(7) post weld heat treatment temperature is 350 DEG C, furnace cooling；
Intensity experiment is tested, and after being welded using the method for this example, the shear strength of molybdenum group glass and kovar alloy can
Up to 9.5MPa.
1 summary sheet of table
Note：◎ represents excellent, and zero represents good, and △ represents general, × represent unqualified.
Claims (7)
1. a kind of laser soldering method for connecting molybdenum group glass/kovar alloy by adding Mo-Mn Ni metal intermediate layers, its feature
It is to comprise the following steps：
(1) purify sample：Glass surface is carried out into purified treatment；Kovar alloy surface film oxide is removed with resistance to water sand paper, from
400 mesh are polishing to 1200 mesh, are polished, and finally carry out defat and go oil processing；
(2) produce oxide-film：Kovar alloy of the step (1) after surface treatment is located in the equipment of evacuation always
Reason, prepares oxide-film in being then placed within oxidation furnace, obtains oxide-film by controlling oxidization time and oxidizing temperature；
(3) prepare transition zone：Tri- kinds of mixed-powders of Mo, Mn, Ni are selected to do transition zone, the composition of its 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 trace element C accounts for 0.5-
1.5%, SiO20.5-1.5% is accounted for, and the additive is PVA, then transition zone is prepared using tablet machine；
(4) weld preheating：Welding " sandwich " formula structure, bottom is glass, and middle is transition zone, and top layer is kovar alloy, three
It is in close contact between person, then " sandwich " the formula structure being in close contact is put in 350-450 DEG C of heating furnace and is preheated,
Preheating time is 20-40min；
(5) laser welding：Glass after preheating, intermediate layer and kovar alloy " sandwich " formula structure are placed on fixture, are swashed
Beam orthogonal is radiated at kovar alloy surface, is welded；
(6) post weld heat treatment：After welding terminates, stress relief annealing is carried out during weldment to be moved to rapidly 350-450 DEG C of heating furnace, so
After cool to room temperature with the furnace, the weldment of reliable glass and kovar alloy is obtained.
2. molybdenum group glass/kovar alloy is connected by adding Mo-Mn Ni metal intermediate layers according to the one kind described in claim 1
Laser soldering method, it is characterised in that in the step (2), the vacuum purification time be 10-30min, suction is 10-2~
10-1MPa。
3. molybdenum group glass/kovar alloy is connected by adding Mo-Mn Ni metal intermediate layers according to the one kind described in claim 1
Laser soldering method, it is characterised in that in the step (2), between 700-850 DEG C, oxidization time is for oxidizing temperature control
10-20min。
4. molybdenum group glass/kovar alloy is connected by adding Mo-Mn Ni metal intermediate layers according to the one kind described in claim 1
Laser soldering method, it is characterised in that in the step (3), transition region thickness be 80-100 μm.
5. molybdenum group glass/kovar alloy is connected by adding Mo-Mn Ni metal intermediate layers according to the one kind described in claim 1
Laser soldering method, it is characterised in that in step (4) (6), the heating furnace for being used be pillar resistance furnace.
6. molybdenum group glass/kovar alloy is connected by adding Mo-Mn Ni metal intermediate layers according to the one kind described in claim 1
Laser soldering method, it is characterised in that in step (5), during laser welding laser instrument be Nd:YAG laser, Laser Welding parameter is such as
Under：Laser power is 550-850W, and speed of welding is 2.5-8.5mm/s, and defocusing amount is ± 4mm, and scanning times are 1-3 roads.
7. molybdenum group glass/kovar alloy is connected by adding Mo-Mn Ni metal intermediate layers according to the one kind described in claim 1
Laser soldering method, it is characterised in that in the step (5), during laser welding, protective gas is argon, and gas flow is preferably
10-25L/min。
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| CN106944741A (en) * | 2017-04-26 | 2017-07-14 | 西安交通大学 | Add the microalloying method that Zr improves molybdenum and molybdenum alloy arc-seam weld obdurability |
| CN107010849A (en) * | 2017-05-10 | 2017-08-04 | 北京工业大学 | The laser welding process method of molybdenum group glass and kovar alloy |
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| CN108623192B (en) * | 2017-03-23 | 2021-04-16 | 南京理工大学 | Titanium alloy-K9 glass composite connection equipment and method based on intermediate layer gradient |
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| CN109487198A (en) * | 2018-12-20 | 2019-03-19 | 西安赛尔电子材料科技有限公司 | It is a kind of for kovar alloy surface rare earth metal-molybdenum binary cementation coating preparation method |
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| US20210053155A1 (en) * | 2019-08-23 | 2021-02-25 | Shenzhenshi Yuzhan Precision Technology Co., Ltd. | Connecting article and method for manufacturing the same, and laser device |
| CN112404728A (en) * | 2019-08-23 | 2021-02-26 | 深圳市裕展精密科技有限公司 | Connecting piece, device, laser equipment and preparation method |
| CN112404728B (en) * | 2019-08-23 | 2023-04-07 | 富联裕展科技(深圳)有限公司 | Connecting piece, device, laser equipment and preparation method |
| CN112846499A (en) * | 2020-12-29 | 2021-05-28 | 武汉华工激光工程有限责任公司 | Ultrafast laser welding method and system for glass and metal packaging |
| CN113909665A (en) * | 2021-10-22 | 2022-01-11 | 哈尔滨工业大学 | Method for diffusion welding of Kovar alloy with molybdenum-rhenium alloy and intermediate layer |
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