CN103922613B - The welding method of kovar alloy and glass - Google Patents
The welding method of kovar alloy and glass Download PDFInfo
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- CN103922613B CN103922613B CN201410169153.9A CN201410169153A CN103922613B CN 103922613 B CN103922613 B CN 103922613B CN 201410169153 A CN201410169153 A CN 201410169153A CN 103922613 B CN103922613 B CN 103922613B
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Abstract
The invention discloses the welding method of a kind of kovar alloy and glass, it comprises the steps: that S1. provides kovar alloy; S2. sanding and polishing kovar alloy; S3. ultrasonic cleaning and cleaning; S4. laser is to the processing of kovar alloy remelting; S5. send in tube furnace and heat. In the welding method of kovar alloy of the present invention and glass, adopt laser instrument to carry out straight line treatment with irradiation kovar alloy surface, instead of adopt stove to process whole kovar alloy, not only reduce energy waste, simultaneously owing to only the region of needs wetting (or sealing-in) being processed, other regions of alloy are not affected, thereby the performance of alloy (metal) is not worsened, and has improved military service performance.
Description
Technical field
The present invention relates to the welding technology field of kovar alloy, relate in particular to the weldering of a kind of kovar alloy and glassConnect method.
Background technology
Glass material is because of high-temperature wearable, anti-corrosion, insulation, and oxidation resistance is strong etc., and feature is widely used,But the low ductility of glass itself, poor impact toughness have limited its application in engineering. Therefore combine glassGlass metal composite joint (welding) material of glass and metal double premium properties arises at the historic moment, and extensively shouldFor microelectronics Packaging, battery, instrument and meter, solar vacuum heat-collecting pipe, prepare composite, because ofThis research glass-to-metal seal is significant.
The method for sealing of glass and metal has a variety of, wherein most study and theoretical more ripe sealing for matingConnect. Matched seal is first metal to be carried out to pre-oxidation treatment before sealing-in, makes metal surface generate a layer thicknessSuitable oxide layer, then metal and glass are placed on to heating and thermal insulation certain hour in stove are then cooled to room temperature,It is then cooling that but matched seal will be heated in stove, thereby the production cycle of matched seal is long.
The quality of glass and metal solder performance is weighed by wetability conventionally, and wherein, wetability refers to solidBody interface is changed into the phenomenon of solid-liquid interface by solid-air interface, wetability represents by angle of wetting. Work as dropWhile dropping in the surface of solids, can occur difformity according to wetability difference, drop is cut solid-liquid contact edgeAngle between line and surface is called angle of wetting. The quality of above-mentioned wettability directly affects glass and metalWelding effect, particularly, angle of wetting is between the two less shows that wetability is better.
Thereby, in above-mentioned matched seal, metal surface through pre-oxidation treatment form oxide layer to glass withThe wetability of metal has a significant impact, oxide layer with the interfacial tension of liquid metal than metal and glass interfaceTension force is low, and therefore oxide layer generally can improve wetability. Therefore traditional glass mates with metal (alloy)In sealing-in, alloy surface is to be all first placed in stove to carry out thermal oxidation in advance, obtains certain thickness oxygenChange layer, then glass is soaking (crying again sealing-in, welding) with metal (alloy). Above-mentioned sealing-in sideMethod will heat in stove carries out after thermal oxide in advance coolingly, is then soaking (sealing-in), thereby is causingProduction cycle long.
In addition,, in existing method for sealing, do not need to soak or the district of sealing-in for metal (alloy)Thermal oxide has also been carried out in territory, has worsened the performance of material, and the military service performance of material is greatly declined, andWhole metal (alloy) is processed, wasted the extra energy.
Summary of the invention
For the problems referred to above, the invention provides the welding method of a kind of kovar alloy and glass.
Laser processing technology, owing to can appointed area being processed to processing, can complete melted alloy surface,Thereby make alloy surface appointed area form certain modified layer, this layer and metal (alloy) directly carry outWetting, can complete wetting. Greatly promote thus the improvement of glass and metal (alloy) sealing-in, simultaneouslyOther regions are not processed, alloy military service performance is also greatly improved.
Based on laser processing technology, to achieve these goals, a kind of kovar alloy of the present invention and glassWelding method, it comprises the steps:
S1., the kovar alloy that carries out sealing-in with glass is provided;
S2. the kovar alloy providing is carried out to surface finish processing;
S3. again to cleaning through the kovar alloy of surface finish processing, after cleaning, dry up for subsequent use;
S4. laser instrument is under control system control, and Emission Lasers is swept the region to be processed of kovar alloyRetouch remelting processing;
S5. the glass welding with kovar alloy is positioned on the machining area of kovar alloy, and willKovar alloy and glass are sent in tube furnace and are heated, and carry out temperature programming when heating, after heating,Be incubated processing, then be cooled to room temperature.
As a further improvement on the present invention, in described step S2, kovar alloy is carried out to surface finish processingTime, utilize sand paper to carry out sanding and polishing to kovar alloy surface.
As a further improvement on the present invention, while cleaning in described step S3, first carry out ultrasonic cleaning,Recycling absolute alcohol or acetone clean.
As a further improvement on the present invention, the thickness of described kovar alloy is 0.5mm～10mm, described inKovar alloy after remelting is processed, surface roughness is less than remelting process before kovar alloy surface roughnessTwice.
As a further improvement on the present invention, in described step S4, the sharp light wavelength of transmitting is800～10640nm, power is 30～700W, sweep speed is 2～26mm/s.
As a further improvement on the present invention, described laser instrument be YAG laser instrument, carbon dioxide laser,Or semiconductor laser.
As a further improvement on the present invention, described step S5 also comprises:
S51., glass dust is provided, is positioned in cylinder, then cylinder is positioned under forcing press, in 5MPaLower pressurization, forms glass blocks;
S52. glass blocks is positioned on the machining area of kovar alloy, and kovar alloy and glass blocks are sentEnter in tube furnace and heat, when heating, carry out temperature programming, after heating, be incubated processing, thenBe cooled to room temperature.
As a further improvement on the present invention, while heating in tube furnace, the even warm area in tube furnaceHeat, when temperature programming, programming rate is 4 DEG C/min, is warming up to 1100 DEG C, insulation 100min,When cooling, controlling rate of temperature fall is 5 DEG C/min, while being reduced to room temperature, stops to temperature.
As a further improvement on the present invention, in tube furnace, heat up and cooling is to enter under atmospheric conditionsRow.
Compared with prior art, the invention has the beneficial effects as follows: the welding of kovar alloy of the present invention and glassMethod is by Optimizing Process Parameters, accurately control laser remolten processing region, power ratio control, sweep speed,Obtain specific modification region, so overcome the deficiency existing in existing pre-oxidation treatment mode.
In addition,, in the welding method of kovar alloy of the present invention and glass, adopt laser instrument to carry out straight line irradiationProcess kovar alloy surface, instead of adopt stove to process whole kovar alloy, not only reduced energySource waste, simultaneously owing to only the region of needs wetting (or sealing-in) being processed, other districts of alloyTerritory is not affected, thereby the performance of alloy (metal) is not worsened, and has improved military service performance.
The welding method of kovar alloy of the present invention and glass also possess energy controllability high, processing heat affected areaNarrow, working (machining) efficiency advantages of higher, can adapt to vibration monitoring better.
Brief description of the drawings
Fig. 1 is the method flow of the detailed description of the invention of the welding method of kovar alloy of the present invention and glassFigure;
Fig. 2 is angle of wetting and wetting or nonwetting (weldering in the welding method of kovar alloy of the present invention and glassConnect performance quality) distribution schematic diagram, wherein in Fig. 2 taking 90 ° as boundary, point to paper left side for wetting,It is nonwetting pointing to paper right side;
Fig. 3 be the kovar alloy that welds together in the welding method of kovar alloy of the present invention and glass withThe angle of wetting test metallograph of glass;
Fig. 4 is in comparative example, does not pass through laser remolten processing, also not through thermal oxidation in advanceThe photo of kovar alloy and glass;
Fig. 5 is in comparative example, not wetting after the kovar alloy of laser remolten processing and glass weldingAngular measurement examination metallograph.
Detailed description of the invention
To the technical scheme in the embodiment of the present invention be described in detail below, obviously, described realityExecuting example is only the present invention's part embodiment, instead of whole embodiment. Based on the enforcement in the present inventionExample, the every other reality that those of ordinary skill in the art obtain under the prerequisite of not making creative workExecute example, all belong to the scope of protection of the invention.
As shown in Figure 1, the welding method of kovar alloy of the present invention and glass, it comprises the steps:
S1., the kovar alloy that carries out sealing-in with glass is provided.
S2. the kovar alloy providing is carried out to surface finish processing. Wherein, kovar alloy being carried out to surface throwsWhen light is processed, utilize sand paper to carry out sanding and polishing to kovar alloy surface.
S3. again to cleaning through the kovar alloy of surface finish processing, after cleaning, dry up for subsequent use. DescribedWhile cleaning in step S3, first carry out ultrasonic cleaning, recycling absolute alcohol or acetone clean,To ensure the clean of kovar alloy machined surface.
S4. laser instrument is under control system control, and Emission Lasers is swept the region to be processed of kovar alloyRetouch remelting processing.
Wherein, the sharp light wavelength of transmitting is 800～10640nm, and power is 30～700W, and sweep speed is2～26mm/s. After the scanning remelting of laser is processed, ensure that kovar alloy surface roughness is less than remeltingThe twice of kovar alloy surface roughness before processing. In present embodiment, the thickness of kovar alloy is0.5mm～10mm. Above-mentioned laser instrument can be that YAG laser instrument, carbon dioxide laser or semiconductor swashLight device. Above-mentioned laser carries out under atmospheric conditions the scanning remelting processing of kovar alloy.
S5. the glass welding with kovar alloy is positioned on the machining area of kovar alloy, and willKovar alloy and glass are sent in tube furnace and are heated, and carry out temperature programming when heating, after heating,Be incubated processing, then be cooled to room temperature, thereby complete the welding of glass and kovar alloy.
As a kind of alternate embodiments, in the time using glass dust to weld, step S5 also comprises:
S51., glass dust is provided, is positioned in cylinder, then cylinder is positioned under forcing press, in 5MPaLower pressurization, forms glass blocks;
S52. glass blocks is positioned on the machining area of kovar alloy, and kovar alloy and glass blocks are sentEnter in tube furnace and heat, when heating, carry out temperature programming, after heating, be incubated processing, thenBe cooled to room temperature.
Wherein, glass dust is pressed into glass blocks, makes it can be not loose in light exercise process, thereby makeWelding can be carried out smoothly. Preferably, glass dust is borosilicate glass dust.
Particularly, while carrying out glass dust compacting, borosilicate glass dust is positioned over to Φ 5mm × 10mmSteel cylinder in, then this cylinder is positioned under forcing press. Under 5MPa condition, suppress, insulation extremelyAfter few 10s, form glass blocks, take out for subsequent use.
In above-mentioned steps S5 and alternate embodiments thereof, while heating in tube furnace, by kovar alloyHeat with the even warm area of glass (powder) in tube furnace, when temperature programming, controlling programming rate is 4 DEG C/ min, and be warming up to 1100 DEG C, insulation 100min, when cooling, controlling rate of temperature fall is 5 DEG C/min, extremelyWhen being reduced to room temperature, temperature stops. The above-mentioned process heating up in tube furnace and lower the temperature is all in atmospheric conditionsUnder carry out.
Below in conjunction with some embodiment, the welding method of kovar alloy of the present invention and glass is explained in detailState.
Embodiment 1
The kovar alloy that carries out sealing-in with glass is provided, sand papering polishing is carried out in its surface, involutoryGold carries out Ultrasonic Cleaning, and uses absolute alcohol to clean, and dries up stand-by.
Use YAG laser instrument, under the control of laser head control system, laser head is to being positioned at machining areaAlloy scans remelting processing, and the condition of processing is atmosphere. Wherein, use optical maser wavelength for 1064nm'sLaser equipment, power is 200W, sweep speed 12mm/s.
Borosilicate glass dust is provided, borosilicate glass dust is carried out to briquet, glass blocks is putPut on the alloy of processing through remelting, send in tube furnace and heat. When heating, control programming rateBe 4 DEG C/min, and be warming up to 1100 DEG C, after insulation 100min, lower the temperature. When cooling, control coolingSpeed is 5 DEG C/min, while being reduced to room temperature, stops to temperature.
Embodiment 2
The kovar alloy that carries out sealing-in with glass is provided, sand papering polishing is carried out in its surface, involutoryGold carries out Ultrasonic Cleaning, and uses acetone to clean, and dries up stand-by.
Use carbon dioxide laser, under the control of laser head control system, laser head is to being positioned at processing districtThe alloy in territory scans remelting processing, and the condition of processing is oxygen. Wherein, using optical maser wavelength is 10640nmLaser equipment, power is 700W, sweep speed 26mm/s.
Borosilicate glass dust is provided, borosilicate glass dust is carried out to briquet, by glassPiece is placed on the alloy of processing through remelting, sends in tube furnace and heats. When heating, control and riseTemperature speed is 4 DEG C/min, and is warming up to 1100 DEG C, after insulation 100min, lowers the temperature. When cooling,Controlling rate of temperature fall is 5 DEG C/min, while being reduced to room temperature, stops to temperature.
Embodiment 3
The kovar alloy that carries out sealing-in with glass is provided, sand papering polishing is carried out in its surface, involutoryGold carries out Ultrasonic Cleaning, and uses acetone to clean, and dries up stand-by.
Use semiconductor laser, under the control of laser head control system, laser head is to being positioned at machining areaAlloy scan remelting processing, the condition of processing is atmosphere. Wherein, using optical maser wavelength is 880nmLaser equipment, power is 30W, sweep speed 2mm/s.
Borosilicate glass dust is provided, borosilicate glass dust is carried out to briquet, by glassPiece is placed on the alloy of processing through remelting, sends in tube furnace and heats. When heating, control and riseTemperature speed is 4 DEG C/min, and is warming up to 1100 DEG C, after insulation 100min, lowers the temperature. When cooling,Controlling rate of temperature fall is 5 DEG C/min, while being reduced to room temperature, stops to temperature.
The present invention is directed to the glass that welds together in above-described embodiment 1,2,3 and the weldability of kovar alloyThe test experiments that can carry out based on wetability angle of wetting, the step of this test experiments is as follows.
As shown in Figure 2, angle of wetting exceedes 90 ° for nonwetting, is less than 90 ° for wetting, and angle is less,Wettability (welding performance) is better.
The glass welding together and kovar alloy are warmed up to 1100 DEG C and be incubated 100 minutes in stove,Cooling rear taking-up in stove. Use is inlayed the resin that metallographic specimen uses alloy is closed together with glass,Use precision linear cutting machine to cut down along the middle of glass blocks, be then set into metallographic specimen. WarpCross after polishing, be placed under metallographic microscope and use low power to take the metallograph at glass blocks edge.
As shown in Figure 3, be the process laser remolten glass welding together after treatment and kovar in embodiment 1The metallograph of alloy angle of wetting. Wherein, add a long straight line L1, edge along the boundary of glass and metalGlass outward flange and draw straight line L2, these two straight lines intersect the angle (getting near glass side) forming and areAngle of wetting. Known according to measuring, this angle of wetting is 28.5 °, thereby shows after laser remolten is processed,Welding performance between glass and kovar alloy is very good.
Carry out similar test experiments for embodiment 2,3, wherein, in embodiment 2, angle of wetting is 30 °,In embodiment 3, angle of wetting is 26 °.
As shown in Figure 4, contrast property ground, through thermal oxide in advance, does not carry out laser treatment for not yetKovar alloy and glass blocks put into stove and carry out wetting experiment, be warmed up to 1100 DEG C and be incubated 100 minutes,After cooling, take out and test.
In photo, because angle of wetting is greater than 90 °, do not need to be prepared into metallographic specimen and observe, fromAnd kovar alloy and glass blocks do not weld together.
As shown in Figure 5, contrast property ground, protects at 700 DEG C for the kovar alloy that does not carry out laser treatmentTemperature 10min carries out thermal oxide in advance, and the whole surface of alloy forms layer of oxide layer. Then by the kovar after oxidationAlloy and glass blocks are put into stove and are carried out wetting experiment, are warmed up to 1100 DEG C and be incubated 100 minutes, cold in stoveBut, being prepared into metallographic specimen observes.
From metallograph, the angle of wetting in this comparative example between L3 and L4 is 45 °, its welding effectPoor compared with the welding effect of kovar alloy of the present invention and glass blocks.
In sum, the welding method of kovar alloy of the present invention and glass is by Optimizing Process Parameters, accurateControl laser remolten processing region, power ratio control, sweep speed, obtained specific modification region,So overcome the deficiency existing in existing pre-oxidation treatment mode.
In addition,, in the welding method of kovar alloy of the present invention and glass, adopt laser instrument to carry out straight line irradiationProcess kovar alloy surface, instead of adopt stove to process whole kovar alloy, not only reduced energySource waste, simultaneously owing to only the region of needs wetting (or sealing-in) being processed, other districts of alloyTerritory is not affected, thereby the performance of alloy (metal) is not worsened, and has improved military service performance.
The welding method of kovar alloy of the present invention and glass also possess energy controllability high, processing heat affected areaNarrow, working (machining) efficiency advantages of higher, can adapt to vibration monitoring better.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned example embodiment,And in the situation that not deviating from spirit of the present invention or essential characteristic, can realize with other concrete formThe present invention. Therefore, no matter from which point, all should regard embodiment as exemplary, and right and wrongRestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to fallAll changes in the implication and the scope that are equal to important document of claim are included in the present invention.
In addition although should be appreciated that this description is described according to embodiment, be not each enforcement,Mode only comprises an independently technical scheme, and this narrating mode of description is only for clarity sake,Those skilled in the art should make description as a whole, and the technical scheme in each embodiment also can be throughAppropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (9)
1. a welding method for kovar alloy and glass, is characterized in that, described kovar alloy and glassThe welding method of glass comprises the steps:
S1., the kovar alloy that carries out sealing-in with glass is provided;
S2. the kovar alloy providing is carried out to surface finish processing;
S3. again to cleaning through the kovar alloy of surface finish processing, after cleaning, dry up for subsequent use;
S4. laser instrument is under control system control, and Emission Lasers is swept the region to be processed of kovar alloyRetouch remelting processing;
S5. the glass welding with kovar alloy is positioned on the machining area of kovar alloy, and willKovar alloy and glass are sent in tube furnace and are heated, and carry out temperature programming when heating, after heating,Be incubated processing, then be cooled to room temperature.
2. the welding method of kovar alloy according to claim 1 and glass, is characterized in that, instituteState in step S2 when kovar alloy is carried out surface finish and processed, utilize sand paper to enter kovar alloy surfaceRow sanding and polishing.
3. the welding method of kovar alloy according to claim 1 and glass, is characterized in that, instituteState while cleaning in step S3, first carry out ultrasonic cleaning, recycling absolute alcohol or acetone clean.
4. the welding method of kovar alloy according to claim 1 and glass, is characterized in that, instituteThe thickness of stating kovar alloy is 0.5mm～10mm, described kovar alloy through remelting process after, rough surfaceDegree is less than the twice of the front kovar alloy surface roughness of remelting processing.
5. the welding method of kovar alloy according to claim 1 and glass, is characterized in that, instituteState in step S4, the sharp light wavelength of transmitting is 800～10640nm, and power is 30～700W, sweep speedBe 2～26mm/s.
6. the welding method of kovar alloy according to claim 1 and glass, is characterized in that, instituteStating laser instrument is YAG laser instrument, carbon dioxide laser or semiconductor laser.
7. the welding method of kovar alloy according to claim 1 and glass, is characterized in that, instituteStating step S5 also comprises:
S51., glass dust is provided, is positioned in cylinder, then cylinder is positioned under forcing press, in 5MPaLower pressurization, forms glass blocks;
S52. glass blocks is positioned on the machining area of kovar alloy, and kovar alloy and glass blocks are sentEnter in tube furnace and heat, when heating, carry out temperature programming, after heating, be incubated processing, thenBe cooled to room temperature.
8. according to the kovar alloy described in claim 1 or 7 and the welding method of glass, it is characterized in that,While heating in tube furnace, the even warm area in tube furnace heats, and when temperature programming, speed heats upDegree is 4 DEG C/min, is warming up to 1100 DEG C, insulation 100min, and when cooling, controlling rate of temperature fall is 5 DEG C/min,While being reduced to room temperature to temperature, stop.
9. according to the kovar alloy described in claim 1 or 7 and the welding method of glass, it is characterized in that,In tube furnace, heat up and lower the temperature and carry out under atmospheric conditions.
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| CN104788024B (en) * | 2015-03-10 | 2017-12-15 | 北京工业大学 | A kind of method that metal surface wetability is improved using high energy beam texturing |
| CN112756779A (en) * | 2020-12-14 | 2021-05-07 | 江苏奥雷光电有限公司 | Welding method of tungsten-copper alloy and thin plate kovar alloy |
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| GB989365A (en) * | 1961-03-29 | 1965-04-14 | Philco Corp | Improvements in or relating to the production of glass-to-metal seals |
| CN101786805A (en) * | 2009-12-25 | 2010-07-28 | 北京天瑞星真空技术开发有限公司 | Sealing method of borosilicate glass and kovar alloy of solar collector tube |
| CN102030486A (en) * | 2010-10-15 | 2011-04-27 | 北京工业大学 | Glass-kovar alloy laser welding method and special fixture therefore |
| CN103172277A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Hermetic seal method of optical glass and Kovar alloy |
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2014
- 2014-04-24 CN CN201410169153.9A patent/CN103922613B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB989365A (en) * | 1961-03-29 | 1965-04-14 | Philco Corp | Improvements in or relating to the production of glass-to-metal seals |
| CN101786805A (en) * | 2009-12-25 | 2010-07-28 | 北京天瑞星真空技术开发有限公司 | Sealing method of borosilicate glass and kovar alloy of solar collector tube |
| CN102030486A (en) * | 2010-10-15 | 2011-04-27 | 北京工业大学 | Glass-kovar alloy laser welding method and special fixture therefore |
| CN103172277A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Hermetic seal method of optical glass and Kovar alloy |
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