CN108161274A - It is a kind of for sealing-in solder of electron tube and preparation method thereof - Google Patents
It is a kind of for sealing-in solder of electron tube and preparation method thereof Download PDFInfo
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- CN108161274A CN108161274A CN201711202707.0A CN201711202707A CN108161274A CN 108161274 A CN108161274 A CN 108161274A CN 201711202707 A CN201711202707 A CN 201711202707A CN 108161274 A CN108161274 A CN 108161274A
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- solder
- sealing
- annealing
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- electron tube
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
It is a kind of for sealing-in solder of electron tube and preparation method thereof, the brazing filler metal alloy ingredient and weight percent are:Cu:30~45, Ni:0.1~2.0, Ti:0~2.0, In:0~5.0, Ag:Surplus.The present invention improves the corrosion resistance and wetability of solder, and solder processing performance is good by adding Ni, Ti, In element in solder.According to alloying component dispensing, alloy ingot blank is prepared using vacuum melting horizontal continuous casting technology and equipment.Ingot blank passes through roughing, intermediate annealing, multiroll rolling and continuous bright annealing technology, can obtain the silver-base solder band of 0.01~1.00mm of thickness.Ingot blank obtains the silver-base solder silk material of diameter 0.1mm~3.0mm by rough, intermediate annealing, accurate drawing and online annealing treatment process.Brazing property is excellent, suitable for the sealing-in and soldering of electron tube.
Description
Technical field
The present invention relates to a kind of silver-base solders and preparation method thereof, belong to welding technology field.
Background technology
Electron tube plays a crucial role in the fields such as military radar, communication, navigation.At civilian aspect,
The demand of the devices such as high-power pulsed magnetron, accelerating tube, microwave communication amplifier also increasingly increases severely.Electron tube is by gold
Category is connected and composed with nonmetallic materials, and soldering is to be welded below base material fusion temperature and connector residual stress is smaller, can
Ensure the structure of precision component and size requirement, be therefore widely used in electron tube sealing-in.
Due to the advantages that Ag72Cu28 solder fusing points are moderate, wettability is good, seam-filling ability is strong, it is widely used in electric true
Pocket part connects, such as stainless steel, kovar alloy, high temperature alloy, and soldering strength is high, and joint quality is good.However, silver belongs to expensive
Metal is the non-renewable resources of state control, and the silver content in solder should be controlled for sustainable development.With China's electric power,
The fast development in the fields such as space flight, aviation, military affairs, the demand to Ag72Cu28 solders are on the increase, and China's scarce resource faces
Huge challenge.Therefore, develop the high-quality welded available for electron tube, low cost, low silver content solder compel in eyebrow
Eyelash.
Invention content
The present invention provides a kind of electron tube silver-base solder and preparation method thereof, it is therefore intended that by improving silver-based pricker
Expect ingredient, reduce the silver content and production cost of solder, obtain the silver-base solder with good brazing property and processing performance.
In order to achieve the above object, the present invention provides following technical solution:
A kind of sealing-in solder for electron tube, alloy composition and weight percent are:Cu:30~45,
Ni:0.1~2.0, Ti:0~5.0, In:0~5.0, Ag:Surplus.
Sealing-in solder as described above, it is preferable that the weight percent of Ti is 0.001~5.0 in the sealing-in solder.
Sealing-in solder as described above, it is preferable that the weight percent of In is 0.001~5.0 in the sealing-in solder.
Sealing-in solder as described above, it is preferable that the sealing-in solder is the band of thickness range 0.01mm~1.00mm
Or the silk material of diameter range 0.1mm~3.0mm.
On the other hand, the present invention provides application of the sealing-in solder as described above in sealing-in electron tube, the envelope
The material for connecing solder brazing is ceramics/ceramics in electron tube, ceramic/metal or metal/metal.
In another aspect, the present invention provides the preparation method of sealing-in solder as described above, include the following steps:
(1) using silver, copper, titanium, indium and CuNi10 intermediate alloys as raw material, match according to following component and weight percentage
Material;Cu:30~45, Ni:0.1~2.0, Ti:0.001~5.0, In:0.001~5.0, Ag:Surplus;
(2) raw metal weighed is placed on to the Al of Vacuum Horizontal Continuous Casting Machine2O3In ceramic crucible, it is heated to 1100 DEG C
~1200 DEG C of progress vacuum meltings, are drawn, shape and sized ingots needed for acquisition by crystallizer cooling and drawing device;
(3) ingot casting prepared by step (2) obtains thick by roughing, intermediate annealing, multiroll rolling and continuous bright annealing
Spend the band of 0.01mm~1.00mm;
Alternatively, ingot casting prepared by step (2) obtains diameter by rough, intermediate annealing, accurate drawing and online annealing
The silk material of 0.1mm~3.0mm.
Preparation method as described above, it is preferable that silver in the step (1), copper, titanium, indium degree of purity be 99.99%.
Preparation method as described above, it is preferable that melting vacuum degree is less than 10 in the step (2)-2Pa, blank traction speed
It spends for 1mm/s~1.5mm/s.
Preparation method as described above, it is preferable that the single pass working modulus 10 of multiroll rolling in the step (3)~
20%.
Preparation method as described above, it is preferable that prepare band in the step (3) or the intermediate anneal temperature of silk material is equal
It is 550 DEG C~600 DEG C, annealing time 2~4 hours.
Preparation method as described above, it is preferable that continuous bright annealing temperature is 560 DEG C~600 in the step (3)
DEG C, protective atmosphere is nitrogen.
Preparation method as described above, it is preferable that online annealing temperature is 560 DEG C~600 DEG C in the step (3).
The advantageous effect of technical solution of the present invention:
1st, added in brazing filler metal alloy suitable Ni can refining alloy microscopic structure, improve mobility and the soldering of solder
Property, the formation of alloy surface oxidizing slag is reduced, improves the anti-dropping capability of solder welding spot.But Ni too high levels can cause solder to melt
Point increases, and solid-liquid phase line interval is excessive, is unfavorable for being formed good soldered fitting, thus preferably Ni constituent contents for 0.1~
2.0wt%.In can form solid solution with Ag, Cu, Ni, can suitably reduce the solid, liquid phase of solder simultaneously as anti-oxidizing elements
Line temperature reduces brazing filler metal melts section, improves the mobility of solder.Ti elements are added, wetability of the solder to ceramics can be improved.
2nd, silver-base solder prepared by the present invention is successfully applied to ceramics/ceramics, ceramic/metal, gold in electron tube
Category/metal welding.
3rd, silver-base solder prepared by the present invention, form are foil and silk material, and surface quality is good, and dimensional accuracy is high, color and luster
It is bright.
4th, preparation method processing cost provided by the invention is low, and production efficiency is high, convenient for industrialization promotion.
Description of the drawings
Fig. 1 is the process flow chart that the present invention prepares silver-based alloy solder.
Fig. 2 is that each solder sprawls experiment photo in experimental example 1.
Specific embodiment
As shown in Figure 1, the technological process that the present invention prepares silver-base solder includes:Raw material is prepared, vacuum level continuous casting, slightly
It rolls, intermediate annealing, multiroll rolling, continuous bright annealing;Or vacuum level continuous casting, rough, intermediate annealing, accurate drawing,
Line annealing and etc..Concrete operation step is as follows:
A. it is according to chemical composition and weight percent:Cu:30~45, Ni:0.1~2.0, Ti:0~5.0, In:0~
5.0, Ag:Surplus dispensing, said components total amount 100%;
B. Al Ag, Cu, Ni, In, CuNi10 alloy raw material weighed being placed in Vacuum Horizontal Continuous Casting Machine2O3Ceramics
In crucible, 1100 DEG C~1200 DEG C are heated to, melting 30~45 minutes is drawn after being cooled down by crystallizer by drawing device,
Blank hauling speed is 1mm/s~1.5mm/s, obtains required shape and sized ingots;
C. when required solder form is band, by ingot casting made from step B after roughing, in 550 DEG C~600 DEG C progress
Intermediate annealing, annealing time 2~4 hours.Ingot blank progress multiroll rolling after annealing, single pass working modulus 10%~20%, later
Continuous bright annealing is carried out at 560 DEG C~600 DEG C, obtains the band of thickness 0.01mm~1.00mm.
When required solder form is silk material, by ingot casting made from step B after rough, in 550 DEG C~600 DEG C carry out
Between anneal, annealing time 2~4 hours.Ingot blank carries out accurate drawing, single pass working modulus 10%~20%, Zhi Hou after annealing
560 DEG C~600 DEG C progress online annealings obtain the silk material of diameter 0.1mm~3.0mm.Comparative example 1 electron tube silver-based pricker
Material strip material
3000 grams and 20000 grams 27000 grams of the silver that purity is 99.99%, copper CuNi10 intermediate alloy dispensings are weighed, true
The Al of empty horizontal caster2O3Melting in ceramic crucible, 1200 DEG C of smelting temperature, smelting time 45 minutes, vacuum degree are less than 10- 2Pa.It is drawn by crystallizer cooling and drawing device, blank hauling speed is 1mm/s, obtains width 200mm, thickness 10mm,
The ingot casting of length 2000mm.Intermediate annealing is carried out after ingot casting roughing, intermediate anneal temperature is 580 DEG C, annealing time 2 hours.It moves back
After fire, strip is handled through multiroll rolling and continuous bright annealing, rolling single pass working modulus 15%, continuous bright annealing temperature
It it is 560 DEG C, protective atmosphere is nitrogen.Obtain the silver-base solder band of thickness 0.05mm.Its chemical composition and weight percent are:
Cu:42, Ni:4.0, Ag:Surplus.
1 electron tube of embodiment is with silver-base solder band (one)
16500 grams and 5000 grams 28500 grams of the silver that purity is 99.99%, copper CuNi10 intermediate alloy dispensings are weighed, true
The Al of empty horizontal caster2O3Melting in ceramic crucible, 1150 DEG C of smelting temperature, smelting time 45 minutes, vacuum degree are less than 10- 2Pa.It is drawn by crystallizer cooling and drawing device, blank hauling speed is 1mm/s, obtains width 200mm, thickness 10mm,
The ingot casting of length 2000mm.Intermediate annealing is carried out after ingot casting roughing, intermediate anneal temperature is 560 DEG C, annealing time 2 hours.It moves back
After fire, strip is handled through multiroll rolling and continuous bright annealing, rolling single pass working modulus 15%, continuous bright annealing temperature
It it is 560 DEG C, protective atmosphere is nitrogen.Obtain the silver-base solder band of thickness 0.05mm.Its chemical composition and weight percent are:
Cu:42, Ni:1.0, Ag:Surplus.
2 electron tube of embodiment is with silver-base solder (two)
Weigh 28250 grams of the silver that purity is 99.99%, copper 16500 grams and 5000 grams CuNi10 intermediate alloys, purity are
99.99% 250 grams of dispensings of titanium, in the Al of Vacuum Horizontal Continuous Casting Machine2O3Melting in ceramic crucible, 1150 DEG C of smelting temperature, melting
45 minutes time, vacuum degree are less than 10-2Pa.It is drawn by crystallizer cooling and drawing device, blank hauling speed is 1mm/s,
Obtain width 200mm, thickness 10mm, the ingot casting of length 2000mm.Intermediate annealing is carried out after ingot casting roughing, intermediate anneal temperature is
560 DEG C, annealing time 2 hours.After annealing, strip is handled through multiroll rolling and continuous bright annealing, rolling single pass processing
Rate 15%, continuous bright annealing temperature are 560 DEG C, and protective atmosphere is nitrogen.Obtain the silver-base solder band of thickness 0.05mm.Its
Chemical composition and weight percent are:Cu:42, Ni:1.0, Ti:0.5, Ag:Surplus.
3 electron tube of embodiment is with silver-base solder (three)
Weigh 28000 grams of the silver that purity is 99.99%, copper 16500 grams and 5000 grams CuNi10 intermediate alloys, purity are
99.99% 250 grams of titanium, 250 grams of dispensings of indium that purity is 99.99%, in the Al of Vacuum Horizontal Continuous Casting Machine2O3In ceramic crucible
Melting, 1150 DEG C of smelting temperature, smelting time 45 minutes, vacuum degree are less than 10-2Pa.It is led by crystallizer cooling and drawing device
Draw, blank hauling speed is 1mm/s, obtains width 200mm, thickness 10mm, the ingot casting of length 2000mm.It is carried out after ingot casting roughing
Intermediate annealing, intermediate anneal temperature are 550 DEG C, annealing time 2 hours.After annealing, strip is through multiroll rolling and continuous bright
Annealing, rolling single pass working modulus 15%, continuous bright annealing temperature is 560 DEG C, and protective atmosphere is nitrogen.Obtain thickness
The silver-base solder band of 0.05mm.Its chemical composition and weight percent are:Cu:42, Ni:1.0, Ti:0.5, In:0.5, Ag:
Surplus.
4 electron tube of embodiment is with silver-base solder (four)
Weigh 28000 grams of the silver that purity is 99.99%, copper 16500 grams and 5000 grams CuNi10 intermediate alloys, purity are
99.99% 250 grams of titanium, 250 grams of dispensings of indium that purity is 99.99%, in the Al of Vacuum Horizontal Continuous Casting Machine2O3In ceramic crucible
Melting, 1150 DEG C of smelting temperature, smelting time 45 minutes, vacuum degree are less than 10-2Pa.It is led by crystallizer cooling and drawing device
Draw, blank hauling speed is 1.5mm/s, obtains diameter of phi 8mm, the ingot casting of length 25mm.Intermediate annealing is carried out after ingot casting is rough,
Intermediate anneal temperature is 550 DEG C, annealing time 2 hours.Wire rod is through accurate drawing and online annealing, drawing single pass after annealing
Working modulus 15%, online annealing temperature are 560 DEG C, obtain the silk material of diameter 0.1mm.Its chemical composition and weight percent are:
Cu:42, Ni:1.0, Ti:0.5, In:0.5, Ag:Surplus.
Experimental example 1
First, the solder prepared respectively to comparative example 1 and embodiment 1-4 carries out fusing point test, obtains test data and is shown in Table 1.
The fusing point of 1 solder of table
Solid-state temperature | Liquidus temperature | Solid-liquid interval delta T | |
Comparative example | 787.1℃ | 825.3℃ | 38.2℃ |
Embodiment 1 | 761.5℃ | 793.0℃ | 31.5℃ |
Embodiment 2 | 762.0℃ | 793.2℃ | 31.2℃ |
Embodiment 3 | 757.2℃ | 776.9℃ | 19.7℃ |
Embodiment 4 | 756.8℃ | 776.2℃ | 19.4℃ |
2nd, it is carried out on kovar alloy in 850 DEG C sprawling experiment with solder prepared by comparative example and embodiment 1-3 respectively,
The results are shown in Figure 2,1 solder of (a) comparative example, 1 solder of (b) embodiment, 2 solder of (c) embodiment, 3 solder of (d) embodiment.Such as
Shown in Fig. 2-d, rectangular centre is solder sample 2, and bottom plate is kovar alloy 1, and wetted part is to sprawl area 3 between sample and bottom plate,
It is best to compare the solder spreading property that each laboratory sample understands prepared by embodiment 3.
3rd, the solder prepared respectively with comparative example and embodiment 1-3 is to electron tube 95Al2O3Ceramics/kovar alloy
Sealing-in is carried out, sealing strength test result is shown in Table 2.
2 sealing strength test result of table
Sealing strength | |
Comparative example | 91.5MPa |
Embodiment 1 | 95.2MPa |
Embodiment 2 | 103.7MPa |
Embodiment 3 | 110.5MPa |
The embodiment of silver based soldering alloy part of the present invention is only enumerated in above-described embodiment, in the technical side of the invention described above
In case:The content of described alloy compositions Ag, Cu, Ni, Ti, the In in prescribed limit can unrestricted choice, no longer arrange one by one herein
It lifts, therefore the technical solution that above description is included should be regarded as protection model illustrative rather than to limit the present patent application patent
It encloses.
Claims (10)
1. a kind of sealing-in solder for electron tube, which is characterized in that the alloy composition and weight of the sealing-in solder
Percentage is:Cu:30~45, Ni:0.1~2.0, Ti:0~5.0, In:0~5.0, Ag:Surplus.
2. sealing-in solder according to claim 1, which is characterized in that the weight percent of Ti is in the sealing-in solder
0.001~5.0.
3. sealing-in solder according to claim 1, which is characterized in that the weight percent of In is in the sealing-in solder
0.001~5.0.
4. sealing-in solder according to any one of claim 1-3, which is characterized in that the sealing-in solder is thickness range
The band of 0.01mm~1.00mm or the silk material of diameter range 0.1mm~3.0mm.
5. application of the sealing-in solder in sealing-in electron tube described in any one of claim 1-4, which is characterized in that institute
The material for stating sealing-in solder brazing is ceramics/ceramics in electron tube, ceramic/metal or metal/metal.
6. the preparation method of the sealing-in solder described in any one of claim 1-4, which is characterized in that this method includes following step
Suddenly:
(1) using silver, copper, titanium, indium and CuNi10 intermediate alloys as raw material, according to the ingredient and weight percentage dispensing;
(2) raw metal weighed is placed on to the Al of Vacuum Horizontal Continuous Casting Machine2O3In ceramic crucible, be heated to 1100 DEG C~
1200 DEG C of progress vacuum meltings, are drawn, shape and sized ingots needed for acquisition by crystallizer cooling and drawing device;
(3) ingot casting prepared by step (2) obtains thickness by roughing, intermediate annealing, multiroll rolling and continuous bright annealing
The band of 0.01mm~1.00mm;
Alternatively, ingot casting prepared by step (2) obtains diameter by rough, intermediate annealing, accurate drawing and online annealing
The silk material of 0.1mm~3.0mm.
7. according to the preparation method described in claim 4, which is characterized in that melting vacuum degree is less than 10 in the step (2)- 2Pa, blank hauling speed are 1mm/s~1.5mm/s.
8. according to the preparation method described in claim 4, which is characterized in that the single pass of multiroll rolling in the step (3)
Working modulus 10~20%.
9. according to the preparation method described in claim 4, which is characterized in that prepare band or silk material in the step (3)
Intermediate anneal temperature is 550 DEG C~600 DEG C, annealing time 2~4 hours.
10. according to the preparation method described in claim 4, which is characterized in that continuous bright annealing temperature in the step (3)
It it is 560 DEG C~600 DEG C, protective atmosphere is nitrogen;Alternatively, online annealing temperature is 560 DEG C~600 DEG C in the step (3).
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110695567A (en) * | 2019-10-21 | 2020-01-17 | 北京航空航天大学 | Silver-based brazing filler metal with low melting point and high plasticity |
CN111375855A (en) * | 2018-12-27 | 2020-07-07 | 丹阳荣鼎金粉科技有限公司 | Heat sink with precision alloy and tungsten-copper alloy composite structure and manufacturing method thereof |
CN112059468A (en) * | 2019-07-26 | 2020-12-11 | 昆明贵金属研究所 | Silver-based brazing filler metal alloy, preparation method thereof, and preparation methods of foil strip and wire material |
CN112518174A (en) * | 2020-12-04 | 2021-03-19 | 杭州华光焊接新材料股份有限公司 | Low-silver solder for welding electric vacuum device and preparation method thereof |
CN114393345A (en) * | 2021-12-30 | 2022-04-26 | 无锡日月合金材料有限公司 | Low-silver vacuum solder with small temperature difference of melting point and flow point |
CN114654131A (en) * | 2020-12-23 | 2022-06-24 | 丹阳市凯鑫合金材料有限公司 | Preparation method of high-temperature-resistant corrosion-resistant nickel-based alloy welding wire |
CN115255716A (en) * | 2022-08-26 | 2022-11-01 | 郑州机械研究所有限公司 | Solder alloy, silver ornament solder, and preparation method and application thereof |
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CN111375855A (en) * | 2018-12-27 | 2020-07-07 | 丹阳荣鼎金粉科技有限公司 | Heat sink with precision alloy and tungsten-copper alloy composite structure and manufacturing method thereof |
CN112059468A (en) * | 2019-07-26 | 2020-12-11 | 昆明贵金属研究所 | Silver-based brazing filler metal alloy, preparation method thereof, and preparation methods of foil strip and wire material |
CN112059468B (en) * | 2019-07-26 | 2021-12-24 | 昆明贵金属研究所 | Silver-based brazing filler metal alloy, preparation method thereof, and preparation methods of foil strip and wire material |
CN110695567A (en) * | 2019-10-21 | 2020-01-17 | 北京航空航天大学 | Silver-based brazing filler metal with low melting point and high plasticity |
CN112518174A (en) * | 2020-12-04 | 2021-03-19 | 杭州华光焊接新材料股份有限公司 | Low-silver solder for welding electric vacuum device and preparation method thereof |
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CN114654131A (en) * | 2020-12-23 | 2022-06-24 | 丹阳市凯鑫合金材料有限公司 | Preparation method of high-temperature-resistant corrosion-resistant nickel-based alloy welding wire |
CN114393345A (en) * | 2021-12-30 | 2022-04-26 | 无锡日月合金材料有限公司 | Low-silver vacuum solder with small temperature difference of melting point and flow point |
CN115255716A (en) * | 2022-08-26 | 2022-11-01 | 郑州机械研究所有限公司 | Solder alloy, silver ornament solder, and preparation method and application thereof |
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