CN103921012B - Preparation method of tungsten-cobalt solder for cathode and preparation method of brazed assembly - Google Patents
Preparation method of tungsten-cobalt solder for cathode and preparation method of brazed assembly Download PDFInfo
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- CN103921012B CN103921012B CN201410135956.2A CN201410135956A CN103921012B CN 103921012 B CN103921012 B CN 103921012B CN 201410135956 A CN201410135956 A CN 201410135956A CN 103921012 B CN103921012 B CN 103921012B
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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
- B23K35/3046—Co as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- 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
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a preparation method of a tungsten-cobalt solder for a cathode and a preparation method of a brazed assembly. The preparation method comprises the following steps: reducing tungsten powder and cobalt powder; grinding the mixture of the reduced tungsten powder and cobalt powder to obtain tungsten-cobalt solder; wherein the weight ratio of the tungsten powder to the cobalt powder is 1: 2-5. The invention also provides a preparation method of the brazing assembly and application of the brazing assembly in a cathode assembly. According to the invention, the tungsten powder and the cobalt powder are subjected to high-temperature reduction to improve the purity of the tungsten powder and the cobalt powder, and the mixture of the tungsten powder and the cobalt powder after reduction in a certain proportion is ground, so that the particle size of the tungsten powder and the cobalt powder is greatly reduced, the uniformity of the tungsten powder and the cobalt powder is improved, and meanwhile, the mixture of the tungsten powder and the cobalt powder after reduction is controlled in a certain proportion, so that the precipitation of a cathode active substance in the welding process can be prevented, and the stability of a cathode substrate is improved.
Description
Technical field
The present invention relates to the preparation method of a kind of tungsten cobalt solder for negative electrode and the preparation side of brazed assembly
Method.
Background technology
In prior art, large-sized travelling-wave tubes cathode base is typically by by refractory metal powder punching press
Make cylindric, then make through high temperature sintering, leaching salt, twice Vehicle Processing and the process of soldering operation.At this
In production technology, welding between spongy body of tungsten and the molybdenum cylinder supporting it is that complete must in cathode base preparation
Indispensable operation.Traditional welding procedure has cathode electron beam weldering and laser beam weldering, but often occurs
Protective gas improper use thus cause the be full of cracks of molybdenum cylinder, embrittlement, in turn result in and come off, welding simultaneously
Journey requires welded and keep between spongy body of tungsten and molybdenum cylinder closely cooperating, otherwise easily cause molybdenum cylinder and first melt
Shrink, cause welding, and be also difficult to ensure that spongy body of tungsten is tight everywhere with molybdenum cylinder after easily causing welding
Closely connected reality, although the two to the eye firm welding.Above-mentioned a variety of causes all can cause because of welding
Improper cause cathode base yield rate relatively low.In order to make up these shortcomings, by between by weldering parent
Fill solder at gap and carry out soldering, reduce part match tolerance with this, thus meet large scale travelling-wave tubes
The requirement of negative electrode development.
When filling solder between spongy body of tungsten and the molybdenum cylinder supporting it, owing to welding gap size is uneven
Even, thus the weld seam siphonage when soldering can be caused uneven, use conventional solder preparation method system
Standby solder can cause the solder when soldering can not fully flow in weld seam so that solder is at spongy body of tungsten end
Form myomata on face and molybdenum cylinder sidewall, cause solder attachment power difference, so that sand holes occur in weld seam,
The phenomenons such as molybdenum cylinder comes off from spongy body of tungsten even occur, affects brazing quality.
Accordingly, it would be desirable to a kind of soldering uniformity is good, material trickling property is good, and what soldering strength was high is used for negative electrode
The preparation method of tungsten cobalt solder.
Content of the invention
The brazing material uniformity that it is an object of the invention to overcome prior art to prepare is not good, trickling property not
Enough, the feature of soldering strength difference, provides a kind of soldering uniformity good, and material trickling property is good, soldering strength
The preparation method of the high tungsten cobalt solder for negative electrode, and use the system of the brazed assembly of this tungsten cobalt solder
Preparation Method and application.
To achieve these goals, the present invention provides the preparation method of a kind of tungsten cobalt solder for negative electrode,
Wherein, the method includes:
(1) tungsten powder and cobalt powder are reduced；
(2) mixture of the tungsten powder after reduction and cobalt powder is ground, obtains tungsten cobalt solder；
Wherein, the weight of described tungsten powder and described cobalt powder is than for 1:2-5.
Present invention also offers the preparation method of a kind of brazed assembly, wherein, the method includes following work
Sequence:
(1) operation of tungsten cobalt solder is prepared by above-mentioned method；
(2) it is fixed on molybdenum cylinder 9 on spongy body of tungsten 10, and by described tungsten cobalt fill solder to described molybdenum
Cylinder 9 inwalls, with the solder bath 11 of the edge formation of described spongy body of tungsten 10 depression, form assembly
Operation；
(3) cool down after described assembly being heated, obtain the operation of brazed assembly.
Present invention also offers tungsten cobalt solder prepared by the above-mentioned preparation method application in cathode base.
The present invention is improved the purity of tungsten powder and cobalt powder by tungsten powder and cobalt powder carry out high temperature reduction, and by one
The mixture of the tungsten powder after the reduction of certainty ratio and cobalt powder is ground, thus it is big to greatly reduce its particle
Little, improve its uniformity, meanwhile, by controlling the mixture of the tungsten powder after reduction and cobalt powder one
Fixed ratio, is prevented from the precipitation of cathode active material during welding, thus adds negative electrode
The stability of matrix.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Brief description
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of specification, with
Detailed description below is used for explaining the present invention together, but is not intended that limitation of the present invention.?
In accompanying drawing:
Fig. 1 represent for the reduction to the present invention after tungsten powder and the device that is ground of the mixture of cobalt powder
Schematic diagram；
Fig. 2 represents the schematic diagram of the assembly for preparing brazed assembly that the present invention provides.
Description of reference numerals
1-the first agate ball 2-the second agate ball
3-agate tank 4-the first lid
5-the second lid 6-outer cover
7-fixes bolt 8-nut
9-molybdenum cylinder 10-spongy body of tungsten
11-solder bath.
Detailed description of the invention
It is described in detail below in conjunction with the detailed description of the invention to the present invention for the accompanying drawing.It should be appreciated that
Detailed description of the invention described herein is merely to illustrate and explains the present invention, is not limited to this
Bright.
The invention provides the preparation method of a kind of tungsten cobalt solder for negative electrode, wherein, the method includes:
(1) tungsten powder and cobalt powder are reduced；
(2) mixture of the tungsten powder after reduction and cobalt powder is ground, obtains tungsten cobalt solder；
Wherein, the weight of described tungsten powder and described cobalt powder is than for 1:2-5.
In the present invention, in order to more efficiently prevent from the analysis of cathode active material during welding
Going out, the weight of preferably described tungsten powder and described cobalt powder is than for 1:2.5-4.5；More preferably 1:3-4.
In the present invention, in order to the reduction reaction making tungsten powder and cobalt powder is more thorough so as to get tungsten powder and
The purity of cobalt powder is higher, in step (1), under the method for reducing tungsten powder and cobalt powder can be
Method A stated or method B.
Tungsten powder and cobalt powder are heat-treated by method A: under an atmosphere of hydrogen respectively.
The mixture of tungsten powder and cobalt powder is heat-treated by method B: under an atmosphere of hydrogen.
When using described method A to be heat-treated, described heat treatment for respectively by tungsten powder and cobalt powder with
The programming rate of 40-180 DEG C/min is warming up to 700-1050 DEG C, and is incubated 30min-1h at such a temperature；
Preferably, described heat treatment is for heating up tungsten powder and cobalt powder with the programming rate of 65-120 DEG C/min respectively
It to 780-960 DEG C, and is incubated 35-45min at such a temperature.
When using described method B to be heat-treated, described heat treatment is for by the mixture of tungsten powder and cobalt powder
It is warming up to 700-1050 DEG C with the programming rate of 40-180 DEG C/min, and be incubated at such a temperature
30min-1h；Preferably, described heat treatment is with 65-120 DEG C/min's by the mixture of tungsten powder and cobalt powder
Programming rate is warming up to 780-960 DEG C, and is incubated 35-45min at such a temperature.
In the present invention, in order to reach more preferable reaction effect, tungsten powder and cobalt powder and hydrogen are most optimally increased
The contact area of gas, molybdenum bowl, for being respectively placed in molybdenum bowl tungsten powder and cobalt powder, is put by preferably described heat treatment
In drying bottle, and drying bottle is placed in molybdenum pipe hydrogen furnace and is heat-treated；Or by tungsten powder and cobalt powder
Mixture be placed in molybdenum bowl, be placed in molybdenum bowl in drying bottle, and drying bottle be placed in molybdenum pipe hydrogen furnace
It is heat-treated；
Additionally, for the contact area better ensuring that tungsten powder and cobalt powder and hydrogen, wherein, with molybdenum bowl
Capacity is 100 parts by volume, and the consumption of described tungsten powder and/or cobalt powder is 1-67 parts by volume；Preferably, with
The capacity of molybdenum bowl is 100 parts by volume, and the consumption of described tungsten powder and/or cobalt powder is 20-50 parts by volume.
Here, " capacity with molybdenum bowl is 100 parts by volume, and the consumption of described tungsten powder and/or cobalt powder is 1-67
Parts by volume " refers to: when tungsten powder and cobalt powder are respectively placed in molybdenum bowl is heat-treated when, with the appearance of molybdenum bowl
Amount is 100 parts by volume, and the consumption of described tungsten powder or cobalt powder is 1-67 parts by volume；When by tungsten powder and cobalt powder
Mixture be placed in when molybdenum bowl is heat-treated, the consumption of the mixture of described tungsten powder and cobalt powder is 1-67
Parts by volume.
In the present invention, described grinding can use various methods known in the art to carry out.In order to
Making the compound particles after grinding be more uniformly distributed, in brazing process, trickling property is more preferable, and described grinding is preferably
Carry out in accordance with the following methods:
(1) it is positioned over the mixture of the tungsten powder after reduction and cobalt powder in the agate tank 3 containing agate ball；
(2) the agate tank 3 being placed with tungsten powder and cobalt powder mixture is sealed；
(3) the agate tank 3 after sealing carries out spin finishing.
In the present invention, in order to make grinding effect more preferable, it is preferable that described agate ball includes 20-40
Second agate ball 2 of first 1 and 30-50 a diameter of 5-15mm of agate ball of a diameter of 10-20mm.
In order to ensure on the premise of reaching required grinding effect, can higher promote grinding efficiency,
In above-mentioned steps (3), described spin finishing is carried out in ball mill, and the rotating speed of described ball mill is arranged
For 60-120 rev/min, ball milling 40-80 minute；Preferably, the rotating speed of described ball mill is set to 80-100
Rev/min, ball milling 50-65 minute.
Present invention also offers the preparation method of a kind of brazed assembly, it is characterised in that the method includes
Following operation:
(1) operation of tungsten cobalt solder is prepared by above-mentioned method；
(2) it is fixed on molybdenum cylinder 9 on spongy body of tungsten 10, and by described tungsten cobalt fill solder to described molybdenum
Cylinder 9 inwalls, with the solder bath 11 of the edge formation of described spongy body of tungsten 10 depression, form assembly
Operation；
(3) cool down after described assembly being heated, obtain the operation of brazed assembly.
In the present invention, as in figure 2 it is shown, described molybdenum cylinder 9 is cylinder-like structure；Described spongy body of tungsten 10
It is three grades of stepped cylindrical body structures.With described spongy body of tungsten bottom for first order cylinder step, successively
It is up respectively second level cylinder step and third level cylinder step (described first order step, described
The diameter of second level step and described third level step is than for 1:0.6-0.9:0.5-0.75, described first order platform
Rank, described second level step and the aspect ratio of described third level step are 1:1.2-2:0.2-0.5), cylinder
Step diameter from the bottom up successively decreases successively, the periphery of the second level cylinder step of described spongy body of tungsten 10
The internal perisporium of wall and described molybdenum cylinder 9 is close to, and forms described depression.Described first order cylinder step end face
There is gap with described molybdenum cylinder 9 bottom surface.
In order to avoid the pollution to brazed assembly for the excessive tungsten cobalt solder, it is preferable that the method also includes,
In step (2), with the tungsten cobalt solder outside needle cleaning solder bath 11.
In the present invention, described heating and cooling is preferably carried out in molybdenum pipe hydrogen furnace.In order to effectively protect
The qualification rate of card brazed assembly, it is preferable that described heating includes the first intensification section and the second intensification section, institute
The programming rate stating the first intensification section with 80-120 DEG C/min is warming up to 1200-1600 DEG C, insulation
0.5-1.5min, described second intensification section is warming up to 1500-1720 DEG C with the programming rate of 30-50 DEG C/min,
Insulation 5-25s.Described cooling includes the first temperature descending section and the second temperature descending section, described first temperature descending section with
The cooling rate of 30-50 DEG C/min is cooled to 1120-1450 DEG C, and described second temperature descending section is with 80-120 DEG C
After the cooling rate of/min is cooled to 15-35 DEG C and keep 10-15min.
Present invention also offers application in cathode base for a kind of tungsten cobalt solder prepared by said method.
Below by embodiment, the present invention is described in detail, but the present invention is not limited in following reality
Execute example.
In the preparation example of the present invention, it is 99.9% that described tungsten powder and cobalt powder are commercially available purity, particle diameter model
Enclose for 3-5 μm.
In the preparation example of the present invention, tungsten powder and the mixture of cobalt powder after reduction are placed on shown in Fig. 1
Device is ground.
Preparation example 1
It is laid in tungsten powder and cobalt powder in molybdenum bowl respectively, and accounts for the 1/3 of molybdenum bowl volume, tungsten powder will be filled
Being transferred in molybdenum pipe hydrogen furnace by drying bottle with the molybdenum bowl of cobalt powder, described molybdenum pipe hydrogen furnace is with 65 DEG C/min
Programming rate at the uniform velocity intensification 12min to 780 DEG C, in the environment of dry hydrogen in molybdenum pipe hydrogen furnace
Carry out the high temperature reduction reaction of 35min；Weigh the tungsten powder obtaining in above-mentioned steps and cobalt in the ratio of 1:3
Powder；It is positioned over the agate ball containing 30 a diameter of 15mm after load weighted tungsten powder and cobalt powder are mixed
In the agate tank 3 of the agate ball 2 of 1 and 40 a diameter of 10mm；Fill tungsten powder and cobalt powder by described
After the agate tank 3 of mixture covers the first lid 4, put in outer cover 6, then screw the second lid 5,
With screwdriver, fixing bolt 7 is screwed, then with spanner, the nut 8 on fixing bolt 7 is screwed, to agate
Tank 3 seals；Agate tank 3 after sealing is placed in the ball mill that rotating speed is 80 revs/min rotation
Within 50 minutes, grind, obtain tungsten cobalt solder.
Preparation example 2
It is laid in tungsten powder and cobalt powder in molybdenum bowl respectively, and accounts for the 1/2 of molybdenum bowl volume, tungsten powder will be filled
Being transferred in molybdenum pipe hydrogen furnace by drying bottle with the molybdenum bowl of cobalt powder, described molybdenum pipe hydrogen furnace is with 88 DEG C/min
Programming rate at the uniform velocity intensification 10min to 880 DEG C, in the environment of dry hydrogen in molybdenum pipe hydrogen furnace
Carry out the high temperature reduction reaction of 40min；In the ratio of 1:3.5 weigh the tungsten powder obtaining in above-mentioned steps and
Cobalt powder；It is positioned over the agate containing 30 a diameter of 15mm after load weighted tungsten powder and cobalt powder are mixed
In the agate tank 3 of the agate ball 2 of ball 1 and 40 a diameter of 10mm；Fill tungsten powder and cobalt by described
After the agate tank 3 of powder mixture covers the first lid 4, put in outer cover 6, then screw the second lid 5,
With screwdriver, fixing bolt 7 is screwed, then with spanner, the nut 8 on fixing bolt 7 is screwed, to agate
Tank 3 seals；Agate tank 3 after sealing is placed in the ball mill that rotating speed is 90 revs/min rotation
Within 60 minutes, grind, obtain tungsten cobalt solder.
Preparation example 3
It is laid in the mixture of tungsten powder and cobalt powder in molybdenum bowl, and accounts for the 2/3 of molybdenum bowl volume, will fill
The molybdenum bowl of tungsten powder and cobalt powder is transferred in molybdenum pipe hydrogen furnace by drying bottle, and described molybdenum pipe hydrogen furnace is with 120
DEG C/programming rate at the uniform velocity intensification 8min to 960 DEG C of min, in molybdenum Guan Qing in the environment of dry hydrogen
Steam stove carries out the high temperature reduction reaction of 40min；Weigh the tungsten obtaining in above-mentioned steps in the ratio of 1:4
Powder and cobalt powder；It is positioned over containing 30 a diameter of 15mm's after load weighted tungsten powder and cobalt powder are mixed
In the agate tank 3 of the agate ball 2 of agate ball 1 and 40 a diameter of 10mm；Fill tungsten powder by described
After covering the first lid 4 with the agate tank 3 of cobalt powder mixture, put in outer cover 6, then screw the second lid
Fixing bolt 7 is screwed by screwdriver, then screws the nut 8 on fixing bolt 7 with spanner by son 5,
Agate tank 3 is sealed；Agate tank after sealing is placed in the ball mill that rotating speed is 100 revs/min
Rotate grinding in 65 minutes, obtain tungsten cobalt solder.
Embodiment 1
Prepare 100 brazed assemblies by the following method.
It is fixed on molybdenum cylinder 9 on spongy body of tungsten 10；By tungsten cobalt fill solder prepared in preparation example 1 extremely
In the solder bath 11 that the edge that described molybdenum cylinder 9 inwall and described spongy body of tungsten 10 cave in is formed, and use magnetic
Pin cleans out the tungsten cobalt solder outside solder bath 11, forms assembly；Described assembly is sent into molybdenum Guan Qing
With the programming rate at the uniform velocity intensification 20min to 1600 DEG C of 80 DEG C/min in steam stove, after insulation 0.5min,
Programming rate at the uniform velocity intensification 4min to 1720 DEG C with 30 DEG C/min again, is incubated 5s；With 30 DEG C/min
Rate of temperature fall at the uniform velocity lower the temperature 20min to 1120 DEG C, then continue at the uniform velocity with the rate of temperature fall of 80 DEG C/min
Lower the temperature and take out after keeping 15min after 12.5min to 20 DEG C, obtain brazed assembly.
Embodiment 2
Prepare 100 brazed assemblies by the following method.
It is fixed on molybdenum cylinder 9 on spongy body of tungsten 10；By tungsten cobalt fill solder prepared in preparation example 1 extremely
In the solder bath 11 that the edge that described molybdenum cylinder 9 inwall and described spongy body of tungsten 10 cave in is formed, and use magnetic
Pin cleans out the tungsten cobalt solder outside solder bath 11, forms assembly；Described assembly is sent into molybdenum Guan Qing
With the programming rate at the uniform velocity intensification 14min to 1400 DEG C of 100 DEG C/min in steam stove, after insulation 1min,
Programming rate at the uniform velocity intensification 5min to 1600 DEG C with 40 DEG C/min again, is incubated 15s；With 40 DEG C/min
Cooling rate at the uniform velocity lower the temperature 8min to 1280 DEG C, then continue at the uniform velocity with the cooling rate of 100 DEG C/min
Lower the temperature and take out after keeping 12min after 12.5min to 20 DEG C, obtain brazed assembly.
Embodiment 3
Prepare 100 brazed assemblies by the following method.
It is fixed on molybdenum cylinder 9 on spongy body of tungsten 10；By tungsten cobalt fill solder prepared in preparation example 1 extremely
In the solder bath 11 that the edge that described molybdenum cylinder 9 inwall and described spongy body of tungsten 10 cave in is formed, and use magnetic
Pin cleans out the tungsten cobalt solder outside solder bath 11, forms assembly；Described assembly is sent into molybdenum Guan Qing
With the programming rate at the uniform velocity intensification 10min to 1200 DEG C of 120 DEG C/min in steam stove, after insulation 1.5min,
Programming rate at the uniform velocity intensification 6min to 1500 DEG C with 50 DEG C/min again, is incubated 25s；With 50 DEG C/min
Cooling rate at the uniform velocity lower the temperature 2min to 1400 DEG C, then continue at the uniform velocity with the cooling rate of 120 DEG C/min
Lower the temperature and take out after keeping 10min after 11.5min to 20 DEG C, obtain brazed assembly.
Embodiment 4
Being prepared according to the embodiment of embodiment 1, except for the difference that, in the present embodiment, tungsten cobalt solder is adopted
Be in preparation example 2 prepare tungsten cobalt solder.
Embodiment 5
Being prepared according to the embodiment of embodiment 2, except for the difference that, in the present embodiment, tungsten cobalt solder is adopted
Be in preparation example 2 prepare tungsten cobalt solder.
Embodiment 6
Being prepared according to the embodiment of embodiment 3, except for the difference that, in the present embodiment, tungsten cobalt solder is adopted
Be in preparation example 2 prepare tungsten cobalt solder.
Embodiment 7
Being prepared according to the embodiment of embodiment 1, except for the difference that, in the present embodiment, tungsten cobalt solder is adopted
Be in preparation example 3 prepare tungsten cobalt solder.
Embodiment 8
Being prepared according to the embodiment of embodiment 2, except for the difference that, in the present embodiment, tungsten cobalt solder is adopted
Be in preparation example 3 prepare tungsten cobalt solder.
Embodiment 9
Being prepared according to the embodiment of embodiment 3, except for the difference that, in the present embodiment, tungsten cobalt solder is adopted
Be in preparation example 3 prepare tungsten cobalt solder.
Comparative example 1
It is prepared according to the embodiment of embodiment 5, except for the difference that, tungsten powder in tungsten cobalt solder used
Different with the ratio of cobalt powder, described tungsten powder is 1:1.5 with the ratio of cobalt powder.
Comparative example 2
It is prepared according to the embodiment of embodiment 5, except for the difference that, tungsten powder in tungsten cobalt solder used
Different with the ratio of cobalt powder, described tungsten powder is 1:6 with the ratio of cobalt powder.
Test case 1
The brazed assembly preparing in embodiment 1-9 and comparative example the 1st, 2 is placed in multiplication factor is 16 times
Observe under microscope, observation situation made specified below:
Grade 1: welding situation is excellent, and basis of microscopic observation does not appears from end without sand holes, solder；
Grade 2: in order, basis of microscopic observation has from molybdenum cylinder end without obvious sand holes, solder in welding
Separate out on a small quantity but do not separate out from spongy body of tungsten end
Grade 3: weld in poor shape, microscope substantially has sand holes under observing, and there is weldering spongy body of tungsten end
Material separates out.
Wherein, grade 1 and grade 2 are qualified for soldering, and grade 3 is defective for soldering.
The soldering qualification rate testing result obtaining is as shown in table 1:
Table 1:
| Grade 1 | Grade 2 | Grade 3 | Qualification rate | |
| Embodiment 1 | 75% | 10% | 15% | 85% |
| Embodiment 2 | 92% | 5% | 3% | 97% |
| Embodiment 3 | 82% | 8% | 10% | 90% |
| Embodiment 4 | 82% | 7% | 11% | 89% |
| Embodiment 5 | 95% | 4% | 1% | 99% |
| Embodiment 6 | 85% | 7% | 7% | 93% |
| Embodiment 7 | 78% | 8% | 14% | 86% |
| Embodiment 8 | 93% | 5% | 2% | 98% |
| Embodiment 9 | 83% | 7% | 10% | 90% |
| Comparative example 1 | 15% | 60% | 25% | 75% |
| Comparative example 2 | 19% | 53% | 28% | 72% |
Test case 2
It is assembled into test case 1 detects qualified brazed assembly in travelling-wave tubes, travelling-wave tubes is placed in power
Spectrum density is 0.016g2Axially test 24 hours respectively along three on the durable bobbing machine of/Hz, add up to 72
The time of vibration of hour.After end to be tested, above-mentioned travelling-wave tubes is used, all can reach normally to make
Condition.
Describe the preferred embodiment of the present invention above in association with accompanying drawing in detail, but, the present invention does not limit
Detail in above-mentioned embodiment, in the technology concept of the present invention, can be to the present invention
Technical scheme carry out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means, in order to avoid need not
The repetition wanted, various possible combinations are no longer illustrated by the present invention separately.
Additionally, also can be combined between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (8)
1. the preparation method for the tungsten cobalt solder of negative electrode, it is characterised in that the method includes:
(1) tungsten powder and cobalt powder are reduced；
(2) mixture of the tungsten powder after reduction and cobalt powder is ground, obtains tungsten cobalt solder；
Wherein, the weight of described tungsten powder and described cobalt powder is than for 1:2-5；
It in step (1), by the method that tungsten powder and cobalt powder reduce is: under an atmosphere of hydrogen, point
Tungsten powder and cobalt powder are not heat-treated；Or under an atmosphere of hydrogen, the mixture of tungsten powder and cobalt powder is entered
Row heat treatment；And
Described heat treatment for being warming up to tungsten powder and cobalt powder with the programming rate of 40-180 DEG C/min
700-1050 DEG C, and it is incubated 30min-60min at such a temperature；
Described heat treatment is: is respectively placed in tungsten powder and cobalt powder in molybdenum bowl, is placed in molybdenum bowl in drying bottle,
And drying bottle is placed in molybdenum pipe hydrogen furnace and is heat-treated；Or the mixture of tungsten powder and cobalt powder is placed in
It in molybdenum bowl, is placed in molybdenum bowl in drying bottle, and drying bottle is placed in molybdenum pipe hydrogen furnace and is heat-treated；
Wherein,
Capacity with molybdenum bowl is 100 parts by volume, and the consumption of described tungsten powder and/or cobalt powder is 1-67 parts by volume；
The method of described grinding includes:
(1) mixture of the tungsten powder after reduction and cobalt powder is positioned over the agate tank (3) containing agate ball
In；
(2) the agate tank (3) being placed with tungsten powder and cobalt powder mixture is sealed；
(3) the agate tank (3) after sealing carries out spin finishing；
In step (1), described agate ball includes first agate of 20-40 a diameter of 10-20mm
Ball (1) and second agate ball (2) of 30-50 a diameter of 5-15mm；
In step (3), described spin finishing is carried out in ball mill, and the rotating speed of described ball mill sets
It is set to 60-120 rev/min, ball milling 40-80 minute.
2. method according to claim 1, wherein, the weight ratio of described tungsten powder and described cobalt powder
For 1:2.5-4.5.
3. method according to claim 2, wherein, the weight ratio of described tungsten powder and described cobalt powder
For 1:3-4.
4. method according to claim 1, wherein, described heat treatment for by tungsten powder and cobalt powder with
The programming rate of 65-120 DEG C/min is warming up to 780-960 DEG C, and is incubated 35-45min at such a temperature.
5. method according to claim 4, wherein, the capacity with molybdenum bowl is 100 parts by volume,
The consumption of described tungsten powder and/or cobalt powder is 20-50 parts by volume.
6. method according to claim 1, wherein, the rotating speed of described ball mill is set to 80-100
Rev/min, ball milling 50-65 minute.
7. the preparation method of a brazed assembly, it is characterised in that the method includes following operation:
(1) operation of tungsten cobalt solder is prepared by the method described in claim 1-6；
(2) it is fixed on molybdenum cylinder (9) on spongy body of tungsten (10), and by described tungsten cobalt fill solder extremely
The solder bath (11) that the edge that described molybdenum cylinder (9) inwall and described spongy body of tungsten (10) cave in is formed
In, form the operation of assembly；
(3) cool down after described assembly being heated, obtain the operation of brazed assembly；Wherein,
In step (3), described heat and be cooled in molybdenum pipe hydrogen furnace carry out；Described heating includes
First intensification section and the second intensification section, described first intensification section is with the programming rate liter of 80-120 DEG C/min
Temperature, to 1200-1600 DEG C, is incubated 0.5-1.5min, and described second intensification section is with the intensification of 30-50 DEG C/min
Speed is warming up to 1500-1720 DEG C, is incubated 5-25s；
Described cooling includes the first temperature descending section and the second temperature descending section, and described first temperature descending section is with 30-50 DEG C
The cooling rate of/min is cooled to 1120-1450 DEG C, and described second temperature descending section is with the fall of 80-120 DEG C/min
Temperature speed be cooled to 15-35 DEG C after and keep 10-15min.
8. method according to claim 7, wherein, the method also includes, in step (2),
Clear up solder bath (11) tungsten cobalt solder outward with needle.
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| CN104525933B (en) * | 2014-11-17 | 2017-01-11 | 安徽华东光电技术研究所 | Cobalt powder treatment method for cathode brazing of dual-mode traveling wave tube |
| CN105269178A (en) * | 2015-11-30 | 2016-01-27 | 广东美的厨房电器制造有限公司 | Solder and production method thereof |
| CN106238961A (en) * | 2016-08-23 | 2016-12-21 | 安徽华东光电技术研究所 | One is applicable to travelling-wave tube negative electrode brazing solder and preparation method |
| CN111633293A (en) * | 2020-06-15 | 2020-09-08 | 安徽华东光电技术研究所有限公司 | Thorium-tungsten hot wire pin brazing method |
| CN113828879B (en) * | 2021-08-12 | 2023-02-28 | 南京三乐集团有限公司 | High-efficiency high-consistency cathode assembly welding method for Ku-waveband communication traveling wave tube |
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| RU2079922C1 (en) * | 1994-08-09 | 1997-05-20 | Государственное научно-производственное предприятие "Алмаз" | Method of fabrication of not cathode for electronic device and composition of solder for fabrication of hot cathode |
| CN1727107A (en) * | 2004-07-30 | 2006-02-01 | 中国科学院电子学研究所 | The solder that is used for impregnated cathode |
| CN100443247C (en) * | 2005-08-31 | 2008-12-17 | 安徽华东光电技术研究所 | Impregnated barium-tungsten cathode solder and method for using same |
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