CN109666833A - A kind of magnetron cathode coil cobalt thorium tungsten alloy material and preparation method thereof - Google Patents
A kind of magnetron cathode coil cobalt thorium tungsten alloy material and preparation method thereof Download PDFInfo
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- CN109666833A CN109666833A CN201811514202.2A CN201811514202A CN109666833A CN 109666833 A CN109666833 A CN 109666833A CN 201811514202 A CN201811514202 A CN 201811514202A CN 109666833 A CN109666833 A CN 109666833A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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Abstract
The invention discloses a kind of magnetron cathode coil cobalt thorium tungsten alloy materials and preparation method thereof, by forming following weight percentage components: Co 0.005~0.04%, Th 0.5~4.0%, surplus is W and inevitable impurity, preparation method adds cobalt salt while being included in blue tungsten doping thorium nitrate, improves the anti-seismic performance of magnetron cathode coil after carbonization by cobalt element refinement crystal particle function.The present invention is in the normally manufacturing step of manufacture magnetron cathode coil thoriatde-tungsten wire, cobalt salt solution is additionally incorporated in doping process, cobalt element is distributed in tungsten basal body by adulterating and mixing powder, make thorium oxide particle is more tiny, Dispersed precipitate more evenly, Grain refinement is played, intensity, reduction brittleness, improvement anti-seismic performance after the carbonization of cathode coil are promoted.
Description
Technical field
The invention belongs to magnetron cathode coil preparation technical fields, and in particular to a kind of magnetron cathode coil cobalt thorium
Tungsten alloy material and preparation method thereof.
Background technique
The material of manufacture magnetron cathode is the common white silk of thorium tungsten using 1%ThO2 now, is made of this material
Thoriated-tungsten wire loop material texture of coarse crystal can occur because carburizing temperature is higher in the carbonisation of magnetron cathode, this thick
Big crystal grain tissue will cause thoriated-tungsten wire circle and be easy fracture of wire, cause entire magnetron can not normal use.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of magnetron cathode coil cobalt thorium tungsten alloy material is provided
Material.
Another object of the present invention is to provide the preparation methods of above-mentioned magnetron cathode coil cobalt thorium tungsten alloy material.
Technical scheme is as follows:
A kind of magnetron cathode coil cobalt thorium tungsten alloy material, by forming following weight percentage components: Co
0.005~0.04%, Th 0.5~4.0%, surplus are W and inevitable impurity, and preparation method is included in blue tungsten doping
Cobalt salt is added while thorium nitrate, improves the antidetonation of magnetron cathode coil after carbonization by cobalt element refinement crystal particle function
Performance.
The above-mentioned magnetron cathode coil preparation method of cobalt thorium tungsten alloy material, includes the following steps:
(1) it adulterates: weighing blue tungsten, thorium nitrate and cobalt salt by the weight percent, blue tungsten and nitre is added in doping pot
While sour thorium adulterates, cobalt salt is added, is mixed by solid-liquid, then dries 6-8h at a temperature of 150-200 DEG C；
(2) it restores: step (1) resulting material is placed in reduction furnace, using 620-980 DEG C, four sections of 90-120min
Temperature control technique is restored, and cobalt thorium tungsten alloy powder is obtained, and reducing atmosphere is hydrogen atmosphere, and the flow of hydrogen is 10-35m3/ h,
The purity of hydrogen is 93-97%；
(3) powder is suppressed: above-mentioned cobalt thorium tungsten alloy powder being placed in batch mixer, 0.5-1.5h and 14-16rpm are carried out
Rolling, obtain granularity be 2-5 μm, loose, dry and uniform powder, then the powder is uniformly fitted into mantle, using 130-
160Mpa carries out the static pressure 80-100s such as liquid, obtains the first cobalt thorium tungalloy bar；
(4) it is sintered: above-mentioned first cobalt thorium tungalloy bar being sent into pre-burning freezing of a furnace, with 1100-1400 DEG C of sintering 20-
40min is placed into incipient fusion machine and is clamped both ends in 2400-2700 DEG C of progress incipient fusion sintering 40-60min, and obtaining density is 17.0-
19.0g/cm3, diameter be 12-30mm the second cobalt thorium tungalloy bar；
(5) pressure processing: above-mentioned second cobalt thorium tungalloy bar is swaged by multi-pass with rotation hammer machine and is machined to 3.3-
3.7mm is re-fed into wire drawing machine and carries out series connection wire drawing, obtains the black silk of cobalt thorium tungsten alloy that diameter is 0.52-0.55mm；
(6) it cleans: by the white silk of cobalt thorium tungsten alloy of the black silk electrobrightening of above-mentioned cobalt thorium tungsten alloy to 0.46-0.50mm, i.e.,
Magnetron cathode coil cobalt thorium tungsten alloy material.
In a preferred embodiment of the invention, the temperature in four sections of temperature control technique be followed successively by 620-680 DEG C,
720-780 DEG C, 820-880 DEG C and 920-980 DEG C, the time is followed successively by 90-10min, 90-100min, 100-110min and 100-
120min。
It is further preferred that the temperature in four sections of temperature control technique is followed successively by 650 DEG C, 750 DEG C, 850 DEG C and 950 DEG C,
Time is followed successively by 90min, 90min, 100min and 120min.
In a preferred embodiment of the invention, in the step (5), the second cobalt thorium tungsten is closed with rotation hammer machine
Gold bar swages by multi-pass and is machined to 3.3-3.7mm.
It is further preferred that the second cobalt thorium tungalloy bar is revolved by multi-pass with rotation hammer machine in the step (5)
Forging is machined to 3.5mm.
In a preferred embodiment of the invention, it in the step (5), is sent into wire drawing machine, passes sequentially through passage
3.0-3.3mm、2.5-2.7mm、2.0-2.3mm、1.4-1.6mm、1.1-1.3mm、1.0-1.1mm、0.85-1.0mm、0.75-
0.85mm, 0.65-0.75mm, 0.6-0.65mm, 0.55-0.6mm and 0.50-0.55mm obtain the black silk of cobalt thorium tungsten alloy.
It is further preferred that in the step (5), be sent into wire drawing machine, pass sequentially through passage 3.2mm, 2.6mm,
2.1mm, 1.5mm, 1.2mm, 1.0mm, 0.9mm, 0.75mm, 0.7mm, 0.6mm, 0.56mm and 0.53mm obtain the cobalt thorium
The black silk of tungsten alloy.
The beneficial effects of the present invention are:
1, in addition the present invention adds in the normally manufacturing step of manufacture magnetron cathode coil thoriatde-tungsten wire in doping process
Enter cobalt salt solution, be distributed to cobalt element in tungsten basal body by adulterating and mixing powder, make thorium oxide particle is more tiny, Dispersed precipitate more
Uniformly, Grain refinement is played, intensity, reduction brittleness, improvement anti-seismic performance after the carbonization of cathode coil are promoted.
2, the cobalt element of the cobalt thorium tungsten alloy filament incorporation in the present invention, forms solid solution, inhibits thorium oxide to grow up, so that oxygen
It is more tiny to change thorium distribution more disperse, grain diameter.
3, the cobalt element of the cobalt thorium tungsten alloy filament incorporation 0.005~0.04% in the present invention, can play thoriatde-tungsten wire material solid
Molten reinforcing, the effect of refined crystalline strengthening can prevent coil tissue recrystal grain to be roughened after the carbonization of magnetron coil temperatures,
Crystal grain is refined, so that coil strength improves after carbonization, brittleness is reduced, and improves the anti-seismic performance of magnetron coil.
Detailed description of the invention
Fig. 1 is the thorium oxide particle in magnetron cathode coil cobalt thorium tungsten alloy material made from the embodiment of the present invention 1
The electron microscope of size and distribution situation.
Fig. 2 is the electron microscope of the thorium oxide granular size in thorium tungsten alloy filament and distribution situation in the prior art.
Fig. 3 is magnetron cathode coil cobalt thorium tungsten alloy material made from the embodiment of the present invention 1 after high temperature cabonization,
The electron microscope of the crystal grain situation of recrystallized structure.
Fig. 4 is that thorium tungsten alloy filament is after high temperature cabonization in the prior art, the electron microscope of the crystal grain situation of recrystallized structure.
Fig. 5 is electronics of the magnetron cathode coil cobalt thorium tungsten alloy material made from the embodiment of the present invention 1 in processing state
Probe elemental analysis result figure.
Fig. 6 is the electricity of magnetron cathode coil cobalt thorium tungsten alloy material after recrystallization made from the embodiment of the present invention 1
Sub- probe elemental analysis result figure.
Specific embodiment
Technical solution of the present invention is further explained and described below by way of specific embodiment combination attached drawing.
Embodiment 1
A kind of magnetron cathode coil cobalt thorium tungsten alloy material, by forming following weight percentage components: Co
0.005~0.04%, Th 0.5~4.0%, surplus are W and inevitable impurity, and preparation method is included in blue tungsten doping
Cobalt salt is added while thorium nitrate, improves the antidetonation of magnetron cathode coil after carbonization by cobalt element refinement crystal particle function
Performance.
The above-mentioned magnetron cathode coil preparation method of cobalt thorium tungsten alloy material, includes the following steps:
(1) it adulterates: weighing blue tungsten, thorium nitrate and cobalt salt by the weight percent, blue tungsten and nitre is added in doping pot
It while sour thorium adulterates, is added cobalt salt (the present embodiment is cobalt chloride), is mixed by solid-liquid, then in 150-200
6-8h is dried at a temperature of DEG C；
(2) restore: step (1) resulting material is placed in reduction furnace, using four sections of temperature control techniques (be followed successively by 650 DEG C/
90min, 750 DEG C/90min, 850 DEG C/100min and 950 DEG C/120min) it is restored, obtain cobalt thorium tungsten alloy powder, reduction
Atmosphere is hydrogen atmosphere, and the flow of hydrogen is 10-35m3/ h, the purity of hydrogen are 93-97%；
(3) powder is suppressed: above-mentioned cobalt thorium tungsten alloy powder being placed in batch mixer, turning over for 0.5-1.5h and 15rpm is carried out
Rolling, obtain granularity be 3.5 μm, loose, dry and uniform powder, then the powder is uniformly fitted into mantle by 2kg, using 130-
160Mpa carries out the static pressure 80-100s such as liquid, obtains the first cobalt thorium tungalloy bar that length is 900mm；
(4) it is sintered: above-mentioned first cobalt thorium tungalloy bar being sent into pre-burning freezing of a furnace, in 1250 DEG C of sintering 25min, is placed into
Both ends are clamped in incipient fusion machine and carry out incipient fusion sintering 40-60min with 2400-2700 DEG C, and obtaining density is 17.5g/cm3, diameter be
The second cobalt thorium tungalloy bar of 18mm；
(5) pressure processing: being swaged by multi-pass by the second cobalt thorium tungalloy bar with rotation hammer machine and be machined to 3.5mm,
Be re-fed into wire drawing machine, pass sequentially through passage 3.2mm, 2.6mm, 2.1mm, 1.5mm, 1.2mm, 1.0mm, 0.9mm, 0.75mm,
0.7mm, 0.6mm, 0.56mm and 0.53mm obtain the black silk of cobalt thorium tungsten alloy that diameter is 0.53mm；
(6) it cleans: by the white silk of cobalt thorium tungsten alloy of the black silk electrobrightening of above-mentioned cobalt thorium tungsten alloy to 0.5mm, i.e., such as Fig. 1,3
With 6 shown in magnetron cathode coil cobalt thorium tungsten alloy material；
(7) the above-mentioned white filament winding of cobalt thorium tungsten alloy is made to the magnetron cathode coil of different dimensions.
As depicted in figs. 1 and 2, magnetron cathode coil manufactured in the present embodiment compares existing skill with cobalt thorium tungsten alloy material
Cobalt thorium tungsten spun gold in art, thorium oxide is more tiny and is more evenly distributed in tungsten basal body.
As shown in Figure 3 and Figure 4, magnetron cathode coil manufactured in the present embodiment is with cobalt thorium tungsten alloy material in benzene atmosphere
It is carbonized, about 2200 DEG C of carburizing temperature, the tungsten recrystal grain after carbonization is more tiny, and thorium tungsten alloy filament system in the prior art
At thoriated-tungsten wire circle carbonization after tungsten grain it is coarseer.
As shown in Figure 5 and Figure 6, magnetron cathode coil manufactured in the present embodiment is equal with the cobalt element of cobalt thorium tungsten alloy material
It is even to be distributed in tungsten basal body, solid solution and solution strengthening are formed, and inhibit Th particle agglomeration to grow up when organizing recrystallization, made again
Th particle is tiny in crystalline structure, is evenly distributed, and plays the role of refining crystal grain and refined crystalline strengthening.
The foregoing is only a preferred embodiment of the present invention, the range that the present invention that therefore, it cannot be limited according to is implemented, i.e.,
Equivalent changes and modifications made in accordance with the scope of the invention and the contents of the specification should still be within the scope of the present invention.
Claims (8)
1. a kind of magnetron cathode coil cobalt thorium tungsten alloy material, it is characterised in that: by group following weight percentage components
At: Co 0.005~0.04%, Th 0.5~4.0%, surplus are that W and inevitable impurity, preparation method are included in indigo plant
Cobalt salt is added while witch culture thorium nitrate, crystal particle function is refined by cobalt element to improve magnetron cathode coil after carbonization
Anti-seismic performance.
2. a kind of preparation method of magnetron cathode coil cobalt thorium tungsten alloy material described in claim 1, it is characterised in that:
Include the following steps:
(1) it adulterates: weighing blue tungsten, thorium nitrate and cobalt salt by the weight percent, blue tungsten and thorium nitrate is added in doping pot
While doping, cobalt salt is added, is mixed by solid-liquid, then dries 6-8h at a temperature of 150-200 DEG C；
(2) it restores: step (1) resulting material being placed in reduction furnace, using the four of 620-980 DEG C and every section 90-120min
Section temperature control technique is restored, and cobalt thorium tungsten alloy powder is obtained, and reducing atmosphere is hydrogen atmosphere, and the flow of hydrogen is 10-35m3/
H, the purity of hydrogen are 93-97%；
(3) powder is suppressed: above-mentioned cobalt thorium tungsten alloy powder being placed in batch mixer, turning over for 0.5-1.5h and 14-16rpm is carried out
Rolling, obtain granularity be 2-5 μm, loose, dry and uniform powder, then the powder is uniformly fitted into mantle, using 130-
160Mpa carries out the static pressure 80-100s such as liquid, obtains the first cobalt thorium tungalloy bar；
(4) be sintered: will in above-mentioned first cobalt thorium tungalloy bar feeding pre-burning freezing of a furnace, with 1100-1400 DEG C of sintering 20-40min, then
It is put into incipient fusion machine and clamps both ends in 2400-2700 DEG C of progress incipient fusion sintering 40-60min, obtaining density is 17.0-19.0g/
cm3, diameter be 12-30mm the second cobalt thorium tungalloy bar；
(5) pressure processing: being swaged by multi-pass by above-mentioned second cobalt thorium tungalloy bar with rotation hammer machine and be machined to 3.3-3.7mm,
It is re-fed into wire drawing machine and carries out series connection wire drawing, obtain the black silk of cobalt thorium tungsten alloy that diameter is 0.52-0.55mm；
(6) it cleans: by the white silk of cobalt thorium tungsten alloy of the black silk electrobrightening of above-mentioned cobalt thorium tungsten alloy to 0.46-0.52mm, i.e., described
Magnetron cathode coil cobalt thorium tungsten alloy material.
3. preparation method as claimed in claim 2, it is characterised in that: the temperature in four sections of temperature control technique is followed successively by 620-
680 DEG C, 720-780 DEG C, 820-880 DEG C and 920-980 DEG C, the time is followed successively by 90-10min, 90-100min, 100-110min
And 100-120min.
4. preparation method as claimed in claim 3, it is characterised in that: the temperature in four sections of temperature control technique is followed successively by 650
DEG C, 750 DEG C, 850 DEG C and 950 DEG C, the time is followed successively by 90min, 90min, 100min and 120min.
5. preparation method as claimed in claim 2, it is characterised in that: in the step (5), with rotation hammer machine by second cobalt
Thorium tungalloy bar swages by multi-pass and is machined to 3.3-3.7mm.
6. preparation method as claimed in claim 5, it is characterised in that: in the step (5), with rotation hammer machine by second cobalt
Thorium tungalloy bar swages by multi-pass and is machined to 3.5mm.
7. preparation method as claimed in claim 2, it is characterised in that: in the step (5), be sent into wire drawing machine, successively lead to
Cross passage 3.0-3.3mm, 2.5-2.7mm, 2.0-2.3mm, 1.4-1.6mm, 1.1-1.3mm, 1.0-1.1mm, 0.85-1.0mm,
0.75-0.85mm, 0.65-0.75mm, 0.6-0.65mm, 0.55-0.6mm and 0.50-0.55mm obtain the cobalt thorium tungsten alloy
Black silk.
8. preparation method as claimed in claim 7, it is characterised in that: in the step (5), be sent into wire drawing machine, successively lead to
Cross passage 3.2mm, 2.6mm, 2.1mm, 1.5mm, 1.2mm, 1.0mm, 0.9mm, 0.75mm, 0.7mm, 0.6mm, 0.56mm and
0.53mm obtains the black silk of cobalt thorium tungsten alloy.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811514202.2A CN109666833B (en) | 2018-12-11 | 2018-12-11 | Cobalt-thorium-tungsten alloy material for magnetron cathode coil and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811514202.2A CN109666833B (en) | 2018-12-11 | 2018-12-11 | Cobalt-thorium-tungsten alloy material for magnetron cathode coil and preparation method thereof |
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| CN109666833B CN109666833B (en) | 2020-05-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110102869A (en) * | 2019-05-16 | 2019-08-09 | 广东省焊接技术研究所（广东省中乌研究院） | A kind of agitating friction weldering stirring head material and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| JPS5585651A (en) * | 1978-12-22 | 1980-06-27 | Toshiba Corp | Tungsten alloy for electron tube cathode heating filament |
| CN101004995A (en) * | 2006-01-20 | 2007-07-25 | 顾进跃 | Method for producing thorium-tungsten wire |
| CN103290294A (en) * | 2012-03-02 | 2013-09-11 | 朱惠冲 | Magnetron cathode, and preparation method and application thereof |
| CN103849804A (en) * | 2014-03-01 | 2014-06-11 | 深圳市威勒达科技开发有限公司 | Non-radiative multi-component composite tungsten negative material for microwave oven magnetron and preparation process of negative material |
-
2018
- 2018-12-11 CN CN201811514202.2A patent/CN109666833B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5585651A (en) * | 1978-12-22 | 1980-06-27 | Toshiba Corp | Tungsten alloy for electron tube cathode heating filament |
| CN101004995A (en) * | 2006-01-20 | 2007-07-25 | 顾进跃 | Method for producing thorium-tungsten wire |
| CN103290294A (en) * | 2012-03-02 | 2013-09-11 | 朱惠冲 | Magnetron cathode, and preparation method and application thereof |
| CN103849804A (en) * | 2014-03-01 | 2014-06-11 | 深圳市威勒达科技开发有限公司 | Non-radiative multi-component composite tungsten negative material for microwave oven magnetron and preparation process of negative material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110102869A (en) * | 2019-05-16 | 2019-08-09 | 广东省焊接技术研究所（广东省中乌研究院） | A kind of agitating friction weldering stirring head material and preparation method thereof |
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