CN100511552C - Dipped barium wolfram cathode and process for manufacture - Google Patents
Dipped barium wolfram cathode and process for manufacture Download PDFInfo
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- CN100511552C CN100511552C CNB2005100942174A CN200510094217A CN100511552C CN 100511552 C CN100511552 C CN 100511552C CN B2005100942174 A CNB2005100942174 A CN B2005100942174A CN 200510094217 A CN200510094217 A CN 200510094217A CN 100511552 C CN100511552 C CN 100511552C
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Abstract
This invention discloses one dipping barium-tungsten cathode with multi functions and its process method, wherein, the cathode comprises addictive, molybdenum cylinder, heater, aluminates; the addictive is composed of iridium powder ruthenium powder and tungsten powder. The process method comprises the following steps: annealing the metal powder and weighting three materials less than 200 for mixing and using molybdenum powder mode to process cathode; heating to 1500-2000 degree less than one hour; putting it into aluminates powder for dipping for 0.5 to 10 minutes in 1500 to 2000 degrees.
Description
Technical field
The present invention relates to the barium-tungsten dispense cathode on a kind of electronic tube tube, relate in particular to a kind of dipped barium-tungsten cathode that contains iridium rhenium tungsten additive.
The invention still further relates to a kind of method for preparing above-mentioned dipped barium-tungsten cathode.
Background technology
With respect to other negative electrodes, traditional dipped barium-tungsten cathode because have that surperficial work function is low, emission current is big, life-span characteristics such as length, better working stability, anti-poisoning and anti-ion bombardment ability be strong, so as electron source, be widely used in all kinds of great-power electronic tube devices, as picture tube of klystron, magnetron, travelling wave tube and high definition high brightness etc.But it exists, and technology is numerous and diverse, difficulty is big, repeatability and defectives such as poor stability, cost height, in addition, along with high power valve improves requirement day by day, original traditional dipped barium-tungsten cathode emission current is big inadequately, the life-span falls short of, working temperature is too high, the imperfect inferior position of job stability does not catch up with development of the situation day by day.
Summary of the invention
The object of the present invention is to provide the dipped barium-tungsten cathode that emission current is big, the life-span long, working temperature is not high.
Another object of the present invention is to provide a kind of method for preparing above-mentioned dipped barium-tungsten cathode, and this preparation method's technology is simple, repeatability and good stability.
For achieving the above object, dipped barium-tungsten cathode provided by the invention comprises additive, molybdenum tube, heater, aluminate, additive consist of iridium powder, rhenium powder, tungsten powder, its weight ratio is that purity is converted to 100% iridium powder: purity is converted to 100% rhenium powder: purity is converted to 100% tungsten powder=1: 1-3: 1-8.
Described iridium powder, rhenium powder, tungsten powder purity are 95-100%.
Described aluminate is the compound that is become at high-temperature firing by a certain percentage by barium monoxide, calcium oxide, aluminium oxide.
Preferred additives consists of purity and is converted to 100% iridium powder: purity is converted to 100% rhenium powder: purity is converted to 100% tungsten powder=1:1.5-2.5:2-3, and described iridium powder, rhenium powder, tungsten powder purity are 99-100%.
Additive iridium powder, rhenium powder can make the tungsten powder in the negative electrode disperse more even, and reduce the work function of tungsten substrate effectively, and the evaporation of the product of active material aluminate in the negative electrode and tungsten substrate pyroreaction is significantly reduced, make above-mentioned negative electrode possess characteristics such as emission current is big, the life-span long, working temperature is not high thereby reach.And the negative electrode that contains this additive is when negative electrode is worked, can effective anti-ion bombardment, and when vacuum degree descends, still can make cathode stabilization work.
The purity of iridium powder, rhenium powder and tungsten powder is high more, and prepared dipped barium-tungsten cathode effect is just good more.
The method of the above-mentioned dipped barium-tungsten cathode of preparation provided by the invention is:
A) iridium powder, rhenium powder and tungsten powder are put into 1000-1500 ℃ of hydrogen furnace annealing respectively.
B) get iridium powder, rhenium powder and tungsten powder by weight, these three kinds of materials are ground to are not less than 200 orders, mixing according to the size of flat-top cathode, is got an amount of mixture, has the pressing mold of molybdenum tube to be pressed into the flat-top cathode in using.
C) cathode of step b preparation is put into the hydrogen stove, when temperature reached 1500-2000 ℃, insulation was not less than 1 hour.
D) cathode that step c is made places the aluminate powder, hydrogen atmosphere, and 1500-2000 ℃ flooded 0.5-10 minute.Floating salt behind the dipping is removed with tungsten wire cotton mass.
E) heater is installed.
In step b, the order number of iridium powder, rhenium powder and tungsten powder is high more, and prepared cathode performance to a certain extent can be better, but in view of cost consideration, so preferred order number is the 300-500 order.
In step c, temperature retention time is long more, and prepared cathode performance can not correspondingly increase, in view of the compromise consideration of negative electrode quality and efficient, so preferred temperature retention time is 1-5 hours.
In steps d, temperature retention time is long more, and prepared cathode performance can not correspondingly increase, and descends on the contrary, in view of the compromise consideration of negative electrode quality and efficient, so preferred temperature retention time is 0.5-2 minutes.
Described cathode diameter is 2-5mm, and thickness is 1-4mm.
The present invention compared with prior art, cathode stabilization is very good, can adapt to the weather and the landform of various complexity, is particularly useful for the military microwave tube of annotating more.
Preparation method of the present invention has the characteristic that traditional handicraft does not possess:
A, because be one-shot forming, need not go twice technology such as copper again through soaking copper in traditional overlay film dipped barium-tungsten cathode production technology, simplified operation, also shortened the production cycle simultaneously.
B, because of being compacting, rather than car system processing, the car line that does not stay because of car system on the cathode plane has guaranteed enough fineness.
C, remove copper because of not needing chemistry, so can not stay the evidence of oxide that causes because of acidifying inside and outside the spongy body of tungsten, guaranteed that spongy body of tungsten possesses fresh that contacts with active material, helping emitting material plays a role effectively, be convenient to the electronics emission, more can not stay residues such as copper only because of removing copper.
D, because of when compacting the negative electrode cavernous body be connected as a single entity with the molybdenum tube, so do not exist because of welding the improper anticathode pollution that causes with the molybdenum tube, also thereby with low cost.
E, because be at same mould compacted under, so each negative electrode (even radian is arranged) all is identical, process repeatability and good stability.
Description of drawings
Fig. 1 is a dipped barium-tungsten cathode structural representation of the present invention.
In Fig. 1, iridium powder, rhenium powder, tungsten powder, aluminate 1, molybdenum tube 2, heater 3, heater leg 4.
Embodiment
The prepared flat-top cathode diameter of the present invention is 3.6mm, and thickness is 2mm.
Technology 1:
1) iridium powder, rhenium powder and tungsten powder are put into 1000 ℃ of hydrogen furnace annealings respectively,, and strengthen its plasticity with thorough purification.
2) take by weighing 10 gram iridium powder, 15 gram rhenium powder, 20 gram tungsten powders, (all having converted is 100%, and the purity of iridium powder is 95%, and the purity of rhenium powder is 96.2%, the purity of tungsten powder is 95.2%), these three kinds of materials are ground to 300 orders, and mixing is got mixture 0.2 gram, with the interior pressing mold that the molybdenum tube is arranged, be pressed into cathode.
3) cathode of step 2 preparation is put into the hydrogen stove, when temperature reaches 1700 ℃, be incubated 5 hours.
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1500 ℃ flooded 5 minutes, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Examination criteria: detection of the present invention with features such as preparation temperature, direct current emission, life-spans as its examination criteria.
Detection method: above-mentioned sample is 2 * 10 in vacuum all
-5Pa, with water-cooled anode diode transmission test platform, cathode life testboard etc. as its detection method.
Except that iridium powder, rhenium powder, tungsten powder purity difference, all the other are identical with technology 1.
Table 1:
Formula number | 1-1 | 1-2 | 1-3 | 1-4 | 1-5 | 1-6 | 1-7 |
Iridium powder purity (%) | 94.5 | 95 | 97 | 98.5 | 99.0 | 99.5 | 99.99 |
Rhenium powder purity (%) | 94.0 | 96.3 | 97.0 | 98.4 | 993 | 99.7 | 99.99 |
Tungsten powder purity (%) | 94.8 | 95.2 | 97.2 | 98.4 | 99.2 | 99.6 | 99.99 |
Direct current emission (A/cm 2) | 1.76 | 2.05 | 2.21 | 2.35 | 2.37 | 2.42 | 2.46 |
Life-span (hour) | 1540 | 1950 | 2230 | 2370 | 2420 | 2450 | 2510 |
Along with iridium powder, rhenium powder, tungsten powder purity improve, the effect of preparation cathode is just good more.
Get prescription 1-7, except that the fineness of iridium powder, rhenium powder, tungsten powder, all the other are identical with technology 1.
Table 2
Formula number | 2-1 | 2-2 | 1—7 | 2-4 | 2-5 | 2-6 |
Iridium powder, rhenium powder, tungsten powder fineness (order) | 180 | 200 | 300 | 400 | 500 | 550 |
Direct current emission (A/cm 2) | 1.75 | 2.05 | 2.46 | 2.47 | 2.47 | 2.48 |
Life-span (hour) | 1560 | 1950 | 2510 | 2520 | 2550 | 2560 |
The order number of iridium powder, rhenium powder, tungsten powder high more (in to a certain degree), prepared cathode performance is good more.
Get prescription 1-7, except that iridium powder, rhenium powder, tungsten powder ratio, all the other are identical with technology 1, and the iridium powder is got 10 grams.
Table 3
Formula number | 3-1 | 3—2 | 1—7 | 3-4 | 3-5 | 3-6 | 3-7 |
Rhenium powder (being equivalent to 100% purity) gram | 8 | 10 | 15 | 20 | 25 | 30 | 35 |
Tungsten powder (being equivalent to 100% purity) gram | 9 | 10 | 20 | 25 | 30 | 80 | 85 |
Direct current emission (A/cm 2) | 1.72 | 2.2 | 2.46 | 2.51 | 2.47 | 2.35 | 1.85 |
Life-span (hour) | 1600 | 2380 | 2510 | 2490 | 2530 | 2400 | 1850 |
Iridium powder, rhenium powder, tungsten powder, its weight ratio are 1: 1-3: 1-8, and the better performances of negative electrode.
Following process is filled a prescription with 1-7.
Technology 2:
1) iridium powder, rhenium powder and tungsten powder are put into 1100 ℃ of hydrogen furnace annealings respectively,, and strengthen its plasticity with thorough purification.
2) take by weighing 10 gram iridium powder, 15 gram rhenium powder, 20 gram tungsten powders, (all converted is 100%) is ground to 300 orders with these three kinds of materials, and mixing is got mixture 0.2 gram, and the pressing mold of molybdenum tube is arranged in using, and is pressed into cathode.
3) cathode of step 2 preparation is put into the hydrogen stove, when temperature reaches 1750 ℃, be incubated 4 hours.
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1600 ℃ flooded 2 minutes, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Technology 3:
1) iridium powder, rhenium powder and tungsten powder are put into 1250 ℃ of hydrogen furnace annealings respectively,, and strengthen its plasticity with thorough purification.
2) take by weighing 10 gram iridium powder, 15 gram rhenium powder, 20 gram tungsten powders, (all converted is 100%) is ground to 300 orders with these three kinds of materials, and mixing is got mixture 0.2 gram, and the pressing mold of molybdenum tube is arranged in using, and is pressed into cathode.
3) cathode of step 2 preparation is put into the hydrogen stove, when temperature reaches 1800 ℃, be incubated 3.5 hours.
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1750 ℃ flooded 1 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Technology 4:
1) iridium powder, rhenium powder and tungsten powder are put into 1400 ℃ of hydrogen furnace annealings respectively,, and strengthen its plasticity with thorough purification.
2) take by weighing 10 gram iridium powder, 15 gram rhenium powder, 20 gram tungsten powders, (all converted is 100%) is ground to 300 orders with these three kinds of materials, and mixing is got mixture 0.2 gram, and the pressing mold of molybdenum tube is arranged in using, and is pressed into cathode
3) cathode of step 2 preparation is put into the hydrogen stove, when temperature reaches 1850 ℃, be incubated 2.5 hours.
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1850 ℃ flooded 0.5 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Technology 5:
1) iridium powder, rhenium powder and tungsten powder are put into 1500 ℃ of hydrogen furnace annealings respectively,, and strengthen its plasticity with thorough purification.
2) take by weighing 10 gram iridium powder, 15 gram rhenium powder, 20 gram tungsten powders, (all converted is 100%) is ground to 300 orders with these three kinds of materials, and mixing is got mixture 0.2 gram, and the pressing mold of molybdenum tube is arranged in using, and is pressed into cathode.
3) cathode of step 2 preparation is put into the hydrogen stove, when temperature reaches 2000 ℃, be incubated 0.5 hour.
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1900 ℃ flooded 0.5 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
The sample number into spectrum of technology 2 preparations is 4-2, and the sample number into spectrum of technology 3 preparations is 4-3, and the like,
Table 4
Numbering | Preparation temperature (℃) | Direct current emission (A/cm 2) | Life-span (hour) |
1—7 | 1500 | 2.46 | 2510 |
4—2 | 1600 | 2.47 | 2470 |
4—3 | 1750 | 2.48 | 2530 |
4—4 | 1850 | 2.50 | 2500 |
4—5 | 2000 | 2.51 | 2530 |
Technology 1-5 all can realize the present invention.
Claims (7)
1, dipped barium-tungsten cathode, comprise additive, molybdenum tube, heater, aluminate, it is characterized in that: additive consist of iridium powder, rhenium powder, tungsten powder, its weight ratio is that purity is converted to 100% iridium powder: purity is converted to 100% rhenium powder: purity is converted to 100% tungsten powder=1: 1-3: 1-8, and described iridium powder, rhenium powder, tungsten powder purity are 95-100%.
2, dipped barium-tungsten cathode according to claim 1, it is characterized in that: the weight ratio of additive is that purity is converted to 100% iridium powder: purity is converted to 100% rhenium powder: purity is converted to 100% tungsten powder=1: 1.5-2.5: 2-3, and described iridium powder, rhenium powder, tungsten powder purity are 99-100%
3, a kind of method for preparing dipped barium-tungsten cathode as claimed in claim 1, its key step is:
A) iridium powder, rhenium powder, tungsten powder are put into 1000-1500 ℃ of hydrogen furnace annealing respectively;
B) get iridium powder, rhenium powder, tungsten powder by weight, three kinds of materials are ground to are not less than 200 orders, mixing according to the size of cathode, is got an amount of mixture, has the pressing mold of molybdenum tube to be pressed into cathode in using;
C) cathode of step b preparation is put into the hydrogen stove, when temperature reached 1500-2000 ℃, temperature retention time was not less than 1 hour;
D) cathode that step c is made places the aluminate powder, hydrogen atmosphere, and 1500-2000 ℃ flooded 0.5-10 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass;
E) heater is installed.
4, method according to claim 3 is characterized in that: the described three kinds of materials of step b are ground to the 300-500 order.
5, method according to claim 3 is characterized in that: the described temperature retention time of step c is 1-5 hour.
6, method according to claim 3 is characterized in that: the described dipping of steps d is 0.5-2 minute.
7, method according to claim 3 is characterized in that: the cathode diameter is 2-5mm, and thickness is 1-4mm.
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