CN104556979A - Beryllia ceramic clamping rod and manufacturing method thereof - Google Patents

Beryllia ceramic clamping rod and manufacturing method thereof Download PDF

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CN104556979A
CN104556979A CN201410829940.1A CN201410829940A CN104556979A CN 104556979 A CN104556979 A CN 104556979A CN 201410829940 A CN201410829940 A CN 201410829940A CN 104556979 A CN104556979 A CN 104556979A
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beryllium oxide
supporting rod
slurry
oxide ceramics
making method
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CN104556979B (en
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王刚
叶均
任鹏道
王钢
储齐晓
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YIBIN HONGXING ELECTRONIC CO Ltd
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Abstract

The invention belongs to the technical field of electronic function ceramic materials, particularly relates to a beryllia ceramic clamping rod and a manufacturing method thereof and aims to solve the technical problem of providing the manufacturing method of the beryllia ceramic clamping rod. The manufacturing method comprises the following steps: A, preparing beryllia powder into a spray granulation material; B, adopting dry pressing preforming and then manufacturing a flaky blank in an isostatic compaction manner; C, feeding the formed flaky blank in a push plate tunnel kiln for primary sintering, and carrying out flattening treatment through the sintering; D, using a flat grinder and a cutting machine to machine the blank into a clamping rod. The clamping rod manufactured by adopting the method is high in dimensional precision, and has the characteristics of high heat conductivity, high strength, good insulating strength, lower dielectric constant and dielectric loss and high chemical stability; the beryllia ceramic clamping rod plays supporting and radiating roles when being applied in a traveling wave tube, and is widely applied in the fields of electronic countermeasures, radar, communication, data transmission and the like.

Description

A kind of beryllium oxide ceramics supporting rod and preparation method thereof
Technical field
The invention belongs to electric function ceramic field of material technology, be specifically related to a kind of beryllium oxide ceramics supporting rod and preparation method thereof.
Background technology
Beryllium oxide ceramics is be the supporting strength member of electron device in defence equipment always.Because beryllium oxide ceramics has the good feature of higher thermal conductivity, good insulativity, thermal-shock resistance, lower loss and chemical stability, so be widely used in space flight, aviation nuclear power engineering do high power device heat radiation, adopted in a large number in electron vacuum device, high power module thick film circuit, packaging, photoelectric device.
Helix TWT relies on the advantage of its aspect such as broadband and high gain, is widely used, in occupation of consequence in current microwave vacuum electron device in fields such as electronic countermeasure, radar, communication and data transmission.In the various characteristics of helix TWT, heat dissipation characteristics is very important, and it is not only the principal element determining travelling-wave tubes average output power, is also the principal element of the Stability and dependability directly affecting travelling-wave tubes work.When helix TWT works, spiral-line due to high-frequency loss and defocus electron beam bombardment and be heated, if these heats can not spread out of timely and effectively, the temperature of spiral-line can be made significantly to increase, when temperature is too high, the decay of average output power can be caused, cause the significantly increase of slow wave loss, even also may cause the damage of whole travelling-wave tubes.
The slow-wave structure of helix TWT is made up of spiral-line, supporting rod and Can.Wherein, the effect of beryllium oxide ceramics supporting rod mainly contains two aspects, and one is support spin line structure, makes spiral-line be able to appropriate be fixed in shell; Two is outwards derived by the heat on spiral-line, provides the heat dissipation channel that good.
At present, preparation technology's flow process of domestic beryllium oxide ceramics supporting rod comprises ceramic material preparation, extrusion forming, burns till, grinds processing, there is the defect of following several respects in this technique: 1, adds more organic additive in ceramic material preparation process, the binder removal time is long and the rear density of beryllium oxide ceramics bar sintering is lower, affect heat conductivility and surfaceness working ability shortcoming, can not machined surface roughness at the supporting rod product being less than 0.8; 2, extrusion forming porcelain preparation cycle utilization ratio that is long, shaping rear porcelain is low, and lapping efficiency is low; 3, beryllium oxide ceramics bar sintering difficulty, needs special protective articles and veteran operator.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of making method of beryllium oxide ceramics supporting rod.The method comprises the following steps:
A, prepare shaping mist projection granulating material:
1., according to weight ratio Yangization Pi ︰ Magnesium Trisilicate=100 ︰ 0.5 ~ 0.55 both are mixed to obtain compound by step;
2., by compound and deionized water step mixes to obtain slurry, and in slurry, add φ 4 ~ 6mm zirconia ball, ball milling slurry is to slurry granularity D 50be not more than 1 μm, 100 ~ 300 eye mesh screens crossed by slurry, more namely obtain beryllium oxide slurry after deironing; According to weight ratio Hun He Liao ︰ Qu Li Shui ︰ φ 4 ~ 6mm zirconia ball=1 ︰ 0.3 ~ 1 ︰ 4 ~ 10;
Step 3., divide loose agent ︰ n-Octanol=100kg ︰ 1kg ︰ 5 ~ 10L ︰ 0.2L ︰ 0.3L ︰ 1 ~ 3L ︰ 2 ~ 5L to be joined in beryllium oxide slurry by other six kinds of raw materials according to the weightmeasurement ratio beryllium oxide slurry material ︰ third alkene acid ︰ polyethylene alcohol solution ︰ the third three sour ︰ of alcohol ︰ oil to mix to obtain mixed slurry, then add deionized water and regulate the viscosity of mixed slurry to be 3 ~ 5mPa.s;
4., by the mixed slurry mist projection granulating after adjusting viscosity step obtains granulation material, obtains shaping mist projection granulating material after 100 ~ 200 eye mesh screens;
B, extrusion forming;
C, sintering;
D, grind processing on request, then cut into supporting rod.
Preferably, the making method of above-mentioned beryllium oxide ceramics supporting rod, in steps A 3., described dispersion agent is any one in water glass, tripoly phosphate sodium STPP, Trisodium Citrate, sodium polyacrylate or poly carboxylic acid sodium.
Preferably, the making method of above-mentioned beryllium oxide ceramics supporting rod, in steps A 3., the massfraction of described polyvinyl alcohol water solution is 10%.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in steps A 3., the preparation method of described polyvinyl alcohol water solution is: be dissolved in by polyvinyl alcohol after crossing 200 eye mesh screens after dissolving completely in the water of 60 ~ 80 DEG C and cool.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in steps A 4., the condition of described mist projection granulating is: inlet temperature 190 ~ 250 DEG C, temperature out 105 ~ 130 DEG C, pumping pressure 0.8 ~ 1.2MPa, and in tower, negative pressure keeps 0 ~ 100Pa.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step B, the concrete steps of described extrusion forming are: by the step 4. first dry-pressing process of the shaping mist projection granulating material of gained, make blank, then isostatic pressed process.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step B, the condition of described dry-pressing process is: pressure 500 ~ 1000kg/cm 2, dwell time 5 ~ 10s.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step B, the condition of described isostatic pressed process is: peak pressure 180 ~ 200MPa, dwell time 30 ~ 60s, one-level venting duration 15 ~ 30s, secondary venting duration 10 ~ 30s.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step C, the concrete steps of described sintering are: by the blank multi-steps sintering after the process of step B isostatic pressed, first paragraph: from room temperature to 600 ~ 650 DEG C, and temperature rise rate is 30 ~ 60 DEG C/h; Second segment: be incubated 2 ~ 4h after being warming up to 1650 ~ 1700 DEG C again, temperature rise rate is 80 ~ 120 DEG C/h; 3rd section: can come out of the stove after Temperature fall, obtain ripe base; Ripe base is put down process again.
Preferably, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step C, described sintering adopts push pedal tunnel kiln sintering.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step C, described multiple putting down is treated to: ripe base overlap is placed or placed separately, and place the object of 5 ~ 10kg above it, control temperature is 1500 DEG C.
Preferably, the making method of above-mentioned beryllium oxide ceramics supporting rod, in step C, when overlap is placed, stack height is not higher than 30mm.
Concrete, the making method of above-mentioned beryllium oxide ceramics supporting rod, step D is concrete in three steps: step one: processing length and width and thickness; Step 2: carry out polished finish, control surface roughness is less than 0.2; Step 3: be cut into supporting rod on request.
Second technical problem to be solved by this invention there is provided the beryllium oxide ceramics supporting rod prepared by the making method of above-mentioned beryllium oxide ceramics supporting rod.
The inventive method, by the research to raw material composition, stuctures and properties, has been selected new raw material, has been decreased the use of organic volatile, thus change traditional raw material, optimize material prescription, improve the compactness of product.Have employed material by wet type mixing and replace conventional dry batch mixing, ensure that the homogeneity that raw material mixes and consistence; Eliminating calcining process makes raw material activity be improved, and reduces ball milling difficulty and sintering temperature; Coordinate formula, original extrusion forming is changed into the mode of isostatic pressed again after dry-pressing, add compactness and the intensity of blank, thus make that the good product quality of preparation, consistence are high, horizontal stable.
Embodiment
A making method for beryllium oxide ceramics supporting rod, comprises the following steps:
A, prepare shaping mist projection granulating material:
1., according to weight ratio Yangization Pi ︰ Magnesium Trisilicate=100 ︰ 0.5 ~ 0.55 both are mixed to obtain compound by step;
2., by compound and deionized water step mixes to obtain slurry, and in slurry, add φ 4 ~ 6mm zirconia ball, ball milling slurry is to slurry granularity D 50be not more than 1 μm, 100 ~ 300 eye mesh screens crossed by slurry, more namely obtain beryllium oxide slurry after deironing; According to weight ratio Hun He Liao ︰ Qu Li Shui ︰ φ 4 ~ 6mm zirconia ball=1 ︰ 0.3 ~ 1 ︰ 4 ~ 10;
Step 3., divide loose agent ︰ n-Octanol=100kg ︰ 1kg ︰ 5 ~ 10L ︰ 0.2L ︰ 0.3L ︰ 1 ~ 3L ︰ 2 ~ 5L to be joined in beryllium oxide slurry by other six kinds of raw materials according to the weightmeasurement ratio beryllium oxide slurry material ︰ third alkene acid ︰ polyethylene alcohol solution ︰ the third three sour ︰ of alcohol ︰ oil to mix to obtain mixed slurry, then add deionized water and regulate the viscosity of mixed slurry to be 3 ~ 5mPa.s;
4., by the mixed slurry mist projection granulating after adjusting viscosity step obtains granulation material, obtains shaping mist projection granulating material after 100 ~ 200 eye mesh screens; The condition of mist projection granulating is: inlet temperature 190 ~ 250 DEG C, temperature out 105 ~ 130 DEG C, pumping pressure 0.8 ~ 1.2MPa, and in tower, negative pressure keeps 0 ~ 100Pa;
B, extrusion forming: by the step 4. first dry-pressing process of the shaping mist projection granulating material of gained, make blank, then isostatic pressed process; The condition of dry-pressing process is: pressure 500 ~ 1000kg/cm 2, dwell time 5 ~ 10s; The condition of isostatic pressed process is: peak pressure 180 ~ 200MPa, dwell time 30 ~ 60s, one-level venting duration 15 ~ 30s, secondary venting duration 10 ~ 30s;
C, sintering: the blank after the process of step B isostatic pressed is adopted push pedal tunnel furnace multi-steps sintering, first paragraph: from room temperature to 600 ~ 650 DEG C, temperature rise rate is 30 ~ 60 DEG C/h; Second segment: be incubated 2 ~ 4h after being warming up to 1650 ~ 1700 DEG C again, temperature rise rate is 80 ~ 120 DEG C/h; 3rd section: can come out of the stove after Temperature fall, obtain ripe base; Ripe base is put down process again; Described multiple putting down is treated to: ripe base overlap is placed or placed separately, and place the object of 5 ~ 10kg above it, control temperature is 1500 DEG C;
D, mill processing:
1. roughing: with precision horizontal surface grinding machine processing length, width and gauge;
2. precision work: carry out polished finish to ceramics with shredder, polishing machine, makes ceramics surfaceness be less than 0.2;
3. be cut into supporting rod: cut into supporting rod with numerically-controlled precise cutting machine, with wear-resisting diamond wheel, the ceramics refined slotted, then cut with diamond wheel.
Concrete, in above-mentioned making method steps A, the massfraction of described polyvinyl alcohol water solution is 10%.
Concrete, in above-mentioned making method steps A, the preparation method of described polyvinyl alcohol water solution is: be dissolved in by polyvinyl alcohol after crossing 200 eye mesh screens after dissolving completely in the water of 60 ~ 80 DEG C and cool.
Preferably, in above-mentioned making method step C, when overlap is placed, stack height is not higher than 30mm.
The beryllium oxide ceramics supporting rod prepared by the making method of above-mentioned beryllium oxide ceramics supporting rod.
Sintering process adopts push pedal tunnel furnace one-time sintering technology, the labour intensity of the personnel that reduce the sintering difficulty of product, shorten firing period, reduce; Precision horizontal surface grinding machine is adopted to roughly grind ceramics, again through row polishing, then the mode by being equipped with the cutting machine of diamond wheel ceramics blank being processed into supporting rod processes beryllium oxide ceramics supporting rod, can guarantee working accuracy, improve working (machining) efficiency and conforming product rate.
It is simple to supporting rod shape requirement that tradition extrudes porcelain bar technique, is applicable to simple and long supporting rod and makes; But along with the development of science and technology, client is more and more higher to the compactness of supporting rod, profile, dimensional requirement, and traditional technology can not meet the demands.
In order to meet modern production to quality product, cost, the requirement of the aspects such as time, present invention process is for preparing the blank of large-size, again follow-up cutting processing is carried out to prepare supporting rod to blank, but through finding, traditional formula, it is inconsistent that technique has compactness by the product of cutting preparation, sintering temperature is higher, product thermal conductivity is on the low side, grain-size is excessive, the shortcomings such as product surface roughness working ability is not enough, so, the present inventor finds after lot of experiments: modify to formula for raw stock, material by wet type mixing is adopted to replace the mode of dry method batch mixing, coordinate dry-pressing again, the pressing mode of isostatic pressed, the process in early stage such as the mode of disposable sintering are adopted to obtain ripe base, supporting rod prepared by cutting has good performance, thus meet the requirement of modern production.
The sponging granulator that embodiment adopts is purchased from the dry factory in Qinghai 3419, and model is DTP-15; The semi-automatic forging press of 630KN is purchased from dry-pressing Nantong forging and stamping factory; 300MPa cold isostatic press is purchased from Chuan Xi machine works.
Embodiment 1
Take beryllium oxide powder body material 50kg, Magnesium Trisilicate 0.25kg, deionized water 50kg, zirconia ball 220kg, beryllium oxide powder body material and Magnesium Trisilicate are mixed to obtain compound, pour deionized water into agitation vat, again zirconia ball is put into agitation vat, open ball grinding stirring machine, rotating speed is 50RPM, and then adds compound, adding rear stirrer adjustment of rotational speed is 130RPM, and the granularity of ball milling 30min test slurry is 0.89 μm;
The slurry of ball milling is crossed 200 eye mesh screens, obtains slurry after deironing and be about 100kg, all pour in the slow agitation vat of sponging granulator; Take vinylformic acid 1kg, polyvinyl alcohol water solution (massfraction is 10%) 10L, glycerol 0.2L, oleic acid 0.3L, SD-00 dispersion agent 2.5L, n-Octanol 4.5L, these raw materials are added and stirs bucket slowly, stir 2h mixing, deionized water adjusting viscosity is added to 5mpa.s in blending process, mist projection granulating obtains granulation material, and (controlling Spray Grain-make Drier inlet temperature is 250 DEG C, temperature out is 110 DEG C, pumping pressure is 1.2MPa, in tower, negative pressure remains on 100Pa), granulation material is crossed 120 mesh sieve extension set process and is obtained shaping mist projection granulating material;
Forming mould (cavity dimension is 127mmx36.3mm) is installed on 63T hydropress, press maximum working pressure (MWP) 25MPa (instrument), shaping mist projection granulating material is put into mold cavity and carries out dry-pressing process, forming pressure is 20MPa (instrument), dwell time 5s, the green compact of shaping 127mmx36.3mmx4mm;
With the good green compact of plastic bag packaging, the fluid cylinder putting into cold isostatic press carries out isostatic pressed process, and pressurization peak pressure is set to 180MPa, and the dwell time is set to 30s, one-level pressure release 15s, secondary pressure release 10s, takes out blank;
When burning till, blank is warmed up to 600 DEG C through 30 DEG C/h, then 80 DEG C/h is warmed up to 1680 DEG C and is incubated 4h, Temperature fall cools, and after ripe burning, is stacked together by ceramics 5 pieces, placing the heavy burden of 5 pieces of load bearing boards (about 5kg) above, is multiple flat in the elevator furnace of 1500 DEG C in final temperature;
After grinding, polishing, cutting, obtain being of a size of thin brilliant supporting rod C1, the C1 various aspects of performance of 0.8mmx2mmx98mm as shown in table 1;
Polishing: ceramics is coarse below 0.2 through glazed surface.
Embodiment 2
Take beryllium oxide powder body material 50kg, Magnesium Trisilicate 0.25kg, deionized water 50kg, zirconia ball 220kg, beryllium oxide powder body material and Magnesium Trisilicate are mixed to obtain compound, pour deionized water into agitation vat, again zirconia ball is put into agitation vat, open ball grinding stirring machine, rotating speed is 50RPM, and then adds compound, adding rear stirrer adjustment of rotational speed is 130RPM, and the granularity of ball milling 30min test slurry is 0.92 μm;
The slurry of ball milling is crossed 200 eye mesh screens, obtains slurry after deironing and be about 100kg, all pour in the slow agitation vat of sponging granulator;
Take vinylformic acid 1kg, polyvinyl alcohol water solution (massfraction is 10%) 10L, glycerol 0.2L, oleic acid 0.3L, SD-00 dispersion agent 3L, n-Octanol 5L, these raw materials are added and stirs bucket slowly, stir 2h mixing, deionized water adjusting viscosity is added to 4mpa.s in blending process, mist projection granulating obtains granulation material, and (controlling Spray Grain-make Drier inlet temperature is 250 DEG C, temperature out is 110 DEG C, pumping pressure is 1.2MPa, in tower, negative pressure remains on 100Pa), granulation material is crossed 120 mesh sieve extension set process and is obtained shaping mist projection granulating material;
Time shaping, forming mould (cavity dimension is 127mmx36.3mm) is installed on 63T hydropress, press maximum working pressure (MWP) 25MPa (instrument), shaping mist projection granulating material is put into mold cavity and carries out dry-pressing process, forming pressure is 20MPa (instrument), dwell time 5s, the green compact of shaping 127mmx36.3mmx4mm;
With the good green compact of plastic bag packaging, the fluid cylinder putting into cold isostatic press carries out isostatic pressed process, and pressurization peak pressure is set to 180MPa, and the dwell time is set to 30s, one-level pressure release 15s, secondary pressure release 10s, takes out blank;
When burning till, blank is warmed up to 650 DEG C through 60 DEG C/h, then 120 DEG C/h is warmed up to 1700 DEG C and is incubated 4h, Temperature fall cools, and after ripe burning, is stacked together by ceramics 5 pieces, placing the heavy burden of 5 pieces of load bearing boards (about 5kg) above, is multiple flat in the elevator furnace of 1500 DEG C in final temperature;
After grinding, polishing, cutting, obtain being of a size of thin brilliant supporting rod C2, the C2 various aspects of performance of 0.8mmx2mmx98mm as shown in table 1;
Polishing: ceramics is coarse below 0.2 through glazed surface.
Comparative example
Beryllium oxide powder 50kg, magnesium oxide 0.125g, aluminum oxide 0.125g, deionized water 40kg, polyvinyl alcohol solution (massfraction 10%) 5kg are put into three-dimensional motion mixer mixing 30min after mixing again; The material mixed is calcined 3h at 1400 DEG C; The material calcined is smashed to pieces, according to weight ratio Liao ︰ Shui ︰ beryllium oxide ball=1 ︰ 1 ︰ 2, three is put into jar mill ball milling 20h again, again the slurry that tank grinds is put into 30-S ball grinding stirring machine and carry out stirring ball-milling, Ball-milling Time 30min according to Jiang Liao ︰ Qu Li Shui ︰ zirconia ball=1 ︰ 1 ︰ 4; Calcine in 1050 DEG C after the slurry of stirring ball-milling is dried; After calcining, grind, put into jar mill ball milling 3h according to the ratio of weight ratio Liao ︰ Jiu Jing ︰ beryllium oxide ball=1 ︰ 2 ︰ 2, the slurry after dispersion mill is crossed 80 eye mesh screens, then obtains beryllium oxide extrusion forming material in 60 DEG C of dryings, for subsequent use;
Methylcellulose gum 5kg, deionized water 25kg, glycerol 0.5kg, oleic acid 0.5kg is taken, mix and blend configuration methocel solution according to weight ratio Jia base Xian Wei Su ︰ Qu Li Shui ︰ Bing tri-Chun ︰ oleic acid=4-5 ︰ 21-25 ︰ 0.5-0.6 ︰ 0.5-0.6.Configure rear for subsequent use;
According to weight ratio, beryllium oxide Fen Liao ︰ methocel solution=100 ︰ 30 of oven dry is taken methocel solution 15kg, be mixed and made into walk with beryllium oxide extrusion forming material, put into vacuum deairing machine, perfect rear old 48h, pugging again, old 24h;
After old mud again pugging 4 times, put into tube extruding machine, extrude into the porcelain bar that length is about 500mm, deposit drying; The porcelain bar of drying is put into high temperature bell jar kiln and carries out binder removal, dump temperature final temperature is 1450 DEG C, and whole binder removal cycle 45h, carries out ripe burning after binder removal, carry out equally at high temperature top-hat kiln, the insulation of sintering top temperature about 1750 DEG C 4h, ripe burning cycle 45h;
Grinding, by porcelain bar circular after ripe burning, by peripheral milling, flat stone mill, hand mill (cannot polishing) mill is processed into the T-shaped supporting rod C3 of 0.8mmx2mmx98mm, and C3 various aspects of performance is as shown in table 1.
National military standard is wherein specially national military standard standard GJB3522A-2011 beryllium oxide ceramics specification, the wherein performance of B-99.
Table 1 each embodiment beryllium oxide ceramics supporting rod performance comparison
As can be seen from Table 1, the beryllium oxide ceramics supporting rod volume density adopting the inventive method to prepare is improved, average grain size reduces, thermal conductivity (25 DEG C, 100 DEG C) performance compares traditional technology C3 entirety raising about 10%, thermal conductivity exceeds military standard of China far away, electric Jie's performance is far superior to the product that traditional method prepares.
In summary it can be seen, product compactness of the present invention is good, and intensity is high, better selects for the higher meticulousr supporting rod of processing request provides one.

Claims (10)

1. a making method for beryllium oxide ceramics supporting rod, is characterized in that: comprise the following steps:
A, prepare shaping mist projection granulating material:
1., according to weight ratio Yangization Pi ︰ Magnesium Trisilicate=100 ︰ 0.5 ~ 0.55 both are mixed to obtain compound by step;
2., by compound and deionized water step mixes to obtain slurry, and in slurry, add φ 4 ~ 6mm zirconia ball, ball milling slurry is to slurry granularity D 50be not more than 1 μm, 100 ~ 300 eye mesh screens crossed by slurry, more namely obtain beryllium oxide slurry after deironing; According to weight ratio Hun He Liao ︰ Qu Li Shui ︰ φ 4 ~ 6mm zirconia ball=1 ︰ 0.3 ~ 1 ︰ 4 ~ 10;
Step 3., divide loose agent ︰ n-Octanol=100kg ︰ 1kg ︰ 5 ~ 10L ︰ 0.2L ︰ 0.3L ︰ 1 ~ 3L ︰ 2 ~ 5L to be joined in beryllium oxide slurry by other six kinds of raw materials according to the weightmeasurement ratio beryllium oxide slurry material ︰ third alkene acid ︰ polyethylene alcohol solution ︰ the third three sour ︰ of alcohol ︰ oil to mix to obtain mixed slurry, then add deionized water and regulate the viscosity of mixed slurry to be 3 ~ 5mPa.s;
4., by the mixed slurry mist projection granulating after adjusting viscosity step obtains granulation material, obtains shaping mist projection granulating material after 100 ~ 200 eye mesh screens;
B, extrusion forming;
C, sintering;
D, grind processing on request, then cut into supporting rod.
2. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 1, is characterized in that: in steps A 3., and described dispersion agent is any one in water glass, tripoly phosphate sodium STPP, Trisodium Citrate, sodium polyacrylate or poly carboxylic acid sodium.
3. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 1, is characterized in that: in steps A 3., and the massfraction of described polyvinyl alcohol water solution is 10%.
4. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 1, it is characterized in that: in steps A 4., the condition of described mist projection granulating is: inlet temperature 190 ~ 250 DEG C, temperature out 105 ~ 130 DEG C, pumping pressure 0.8 ~ 1.2MPa, in tower, negative pressure keeps 0 ~ 100Pa.
5. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 1, it is characterized in that: in step B, the concrete steps of described extrusion forming are: by the step 4. first dry-pressing process of the shaping mist projection granulating material of gained, make blank, then isostatic pressed process.
6. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 5, is characterized in that: in step B, and the condition of described dry-pressing process is: pressure 500 ~ 1000kg/cm 2, dwell time 5 ~ 10s.
7. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 5, it is characterized in that: in step B, the condition of described isostatic pressed process is: peak pressure 180 ~ 200MPa, dwell time 30 ~ 60s, one-level venting duration 15 ~ 30s, secondary venting duration 10 ~ 30s.
8. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 1, it is characterized in that: in step C, the concrete steps of described sintering are: by the blank multi-steps sintering after the process of step B isostatic pressed, first paragraph: from room temperature to 600 ~ 650 DEG C, temperature rise rate is 30 ~ 60 DEG C/h; Second segment: be incubated 2 ~ 4h after being warming up to 1650 ~ 1700 DEG C again, temperature rise rate is 80 ~ 120 DEG C/h; 3rd section: can come out of the stove after Temperature fall, obtain ripe base; Ripe base is put down process again.
9. the making method of a kind of beryllium oxide ceramics supporting rod according to claim 8, is characterized in that: in step C, and described multiple putting down is treated to: ripe base overlap is placed or placed separately, and place the object of 5 ~ 10kg above it, control temperature is 1500 DEG C.
10. the beryllium oxide ceramics supporting rod prepared by the making method of the beryllium oxide ceramics supporting rod described in any one of claim 1 ~ 9.
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CN110105055A (en) * 2019-06-20 2019-08-09 宜宾红星电子有限公司 The production method that thin film circuit polishes substrate with beryllium oxide ceramics
CN113773059A (en) * 2021-09-24 2021-12-10 宜宾红星电子有限公司 Manufacturing process of miniaturized ceramic window sheet for high-frequency electric vacuum device
CN114538933A (en) * 2020-11-24 2022-05-27 娄底市安地亚斯电子陶瓷有限公司 Method for manufacturing travelling wave tube clamping rod
CN115179395A (en) * 2022-07-19 2022-10-14 宜宾红星电子有限公司 Molding method for high-flatness ceramic substrate

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101219899A (en) * 2008-01-10 2008-07-16 电子科技大学 Process for producing beryllium oxide ceramics material with high heat-conduction and high breaking strength
CN101271803A (en) * 2007-03-21 2008-09-24 中国科学院电子学研究所 Helix TWT slow wave component and production method
CN103693946A (en) * 2013-11-21 2014-04-02 宜宾红星电子有限公司 High-thermal conductivity TiO2-containing microwave attenuating ceramic and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101271803A (en) * 2007-03-21 2008-09-24 中国科学院电子学研究所 Helix TWT slow wave component and production method
CN101219899A (en) * 2008-01-10 2008-07-16 电子科技大学 Process for producing beryllium oxide ceramics material with high heat-conduction and high breaking strength
CN103693946A (en) * 2013-11-21 2014-04-02 宜宾红星电子有限公司 High-thermal conductivity TiO2-containing microwave attenuating ceramic and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819832A (en) * 2016-03-29 2016-08-03 宜宾红星电子有限公司 Beryllium oxide/silicon carbide ceramic composite microwave attenuation ceramic and preparation method thereof
CN105819832B (en) * 2016-03-29 2018-09-18 宜宾红星电子有限公司 Beryllium oxide/silicon carbide compound microwave attenuative ceramics and preparation method thereof
CN110105055A (en) * 2019-06-20 2019-08-09 宜宾红星电子有限公司 The production method that thin film circuit polishes substrate with beryllium oxide ceramics
CN114538933A (en) * 2020-11-24 2022-05-27 娄底市安地亚斯电子陶瓷有限公司 Method for manufacturing travelling wave tube clamping rod
CN114538933B (en) * 2020-11-24 2022-11-22 娄底市安地亚斯电子陶瓷有限公司 Method for manufacturing travelling wave tube clamping rod
CN113773059A (en) * 2021-09-24 2021-12-10 宜宾红星电子有限公司 Manufacturing process of miniaturized ceramic window sheet for high-frequency electric vacuum device
CN115179395A (en) * 2022-07-19 2022-10-14 宜宾红星电子有限公司 Molding method for high-flatness ceramic substrate

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