CN108516837A - A kind of microwave attenuative ceramics and preparation method thereof - Google Patents
A kind of microwave attenuative ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of microwave attenuative ceramics and preparation method thereof, belong to absorbing material technical field.The present invention builds contact point by the way that aluminum nitride powder ball milling to be dispersed into nanometer sheet stratiform boron nitride spacing, it is formed with high heat conductance, moderate dielectric constant, good chemically and thermally stability, the framework material of very high resistivity, there is good thermal conductivity and electric conductivity using metal Mo simultaneously, and coefficient of expansion the characteristics of being close with aluminium nitride, the conductive phase granules such as Mo are uniformly distributed in ceramic material, improve the dielectric loss of material, make material that integrally there is high heat conductance, the excellent thermal property such as low elastic modulus and coefficient of thermal expansion, to which realization prepares the target of the novel microwave attenuating material of excellent combination property；Porcelain body densified sintering product of the present invention, almost without stomata, the material of irregular grain morphology makes absorption and scattering area increase, the microwave attenuation ability of reinforcing material when with microwave action.
Description
Technical field
The present invention relates to a kind of microwave attenuative ceramics and preparation method thereof, belong to absorbing material technical field.
Background technology
Microwave attenuating material is a kind of energy electromagnetic wave absorption, and converts thereof into thermal energy and be transported to outside material bodies or make electricity
What magnetic wave disappeared by interference, and the functional material of the reflection to electromagnetic wave, scattering and projection all very littles.In recent years, high heat conduction
Microwave attenuating material causes the extensive attention of scientific research personnel.
With the rapid development of modern electronic technology, microwave electron tube towards micromation, lighting, high integration,
High reliability, high-power output direction develop, this is just badly in need of that high heat conduction microwave attenuating material is wanted to be used as body attenuator or damage
The critical components such as consumption button are supported to develop skill, and to cut off feedback approach, improve the job stability of device.Lack microwave to decline
Subtract material, microwave electron tube, especially high power device will be unable to normal use.
HIGH-POWERED MICROWAVES electron tube is to the basic demand of attenuating material：（1）Dielectric constant is high and imaginary part is controllable,
It is to realize attenuating material high attenuation, can bear one of powerful key, the controllable purpose of imaginary part is to meet different pipes
The travelling-wave tubes requirement of type；（2）Matrix has good thermal conductivity, and heat caused by microwave attenuation is transferred out in time
It goes, maintains the normal operating conditions of travelling-wave tubes；（3）High temperature and chemical stability are preferable, ensure that material is amenable to entire tubulation work
Skill process and performance is constant；（4）Certain mechanical strength, it is without damage during shelving or pipe use to ensure, suitably
Linear expansion coefficient, meet the welding demand of attenuation ceramic and pipe inner metal component；（5）Material wishes simple for process, easy in the preparation
In control, reproducible, high yield rate.Lack microwave attenuating material, microwave electron tube, especially high power device will not
It can normal use.
Microwave attenuation porcelain used in domestic microwave tube mainly adds not in aluminium oxide or beryllium oxide dielectric phase
Decay together the composite material mutually formed.Wherein, carburizing Woelm Alumina attenuation ceramic makes microwave reflection amount due to its porous feature
Obtained certain application less, but the disadvantage is that discharge quantity is big, intensity is relatively low, decaying distributed mutually unevenness hook, carburizing yield rate compared with
Low, it is low that porous structure is allowed to thermal conductivity, and certain obstacle is caused to high power tube use.Therefore, to novel microwave decaying material
The research of material is extremely urgent.
Invention content
The technical problems to be solved by the invention：Uneven for existing microwave attenuative ceramics decaying distributed mutually, thermal conductivity is low
Under, the problem of causing obstacle to high power tube use, provides a kind of microwave attenuative ceramics and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
The microwave attenuative ceramics is made of the sintering of following weight parts raw material：20 ~ 30 parts of nanometer sheet stratiform boron nitride, 30 ~ 50 parts
Nano aluminum nitride, 20 ~ 30 parts of silicon carbide, 10 ~ 20 parts of molybdenum powders, 1 ~ 3 part of calcirm-fluoride, 1 ~ 3 part of aluminium oxide.
The nanometer sheet stratiform boron nitride is that boric acid is mixed and heated to 50~60 DEG C with deionized water, adds urea and rises
Temperature washs dry be made to being evaporated to dryness under reduced pressure after 60~70 DEG C after high-temperature calcination.
The boric acid, deionized water, the parts by weight of urea be 150~200 parts of boric acid, 1200 ~ 1500 parts of deionized waters,
300~400 parts of urea.
The high-temperature burning process be under nitrogen atmosphere, with 20 DEG C/min rates be warming up to 800~900 DEG C calcining 3~
6h。
The nano aluminum nitride is yttrium nitrate, the dissolving of calcium nitrate, aluminum nitrate, glucose in deionized water, then depressurizes steaming
Be sent to it is dry, after calcination processing nitrogen treatment be made.
The yttrium nitrate, calcium nitrate, aluminum nitrate, glucose, deionized water parts by weight be 1~3 part of yttrium nitrate, 1~2 part
Calcium nitrate, 200~300 parts of aluminum nitrates, 20~40 parts of glucose, 300~500 parts of deionized waters.
The calcination processing process is to be warming up to 600~700 DEG C of calcinings under carbon monoxide atmosphere with 20 DEG C/min rates
1~2h.
The nitrogen treatment process is 19 to be passed through volume ratio with 100~200mL/min rates：1 nitrogen and hydrogen mixture, and
It is warming up to 1300~1600 DEG C of 3~4h of nitrogen treatment with 20 DEG C/min rates.
A kind of preparation method of the microwave attenuative ceramics, the specific steps are：
（1）Boric acid and deionized water are mixed and heated to 50~60 DEG C, depressurizes and steams after adding urea and being warming up to 60~70 DEG C
It is sent to dry, obtains presoma；
（2）Presoma is placed in Muffle furnace, is washed simultaneously for 1% hydrochloric acid and absolute ethyl alcohol with mass fraction successively after high-temperature calcination
It is dry, obtain nanometer sheet stratiform boron nitride；
（3）It takes yttrium nitrate, calcium nitrate, aluminum nitrate, glucose to be added in deionized water to dissolve, then is evaporated to dryness under reduced pressure, obtain solid
Powder；
（4）Solid powder is placed in Muffle furnace nitrogen treatment after calcination processing, obtains nano aluminum nitride；
（5）Nanometer sheet stratiform boron nitride, nano aluminum nitride, silicon carbide, molybdenum powder, calcirm-fluoride, aluminium oxide are taken, is packed into after ball milling mixing
In mold, discharge plasma sintering is carried out at 8 ~ 10MPa pressure, 1600 ~ 1700 DEG C, and microwave attenuation pottery is obtained after being cooled to room temperature
Porcelain.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention builds contact point by the way that aluminum nitride powder ball milling to be dispersed into nanometer sheet stratiform boron nitride spacing, is formed
There are high heat conductance, moderate dielectric constant, good chemically and thermally stability, the framework material of very high resistivity, while profit
There is good thermal conductivity and electric conductivity with metal Mo, and the characteristics of the coefficient of expansion is close with aluminium nitride, in ceramic material
Be uniformly distributed the conductive phase granules such as Mo, improve the dielectric loss of material, make material integrally have high heat conductance, low elastic modulus and
The excellent thermal property such as coefficient of thermal expansion, to which realization prepares the target of the novel microwave attenuating material of excellent combination property；
（2）The present invention makes sintering aid generate liquid phase by high temperature sintering, and solid phase particles can be soaked by liquid phase, and molecule is pollinated
The influence for the capillary tension that body ambient liquid phase generates is into rearrangement, and the frictional force that liquid phase itself can also be such that particle re-arrangement generates subtracts
Small, while reducing hole, particle more closely arranges, and sintered density accordingly improves so that ceramic crystalline grain in irregular,
Crystal particle dimension difference is larger, porcelain body densified sintering product, almost without stomata, the material of irregular grain morphology with microwave action
When, so that absorption and scattering area is increased, the microwave attenuation ability of reinforcing material.
Specific implementation mode
It takes 150~200g boric acid, is added in 1.2~1.5L deionized waters, 50 are heated with stirring to 300~400r/min~
It 60 DEG C, adds 300~400g urea and is warming up to 60~70 DEG C, be evaporated to dryness under reduced pressure after continuing 30~40min of stirring, before obtaining
Drive body, presoma is placed in Muffle furnace, under nitrogen atmosphere, with 20 DEG C/min rates be warming up to 800~900 DEG C calcining 3~
6h takes out product after being cooled to room temperature, and is to use absolute ethyl alcohol washed product again after 1% hydrochloric acid washed product 1 ~ 2 time with mass fraction
It 1~2 time, being transferred in drying box after washing, dry 6~8h, obtains nanometer sheet stratiform boron nitride at 80~90 DEG C, take 1~
3g yttrium nitrates, 1~2g calcium nitrate, 200~300g aluminum nitrates, 20~40g glucose are added in 300~500mL deionized waters, with
300~400r/min stirs 30 ~ 40min, then is placed on Rotary Evaporators and is evaporated to dryness under reduced pressure, and solid powder is obtained, by solid powder
End is placed in Muffle furnace, under carbon monoxide atmosphere, with 20 DEG C/min rates be warming up to 600~700 DEG C calcining 1~2h, then with
It is 19 that 100~200mL/min rates, which are passed through volume ratio,：1 nitrogen and hydrogen mixture, and it is warming up to 1300 with 20 DEG C/min rates~
1600 DEG C of 3~4h of nitrogen treatment, are cooled to room temperature to obtain nano aluminum nitride, and 20 ~ 30g nanometer sheet stratiform boron nitride, 30 ~ 50g is taken to receive
Rice aluminium nitride, 20 ~ 30g silicon carbide, 10 ~ 20g molybdenum powders, 1 ~ 3g calcirm-fluoride, 1 ~ 3g aluminium oxide, be fitted into ball mill with 200 ~
240r/min 10 ~ 20h of ball milling, the powder that ball milling finishes is fitted into mold, is carried out at 8 ~ 10MPa pressure, 1600 ~ 1700 DEG C
Discharge plasma sintering obtains microwave attenuative ceramics after being cooled to room temperature.
Example 1
150g boric acid is taken, is added in 1.2L deionized waters, is heated with stirring to 50 DEG C with 300r/min, adds 300g urea and rise
Temperature continues to be evaporated to dryness under reduced pressure after stirring 30min, obtains presoma, presoma is placed in Muffle furnace, in nitrogen atmosphere to 60 DEG C
Under, 800 DEG C of calcining 3h are warming up to 20 DEG C/min rates, product is taken out after being cooled to room temperature, is 1% salt pickling with mass fraction
Absolute ethyl alcohol washed product being used again 1 time after washing product 1 time, being transferred in drying box after washing, dry 6h, must receive at 80 DEG C
Rice sheet boron nitride, takes 1g yttrium nitrates, 1g calcium nitrate, 200g aluminum nitrates, and 20g glucose is added in 300mL deionized waters, with
300r/min stirs 30min, then is placed on Rotary Evaporators and is evaporated to dryness under reduced pressure, and obtains solid powder, solid powder is placed in horse
Not in stove, under carbon monoxide atmosphere, 600 DEG C of calcining 1h are warming up to 20 DEG C/min rates, then be passed through with 100mL/min rates
Volume ratio is 19：1 nitrogen and hydrogen mixture, and 1300 DEG C of nitrogen treatment 3h are warming up to 20 DEG C/min rates, it is cooled to room temperature
Nano aluminum nitride takes 20g nanometer sheet stratiform boron nitride, 30g nano aluminum nitrides, 20g silicon carbide, 10g molybdenum powders, 1g calcirm-fluoride, 1g
Aluminium oxide is fitted into ball mill with 200r/min ball milling 10h, the powder that ball milling finishes is fitted into mold, in 8MPa pressure,
Discharge plasma sintering is carried out at 1600 DEG C, and microwave attenuative ceramics is obtained after being cooled to room temperature.
Example 2
180g boric acid is taken, is added in 1.3L deionized waters, is heated with stirring to 55 DEG C with 350r/min, adds 350g urea and rise
Temperature continues to be evaporated to dryness under reduced pressure after stirring 35min, obtains presoma, presoma is placed in Muffle furnace, in nitrogen atmosphere to 65 DEG C
Under, 850 DEG C of calcining 5h are warming up to 20 DEG C/min rates, product is taken out after being cooled to room temperature, is 1% salt pickling with mass fraction
Absolute ethyl alcohol washed product being used again 1 time after washing product 1 time, being transferred in drying box after washing, dry 7h, must receive at 85 DEG C
Rice sheet boron nitride, takes 2g yttrium nitrates, 1g calcium nitrate, 250g aluminum nitrates, and 30g glucose is added in 400mL deionized waters, with
350r/min stirs 35min, then is placed on Rotary Evaporators and is evaporated to dryness under reduced pressure, and obtains solid powder, solid powder is placed in horse
Not in stove, under carbon monoxide atmosphere, 650 DEG C of calcining 1h are warming up to 20 DEG C/min rates, then be passed through with 150mL/min rates
Volume ratio is 19：1 nitrogen and hydrogen mixture, and 1500 DEG C of nitrogen treatment 3h are warming up to 20 DEG C/min rates, it is cooled to room temperature
Nano aluminum nitride takes 25g nanometer sheet stratiform boron nitride, 40g nano aluminum nitrides, 25g silicon carbide, 15g molybdenum powders, 2g calcirm-fluoride, 2g
Aluminium oxide is fitted into ball mill with 220r/min ball milling 15h, the powder that ball milling finishes is fitted into mold, in 9MPa pressure,
Discharge plasma sintering is carried out at 1650 DEG C, and microwave attenuative ceramics is obtained after being cooled to room temperature.
Example 3
200g boric acid is taken, is added in 1.5L deionized waters, is heated with stirring to 60 DEG C with 400r/min, adds 400g urea and rise
Temperature continues to be evaporated to dryness under reduced pressure after stirring 40min, obtains presoma, presoma is placed in Muffle furnace, in nitrogen atmosphere to 70 DEG C
Under, 900 DEG C of calcining 6h are warming up to 20 DEG C/min rates, product is taken out after being cooled to room temperature, is 1% salt pickling with mass fraction
Absolute ethyl alcohol washed product being used again 2 times after washing product 2 times, being transferred in drying box after washing, dry 8h, must receive at 90 DEG C
Rice sheet boron nitride, takes 3g yttrium nitrates, 2g calcium nitrate, 300g aluminum nitrates, and 40g glucose is added in 500mL deionized waters, with
400r/min stirs 40min, then is placed on Rotary Evaporators and is evaporated to dryness under reduced pressure, and obtains solid powder, solid powder is placed in horse
Not in stove, under carbon monoxide atmosphere, 700 DEG C of calcining 2h are warming up to 20 DEG C/min rates, then be passed through with 200mL/min rates
Volume ratio is 19：1 nitrogen and hydrogen mixture, and 1600 DEG C of nitrogen treatment 4h are warming up to 20 DEG C/min rates, it is cooled to room temperature
Nano aluminum nitride takes 30g nanometer sheet stratiform boron nitride, 50g nano aluminum nitrides, 30g silicon carbide, 20g molybdenum powders, 3g calcirm-fluoride, 3g
Aluminium oxide is fitted into ball mill with 240r/min ball milling 20h, the powder that ball milling finishes is fitted into mold, in 10MPa pressure,
Discharge plasma sintering is carried out at 1700 DEG C, and microwave attenuative ceramics is obtained after being cooled to room temperature.
Reference examples：The microwave attenuating material of Guangdong company production.
The microwave attenuating material of example and reference examples is detected, specific detection is as follows：
Dielectric properties：The thin discs sample obtained after SPS is sintered is ground off into surface carbon paper, sanding and polishing, and burning infiltration silver electricity
After extremely, the capacitance of sample is measured with Agilent4284A type precise impedance analyzers in 1000Hz ~ 1MHz frequency ranges and dielectric is damaged
Tangent is consumed, and calculates the dielectric constant of material according to formula.
Resistivity：The volume resistance of sample is measured using the Cp-Rp patterns of Agilent4284A type precise impedance analyzers,
Then the resistivity of sample is calculated with formula.
Thermal conductivity is tested：Material is accurately measured using German Nai Chi companies NETZSCHLFA457 laser Conduction Coefficient Detector Basings
Thermal diffusivity, in the thermal conductivity by thermal diffusivity numerical computations material.
Specific testing result such as table 1.
1 performance characterization contrast table of table
As shown in Table 1, the microwave attenuating material that prepared by the present invention has good dielectricity, resistivity and thermal conductivity, meets
Indices requirement.
Claims (9)
1. a kind of microwave attenuative ceramics, which is characterized in that the microwave attenuative ceramics is made of the sintering of following weight parts raw material：20
~ 30 parts of nanometer sheet stratiform boron nitride, 30 ~ 50 parts of nano aluminum nitrides, 20 ~ 30 parts of silicon carbide, 10 ~ 20 parts of molybdenum powders, 1 ~ 3 part of fluorination
Calcium, 1 ~ 3 part of aluminium oxide.
2. a kind of microwave attenuative ceramics as described in claim 1, which is characterized in that the nanometer sheet stratiform boron nitride is boric acid
50~60 DEG C are mixed and heated to deionized water, add urea and is evaporated to dryness under reduced pressure after being warming up to 60~70 DEG C, through high temperature
Dry be made is washed after calcining.
3. a kind of microwave attenuative ceramics as claimed in claim 2, which is characterized in that the boric acid, deionized water, urea weight
Amount part is 150~200 parts of boric acid, 1200 ~ 1500 parts of deionized waters, 300~400 parts of urea.
4. a kind of microwave attenuative ceramics as claimed in claim 2, which is characterized in that the high-temperature burning process is in nitrogen atmosphere
Under enclosing, 800~900 DEG C of 3~6h of calcining are warming up to 20 DEG C/min rates.
5. a kind of microwave attenuative ceramics as described in claim 1, which is characterized in that the nano aluminum nitride is yttrium nitrate, nitre
Sour calcium, aluminum nitrate, glucose dissolving in deionized water, then are evaporated to dryness under reduced pressure, and nitrogen treatment is made after calcination processing.
6. a kind of microwave attenuative ceramics as claimed in claim 5, which is characterized in that the yttrium nitrate, calcium nitrate, aluminum nitrate,
Glucose, deionized water parts by weight be 1~3 part of yttrium nitrate, 1~2 part of calcium nitrate, 200~300 parts of aluminum nitrates, 20~40 parts
Glucose, 300~500 parts of deionized waters.
7. a kind of microwave attenuative ceramics as claimed in claim 5, which is characterized in that the calcination processing process is in an oxidation
Under carbon atmosphere, 600~700 DEG C of 1~2h of calcining are warming up to 20 DEG C/min rates.
8. a kind of microwave attenuative ceramics as claimed in claim 5, which is characterized in that the nitrogen treatment process be with 100~
It is 19 that 200mL/min rates, which are passed through volume ratio,:1 nitrogen and hydrogen mixture, and it is warming up to 1300~1600 DEG C with 20 DEG C/min rates
3~4h of nitrogen treatment.
9. a kind of preparation method of microwave attenuative ceramics as described in claim 1 ~ 7 any one, which is characterized in that specific step
Suddenly it is：
（1）Boric acid and deionized water are mixed and heated to 50~60 DEG C, depressurizes and steams after adding urea and being warming up to 60~70 DEG C
It is sent to dry, obtains presoma；
（2）Presoma is placed in Muffle furnace, is washed simultaneously for 1% hydrochloric acid and absolute ethyl alcohol with mass fraction successively after high-temperature calcination
It is dry, obtain nanometer sheet stratiform boron nitride；
（3）It takes yttrium nitrate, calcium nitrate, aluminum nitrate, glucose to be added in deionized water to dissolve, then is evaporated to dryness under reduced pressure, obtain solid
Powder；
（4）Solid powder is placed in Muffle furnace nitrogen treatment after calcination processing, obtains nano aluminum nitride；
（5）Nanometer sheet stratiform boron nitride, nano aluminum nitride, silicon carbide, molybdenum powder, calcirm-fluoride, aluminium oxide are taken, is packed into after ball milling mixing
In mold, discharge plasma sintering is carried out at 8 ~ 10MPa pressure, 1600 ~ 1700 DEG C, and microwave attenuation pottery is obtained after being cooled to room temperature
Porcelain.
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