CN107602156A - A kind of microwave-absorbing ceramic and preparation method thereof - Google Patents
A kind of microwave-absorbing ceramic and preparation method thereof Download PDFInfo
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- CN107602156A CN107602156A CN201710951568.5A CN201710951568A CN107602156A CN 107602156 A CN107602156 A CN 107602156A CN 201710951568 A CN201710951568 A CN 201710951568A CN 107602156 A CN107602156 A CN 107602156A
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Abstract
The present invention relates to a kind of preparation method of microwave-absorbing ceramic, including herein below：(1) mixed liquor of zinc acetate, aluminium compound, alcamine compound and good solvent is taken, molar concentration of the zinc acetate in mixed liquor is 0.1~1mol/L, and zinc acetate is 1 with alcamine compound mol ratio:1, Al and Zn mol ratio is 0 0.02:1, stood after stirring, obtain presoma；(2) by porous alumina ceramic impregnation in the presoma, precast body is made, after heat treatment obtains infused ceramic；(3) impregnation in presoma by the infused ceramic, is then heat-treated again；This step repeats, and obtains the infused ceramic that zinc oxide content is 7.0 11.5wt%；(4) heat up, be heat-treated under protective atmosphere, produce microwave-absorbing ceramic material.ZnO is synthesized using wet chemistry method, product ZnO granular size, recrystallization temperature, obtained ZnO/Al can be greatly lowered2O3ZnO in complex phase ceramic is evenly distributed, and is advantageous to improve the absorbing property of material.
Description
Technical field
The invention belongs to absorbing material technical field, and in particular to a kind of microwave-absorbing ceramic and preparation method thereof.
Background technology
Absorbing material is to refer to the incident electromagnetic wave energy of attenuation by absorption, and its electromagnetic energy is converted into heat energy or other shapes
Formula energy dissipation is fallen, so as to reduce a kind of material of reflection of electromagnetic wave or transmission.Absorbing material can be divided into magnetic loss type and Jie
The class of dielectric loss type two.Most of magnetic material is limited by Curie temperature, can only provide stable wave absorbtion at a lower temperature
Energy.When environment temperature rise to a certain extent, magnetic loss defunctionalization.Therefore, dielectric loss type absorbing material is inhaled as high temperature
The inevitable choice of wave material.
Under normal circumstances, the electronic component in device is needed in room temperature or under relatively less high environment temperature
Stable working condition could be kept.Absorbing material does not need only to have good absorbing property used by this is required, and
And higher environment temperature is resistant to, also need to that there is low thermal conductivity in addition.
The content of the invention
The present invention is directed to prior art weak point, there is provided a kind of microwave-absorbing ceramic and preparation method thereof.
To achieve the above object, technical scheme provided by the invention is：
A kind of preparation method of microwave-absorbing ceramic, including herein below：
(1) mixed liquor of zinc acetate, aluminium compound, alcamine compound and good solvent is taken, zinc acetate is in mixed liquor
Molar concentration be 0.1~1mol/L, zinc acetate is 1 with alcamine compound mol ratio:1, Al and Zn mol ratio is 0-
0.02:1, stood after stirring, obtain presoma；
(2) by porous alumina ceramic impregnation in the presoma, precast body is made, is after heat treatment soaked
Stain ceramics；
(3) impregnation in presoma by the infused ceramic, is then heat-treated again；This step repeats, and obtains
Zinc oxide content is 7.0-11.5wt% infused ceramic；
(4) heat up, be heat-treated under protective atmosphere, produce microwave-absorbing ceramic material.
Above scheme, when the mol ratio for Al and Zn is 0, it is understood that calorize conjunction is not contained in mixed liquor
Thing.
Further, in step (1), the preparation method of the presoma is：24- is stood after mixed liquor is stirred
48h, obtain presoma.
Further, the aluminium compound is selected from aluminum nitrate or alchlor.
Further, the alcamine compound is selected from monoethanolamine or diethanol amine.
Further, the good solvent is selected from ethylene glycol, isopropanol or ethylene glycol monomethyl ether.
Applicant is found surprisingly that loads zinc oxide in the range of 8.2-12.4GHz compared with low porosity porous alumina ceramic
With good absorbing property, and load capacity is few, solves the problems, such as that improving absorbing property needs to increase load capacity.And increase negative
Carrying capacity needs to make the porosity of porous alumina ceramic to increase, there is provided more spaces separate out zinc oxide, so as to increase suction ripple
The content of agent, but study find the excessive absorption being unfavorable for electromagnetic wave of wave absorbing agent content, and with porosity increase also
Structural strength step-down can be caused.Preferably, the porous alumina ceramic porosity is 28-35%；Further, it is selected from
30%.
Further, heat treatment temperature is 300-500 DEG C in step (2) and step (3), a length of 0.5-2h during heat treatment.
Further, heat treatment temperature is 600-800 DEG C in step (4), a length of 2-4h during heat treatment.
Further, the flow of protective atmosphere is 25-100ml/min in step (4).
Further, heating rate is 1-5 DEG C/min in step (4).
Present invention also offers microwave-absorbing ceramic made from the preparation method of the microwave-absorbing ceramic, aoxidized in the microwave-absorbing ceramic
Zn content is 7.0-11.5wt%.
Beneficial effect of the present invention：
First, ZnO is synthesized using wet chemistry method, product ZnO granular size, recrystallization temperature can be greatly lowered, obtain
ZnO/Al2O3ZnO in complex phase ceramic is evenly distributed, and is advantageous to improve the absorbing property of material.
2nd, the aluminium element of doping is sufficiently mixed uniformly in the liquid phase in the form of salting liquid with zinc oxide precursor, makes it
It can on an atomic scale realize and be uniformly distributed, so as to ensure the uniformity of product component.The minor-alloying element Al of doping enters ZnO
Lattice forms foreign atom, can improve ZnO carrier concentration, so as to increase electrical conductivity, strengthens dielectric loss, is advantageous to absorb
Electromagnetic wave.
3rd, each phase heat treatment temperature of the present invention is low, ensures stability and chemical compatibility between matrix and wave absorbing agent,
Be advantageous to simplify preparation technology, and energy consumption can also be reduced.
4th, zinc oxide and porous alumina ceramic the microwave-absorbing ceramic material with reference to made from structure under 300 DEG C of high temperature above
Still stable and good with matrix compatibility, absorbing property is stable at high temperature.
Brief description of the drawings
Fig. 1 is the microwave-absorbing ceramic fracture apperance stereoscan photograph prepared by embodiment 4.
Fig. 2 is complex dielectric permittivity figure of the microwave-absorbing ceramic in the range of normal temperature, 8.2-12.4GHz prepared by embodiment 3,4.
Fig. 3 is stickogram of the microwave-absorbing ceramic in the range of normal temperature, 8.2~12.4GHz prepared by embodiment 3,4.
Fig. 4 be microwave-absorbing ceramic prepared by embodiment 3,4 at 300 DEG C, the complex dielectric permittivity in the range of 8.2~12.4GHz
Figure.
Fig. 5 be microwave-absorbing ceramic prepared by embodiment 3,4 at 300 DEG C, the stickogram in the range of 8.2~12.4GHz.
Fig. 6 is the microwave-absorbing ceramic fracture apperance stereoscan photograph prepared by embodiment 5.
Embodiment
Fig. 1 is that ZnO/Al is prepared in embodiment 42O3Complex phase porous ceramics fracture apperance stereoscan photograph, can from figure
To see that ZnO particle is evenly distributed in porous alumina ceramic, ZnO particle particle diameter 200nm or so.
Fig. 2 is Al element dopings (embodiment 4) and the ZnO/Al undoped with (embodiment 3)2O3Complex phase porous ceramics is normal
Temperature, the complex dielectric permittivity in the range of 8.2~12.4GHz, method of testing is waveguide method, as a result illustrates that Al element dopings can be carried significantly
The real part of permittivity and imaginary part of high complex phase ceramic, 1% Al element dopings ZnO/Al2O3Complex phase ceramic has medium relative dielectric damage
Characteristic is consumed, loss tangent value is approximately 0.35.
Fig. 3 is Al element dopings (embodiment 4) and the ZnO/Al undoped with (embodiment 3)2O3Complex phase porous ceramics is normal
Temperature, the reflectance factor in the range of 8.2~12.4GHz, as a result shows Al element dopings ZnO/Al2O3Complex phase porous ceramics has excellent
Different absorbing property, reflectance factor reach minimum -25dB in 9.4GHz, it is meant that the electromagnetic wave energy more than 99% is inhaled
Receive.
ZnO/Al2O3 complex phase porous ceramics fracture apperance stereoscan photographs, corresponding Al is prepared in Fig. 6 embodiments 5
It is doped to Al in embodiment 4 corresponding to 2%, Fig. 1 and is doped to 1%.It is can be found that from the SEM photograph contrast of two groups of samples：With
The increase of Al element doping ratios, it is significantly reduced the size of ZnO particle.Further, research finds Al element dopings to ZnO
In lattice, because the difference of Al and Zn atomic radiuses generates crystal lattice stress, so as to inhibit growing up for ZnO crystal grain.Therefore with
The increase of Al element dopings ratio, ZnO crystallite dimensions reduce therewith.
The present invention is further detailed explanation for example below, wherein being selected from aluminum nitrate, alcamines with aluminium compound
Compound is selected from monoethanolamine, good solvent is selected from exemplified by ethylene glycol, but finds that aluminium compound is selected from alchlor, alcohol by experiment
Aminated compounds is selected from diethanol amine, good solvent can realize the object of the invention selected from isopropanol or ethylene glycol monomethyl ether, herein
Place does not list specifically in embodiment, but can not think that the present invention can not use these materials.
Embodiment 1
(1) using ethylene glycol as solvent, zinc acetate, monoethanolamine are added, by standing 24h after stirring at room temperature, is obtained
Zinc acetate colloidal sol.The molar concentration of zinc acetate in the solution is 0.1mol/L, and zinc acetate is 1 with monoethanolamine mol ratio:1.
(2) porous alumina ceramic is impregnated into vacuum impregnation or pressure impregnation 0.5h in the colloidal sol of step 1.
(3) precast body in step 2 is heat-treated 2h at 300 DEG C, obtains the complex phase infused ceramic of single-steeping.
(4) complex phase ceramic in step 3 is impregnated into the colloidal sol of step 1, be heat-treated according to step 3, circulated with this
15 times, obtain the complex phase ceramic that ZnO content is 7.3wt%.
(5) by precast body in step 4,600 DEG C of heat treatment 4h, protective atmosphere are argon gas or nitrogen under protective atmosphere, are flowed
It is 1 DEG C/min to measure as 25ml/min, heating rate, obtains and inhales wave mode ZnO/Al2O3Complex phase porous ceramics.
Embodiment 2
(1) using ethylene glycol as solvent, zinc acetate, monoethanolamine are added, by standing 24h after stirring at room temperature, is obtained
Zinc acetate colloidal sol.The molar concentration of zinc acetate in the solution is 0.2mol/L, and zinc acetate is 1 with monoethanolamine mol ratio:1.
(2) porous alumina ceramic is impregnated into vacuum impregnation or pressure impregnation 2h in the colloidal sol of step 1.
(3) precast body in step 2 is heat-treated 2h at 350 DEG C, obtains the complex phase infused ceramic of single-steeping.
(4) complex phase ceramic in step 3 is impregnated into the colloidal sol of step 1, be heat-treated according to step 3, circulated with this
12 times, obtain the complex phase ceramic that ZnO content is 8.7wt%.
(5) by precast body in step 4,650 DEG C of heat treatment 4h, protective atmosphere are argon gas or nitrogen under protective atmosphere, are flowed
It is 2 DEG C/min to measure as 50ml/min, heating rate, obtains and inhales wave mode ZnO/Al2O3Complex phase porous ceramics.
Embodiment 3
(1) using ethylene glycol as solvent, zinc acetate, monoethanolamine are added, by standing 36h after stirring at room temperature, is obtained
Zinc acetate colloidal sol.The molar concentration of zinc acetate in the solution is 0.5mol/L, and zinc acetate is 1 with monoethanolamine mol ratio:1.
(2) porous alumina ceramic is impregnated into vacuum impregnation or pressure impregnation 2h in the colloidal sol of step 1.
(3) precast body in step 2 is heat-treated 1.5h at 400 DEG C, obtains the complex phase infused ceramic of single-steeping.
(4) complex phase ceramic in step 3 is impregnated into the colloidal sol of step 1, be heat-treated according to step 3, circulated with this
10 times, obtain the complex phase ceramic that ZnO content is 11.2wt%.
(5) by precast body in step 4,700 DEG C of heat treatment 3h, protective atmosphere are argon gas or nitrogen under protective atmosphere, are flowed
It is 3 DEG C/min to measure as 100ml/min, heating rate, obtains and inhales wave mode ZnO/Al2O3Complex phase porous ceramics.
Embodiment 4
(1) using ethylene glycol as solvent, zinc acetate, aluminum nitrate, monoethanolamine are added, by standing after stirring at room temperature
36h, obtain zinc acetate colloidal sol.The molar concentration of zinc acetate in the solution is that 0.5mol/L, Al and Zn mol ratio are 0.01:1,
Zinc acetate is 1 with monoethanolamine mol ratio:1.
(2) porous alumina ceramic is impregnated into vacuum impregnation or pressure impregnation 2h in the colloidal sol of step 1.
(3) precast body in step 2 is heat-treated 1.5h at 400 DEG C, obtains the complex phase infused ceramic of single-steeping.
(4) complex phase ceramic in step 3 is impregnated into the colloidal sol of step 1, be heat-treated according to step 3, circulated with this
10 times, obtain the complex phase ceramic that ZnO content is 11.2wt%.
(5) by precast body in step 4,700 DEG C of heat treatment 3h, protective atmosphere are argon gas or nitrogen under protective atmosphere, are flowed
It is 3 DEG C/min to measure as 100ml/min, heating rate, obtains and inhales wave mode ZnO/Al2O3Complex phase porous ceramics.
Embodiment 5
(1) using ethylene glycol as solvent, zinc acetate, aluminum nitrate, monoethanolamine are added, by standing after stirring at room temperature
48h, obtain zinc acetate colloidal sol.The molar concentration of zinc acetate in the solution is that 0.8mol/L, Al and Zn mol ratio are 2%, second
Sour zinc is 1 with monoethanolamine mol ratio:1.
(2) porous alumina ceramic is impregnated into vacuum impregnation 0.5h combination pressures in the colloidal sol of step 1 and impregnates 0.5h.
(3) precast body in step 2 is heat-treated 1h at 450 DEG C, obtains the complex phase infused ceramic of single-steeping.
(4) complex phase ceramic in step 3 is impregnated into the colloidal sol of step 1, be heat-treated according to step 3,7 are circulated with this
It is secondary, obtain the complex phase ceramic that ZnO content is 9.6wt%.
(5) by precast body in step 4,750 DEG C of heat treatment 2h, protective atmosphere are argon gas or nitrogen under protective atmosphere, are flowed
It is 4 DEG C/min to measure as 100ml/min, heating rate, obtains and inhales wave mode ZnO/Al2O3Complex phase porous ceramics.
Embodiment 6
(1) using ethylene glycol as solvent, zinc acetate, monoethanolamine are added, by standing 48h after stirring at room temperature, is obtained
Zinc acetate colloidal sol.The molar concentration of zinc acetate in the solution is 1mol/L, and zinc acetate is 1 with monoethanolamine mol ratio:1.
(2) porous alumina ceramic is impregnated into vacuum impregnation 1h combination pressures in the colloidal sol of step 1 and impregnates 1h.
(3) precast body in step 2 is heat-treated 0.5h at 500 DEG C, obtains the complex phase infused ceramic of single-steeping.
(4) complex phase ceramic in step 3 is impregnated into the colloidal sol of step 1, be heat-treated according to step 3,5 are circulated with this
It is secondary, obtain the complex phase ceramic that ZnO content is 9.1wt%.
(5) by precast body in step 4,800 DEG C of heat treatment 2h, protective atmosphere are argon gas or nitrogen under protective atmosphere, are flowed
It is 5 DEG C/min to measure as 50ml/min, heating rate, obtains and inhales wave mode ZnO/Al2O3Complex phase porous ceramics.
It is as follows that the normal temperature dielectric constant of complex phase porous ceramics, the parameter of absorbing property is made in embodiment 1-6：
As can be seen from the table：Embodiment 1,2 and 6 is situated between because the mass fraction of ZnO in complex phase porous ceramics is smaller
Electric constant real part, imaginary part are all smaller, and absorbing property is poor；ZnO content in embodiment 5 is only second to embodiment 3 and 4, Al element
Doping ratio is 2%, and doping ratio is maximum, and the reflectance factor finally measured is -9.6dB.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those skilled in the art disclosed herein technical scope in, can without the change that creative work is expected or
Replace, should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be limited with claims
Fixed protection domain is defined.
Claims (10)
1. a kind of preparation method of microwave-absorbing ceramic, it is characterised in that including herein below：
(1) mixed liquor of zinc acetate, aluminium compound, alcamine compound and good solvent, zinc acetate rubbing in mixed liquor are taken
Your concentration is 0.1~1mol/L, and zinc acetate is 1 with alcamine compound mol ratio:1, Al and Zn mol ratio is 0-0.02:1,
Stood after stirring, obtain presoma；
(2) by porous alumina ceramic impregnation in the presoma, precast body is made, after heat treatment obtains dipping pottery
Porcelain；
(3) impregnation in presoma by the infused ceramic, is then heat-treated again；This step repeats, and is aoxidized
Zn content is 7.0-11.5wt% infused ceramic；
(4) heat up, be heat-treated under protective atmosphere, produce microwave-absorbing ceramic material.
2. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：In step (1), the system of the presoma
Preparation Method is：24-48h is stood after mixed liquor is stirred, obtains presoma.
3. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：The aluminium compound be selected from aluminum nitrate or
Alchlor.
4. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：The alcamine compound is selected from ethanol
Amine or diethanol amine.
5. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：The good solvent be selected from ethylene glycol,
Isopropanol or ethylene glycol monomethyl ether.
6. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：It is heat-treated in step (2) and step (3)
Temperature is 300-500 DEG C, a length of 0.5-2h during heat treatment.
7. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：The porous alumina ceramic porosity
For 28-35%.
8. the preparation method of microwave-absorbing ceramic according to claim 6, it is characterised in that：The porous alumina ceramic porosity
For 30%.
9. the preparation method of microwave-absorbing ceramic according to claim 1, it is characterised in that：Heat treatment temperature is in step (4)
600-800 DEG C, a length of 2-4h during heat treatment.
10. according to microwave-absorbing ceramic made from the preparation method of any microwave-absorbing ceramics of claim 1-9, it is characterised in that：Institute
It is 7.0-11.5wt% to state zinc oxide content in microwave-absorbing ceramic.
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| CN109650933A (en) * | 2019-01-28 | 2019-04-19 | 陕西科技大学 | A kind of porous C o3O4/Al2SiO5Low-density inhales wave mode complex phase ceramic and preparation method thereof |
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