CN101723662A - Dielectric adjustable BST-MB two-phase compound microwave ceramic material and method for preparing same - Google Patents
Dielectric adjustable BST-MB two-phase compound microwave ceramic material and method for preparing same Download PDFInfo
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Abstract
The invention belongs to the technical field of electric materials and devices, in particular to a dielectric adjustable BST-MB two-phase compound microwave ceramic material and a method for preparing the same. The dielectric adjustable two-phase compound microwave ceramic material consists of BaxSr1-xTiO3 and Mg2B2O6. The dielectric adjustable BST-MB two-phase compound microwave ceramic material has the advantages of low sintering temperature and big change of a dielectric constant along with the change of external DC electric fields and is applicable to the two-phase compound microwave ceramic medium ferroelectric phase shifter material of a adjustable microwave device.
Description
Technical field
The invention belongs to electronic material and device technology field, be specifically related to adjustable BST-MB two-phase composite microwave ceramic material of a kind of dielectric and preparation method thereof.
Background technology
Ba
xSr
1-xTiO
3(strontium-barium titanate BST) is BaTiO
3And SrTiO
3Unlimited Solid solution, have excellent dielectric properties: specific inductivity is easy to adjust, low-dielectric loss, good ferroelectric, piezoelectricity, withstand voltage, insulation and tunable performance can be widely used in the little and capacious miniature capacitor of volume, ultra-large dynamic RAM, tuning microwave device, ferroelectric phase shifter etc.The strontium-barium titanate material is generally believed it is the most promising ferroelectric phase shift material, aspect microwave adjustable device (as phase shifter, wave filter, variable condenser and retarding line etc.) obtain increasingly extensive concern, especially aspect microwave phase shifter especially at present research focus.
1994, American National military field engineering lab material L.C.Sengupta of portion and u.s.a. military affairs research laboratory microwave and the W.C.Drach of photoelectricity portion, in the report of survey of " strontium-barium titanate (BST) the phase shifter material electrology characteristic " submitted to mil, propose, make phase shifter if the BST ferroelectric material can replace Ferrite Material, Phased Array Radar Antenna will face a huge revolution.But the BST stupalith with high-k is difficult to satisfy the impedance matching and the powerful requirement of itself and driving source inside, and it has bigger dielectric loss under microwave frequency band, and this has all limited its application in the microwave adjustable device field greatly.Therefore, how to prepare both had moderate specific inductivity, low dielectric loss, the material that has high dielectric adjustable again is technological difficulties.
As the adjustable dielectric materials of microwave, in order to obtain better application in microwave device, material should have the higher figure of merit (ratio of tunable performance and dielectric loss).Thereby adjustable dielectric materials should have following performance: under microwave frequency, on the one hand, specific inductivity is low, dielectric loss low (it is high that quality factor q is wanted); On the other hand, under the direct-current biasing electric field, it is big that the variation of specific inductivity is wanted, and promptly has higher tunable performance.
For solving above-mentioned technological difficulties, many investigators mainly form composite structure by add non-ferroelectric microwave dielectric material in strontium-barium titanate, reduce dielectric loss under specific inductivity and the microwave frequency band thereby reach, and make it can be used for microwave adjustable device.Sengupta etc. have carried out systematic research and have applied for related U.S. patent the compound of BST and non-ferroelectric material MgO, though the specific inductivity of this matrix material and loss have obtained reduction to a certain extent, but along with the increase of MgO content, the temperature dependent properties of its specific inductivity and dielectric tunable characteristic but sharply descend.Dong Xianlin etc. are at BST stupalith and Mg
2SiO
4-MgO has also done certain research work in compound aspect.But the sintering temperature by the material after these means modifications is generally all about 1400 ℃, and because the introducing of second phase, rate that dielectric is adjustable can worsen rapidly.These have all limited its application on ferroelectric phase shifter.
Dielectric material with adjustable and high Q value microwave dielectric material are compound, because it has kept the high modulation characteristic of dielectric material with adjustable, the high Q characteristic that can also have microwave material realizes the function leap of 1+1＞2, and becomes another approach of optimizing dielectric material with adjustable microwave property.
This seminar is in early days at Ba
1-xSr
xTiO
3-Mg
2TiO
4A few thing has been done in the composite ceramic material aspect, has obtained very big progress.Yet, Ba
1-xSr
xTiO
3With Mg with excellent microwave dielectric property
3B
2O
6(ε
r=7.0, Q.f=230900 f=11.8GHz) compound and Dielectric Properties is not seen relevant report as yet.
Summary of the invention
The purpose of this invention is to provide the adjustable Ba of a kind of dielectric
xSr
1-xTiO
3-Mg
3B
2O
6(BST-MB) two-phase composite microwave ceramic material and preparation method thereof.
Two-phase composite microwave ceramic material provided by the present invention comprises following component by mass percent:
Ba
xSr
1-xTiO
3(x＝0.3～0.8)????????10.0wt.％～90.0wt.％
Mg
3B
2O
6??????????????????????????10.0wt.％～90.0wt.％。
Preferably, described two-phase composite microwave ceramic material comprises following component by mass percent:
Ba
xSr
1-xTiO
3(x＝0.3～0.8)????????40.0wt.％～90.0wt.％
Mg
3B
2O
6??????????????????????????10.0wt.％～60.0wt.％。
Above-mentioned Ba
xSr
1-xTiO
3In, the x value is represented mol ratio, and the preferred value of x is 0.5.
The preparation method of two-phase composite microwave ceramic material of the present invention specifically comprises the steps:
1, adopt solid reaction process to prepare Ba
xSr
1-xTiO
3(x=0.3～0.8) obtains Ba after the grinding
xSr
1-xTiO
3(x=0.3～0.8) powder is specially:
Adopt traditional electronic ceramic powder preparation technology,, select BaTiO for use by solid reaction process
3Powder and SrTiO
3Powder is a main raw material, according to making compound after certain Ba/Sr molar ratio ingredient mixing, the compound for preparing is placed nylon ball grinder, add zirconia ball, added dehydrated alcohol or deionized water ball milling 20～24 hours, the compound of gained is put into crystallizing dish, in baking oven,, grind and promptly obtain composite powder, put into alumina crucible then with after 100 ℃ of oven dry, with process furnace it is heated, heating curve is: from room temperature, be warming up to 1100 ℃～1200 ℃ with the temperature rise rate of 3 ℃/min, be incubated 2～4 hours, with the process furnace cool to room temperature, obtain Ba after the grinding then
xSr
1-xTiO
3(x=0.3～0.8) powder;
2, adopt solid reaction process to prepare Mg
3B
2O
6, obtain Mg after the grinding
3B
2O
6Powder;
According to the synthetic Mg of following reaction equation
3B
2O
6Powder:
3MgO+2H
3BO
3＝Mg
3B
2O
6+3H
2O
Take by weighing MgO powder and H respectively according to the mole proportioning
3BO
3Powder makes compound after mixing, then compound is placed nylon ball grinder, add zirconia ball, add dehydrated alcohol or deionized water, ball milling 20～24 hours, the compound of gained is put into crystallizing dish, in baking oven,, grind and promptly obtain composite powder, put into alumina crucible then with after 100 ℃ of oven dry, with process furnace it is heated pre-burning, obtain monophasic Mg after the grinding
3B
2O
6Powder;
3, Ba
xSr
1-xTiO
3-Mg
3B
2O
6Compound:
Take by weighing compound according to following set of dispense ratio, add zirconia ball, add dehydrated alcohol or deionized water, ball milling 20～24 hours is put into crystallizing dish with the compound of gained, with after 100 ℃ of oven dry, grind in baking oven, and 200 mesh sieves obtains composite powder excessively;
Ba
1-xSr
xTiO
3(x＝0.3～0.8)???????90.0wt.％～10.0wt.％
Mg
3B
2O
6?????????????????????????10.0wt.％～90.0wt.％；
4, adopting mass percent is that 8～10% polyvinyl alcohol water solution (PVA) carries out granulation as binding agent to above-mentioned composite powder, under 10～100MPa pressure, is pressed into the ceramic green sheet of desired size size by forming mould;
5, the ceramic green sheet that makes in the step 4 through 550 ℃～600 ℃ row is sticking handle after, 1050 ℃～1100 ℃ insulations 2～4 hours down, can obtain described composite microwave ceramic material.
Preferably, in the described step 1, BaTiO
3And SrTiO
3The purity of powder is 99.90%.
Preferably, in the described step 2, H
3BO
3Molar weight excessive 3%.Since in the process of pre-burning, H
3BO
3Dehydration along with the rising of temperature, and is followed B about 600 ℃
2O
3Volatilization.
Above-mentioned term " molar weight excessive 3% " is meant H in blending process
3BO
3Actual molar quantity and the H that calculates according to reaction formula
3BO
3Molar weight compare excessive 3%.
Preferably, in the pre-burning process in the described step 2, the calcined temperature curve is: 30 ℃ of-600 ℃ of (2h)-1150 ℃ (insulation 4h)-cool to the furnace room temperature (5h); Wherein, the implication of above-mentioned calcined temperature curve is: at first with the compound behind the ball milling from room temperature, be warming up to 600 ℃ with the temperature rise rate of 3 ℃/min, 600 ℃ of insulations 2 hours; Temperature rise rate with 3 ℃/min was warming up to 1100 ℃ then, 1100 ℃ of insulations 4 hours; Cool to room temperature then with the furnace.
Preferably, in the described step 2, the purity of described MgO powder is 99.90%, described H
3BO
3The purity of powder is 99.5%.
Among the above-mentioned preparation method, step 1, in the mechanical milling process of step 2 and step 3, the mass ratio of zirconia ball and ball milling material is 1.2～1.5: 1; The mass ratio of dehydrated alcohol or deionized water and ball milling material is 1.5～3.0: 1; Wherein, the ball milling material described in the step 1 is meant BaTiO
3And SrTiO
3Compound, the ball milling material described in the step 2 is meant MgO and H
3BO
3Compound, the ball milling material described in the step 3 is meant Ba
xSr
1-xTiO
3-Mg
3B
2O
6The compound material of forming.
Preferably, the row in the described step 5 is sticking to be treated to: from room temperature, be warming up to a certain temperature (comprising 550 ℃ and 600 ℃) between 550～600 ℃ with the temperature rise rate of 1 ℃/min, be incubated 6 hours under this temperature condition, cool to room temperature then with the furnace.
Composite microwave ceramic material of the present invention has low-k (specific inductivity is 50～2500), high tunable characteristic (T=12.3%～23.9%), sintering temperature and low (1050 ℃～1100 ℃).Simultaneously, composite microwave ceramic material of the present invention can be used for two-phase composite microwave ceramic material of adjustable microwave device and preparation method thereof, also can provide certain experimental basis to specific inductivity and this contradiction of dielectric adjustable mutual restriction about the BST matrix material simultaneously.It is low that matrix material has sintering temperature, and specific inductivity changes greatly with applying direct current electric field, is suitable for the two-phase composite microwave medium ceramic ferroelectric phase shifter material of adjustable microwave device.
The present invention adopts traditional electronic ceramic technology, selects microwave dielectric material Mg for use
3B
2O
6To carry out two phase gradients compound with the strontium-barium titanate ferroelectric material of different B a/Sr component, and development obtains a kind of low-k that has, high tunable characteristic, sintering temperature and low, and can be used for the Ba of adjustable microwave device
1-xSr
xTiO
3-Mg
3B
2O
6Two-phase composite microwave ceramic material, it has following principal feature:
(1) sintering temperature and low is 1050 ℃～1100 ℃, and the introducing of second phase, and the adjustable rate of dielectric does not rapidly reduce, on the contrary with ferroelectric material BST compound after, its dielectric adjustable adjustability with pure BST in certain ratio range is suitable.
(2) pass through Ba
1-xSr
xTiO
3(x=0.3～0.8)-Mg
3B
2O
6The variation of two-phase plural components content, the specific inductivity of composite ceramic material can be adjustable continuously between 50～2500, can obtain the material system of specific inductivity seriation, widened the range of application of material;
(3) under the applying direct current electric field effect, described composite microwave ceramic material has higher dielectric tunable characteristic (〉=10%);
(4) this composite ceramic material is with Ba
1-xSr
xTiO
3(x=0.3～0.8) and Mg
3B
2O
6The two-phase form independently exists, and does not have the generation of other dephasign, has excellent dielectric properties;
(5) adopt traditional electronic ceramic technology, technology is simple, and cost is low, the side effect of material system environment-protecting asepsis, and excellent performance is applicable to the exploitation and the design of adjustable microwave device.
Description of drawings
Fig. 1, (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6The X-ray diffraction analysis collection of illustrative plates of two-phase composite microwave ceramic material.
Fig. 2, (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6The relation curve of two-phase composite microwave ceramic material specific inductivity and loss and temperature under f=10kHz.
Fig. 3, (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6The relation curve of two-phase composite microwave ceramic material specific inductivity and external dc field intensity under 10kHz.
Embodiment
Embodiment 1-5 prepares (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6Two-phase composite microwave ceramic material:
(1) according to Ba
0.5Sr
0.5TiO
3Stoichiometric ratio, take by weighing 70.038g BaTiO
3With 55.112g SrTiO
3Powder places nylon ball grinder, adds zirconia ball, adds dehydrated alcohol or deionized water, ball milling 24 hours, and discharging oven dry back obtains Ba 1200 ℃ of pre-burnings 4 hours after the grinding
0.5Sr
0.5TiO
3Powder is stand-by.
(2) take by weighing 30.225g MgO, 31.070g H respectively
3BO
3Excessive H with 0.932g
3BO
3Powder places nylon ball grinder, adds zirconia ball, adds dehydrated alcohol or deionized water, ball milling 24 hours, and discharging oven dry back obtains Mg 1150 ℃ of pre-burnings 4 hours after the grinding
3B
2O
6Powder is stand-by, and wherein the calcined temperature curve is: at first from room temperature, be warming up to 600 ℃ with the temperature rise rate of 3 ℃/min, 600 ℃ of insulations 2 hours; And then be warming up to 1150 ℃, and 1150 ℃ of insulations 4 hours with the temperature rise rate of 3 ℃/min; Cool to room temperature then with the furnace.
Take by weighing above-mentioned synthetic Ba respectively according to plural components proportioning in the table 1
0.5Sr
0.5TiO
3, Mg
3B
2O
6Stand-by powder:
Table 1. (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6The two-phase composite microwave ceramic material proportioning
| Prescription | ??SampleA??(x＝0.10) | ??SampleB??(x＝0.20) | ??SampleC??(x＝0.40) | ??SampleD??(x＝0.60) |
| ??Ba 0.5Sr 0.5TiO 3 | ??27.0g | ??24.0g | ??18.0g | ??12.0g |
| ??Mg 3B 2O 6 | ??3.0g | ??6.0g | ??12.0g | ??18.0g |
(3) compound of above-mentioned each prescription is put into nylon ball grinder, added zirconia ball and dehydrated alcohol ball milling 24 hours, discharging oven dry back powder is crossed 200 mesh sieves, according to traditional electronic ceramic technology, adopting mass percent is that 8% polyvinyl alcohol (PVA) carries out granulation as binding agent, under 15MPa pressure, dry method is pressed into diameter
Green sheet, (the sticking concrete steps of handling of row are: from room temperature through the sticking processing of 550 ℃ rows, temperature rise rate with 1 ℃/min is warming up to 550 ℃, be incubated 6 hours down at 550 ℃, cool to room temperature then with the furnace) after, sample is under air atmosphere, and sintering temperature is 1100 ℃, be incubated after 4 hours, obtain (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6The two-phase composite microwave ceramic sample.The ceramics sample that makes is carried out polishing both surfaces, quilt silver earlier, carry out analysis of thing phase composition and dielectric properties test behind the silver ink firing, its relevant dielectric properties see Table 2.
Table 2. (1-x) Ba
0.5Sr
0.5TiO
3-xMg
3B
2O
6The relevant dielectric properties of two-phase composite microwave ceramic material
| The composite microwave ceramic material dielectric properties | ??SampleA??(x＝0.10) | ??SampleB??(x＝0.20) | ??SampleC??(x＝0.40) | ??SampleD??(x＝0.60) |
| Curie temperature T C(℃)@10kHz | ??-32.2 | ??-31.7 | ??-26.4 | ??-31.8 |
| ??ε r(20 ℃ of) @10kHz of room temperature | ??558 | ??485 | ??280 | ??63 |
| Tan δ (20 ℃ of) @10kHz of room temperature | ??0.002 | ??0.002 | ??0.008 | ??0.004 |
| Dielectric adjustable K (30kV/cm, 20 ℃ of) @10kHz | ??21.9％ | ??23.1％ | ??23.9％ | ??12.3％ |
Embodiment Sample A-Sample D prepared (1-x) Ba that fills a prescription
0.5Sr
0.5TiO
3-xMg
3B
2O
6The X-ray diffraction analysis collection of illustrative plates of two-phase composite microwave ceramic material as shown in Figure 1, the result shows with Ba
0.5Sr
0.5TiO
3And Mg
3B
2O
6Pure two-phase form coexistence does not have other dephasigns to generate; Embodiment Sample A-Sample D prepared (1-x) Ba that fills a prescription
0.5Sr
0.5TiO
3-xMg
3B
2O
6The relation curve of the specific inductivity of two-phase composite microwave ceramic material and loss and temperature as shown in Figure 2, the result shows along with Mg
3B
2O
6The increase of content, Curie shifts at the peak high temperature and broadened, inhibition, and specific inductivity significantly reduces; Embodiment Sample A-Sample D prepared (1-x) Ba that fills a prescription
0.5Sr
0.5TiO
3-xMg
3B
2O
6The relation of the specific inductivity of two-phase composite microwave ceramic material and external dc field intensity as shown in Figure 3, test result shows along with Mg
3B
2O
6Mg is being added in the increase of content
3B
2O
6Be 40% o'clock, its dielectric adjustable still keeps T=23.9%, and specific inductivity is also significantly reduced simultaneously.
Embodiment 6 preparation Ba
0.3Sr
0.7TiO
3-Mg
3B
2O
6Two-phase composite microwave ceramic material:
(1) according to Ba
0.3Sr
0.7TiO
3Stoichiometric ratio, take by weighing 42.023g BaTiO
3With 77.157g SrTiO
3Powder places nylon ball grinder, add zirconia ball (mass ratio of zirconia ball and ball milling material is 1.2: 1) and dehydrated alcohol (mass ratio of dehydrated alcohol and ball milling material is 1.5: 1), ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 4 hours after the grinding
0.3Sr
0.7TiO
3Powder is stand-by.
(2) take by weighing 30.225g MgO, 31.070g H respectively
3BO
3Excessive H with 0.932g
3BO
3Powder places nylon ball grinder, add zirconia ball (mass ratio of zirconia ball and ball milling material is 1.2: 1) and dehydrated alcohol (mass ratio of dehydrated alcohol and ball milling material is 1.5: 1), ball milling 24 hours, discharging oven dry back obtains Mg 1150 ℃ of pre-burnings 4 hours after the grinding
3B
2O
6Powder is stand-by.
According to Ba
0.3Sr
0.7TiO
3And Mg
3B
2O
6Weight ratio be that 1: 9 batching takes by weighing above-mentioned synthetic Ba respectively
0.3Sr
0.7TiO
3, Mg
3B
2O
6Stand-by powder.
Above-mentioned compound is put into nylon ball grinder, added zirconia ball (mass ratio of zirconia ball and ball milling material is 1.2: 1) and dehydrated alcohol (mass ratio of dehydrated alcohol and ball milling material is 1.5: 1) ball milling 20 hours, discharging oven dry back powder is crossed 200 mesh sieves, according to traditional electronic ceramic technology, adopting mass percent is that 8% polyvinyl alcohol (PVA) carries out granulation as binding agent, under 10MPa pressure, dry method is pressed into diameter
Green sheet, (the sticking concrete steps of handling of row are: from room temperature through the sticking processing of 550 ℃ rows, temperature rise rate with 1 ℃/min is warming up to 580 ℃, be incubated 6 hours down at 580 ℃, cool to room temperature then with the furnace) after, sample is under air atmosphere, and sintering temperature is 1100 ℃, be incubated after 2 hours, obtain Ba
0.3Sr
0.7TiO
3-Mg
3B
2O
6The two-phase composite microwave ceramic sample.
(3) according to Ba
0.7Sr
0.3TiO
3Stoichiometric ratio, take by weighing 98.054g BaTiO
3With 33.067g SrTiO
3Powder places nylon ball grinder, add zirconia ball (mass ratio of zirconia ball and ball milling material is 1.5: 1) and deionized water (mass ratio of deionized water and ball milling material is 3.0: 1), ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 2 hours after the grinding
0.7Sr
0.3TiO
3Powder is stand-by.
(4) take by weighing 30.225g MgO, 31.070g H respectively
3BO
3Excessive H with 0.932g
3BO
3Powder places nylon ball grinder, adds zirconia ball, adds dehydrated alcohol or deionized water, ball milling 24 hours, and discharging oven dry back obtains Mg 1150 ℃ of pre-burnings 4 hours after the grinding
3B
2O
6Powder is stand-by.
According to Ba
0.7Sr
0.3TiO
3And Mg
3B
2O
6Weight ratio be that 9: 1 batchings take by weighing above-mentioned synthetic Ba respectively
0.3Sr
0.7TiO
3, Mg
3B
2O
6Stand-by powder.
Above-mentioned compound is put into nylon ball grinder, added zirconia ball (mass ratio of zirconia ball and ball milling material is 1.5: 1) and dehydrated alcohol (mass ratio of dehydrated alcohol and ball milling material is 3.0: 1) ball milling 24 hours, discharging oven dry back powder is crossed 200 mesh sieves, according to traditional electronic ceramic technology, adopting mass percent is that 10% polyvinyl alcohol (PVA) carries out granulation as binding agent, under 10MPa pressure, dry method is pressed into diameter
Green sheet, (the sticking concrete steps of handling of row are: from room temperature through the sticking processing of 600 ℃ rows, temperature rise rate with 1 ℃/min is warming up to 550 ℃, be incubated 6 hours down at 550 ℃, cool to room temperature then with the furnace) after, sample is under air atmosphere, and sintering temperature is 1050 ℃, be incubated after 2 hours, obtain Ba
0.7Sr
0.3TiO
3-Mg
3B
2O
6The two-phase composite microwave ceramic sample.
Claims (9)
1. two-phase composite microwave ceramic material that dielectric is adjustable, form by following component by mass percent:
Ba
xSr
1-xTiO
3，x＝0.3～0.8?????10.0wt.％～90.0wt.％
Mg
3B
2O
6???????????????????????10.0wt.％～90.0wt.％。
2. the adjustable two-phase composite microwave ceramic material of dielectric according to claim 1 is characterized in that the two-phase composite microwave ceramic material that described dielectric is adjustable is made up of following component by mass percent:
Ba
xSr
1-xTiO
3，x＝0.3～0.8?????40.0wt.％～90.0wt.％
Mg
3B
2O
6???????????????????????10.0wt.％～60.0wt.％。
3. the adjustable two-phase composite microwave ceramic material of arbitrary dielectric described in claim 1 or 2 is characterized in that described Ba
xSr
1-xTiO
3In, x is 0.5.
4. the preparation method of the adjustable two-phase composite microwave ceramic material of the arbitrary dielectric described in the claim 1-3 comprises the steps:
1) adopt solid reaction process to prepare Ba
xSr
1-xTiO
3Powder, x=0.3～0.8;
2) adopt solid reaction process to prepare Mg
3B
2O
6Powder;
3) take by weighing the Ba that makes in the step 1)
xSr
1-xTiO
3Powder and step 2) in the Mg that makes
3B
2O
6After powder mixes, put into nylon ball grinder, add zirconia ball simultaneously, add dehydrated alcohol or deionized water, ball milling 20～24 hours makes composite powder with the compound drying of gained and after grinding, wherein, and described Ba
xSr
1-xTiO
3Powder and Mg
3B
2O
6Powder carries out proportioning according to following mass percent:
Ba
xSr
1-xTiO
3，x＝0.3～0.8?????????10.0wt.％～90.0wt.％
Mg
3B
2O
6???????????????????????????10.0wt.％～90.0wt.％；
4) adopt binding agent that the composite powder that makes in the step 3) is carried out granulation, under 10～100MPa pressure, be pressed into the ceramic green sheet then;
5) after the ceramic green sheet that makes in the step 4) glued processing through row, insulation was 2～4 hours under 1050 ℃～1100 ℃, can obtain described composite microwave ceramic material.
5. the preparation method of the adjustable two-phase composite microwave ceramic material of the dielectric described in claim 4 is characterized in that described step 2) in, H
3BO
3Molar weight excessive 3%.
6. the preparation method of the adjustable two-phase composite microwave ceramic material of the dielectric described in claim 4 is characterized in that described step 2) in adopt solid reaction process to prepare Mg
3B
2O
6The concrete steps of powder are: take by weighing MgO powder and H respectively according to the mole proportioning
3BO
3Powder makes compound after mixing, then compound is placed nylon ball grinder, add zirconia ball, add dehydrated alcohol or deionized water, ball milling 20～24 hours is put into crystallizing dish with the compound of gained, in baking oven with after 100 ℃ of oven dry, grind and promptly obtain composite powder, obtain monophasic Mg after pre-burning and the grinding
3B
2O
6Powder.
7. the preparation method of the adjustable two-phase composite microwave ceramic material of the dielectric described in claim 6, it is characterized in that, the concrete steps of described pre-burning are: at first the compound behind the ball milling is put into alumina crucible, put into process furnace simultaneously, from room temperature, temperature rise rate with 3 ℃/min was warming up to 600 ℃, 600 ℃ of insulations 2 hours; Temperature rise rate with 3 ℃/min was warming up to 1150 ℃ then, 1150 ℃ of insulations 4 hours; Cool to room temperature then with the furnace.
8. as the preparation method of the adjustable two-phase composite microwave ceramic material of dielectric as described in the claim 4, it is characterized in that the binding agent in the described step 4) is that mass percent is 8～10% polyvinyl alcohol water solution.
9. as the preparation method of the adjustable two-phase composite microwave ceramic material of dielectric as described in the claim 4, it is characterized in that the sticking temperature of the row in the described step 5) is 550～600 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910199981A CN101723662A (en) | 2009-12-04 | 2009-12-04 | Dielectric adjustable BST-MB two-phase compound microwave ceramic material and method for preparing same |
Applications Claiming Priority (1)
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| CN103964841A (en) * | 2014-04-22 | 2014-08-06 | 华中科技大学 | Microwave tuning composite ceramic material and preparation method thereof |
| CN110423093A (en) * | 2019-09-03 | 2019-11-08 | 浙江大学 | Ultralow dielectric microwave dielectric material and preparation method thereof |
| CN111925190A (en) * | 2020-07-02 | 2020-11-13 | 杭州电子科技大学 | Mg3B2O6-CaTiO3Composite microwave dielectric ceramic material and preparation method thereof |
| CN113557582A (en) * | 2019-03-11 | 2021-10-26 | 康姆艾德公司 | Variable capacitor for radio frequency power applications |
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|---|---|---|---|---|
| CN103964841A (en) * | 2014-04-22 | 2014-08-06 | 华中科技大学 | Microwave tuning composite ceramic material and preparation method thereof |
| CN103964841B (en) * | 2014-04-22 | 2015-10-28 | 华中科技大学 | A kind of microwave-tuned composite ceramic material and preparation method thereof |
| CN113557582A (en) * | 2019-03-11 | 2021-10-26 | 康姆艾德公司 | Variable capacitor for radio frequency power applications |
| US11901160B2 (en) | 2019-03-11 | 2024-02-13 | Comet Ag | Variable capacitor for RF power applications |
| CN110423093A (en) * | 2019-09-03 | 2019-11-08 | 浙江大学 | Ultralow dielectric microwave dielectric material and preparation method thereof |
| CN110423093B (en) * | 2019-09-03 | 2020-10-16 | 浙江大学 | Microwave dielectric material with ultralow dielectric constant and preparation method thereof |
| CN111925190A (en) * | 2020-07-02 | 2020-11-13 | 杭州电子科技大学 | Mg3B2O6-CaTiO3Composite microwave dielectric ceramic material and preparation method thereof |
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