CN116969760A - Ca-Sm-Al-Ti-based microwave dielectric ceramic material and preparation method thereof - Google Patents
Ca-Sm-Al-Ti-based microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 34
- 229910018575 Al—Ti Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 239000004576 sand Substances 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 7
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 7
- 235000006748 manganese carbonate Nutrition 0.000 claims abstract description 7
- 229940093474 manganese carbonate Drugs 0.000 claims abstract description 7
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 7
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001954 samarium oxide Inorganic materials 0.000 claims abstract description 7
- 229940075630 samarium oxide Drugs 0.000 claims abstract description 7
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- 239000007921 spray Substances 0.000 claims abstract description 7
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 239000011787 zinc oxide Substances 0.000 claims abstract description 7
- 238000003801 milling Methods 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 abstract description 12
- 229910052573 porcelain Inorganic materials 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000003989 dielectric material Substances 0.000 abstract description 2
- 238000005452 bending Methods 0.000 abstract 1
- 238000004891 communication Methods 0.000 description 9
- 238000005457 optimization Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The application provides a Ca-Sm-Al-Ti based microwave dielectric material and a preparation method thereof, wherein the material comprises the following raw materials in percentage by weight: 29 to 39 percent of calcium carbonate, 33 to 46 percent of samarium oxide, 13 to 20 percent of aluminum oxide, 3 to 10 percent of titanium dioxide, 0.5 to 1 percent of zinc oxide, 0.15 to 0.5 percent of lithium carbonate, 0.05 to 0.3 percent of zirconium dioxide, 0.1 to 0.5 percent of silicon dioxide and 0.08 to 0.20 percent of manganese carbonate. The Ca-Sm-Al-Ti based microwave porcelain material is prepared by the steps of proportioning, mixing, drying, presintering, ball milling, sand milling, spray granulation, blank pressing, sintering and the like, and has a dielectric constant of 25-29, qf of more than or equal to 60000GHz and a frequency temperature coefficient tau f (-40-130 ℃ C.). <.+ -. 3 ppm/. Degree.C. The material has uniform crystal structure and high ceramic bending strength, and is suitable for manufacturing various microwave components; meanwhile, all the ceramic materials adopt industrial electronic grade raw materials; the industrial mass production of the porcelain is realized through the fine control of the key process, andcompared with the similar foreign microwave materials, the cost advantage is obvious.
Description
Technical Field
The application relates to the field of electronic information functional materials, in particular to a Ca-Sm-Al-Ti-based microwave dielectric ceramic material and a preparation method thereof.
Background
The microwave dielectric ceramic material as one new kind of electronic functional material has high Qf value, low dielectric loss, high dielectric constant epsilonr and frequency temperature coefficient tau f Stable and the like, is a core basic material of novel microwave circuits and devices including a dielectric resonator, a filter, an oscillator, a duplexer, an antenna, a dielectric substrate and the like, and has wide application in modern microwave communication and satellite navigation systems and equipment. In recent years, as microwave technology equipment is rapidly developed to be miniaturized, integrated and low in power consumption, particularly to be used in large quantities and low in price, a large number of microwave dielectric ceramic materials suitable for various microwave frequency bands have been developed. Because of different regions and different use scenes, the environmental temperature spans are larger, the high-density integration and the heat dissipation capacity of a small space range are limited, and the microwave device is heated, the problem of the stability of the whole machine in a wide temperature range is solved, thereby providing higher requirements on the frequency temperature coefficient of the microwave dielectric ceramic material and the frequency temperature coefficient tau f <±3ppm/℃。
An ultra-low loss microwave dielectric ceramic with a dielectric constant of about 20 (er=18 to 22, qf >60000ghz,
τ f <5ppm/°c) has an important role in mobile data communications, satellite communications, and other microwave communications, and low-loss microwaves are now availableThe dielectric ceramics mainly comprise: 1) Ba (Mg) 1/3 Ta 2/3 )O 3 (εr＝25，Qf>250000GHz，τ f <5ppm/°c) based ceramic; 2) Ba (Zn) 1/3 Ta 2/3 )O 3 (εr＝29，Q＝15,000at 11GHz，τ f <5ppm/°c) based ceramic; 3) MgTiO 3 -CaTiO 3 (εr≈21，Q≈8000at 7GHz，andτ f About 0 ppm/. Degree.C.ceramic; 4) LaAlO 3 (εr＝23，Qf＝68000GHz，τ f = -44ppm/°c). These materials belong to the typical perovskite structure. But Ba (Mg) 1/ 3 Ta 2/3 )O 3 And Ba (Zn) 1/3 Ta 2/3 )O 3 Has the problems of high sintering temperature, harsh preparation conditions and expensive raw materials, and LaAlO 3 The sintering temperature is high and the temperature coefficient is higher, while MgTiO 3 -CaTiO 3 The problems of dielectric loss and large frequency temperature coefficient are solved, so that the search for a new system with excellent microwave dielectric property is an important subject. With K 2 NiF 4 Structural MRAlO 4 (m=sr, ca; r=la, Y, nd, sm) has good microwave dielectric properties, in addition, MRAlO 4 Microwave dielectric ceramics and Ba (Mg) 1/3 Ta 2/3 )O 3 ，Ba(Zn 1/3 Ta 2/3 )O 3 And Ba (Zn) 1/3 Nd 2/3 )O 3 Compared with the prior art, the alloy does not contain valuable raw materials such as Ta, nd and the like, and has obvious cost advantage, thereby attracting great attention.
Disclosure of Invention
The application aims to provide a microwave dielectric ceramic material with an ultralow frequency temperature coefficient in a wide temperature range and a preparation method thereof, so as to solve the problems of larger frequency temperature coefficient and poor performance reliability of the conventional microwave dielectric ceramic material with a dielectric constant of about 25. The Ca-Sm-Al-Ti based microwave dielectric material with high Qf value, ultralow frequency temperature coefficient and adjustable dielectric constant is suitable for manufacturing microwave communication components such as a dielectric filter, a dielectric resonator, a dielectric antenna and the like in the modern communication technology.
The technical scheme adopted by the application is as follows:
the Ca-Sm-Al-Ti based microwave dielectric ceramic material comprises the following raw materials in percentage by weight: 29 to 39 percent of calcium carbonate, 33 to 46 percent of samarium oxide, 13 to 20 percent of aluminum oxide, 3 to 10 percent of titanium dioxide, 0.5 to 1 percent of zinc oxide, 0.15 to 0.5 percent of lithium carbonate, 0.05 to 0.3 percent of zirconium dioxide, 0.1 to 0.5 percent of silicon dioxide and 0.08 to 0.20 percent of manganese carbonate.
As the optimal preferable formula, the raw materials comprise the following components in parts by weight: 36.32% of calcium carbonate, 42.76% of samarium oxide, 15.26% of aluminum oxide, 4.32% of titanium dioxide, 0.76% of zinc oxide, 0.25% of lithium carbonate, 0.15% of zirconium dioxide, 0.1% of silicon dioxide and 0.08% of manganese carbonate.
The application also provides a preparation method of the microsphere blocking remover, which comprises the following steps: and mixing the raw materials containing the surfactant, the solubilizer and the stabilizer with water according to the mass percentage to obtain the blocking remover.
The application also aims to provide a preparation method of the Ca-Sm-Al-Ti-based microwave dielectric ceramic material, which comprises the following steps:
step 1: proportioning materials
Weighing the raw materials according to a raw material formula, and mixing to obtain a mixture;
step 2: mixing material
Placing the mixture obtained in the step 1 into a ball mill for wet ball milling to obtain slurry raw materials;
step 3: drying
Drying the slurry raw material, granulating the dried raw material, and pressing the granulated raw material into a cylindrical material block;
step 4: presintering process
Placing the obtained material block in a high-temperature tunnel sintering furnace for presintering;
step 5: ball milling
Placing the pre-sintered powder into a ball mill for wet ball milling to obtain slurry;
step 6: sanding
Pumping the slurry into a stirring tank of a sand mill for sand milling;
step 7: spray granulation
Adding an adhesive into the sanded slurry, uniformly mixing, and then carrying out spray granulation;
step 8: pressing the powder into a green body;
step 9: sintering
Sintering the green body in a high-temperature box-type sintering furnace according to a set temperature curve to obtain the microwave dielectric ceramic material.
As further optimization of the technical scheme, in the step 2, the mixture, ball milling beads and deionized water are placed in a row ball mill according to the mass ratio of 1:2.0:2.0 for wet ball milling, and the ball milling time is 10 hours, so that slurry raw materials are obtained.
As a further optimization of the above technical solution, the specific operation of step 3: the slurry raw material is placed in a constant temperature oven at 150-200 ℃ for drying, and the dried raw material is granulated and then pressed into cylindrical material blocks with the diameter of 80mm and the thickness of 40 mm.
As a further optimization of the above technical scheme, the burn-in temperature in step 4 is 1280±10 ℃, and the burn-in time is 4 hours.
As a further optimization of the technical scheme, the ball milling time in the step 5 is 10 hours.
As a further optimization of the above technical solution, the sanding time in step 6 is 10h.
As a further optimization of the above technical solution, the specific operation of step 7: adding 10% polyvinyl alcohol solution into the sanded slurry, wherein the weight of the added adhesive is 4% -6% of the weight of the slurry, and spraying and granulating after uniformly mixing to obtain powder with the average particle size of 90-130 mu m.
As a further optimization of the above technical solution, the specific operation of step 9: sintering the green body in a high-temperature box-type sintering furnace according to a set temperature curve, wherein the glue discharging temperature zone is 400-600 ℃, the heat preservation is carried out for 3 hours, the high-temperature sintering temperature zone is 1370-1400 ℃, and the sintering time is 3-5 hours, so that the Ca-Sm-Al-Ti-based microwave dielectric ceramic material is obtained.
The application has the beneficial effects that:
1. the application uses 36.32% of calcium carbonate, 42.76% of samarium oxide, 15.26% of aluminum oxide, 4.32% of titanium dioxide and 0.7% of zinc oxide6 percent of lithium carbonate 0.25 percent, 0.15 percent of zirconium dioxide 0.1 percent of silicon dioxide 0.08 percent of manganese carbonate are used as raw materials, and the solid phase method is adopted for one-step synthesis, thereby solving the problem of poor material uniformity caused by mixing a plurality of synthetic materials, and solving the problem of larger frequency temperature coefficient under the wide temperature range (-40 ℃ to 130 ℃)>Soil at 10 ppm/DEG C) and the stability of the microwave device is poor under a complex temperature environment, and the prepared microwave dielectric ceramic material has good uniformity and meets the requirements of the microwave device. The powder is sintered at 1370-1400 ℃ to obtain the microwave dielectric ceramic device with microwave performance. The ceramic material can form a ceramic material with a room temperature dielectric constant of 25-29, a Qf value of more than or equal to 60000GHz and a temperature coefficient T by adjusting the proportion of raw material synthesis and additive materials f (-40～-130℃)：<The soil with the concentration of 3 ppm/DEG C can meet the requirement of high frequency stability of the current mobile communication and microwave communication, and is particularly suitable for being used in environments with large temperature difference.
2. The application uses Ca/Ti to cooperatively replace CaSmAlO 4 +CaTiO 3 The composite system is doped and modified, so that the microwave dielectric property of the composite system is improved, the dielectric constant of porcelain is improved, and the temperature coefficient of resonant frequency is improved; at the same time introduce ZnO, zrO 2 ，Li 2 CO 3 、MnCO 3 、SiO 2 The additive reduces the sintering temperature of the composite system and keeps a higher QF value, realizes the adjustability of the temperature coefficient of the resonant frequency of the microwave ceramic powder within a required range, and meets the performance requirements of components such as filters, resonators and the like for the microwave communication system.
3. The porcelain material is all made of industrial electronic grade raw materials; the industrial scale production of the porcelain is realized through the fine control of the sand milling granularity and the proper one-time presintering temperature process, and compared with the foreign similar microwave materials, the porcelain has obvious cost advantage.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of the present application.
FIG. 2 is an SEM image of a Ca-Sm-Al-Ti based microwave dielectric ceramic material.
FIG. 3 is a XRD analysis pattern of a sintered block at 1300 ℃.
Fig. 4 is a block XRD analysis pattern at 1280 ℃.
FIG. 5 is a XRD analysis pattern of a sintered block at 1250 ℃.
FIG. 6 is a graph showing the distribution of porcelain powder after sieving with a 80-270 mesh sieve.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. Thus, the following detailed description of the embodiments of the application, as presented in the figures, is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The application provides a Ca-Sm-Al-Ti-based microwave dielectric ceramic material, which comprises the following raw materials in percentage by weight: 29 to 39 percent of calcium carbonate, 33 to 46 percent of samarium oxide, 13 to 20 percent of aluminum oxide, 3 to 10 percent of titanium dioxide, 0.5 to 1 percent of zinc oxide, 0.15 to 0.5 percent of lithium carbonate, 0.05 to 0.3 percent of zirconium dioxide, 0.1 to 0.5 percent of silicon dioxide and 0.08 to 0.20 percent of manganese carbonate.
The mass percentages of the raw materials in each example are shown in Table 1
TABLE 1 chemical raw material proportions
SEM pictures of Ca-Sm-Al-Ti based microwave dielectric ceramic materials prepared according to formulation 2 of Table 1 are shown in FIG. 2. As can be seen from FIG. 2, the Ca-Sm-Al-Ti based microwave dielectric ceramic prepared in the embodiment has uniform grain size distribution, no obvious pores on the surface of the ceramic, and clear and compact grain boundaries.
The embodiment also provides a preparation method of the Ca-Sm-Al-Ti-based microwave dielectric ceramic material, which comprises the following steps:
step 1: proportioning materials
Weighing the raw materials according to a raw material formula, and mixing to obtain a mixture;
step 2: mixing material
Placing the mixture obtained in the step 1 into a ball mill for wet ball milling to obtain slurry raw materials;
step 3: drying
Drying the slurry raw material, granulating the dried raw material, and pressing the granulated raw material into a cylindrical material block;
step 4: presintering process
Placing the obtained material block in a high-temperature tunnel sintering furnace for presintering;
step 5: ball milling
Placing the pre-sintered powder into a ball mill for wet ball milling to obtain slurry;
step 6: sanding
Pumping the slurry into a stirring tank of a sand mill for sand milling;
step 7: spray granulation
Adding an adhesive into the sanded slurry, uniformly mixing, and then carrying out spray granulation;
step 8: pressing the powder into a green body;
step 9: sintering
Sintering the green body in a high-temperature box-type sintering furnace according to a set temperature curve to obtain the microwave dielectric ceramic material.
The following table shows the particle size comparisons of different ball water ratios:
TABLE 2 particle size comparison of different ball Water ratios
As can be seen from table 2 above, when the mix, ball-milled beads, deionized water were mixed according to 1:2.0:2.0, and the slurry granularity is 1.8-2.0 mu m when the ball milling time is 10 hours, and the granularity is proper, and the material is dilute and discharged quickly.
The specific operation of the step 3 is as follows: the slurry raw material is placed in a constant temperature oven at 150-200 ℃ for drying, and the dried raw material is granulated and then pressed into cylindrical material blocks with the diameter of 80mm and the thickness of 40 mm.
In the presintering process of the step 4, by analyzing the main crystal phases after the presintering of the baked blocks at different temperatures, it can be seen from the diffraction patterns (shown in fig. 3-5) that after the presintering at 1280 ℃, the main crystal phases are relatively close to the standard patterns, and each performance index is optimal.
The ball milling time in the step 5 is 10 hours.
In the step 6, the granularity of the slurry is mainly adjusted by adjusting the grinding time, and meanwhile, the comprehensive efficiency of mass production is considered to achieve the optimal production condition, the following table is a slurry granularity parameter table under different time, and the comprehensive optimal time is 10 hours.
The specific operation of the step 7 is as follows: adding 10% polyvinyl alcohol solution into the sanded slurry, wherein the weight of the added adhesive is 4% -6% of the weight of the slurry, uniformly mixing, and then spraying and granulating to obtain powder with the average particle size of about 115um, wherein the particle size distribution approximately accords with the normal distribution to be optimal, as shown in figure 6.
The specific operation of the step 8 is as follows: the powder is pressed into green bodies with the diameter of 25mm and the thickness of 13mm in a semi-automatic sample pressing machine.
The specific operation of the step 9: sintering the green body in a high-temperature box-type sintering furnace according to a set temperature curve, wherein the glue discharging temperature zone is 400-600 ℃, the heat preservation is carried out for 3 hours, the high-temperature sintering temperature zone is 1370-1400 ℃, and the sintering time is 3-5 hours, so that the Ca-Sm-Al-Ti-based microwave dielectric ceramic material is obtained.
Performance test: the performance test is carried out by using Agilent E5071C network analyzer and parallel plate method, and the test system comprises network analyzer, computer analysis software, test fixture, positive and negative temperature boxes, etc.
The chemical feed formulations and sample test data for the ten examples are given below, respectively in table 3.
Table 3 sample test data
The innovation of the application is that CaSmAlO is adopted 4 +CaTiO 3 Based on the composite system, by selecting proper raw material proportion and modified additive, the sintering temperature of the composite system is reduced, meanwhile, a higher QF value is maintained, and a near-zero resonance frequency temperature coefficient is maintained, so that the adjustability of the dielectric constant of the microwave ceramic powder is realized, and the high stability performance requirements of components such as filters, resonators and the like for the microwave communication system are met.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (10)
1. The Ca-Sm-Al-Ti based microwave dielectric ceramic material comprises the following raw materials in percentage by weight: 29 to 39 percent of calcium carbonate, 33 to 46 percent of samarium oxide, 13 to 20 percent of aluminum oxide, 3 to 10 percent of titanium dioxide, 0.5 to 1 percent of zinc oxide, 0.15 to 0.5 percent of lithium carbonate, 0.05 to 0.3 percent of zirconium dioxide, 0.1 to 0.5 percent of silicon dioxide and 0.08 to 0.20 percent of manganese carbonate.
2. The Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 1, wherein the raw materials comprise, in weight percent: 36.32% of calcium carbonate, 42.76% of samarium oxide, 15.26% of aluminum oxide, 4.32% of titanium dioxide, 0.76% of zinc oxide, 0.25% of lithium carbonate, 0.15% of zirconium dioxide, 0.1% of silicon dioxide and 0.08% of manganese carbonate.
3. The method for preparing the Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 1 or 2, which is characterized by comprising the following steps:
step 1: proportioning materials
Weighing the raw materials according to a raw material formula, and mixing to obtain a mixture;
step 2: mixing material
Placing the mixture obtained in the step 1 into a ball mill for wet ball milling to obtain slurry raw materials;
step 3: drying
Drying the slurry raw material, granulating the dried raw material, and pressing the granulated raw material into a cylindrical material block;
step 4: presintering process
Placing the obtained material block in a high-temperature tunnel sintering furnace for presintering;
step 5: ball milling
Placing the pre-sintered powder into a ball mill for wet ball milling to obtain slurry;
step 6: sanding
Pumping the slurry into a stirring tank of a sand mill for sand milling;
step 7: spray granulation
Adding an adhesive into the sanded slurry, uniformly mixing, and then carrying out spray granulation;
step 8: pressing the powder into a green body;
step 9: sintering
Sintering the green body in a high-temperature box-type sintering furnace according to a set temperature curve to obtain the microwave dielectric ceramic material.
4. The method for preparing the Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein in the step 2, the mixture, ball milling beads and deionized water are placed in a row ball mill according to the mass ratio of 1:2.0:2.0 for wet ball milling for 10 hours, so as to obtain slurry raw materials.
5. The method for preparing the Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein the specific operation of the step 3 is as follows: the slurry raw material is placed in a constant temperature oven at 150-200 ℃ for drying, and the dried raw material is granulated and then pressed into cylindrical material blocks with the diameter of 80mm and the thickness of 40 mm.
6. The method for preparing a Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein the pre-sintering temperature in the step 4 is 1250+/-10 ℃ and the pre-sintering time is 4 hours.
7. The method for preparing a Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein the ball milling time in the step 5 is 10h.
8. A method for preparing a Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein the sanding time of step 6 is 10 hours.
9. The method for preparing the Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein the specific operation of the step 7 is as follows: adding 10% polyvinyl alcohol solution into the sanded slurry, wherein the weight of the added adhesive is 4% -6% of the weight of the slurry, and spraying and granulating after uniformly mixing to obtain powder with the average particle size of 90-130 mu m.
10. The method for preparing the Ca-Sm-Al-Ti based microwave dielectric ceramic material according to claim 3, wherein the specific operation of the step 9 is as follows: sintering the green body in a high-temperature box-type sintering furnace according to a set temperature curve, wherein the glue discharging temperature zone is 400-600 ℃, the heat preservation is carried out for 3 hours, the high-temperature sintering temperature zone is 1370-1400 ℃, and the sintering time is 3-5 hours, so that the Ca-Sm-Al-Ti-based microwave dielectric ceramic material is obtained.
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