CN113979730A - Preparation method of dielectric ceramic material - Google Patents
Preparation method of dielectric ceramic material Download PDFInfo
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- CN113979730A CN113979730A CN202111445102.0A CN202111445102A CN113979730A CN 113979730 A CN113979730 A CN 113979730A CN 202111445102 A CN202111445102 A CN 202111445102A CN 113979730 A CN113979730 A CN 113979730A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 22
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 15
- 229920003023 plastic Polymers 0.000 claims description 14
- 239000004033 plastic Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012778 molding material Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims 2
- 238000004891 communication Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 17
- 239000007921 spray Substances 0.000 description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- -1 rare earth metal lanthanum sesquioxide Chemical class 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006880 cross-coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
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Abstract
The invention relates to the technical field of ceramic materials, and discloses a preparation method of a medium ceramic material. The dielectric ceramic material prepared by the method has lower porosity, higher quality factor and frequency temperature coefficient close to 0, and is suitable for the communication field, such as antenna, Monoblock, RFID, filter and the like.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a preparation method of a dielectric ceramic material.
Background
The dielectric ceramic material is a polycrystal formed by irregularly gathering fine crystal grains obtained by mixing, molding and sintering raw materials with necessary components and through a solid-phase reaction between powder particles and a sintering process. In recent years, dielectric ceramic materials are widely used in various fields such as electronic components or mechanical components, and with the rapid development of mobile communication, the demand of the dielectric ceramic materials is increasing, the low dielectric constant can reduce the cross coupling loss between the materials and the electrodes and improve the transmission rate of electric signals, the high quality factor is beneficial to improving the selectivity of the working frequency of the device, and the frequency temperature coefficient close to 0 is beneficial to improving the frequency temperature stability of the device. This puts higher demands on the dielectric ceramic material.
Disclosure of Invention
The invention aims to provide a preparation method of a dielectric ceramic material, which has a high quality factor and a frequency temperature coefficient close to 0.
In order to solve the problems, the invention provides the following scheme:
a preparation method of a dielectric ceramic material comprises the following steps:
s1: mixing 11.1-37.0% of lanthanum oxide, 4.0-11.9% of aluminum oxide, 14.0-47.0% of titanium dioxide, 13.0-34.2% of magnesium oxide and 6.0-9.5% of calcium carbonate according to mass fraction;
s2: adding deionized water to form a mixture;
s3: grinding the mixture into primary slurry by using a ball mill;
s4: filtering and dehydrating the primary slurry by using a filter press;
s5: drying the dehydrated primary slurry and crushing the dried primary slurry into powder;
s6: pre-sintering the powder;
s7: adding powder and deionized water into the ball mill for secondary ball milling to obtain secondary slurry;
s8: adding an adhesive into the secondary slurry, stirring and granulating to obtain powder particles;
s9: carrying out compression molding on the powder particles;
s10: heating and plastic removing are carried out on the formed material;
s11: the obtained molding material is sent to a sintering furnace for sintering.
The addition of the rare earth metal lanthanum sesquioxide not only reduces the porosity of the dielectric ceramic material, enables the structure to be more compact, but also effectively reduces the dielectric loss and improves the quality factor; in addition, the medium ceramic material is compounded by adopting a plurality of materials with different frequency temperature coefficients, so that the offset of positive and negative frequency temperature coefficient values is realized, the frequency temperature coefficient close to 0 is possessed, and a stable resonant frequency can be ensured, so that the medium ceramic material can stably work under the change of ambient temperature, can be suitable for a plurality of communication fields, such as antennas, Monoblock, RFID and filters, and has wide application prospect.
Preferably, the pre-sintering temperature of the powder is set to be 1000-1200 ℃, and the pre-sintering time is set to be 3-5 h.
Preferably, the pressure during the press molding is 1.6 to 2.2t/cm2。
Preferably, the temperature for heating and plastic removal is set to be 600-800 ℃ and kept for 60-90 min, and the temperature rise speed for heating and plastic removal is less than 0.5 ℃/min.
Preferably, the sintering temperature of the molding material is set to be 1320-1380 ℃, the sintering time is 2-4 h, the temperature rise speed before 1280 ℃ is less than 2.5 ℃/min, and the temperature rise speed after 1280 ℃ is less than 0.5 ℃/min.
Preferably, the particle size distribution of the primary slurry is in the range of 0.8 to 2.0 μm.
Preferably, the particle size distribution of the secondary slurry is within the range of 1.5-3 μm.
Compared with the prior art, the invention has the advantages that: the invention greatly improves the quality factor and the strength of the material while reducing the porosity of the dielectric ceramic material, thereby ensuring that the product is not easy to damage in the production process, indirectly improving the yield of the product and being more convenient for production. The dielectric constant of the dielectric ceramic prepared by the invention is about 28, the quality factor value is higher, and the frequency temperature coefficient is nearly 0.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention, in which:
FIG. 1 is a flow chart of the production of a powder material in a dielectric ceramic material according to the present invention;
FIG. 2 shows the performance test results of a powder sample in a dielectric ceramic material according to the present disclosure;
Detailed Description
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
The invention discloses a preparation method of a dielectric ceramic material, which comprises the following steps:
mixing 11.1-37.0% of lanthanum oxide, 4.0-11.9% of aluminum oxide, 14.0-47.0% of titanium dioxide, 13.0-34.2% of magnesium oxide and 6.0-9.5% of calcium carbonate by mass, adding 80-90% of deionized water by weight of raw materials, and grinding into slurry with the particle size of 0.8-2.0 microns by using a ball mill. Wherein, the purity of all raw materials is 99.5%, and the lining material of the ball mill is polyurethane.
And filtering and dehydrating the slurry by using a filter press, drying the filtered and dehydrated slurry, crushing the dried slurry into powder with the particle size of less than 0.5mm, and then presintering the powder at the presintering temperature of 1000-1200 ℃ for 3-5 h.
And performing secondary ball milling on the pre-sintered powder and deionized water with the weight being 50-80% of the weight of the raw materials by using a ball mill to obtain secondary slurry with the particle size being 1.5-3 mu m.
Adding adhesive into the secondary slurry, stirring, controlling the temperature of the slurry entering the spray tower, granulating, and making the powder into spherical and fluid powder particles with good particle ball precision and uniform particles. Wherein, the formula of the adhesive is as follows: 3-10% of polyvinyl alcohol and 90-97% of distilled water. The weight of the added adhesive is 13% of the weight of the raw materials, the inlet temperature is controlled to be 250-300 ℃, and the outlet temperature is controlled to be 90-120 ℃.
Then the powder obtained by spray granulation is molded by a die pressing process, the powder particles with spherical fluidity are made into a material with a required shape, and the pressure during molding is set to be 1.6-2.2 t/cm2And then heating the molded material to 600-800 ℃, and keeping the temperature for 60-90 min, wherein the heating speed is less than 0.5 ℃/min for plastic removal.
And finally, conveying the molding material subjected to plastic removal treatment to a sintering furnace for sintering, wherein the sintering temperature is set to be 1320-1380 ℃, the sintering time is 2-4 h, the heating rate is less than 2.5 ℃/min before 1280 ℃, and the heating rate is less than 0.5 ℃/min after 1280 ℃, so that the dielectric ceramic material can be obtained.
Example 1
In this example, 11.1% by weight of lanthanum oxide, 11.9% by weight of aluminum oxide, 47.0% by weight of titanium dioxide, 20.5% by weight of magnesium oxide, and 9.5% by weight of calcium carbonate were mixed with deionized water 80% by weight of the raw materials, and the mixture was subjected to primary ball milling, dehydration, drying, presintering at 1000 ℃ for 5 hours, and then deionized water 50% by weight of the raw materials was added to perform secondary ball milling, followed by spray granulation (inlet temperature 250 ℃ C., outlet temperature 90 ℃ C.), and then the pressure was set to 1.9t/cm2Performing compression molding, heating at a temperature rise rate of less than 0.5 deg.C/min, maintaining at 600 deg.C for 90min, heating for plastic removal, and finally sintering at 1300 deg.C for 4h, wherein the temperature rise rate is less than 2.5 deg.C/min before 1280 deg.C, and less than 0.5 deg.C/min after 1280 deg.C.
Example 2
In the embodiment, 24.3 percent of lanthanum oxide, 9.0 percent of aluminum oxide, 23.0 percent of titanium dioxide, 34.2 percent of magnesium oxide and 9.5 percent of calcium carbonate by mass are mixed with deionized water which accounts for 90 percent of the weight of the raw materials, the mixture is subjected to primary ball milling, dehydration, drying and presintering for 3 hours at 1200 ℃, then deionized water which accounts for 80 percent of the weight of the raw materials is added for secondary ball milling, and then spray granulation is carried out (the inlet temperature is 300 ℃ and the outlet temperature is 120 ℃), and then the pressure is set to be 2.2t/cm2Performing compression molding, heating at a temperature rise rate of less than 0.5 deg.C/min, maintaining at 800 deg.C for 60min, heating for plastic removal, and finally sintering at 1380 deg.C for 2h, wherein the temperature rise rate is less than 2.5 deg.C/min before 1280 deg.C, and is less than 0.5 deg.C/min after 1280 deg.C.
Example 3
In this example, 33.0% by mass of lanthanum oxide, 4.0% by mass of aluminum oxide, 42.0% by mass of titanium dioxide, 13.0% by mass of magnesium oxide, and 8.0% by mass of calcium carbonate were mixed with deionized water 85% by weight of the raw materials, and the mixture was subjected to primary ball milling, dehydration, drying, presintering at 1100 ℃ for 4 hours, and then deionized water 60% by weight of the raw materials was added to perform secondary ball milling, followed by spray granulation (inlet temperature 270 ℃ C., outlet temperature 100 ℃ C.), and then the pressure was set to 2.0t/cm2Performing compression molding, heating at a temperature rise rate of less than 0.5 ℃/min, keeping at 700 ℃ for 75min, heating for plastic removal, finally sintering at 1340 ℃ for 3h, wherein the temperature rise rate is less than 2.5 ℃/min before 1280 ℃, and is less than 0.5 ℃/min after 1280 ℃.
Example 4
In this example, lanthanum oxide 37.0 wt%, aluminum oxide 10.0 wt%, titanium dioxide 14.0 wt%, magnesium oxide 33.0 wt%, and calcium carbonate 6.0 wt% were mixed with deionized water 80 wt% of the raw materials, and were subjected to primary ball milling, wherein the primary slurry particle size was about 1.2 μm; dehydrating, drying, presintering at 1180 ℃ for 4 hours, adding deionized water accounting for 70% of the weight of the raw materials, and carrying out secondary ball milling to obtain secondary slurry with the particle size of about 1.6 microns; adding 9% polyvinyl alcohol binder, stirring, spray granulating (inlet temperature of 280 deg.C, outlet temperature of 110 deg.C), and setting pressure to 1.8t/cm2Performing compression molding, heating at a temperature rise rate of less than 0.5 deg.C/min, maintaining at 700 deg.C for 75min, heating for plastic removal, and finally sintering at 1350 deg.C for 3h, wherein the temperature rise rate is less than 2.5 deg.C/min before 1280 deg.C, and less than 0.5 deg.C/min after 1280 deg.C. The dielectric ceramic material prepared in this example has a dielectric constant of 28.24, a quality constant of 72169, and a temperature coefficient of frequency of 2.2 ppm/deg.C.
Example 5
In the embodiment, 37.0% by mass of lanthanum oxide, 10.0% by mass of aluminum oxide, 14.0% by mass of titanium dioxide, 33.0% by mass of magnesium oxide, 6.0% by mass of calcium carbonate and deionized water accounting for 85% of the weight of the raw materials are mixed and subjected to primary ball milling, and the particle size of primary slurry is about 1.2 μm; dehydrating, drying, presintering at 1180 ℃ for 4 hours, adding deionized water accounting for 70% of the weight of the raw materials, and carrying out secondary ball milling to obtain secondary slurry with the particle size of about 1.6 microns; adding 9% polyvinyl alcohol adhesive, stirring, and spray granulating (inlet temperature 2)60 ℃ and an outlet temperature of 110 ℃ and subsequently a pressure of 1.8t/cm2Performing compression molding, heating at a temperature rise rate of less than 0.5 ℃/min, keeping at 700 ℃ for 75min, performing heating plastic removal, and finally sintering at 1320 ℃ for 4h, wherein the temperature rise rate is less than 2.5 ℃/min before 1280 ℃, and is less than 0.5 ℃/min after 1280 ℃. The dielectric ceramic material prepared in this example has a dielectric constant of 27.84, a quality constant of 56284, and a temperature coefficient of frequency of 8.6 ppm/deg.C.
Example 6
In the embodiment, 37.0% by mass of lanthanum oxide, 10.0% by mass of aluminum oxide, 14.0% by mass of titanium dioxide, 33.0% by mass of magnesium oxide, 6.0% by mass of calcium carbonate and deionized water accounting for 85% of the weight of the raw materials are mixed and subjected to primary ball milling, and the particle size of primary slurry is about 1.2 μm; dehydrating, drying, presintering at 1180 ℃ for 4 hours, adding deionized water accounting for 70% of the weight of the raw materials, and carrying out secondary ball milling to obtain secondary slurry with the particle size of about 1.6 microns; adding 9% polyvinyl alcohol binder, stirring, spray granulating (inlet temperature 270 deg.C, outlet temperature 105 deg.C), and setting pressure to 1.8t/cm2Performing compression molding, heating at a temperature rise rate of less than 0.5 deg.C/min, maintaining at 600 deg.C for 60min, heating for plastic removal, and finally sintering at 1380 deg.C for 4h, wherein the temperature rise rate is less than 2.5 deg.C/min before 1280 deg.C, and is less than 0.5 deg.C/min after 1280 deg.C. The dielectric ceramic material prepared in this example has a dielectric constant of 28.18, a quality constant of 68299, and a temperature coefficient of frequency of 5.9 ppm/DEG C.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or any other related technical fields, are included in the scope of the present invention.
Claims (7)
1. The preparation method of the dielectric ceramic material is characterized by comprising the following steps of:
s1: mixing 11.1-37.0% of lanthanum oxide, 4.0-11.9% of aluminum oxide, 14.0-47.0% of titanium dioxide, 13.0-34.2% of magnesium oxide and 6.0-9.5% of calcium carbonate according to mass fraction;
s2: adding deionized water to form a mixture;
s3: grinding the mixture into primary slurry by using a ball mill;
s4: filtering and dehydrating the primary slurry by using a filter press;
s5: drying the dehydrated primary slurry and crushing the dried primary slurry into powder;
s6: pre-sintering the powder;
s7: adding the powder and the deionized water into the ball mill for secondary ball milling to obtain secondary slurry;
s8: adding an adhesive into the secondary slurry, stirring and granulating to obtain powder particles;
s9: carrying out compression molding on the powder particles;
s10: heating and plastic removing are carried out on the formed material;
s11: the obtained molding material is sent to a sintering furnace for sintering.
2. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein the pre-sintering temperature of the powder is set to 1000-1200 ℃, and the pre-sintering time of the powder is set to 3-5 h.
3. A preparation method according to claim 1, wherein the pressure for molding the powder particles is set to 1.6-2.2 t/cm2。
4. The preparation method of the dielectric ceramic material as claimed in claim 1, wherein the temperature of heating and plastic removal is set to be 600-800 ℃ and kept for 60-90 min, and the temperature rise speed of heating and plastic removal is less than 0.5 ℃/min.
5. The method for preparing a dielectric ceramic material according to claim 1, wherein the sintering temperature of the molding material is set to 1320-1380 ℃, the sintering time is set to 2-4 h, the temperature rising speed before 1280 ℃ is less than 2.5 ℃/min, and the temperature rising speed after 1280 ℃ is less than 0.5 ℃/min.
6. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein the primary slurry has a particle size distribution within a range of 0.8 to 2.0 μm.
7. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein the particle size distribution of the secondary slurry is in the range of 1.5 to 3 μm.
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| CN111233462A (en) * | 2020-03-21 | 2020-06-05 | 东莞市钧鹏电子科技有限公司 | Medium microwave dielectric ceramic powder and preparation method thereof |
| CN111517791A (en) * | 2020-04-30 | 2020-08-11 | 福鼎市溥昱电子科技有限公司 | Low-temperature sintered medium-dielectric-constant microwave dielectric ceramic material and preparation method thereof |
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| US5147835A (en) * | 1991-03-05 | 1992-09-15 | Motorola, Inc. | Composite titanate aluminate dielectric material |
| JP2012184122A (en) * | 2011-03-03 | 2012-09-27 | Kyocera Corp | Dielectric ceramic, and dielectric filter having the same |
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