CN117142849A - Method for growing zinc-magnesium-titanium microwave ceramics based on skeleton effect - Google Patents
Method for growing zinc-magnesium-titanium microwave ceramics based on skeleton effect Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- YDXYFUGPRPJJJY-UHFFFAOYSA-N [Zn].[Ti].[Mg] Chemical compound [Zn].[Ti].[Mg] YDXYFUGPRPJJJY-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000000694 effects Effects 0.000 title claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000011777 magnesium Substances 0.000 claims abstract description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011701 zinc Substances 0.000 claims abstract description 18
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 45
- 238000000498 ball milling Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 239000002002 slurry 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 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000004484 Briquette Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000005476 size effect Effects 0.000 abstract description 4
- 239000011787 zinc oxide Substances 0.000 abstract description 4
- 239000000945 filler Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 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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- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
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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 invention belongs to the field of microwave dielectric ceramic materials, and particularly provides a method for growing zinc-magnesium-titanium microwave ceramic based on a skeleton effect, so that the prepared zinc-magnesium-titanium microwave dielectric ceramic material has low dielectric constant and low dielectric loss, and is suitable for manufacturing ceramic substrates with excellent performance. The invention adopts Zn 0.7 Mg 0.3 TiO 3 The system is characterized in that from the original particle size of raw materials, micron-sized titanium dioxide raw materials are used as a main framework, nano-sized zinc oxide and magnesium oxide raw materials are used as sintering fillers, and a cementing structure similar to concrete is formed, so that the sintering characteristic can be greatly improved, bubbles are avoided, and the mechanical strength of ceramic is enhanced; finally, the invention utilizes the skeleton effect (particle size effect) to improve Zn 0.7 Mg 0.3 TiO 3 The sinterability of the microwave dielectric ceramic gave a dielectric constant of 21.714, a Q×f= 48486.6 and a temperature stability factor of the resonant frequency of-46.3 ppThe microwave dielectric ceramic material with m/DEG C is expected to be used for manufacturing ceramic substrates.
Description
Technical Field
The invention belongs to the field of microwave dielectric ceramic materials, and provides a method for growing zinc-magnesium-titanium microwave ceramic based on a skeleton effect.
Background
Zn 0.7 Mg 0.3 TiO 3 Materials are commonly used for electronic components such as dielectric substrates and dielectric antennas in 5G communication circuits, and microwave frequency devices in filters and resonators. As a novel electronic material, the microwave dielectric ceramic has the characteristics of excellent performance, high reliability, small volume and the like; their abundant physicochemical properties depend on many factors such as phase composition, sintering temperature and synthesis method, and many scholars have made extensive studies on these aspects; however, the effect of various particle size materials on their physicochemical properties is unknown. Therefore, the research of modifying the zinc-magnesium-titanium microwave ceramic by controlling the particle size becomes the focus of the research of the invention.
In general, the finer the powder particles, the tighter the contact between them, the shorter the sintering chamber diffusion path, and the greater the sintering driving force-surface energy; however, the rapid growth of grains of the ultra-fine powder particles during high temperature sintering may cause abnormal growth, and may adsorb impurities due to the relatively high surface activity. Currently, zn synthesized by conventional solid phase method 0.7 Mg 0.3 TiO 3 The microwave dielectric ceramic material has high dielectric loss and high temperature coefficient of vibration cavity frequency; in order to improve the sinterability, the particle size of the raw materials such as zinc oxide, magnesium oxide and titanium dioxide is controlled, so that the raw materials have more excellent performance by utilizing the particle size effect of the materials.
Disclosure of Invention
The invention aims to provide a method for growing zinc-magnesium-titanium microwave ceramics based on a skeleton effect, so that the prepared zinc-magnesium-titanium microwave dielectric ceramic material has low dielectric constant and low dielectric loss, and is suitable for manufacturing ceramic substrates with excellent performances. The invention adoptsWith Zn 0.7 Mg 0.3 TiO 3 The system is characterized in that from the original particle size of raw materials, micron-sized titanium dioxide raw materials are used as a main framework, nano-sized zinc oxide and magnesium oxide raw materials are used as sintering fillers, and a cementing structure similar to concrete is formed, so that the sintering characteristic can be greatly improved, bubbles are avoided, and the mechanical strength of ceramic is enhanced; finally, the invention utilizes the skeleton effect (particle size effect) to improve Zn 0.7 Mg 0.3 TiO 3 The sinterability of the microwave dielectric ceramic gives a microwave dielectric ceramic material having a dielectric constant of 21.714, Q×f= 48486.6 and a temperature stability factor of resonance frequency of-46.3 ppm/. Degree.C, and is expected to be used for manufacturing a ceramic substrate.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the method for growing the zinc-magnesium-titanium microwave ceramic based on the skeleton effect is characterized by comprising the following steps of:
a. zinc oxide powder, magnesia powder and titanium dioxide powder are used as raw materials, and the raw materials are mixed according to Zn 0.7 Mg 0.3 TiO 3 The components are respectively weighed and mixed; wherein each raw material consists of two kinds of powder with the grain diameter of 25-50wt% of micron-sized (grain diameter) powder and 50-75wt% of nano-sized (grain diameter) powder respectively;
b. performing primary ball milling on the mixed raw materials, and drying and grinding the slurry after ball milling to obtain precursor powder;
c. calcining the precursor powder for 2-4 hours at 850-950 ℃ to obtain a presintered material;
d. performing secondary ball milling on the presintered material, and drying and grinding the slurry after ball milling to obtain Zn 0.7 Mg 0.3 TiO 3 Powder;
e. zn is added 0.7 Mg 0.3 TiO 3 Granulating the powder by using a polyvinyl alcohol adhesive, sieving, and briquetting to obtain a blank;
f. sintering the blank for 4-6 hours at 1150-1200 ℃ to obtain the zinc-magnesium-titanium microwave ceramic material.
Further, in the step a, the ratio of the micro-sized powder to the nano-sized powder may be the same or different for the three raw materials.
Further, in the step b and the step d, the same wet ball milling is adopted for both the primary ball milling and the secondary ball milling, the wet ball milling is carried out in a planetary ball mill, deionized water and absolute ethyl alcohol are used as solvents, agate beads are used as ball milling media, the mass ratio of raw materials to the solvents is 1:1.5, the volume ratio of the deionized water to the absolute ethyl alcohol in the solvents is 1:1, and the ball milling time is 12 hours.
Further, in the step b and the step d, the drying temperature was 85℃and the drying time was 24 hours.
Further, in step e, the amount of binder is 10-15ml; the sieving process is as follows: sequentially sieving with 40 mesh and 100 mesh, and collecting particles between 40 mesh and 100 mesh; the pressure of the briquette forming is 15-20Kg/cm 2 The time is 2-3 minutes, and the mixture is pressed into a cylindrical blank body.
Based on the technical scheme, the invention has the beneficial effects that:
the invention provides a method for growing zinc-magnesium-titanium microwave ceramics based on skeleton effect, which adopts a solid phase method to prepare Zn through proportioning, primary ball milling, presintering, secondary ball milling, granulating and high-temperature sintering 0.7 Mg 0.3 TiO 3 Microwave dielectric ceramics; on the basis of the solid phase method, the invention prepares Zn 0.7 Mg 0.3 TiO 3 Starting from the particle size of the raw materials of the system, the particle sizes of the zinc oxide powder, the magnesium oxide powder and the titanium dioxide powder are controlled, and the skeleton effect (particle size effect) is utilized to obviously improve Zn 0.7 Mg 0.3 TiO 3 The sinterability of the microwave dielectric ceramic; the method comprises the following steps: the nano-scale titanium dioxide raw material is used as a main framework (25-50 wt%), the nano-scale zinc oxide and magnesium oxide raw material are used as sintering filler (50-75 wt%), and a cementing structure similar to concrete is formed, so that the structure can greatly improve the sintering characteristic, avoid the generation of bubbles and enhance the mechanical strength of ceramics; finally, the invention obtains the microwave dielectric ceramic material with the dielectric constant of 21.714, Q multiplied by f= 48486.6 and the temperature stability coefficient of the resonant frequency of-46.3 ppm/DEG C, which is expected to be used for manufacturing the performanceAn excellent ceramic substrate; and the microwave dielectric ceramic material prepared by the method has stable performance and good consistency, and is beneficial to realizing the industrial production of ceramic substrates.
Drawings
FIG. 1 is an X-ray diffraction pattern of a Zn-Mg-Ti based microwave dielectric ceramic in example 2 of the present invention.
FIG. 2 is an SEM image of a Zn-Mg-Ti-based microwave dielectric ceramic according to example 2 of the invention.
FIG. 3 is a graph showing dielectric properties of Zn-Mg-Ti based microwave dielectric ceramics in example 1, example 2 and comparative example according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The embodiment provides a method for growing zinc-magnesium-titanium-based microwave dielectric ceramic based on a skeleton effect, wherein the chemical expression of the zinc-magnesium-titanium-based microwave dielectric ceramic is as follows: zn (zinc) 0.7 Mg 0.3 TiO 3 The method specifically comprises the following steps:
a. zinc oxide powder, magnesia powder and titanium dioxide powder are used as raw materials, and the raw materials are mixed according to Zn 0.7 Mg 0.3 TiO 3 The components are respectively weighed and mixed with zinc oxide powder, magnesium oxide powder and titanium dioxide powder; wherein each raw material consists of two kinds of powder with particle diameters, namely 50wt% of micron-sized (particle diameter) powder and 50wt% of nano-sized (particle diameter) powder;
b. putting the mixed raw materials into a planetary ball mill, and performing wet ball milling by taking deionized water and absolute ethyl alcohol as solvents and agate beads as ball milling media, wherein the mass ratio of the raw materials to the solvents is 1:1.5, the volume ratio of the deionized water to the absolute ethyl alcohol in the solvents is 1:1, and the ball milling time is 12 hours; drying the obtained slurry in an oven at 85 ℃ after ball milling is finished, and grinding to obtain precursor powder;
c. calcining the precursor powder for 2 hours at 850 ℃ to obtain a presintered material;
d、b, performing secondary ball milling on the presintered material, wherein the secondary ball milling adopts the same wet ball milling in the step b; after ball milling, drying the obtained slurry in an oven at 85 ℃ and grinding to obtain Zn 0.7 Mg 0.3 TiO 3 Powder;
e. zn is added 0.7 Mg 0.3 TiO 3 Granulating and sieving the powder by using a polyvinyl alcohol (PVA, 10%) adhesive, wherein the dosage of the adhesive is 12ml, and the sieving process is as follows: sequentially sieving with 40 mesh and 100 mesh, and collecting particles between 40 mesh and 100 mesh; then the obtained granules are subjected to 15Kg/cm 2 Briquetting is carried out under the pressure of (2) for 2 minutes, and a cylindrical blank body (phi multiplied by h:12mm multiplied by 6 mm) is obtained by pressing;
f. sintering the blank for 4 hours at 1150 ℃ to obtain the zinc-magnesium-titanium-based microwave dielectric ceramic material.
The zinc-magnesium-titanium-based microwave dielectric ceramic material prepared in the embodiment is tested, the dielectric constant is 22.154, Q multiplied by f= 31017.6, and the temperature stability coefficient of the resonant frequency is-38.8 ppm/DEG C.
Example 2
The embodiment provides a method for growing zinc-magnesium-titanium-based microwave dielectric ceramic based on a skeleton effect, wherein the chemical expression of the zinc-magnesium-titanium-based microwave dielectric ceramic is as follows: zn (zinc) 0.7 Mg 0.3 TiO 3 The only difference from example 1 is that: in step a, each raw material is composed of two kinds of powder having particle diameters, namely 25wt% of micron-sized (particle diameter) powder and 75wt% of nano-sized (particle diameter) powder.
The zinc-magnesium-titanium-based microwave dielectric ceramic material prepared in the embodiment is tested, wherein an X-ray diffraction spectrum is shown in figure 1, and as can be seen from the figure, the microwave dielectric ceramic material Zn 0.7 Mg 0.3 TiO 3 Has good crystallinity; SEM images are shown in fig. 2, from which it can be seen that the microstructure of the sample shows dense and well-packed grains; in addition, the dielectric constant of the Zn-Mg-Ti-based microwave dielectric ceramic material is 21.714, Q×f= 48486.6, and the temperature stability coefficient of the resonance frequency is-46.3 ppm/. Degree.C.
Comparative example
The comparative example provides a method for growing zinc-magnesium-titanium-based microwave dielectric ceramics based on a skeleton effect, wherein the chemical expression of the zinc-magnesium-titanium-based microwave dielectric ceramics is as follows: zn (zinc) 0.7 Mg 0.3 TiO 3 The only difference from example 1 is that: in step a, each raw material is composed of two kinds of powder having particle diameters, namely 75wt% of micron-sized (particle diameter) powder and 25wt% of nano-sized (particle diameter) powder.
Comparing the dielectric properties of the above-mentioned examples 1, 2 with those of the comparative examples, the results are shown in FIG. 3, and it is seen from the graph that examples 1, 2 have better dielectric properties because a cement structure similar to concrete is formed by controlling the particle sizes of the raw materials of zinc oxide powder, magnesium oxide powder and titanium dioxide powder, which can greatly improve sintering characteristics and avoid the generation of bubbles in the material.
While the invention has been described in terms of specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the equivalent or similar purpose, unless expressly stated otherwise; all of the features disclosed, or all of the steps in a method or process, except for mutually exclusive features and/or steps, may be combined in any manner.
Claims (5)
1. The method for growing the zinc-magnesium-titanium microwave ceramic based on the skeleton effect is characterized by comprising the following steps of:
a. zinc oxide powder, magnesia powder and titanium dioxide powder are used as raw materials, and the raw materials are mixed according to Zn 0.7 Mg 0.3 TiO 3 The components are respectively weighed and mixed; wherein each raw material consists of two kinds of powder with the grain diameter of 25-50wt% of micron-sized (grain diameter) powder and 50-75wt% of nano-sized (grain diameter) powder respectively;
b. performing primary ball milling on the mixed raw materials, and drying and grinding the slurry after ball milling to obtain precursor powder;
c. calcining the precursor powder for 2-4 hours at 850-950 ℃ to obtain a presintered material;
d. will burn inPerforming secondary ball milling on the material, and drying and grinding the slurry after ball milling to obtain Zn 0.7 Mg 0.3 TiO 3 Powder;
e. zn is added 0.7 Mg 0.3 TiO 3 Granulating the powder by using a polyvinyl alcohol adhesive, sieving, and briquetting to obtain a blank;
f. sintering the blank for 4-6 hours at 1150-1200 ℃ to obtain the zinc-magnesium-titanium microwave ceramic material.
2. The method for growing zinc-magnesium-titanium microwave ceramics based on the skeleton effect according to claim 1, wherein in the step a, the proportion of the micron-sized powder to the nanometer-sized powder can be the same or different for the three raw materials.
3. The method for growing zinc-magnesium-titanium microwave ceramics based on the skeleton effect according to claim 1, wherein in the step b and the step d, the same wet ball milling is adopted for both the primary ball milling and the secondary ball milling, the wet ball milling is carried out in a planetary ball mill, deionized water and absolute ethyl alcohol are used as solvents, agate beads are used as ball milling media, the mass ratio of raw materials to solvents is 1:1.5, the volume ratio of the deionized water to the absolute ethyl alcohol in the solvents is 1:1, and the ball milling time is 12 hours.
4. The method for growing zinc magnesium titanium microwave ceramics based on the skeleton effect according to claim 1, characterized in that in the step b and the step d, the drying temperature is 85 ℃ and the drying time is 24 hours.
5. The method for growing zinc magnesium titanium microwave ceramics based on the skeleton effect according to claim 1, characterized in that in step e, the amount of binder is 10-15ml; the sieving process is as follows: sequentially sieving with 40 mesh and 100 mesh, and collecting particles between 40 mesh and 100 mesh; the pressure of the briquette forming is 15-20Kg/cm 2 The time is 2-3 minutes, and the mixture is pressed into a cylindrical blank body.
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