Microwave ceramic material, preparation method and application thereof
By adjusting the composition and additives of CaMg(Zr0.05Si1.95)O6 and SrxBa(2-x)TiSi2O8, microwave ceramic materials with excellent dielectric properties were prepared, which solved the shortcomings of existing materials in high-frequency applications, expanded their application range and improved device performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- BEIJING YUAN LIU HONG YUAN ELECTRONIC TECHNOLOGY CO LTD
- Filing Date
- 2024-07-29
- Publication Date
- 2026-06-19
AI Technical Summary
Existing low dielectric constant microwave ceramic materials suffer from narrow sintering temperature range, non-dense microstructure, difficulty in phase control, difficulty in unifying low dielectric constant, quality factor and near-zero temperature coefficient, and poor resistance to reduction, which limits their application in high-frequency components.
Microwave ceramic materials with a dielectric constant of 6.2–8.3, dielectric loss <1 × 10⁻⁴, and adjustable capacitance temperature coefficient were prepared by using CaMg(Zr0.05Si1.95)O₆ and SrxBa(2-x)TiSi₂O₈ as the base materials and adding B₂O₃, SiO₂, and ZnO as sintering aids and manganese, aluminum, cobalt, niobium, and cerium compounds as modifying additives to adjust dielectric properties and microstructure.
It achieves controllable dielectric constant, low dielectric loss, and adjustable temperature coefficient, expanding the application range of microwave ceramic materials. It is suitable for the manufacture of microwave devices such as multilayer ceramic capacitors, single-layer capacitors, and microwave substrates, and has a high insulation resistivity.
Abstract
Description
Technical Field
[0001] This invention belongs to the field of ceramic materials technology, specifically relating to a microwave ceramic material, its preparation method, and its application. Background Technology
[0002] With the rapid development of 5G communication technology, higher frequencies are an inevitable trend in the development of microwave components. As the operating frequency of communication equipment expands into the millimeter-wave band, signal delay becomes more prominent, placing higher demands on the performance of microwave dielectric ceramics, a key material in communication equipment. Compared with dielectric and high dielectric constant materials, low dielectric constant materials can reduce the interaction coupling loss between the substrate and metal electrodes, shortening the signal propagation delay time between chips. As communication technology gradually moves towards millimeter waves, the requirements for the microwave dielectric properties of multilayer ceramic capacitors (MLCCs) are also increasing, demanding low dielectric constants (ε). r <10) To improve the information transmission rate of the device, lower high-frequency dielectric loss (tanδ<0.0005) to enhance the frequency selectivity of the device and reduce energy consumption, and near-zero frequency temperature coefficient to ensure the working stability of the signal during resonance and transmission.
[0003] Currently, research on low dielectric constant materials mainly focuses on material systems such as Al2O3, Mg2SiO4, AWO4 (where A is Ca, Sr, or Ba), phosphates, and R2BaCuO5 (where R is Y, Sm, or Yb). For example, Chinese patent CN106587987A discloses a C0G characteristic microwave dielectric material with a dielectric constant of 10–20, mainly by substituting Ca or Sr at the A-site of MgTiO3 to adjust the dielectric constant and temperature coefficient. However, the dielectric constant of this ceramic material is greater than 10, thus limiting its application at higher frequency bands. Another example is Chinese patent CN111635222A, which discloses a high-temperature sintering (1350–1475℃) low dielectric constant (ε... r Microwave dielectric materials with a frequency stability coefficient τ of 6.3 to 6.8 (τ = 6.3 to 6.8) have a high frequency stability coefficient τ. f = -47ppm / ℃ (dielectric constant τ) ε The dielectric constant is approximately 74 ppm / ℃, and the sintering temperature is too high, thus limiting the application range of this material. Most existing low dielectric constant materials suffer from various problems such as narrow sintering temperature range, insufficient microstructure, difficulty in phase control, difficulty in unifying low dielectric constant, quality factor, and near-zero temperature coefficient, and poor resistance to reduction, which limit their practical application in high-frequency components. Summary of the Invention
[0004] In view of this, the present invention provides a microwave ceramic material, its preparation method, and its application. The dielectric constant of the microwave ceramic material provided by the present invention is controllable in the range of 6.2 to 8.3, and its dielectric loss is <1×10⁻⁶. -4 The capacity temperature coefficient is adjustable (meeting CF(0±15)ppm / ℃, CG(0±30)ppm / ℃ and AG(100±30)ppm / ℃), while also having a high insulation resistivity (>1×10⁻⁶). 13 The Ω·cm) has expanded the application range of microwave ceramic materials.
[0005] To address the aforementioned technical problems, this invention provides a microwave ceramic material comprising the following components in weight percentage:
[0006]
[0007] Where 0 ≤ x ≤ 1.46;
[0008] The sintering aid is one or more of B2O3, SiO2 and ZnO;
[0009] The modified additive is one or more of manganese compounds, aluminum compounds, cobalt compounds, niobium compounds, and cerium compounds.
[0010] Preferably, the CaMg(Zr) 0.05 Si 1.95 The preparation method of O6 includes the following steps:
[0011] CaCO3, Mg(OH)2, ZrO2, and SiO2 are first mixed and then calcined to obtain the CaMg(ZrO2)2 mixture. 0.05 Si 1.95 )O6.
[0012] Preferably, the first mixture is produced by wet ball milling;
[0013] The first calcination temperature is 1150-1200℃, and the time is 2-5 hours.
[0014] Preferably, the Sr x Ba (2-x) The preparation method of TiSi2O8 includes the following steps:
[0015] The SrCO3, BaCO3, TiO2 and SiO2 are mixed and then calcined a second time to obtain the Sr x Ba (2-x) TiSi2O8.
[0016] Preferably, the second mixing is performed by wet ball milling;
[0017] The second calcination temperature is 1100-1170℃, and the time is 2-4 hours.
[0018] Preferably, the manganese compound is an oxide of manganese and / or manganese carbonate;
[0019] The aluminum compound is one or more of aluminum oxide, aluminum hydroxide, and aluminum carbonate;
[0020] The cobalt compound is an oxide of cobalt and / or cobalt carbonate;
[0021] The niobium compound is an oxide of niobium and / or niobium hydroxide;
[0022] The cerium compound is an oxide of cerium and / or cerium carbonate.
[0023] Preferably, when the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, the mass percentage of each component oxide in the modifying additive relative to the microwave ceramic material is:
[0024] MnO 0.10~0.34wt%;
[0025] Al2O3 1.52~4.69wt%;
[0026] CoO 0.15~0.34wt%;
[0027] Nb₂O₅ 0–3.82 wt%;
[0028] CeO2 0–0.29 wt%.
[0029] The present invention also provides a method for preparing the microwave ceramic material described in the above technical solution, comprising the following steps:
[0030] CaMg(Zr) 0.05 Si 1.95 O6、Sr x Ba (2-x) The microwave ceramic material is obtained by mixing TiSi2O8, sintering aids, and modifying additives.
[0031] Preferably, the process before mixing further includes: subjecting the sintering aid to a third calcination; the third calcination temperature is 550–650°C, and the time is 2–4 hours;
[0032] The mixing is performed by wet ball milling, and the wet ball milling time is 5 to 10 hours.
[0033] The present invention also provides the application of microwave ceramic materials prepared by the above-described method in the preparation of microwave devices.
[0034] This invention provides a microwave ceramic material comprising the following components in weight percentage: 77.93–83.84 wt% CaMg(Zr) 0.05 Si 1.95 O6, 11.27~12.12wt% Sr x Ba (2-x) TiSi₂O₈, 1.77–2.82 wt% sintering aid and 1.77–9.48 wt% modifying additive; wherein 0 ≤ x ≤ 1.46; the sintering aid is one or more of B₂O₃, SiO₂, and ZnO; the modifying additive is one or more of manganese compounds, aluminum compounds, cobalt compounds, niobium compounds, and cerium compounds. This invention uses CaMg(ZnO)₂O₈ as the base material. 0.05 Si 1.95 Based on O6 microwave dielectric ceramics, by adjusting the auxiliary material (Sr) x Ba (2-x) The composition and dosage of TiSi2O8 and modifying additives are used to adjust the dielectric properties and microstructure of microwave dielectric ceramic materials, making their temperature coefficient adjustable within the temperature range of -55℃ to 125℃, meeting the temperature characteristic requirements of CF (0±15)ppm / ℃, CG (0±30)ppm / ℃ and AG (100±30)ppm / ℃ in GB / T 5596; and the microwave dielectric ceramic material provided by this invention has a high insulation resistivity (>10). 13 (Ω·cm), expanding its application scope.
[0035] The low dielectric constant microwave ceramic material provided by this invention has a simple preparation process, is easy to mass-produce, has low raw material cost and is environmentally friendly, and can be used in the manufacture of microwave devices such as multilayer ceramic capacitors, single-layer capacitors and microwave substrates. Detailed Implementation
[0036] This invention provides a microwave ceramic material comprising the following components in weight percentage:
[0037]
[0038] Where 0 ≤ x ≤ 1.46;
[0039] The sintering aid is one or more of B2O3, SiO2 and ZnO;
[0040] The modified additive is one or more of manganese compounds, aluminum compounds, cobalt compounds, niobium compounds, and cerium compounds.
[0041] In this invention, unless otherwise specified, all raw materials are conventional commercially available products, and the purity of all raw materials is preferably 99% or higher.
[0042] The microwave ceramic material provided by this invention comprises 77.93–83.84 wt% CaMg(Zr) based on mass percentage. 0.05 Si 1.95 The CaMg(Zr)O6 content is preferably 79.27–83 wt%, more preferably 79.46–81.65 wt%. In this invention, the CaMg(Zr)O6 content is... 0.05 Si 1.95 The preferred method for preparing O6 includes the following steps:
[0043] CaCO3, Mg(OH)2, ZrO2, and SiO2 are first mixed and then calcined to obtain the CaMg(ZrO2)2 mixture. 0.05 Si 1.95 )O6.
[0044] In this invention, the first mixing is preferably wet ball milling. The dispersant used in the wet ball milling is preferably water, and the water is preferably deionized water; the milling balls used in the wet ball milling are preferably zirconia balls. This invention does not have special requirements for the rotation speed and time of the wet ball milling, as long as the mixing is uniform. In this invention, the first mixing preferably further includes: drying and sieving the first mixed product sequentially. This invention does not have special requirements for the drying, as long as the solvent is removed. In this invention, the aperture of the sieve used for sieving is preferably 60-100 mesh, more preferably 100 mesh. This invention preferably uses the undersize material for a first calcination.
[0045] In this invention, the temperature of the first calcination is preferably 1150-1200℃, more preferably 1160-1180℃; the time of the first calcination is preferably 2-5h, more preferably 3-4h.
[0046] In this invention, the CaMg(Zr) 0.05 Si 1.95 The main material is O6, and the CaMg(Zr) is used as the main material. 0.05 Si 1.95 The presence of a small amount of Zr in O6 can broaden the sintering temperature, stabilize the phase structure, and suppress the formation of the impurity phase Ca2MgSi2O7.
[0047] The microwave ceramic material provided by this invention comprises 11.27–12.12 wt% Sr, based on mass percentage. x Ba (2-x) TiSi₂O₈, preferably 11.49–12 wt%. In this invention, 0 ≤ x ≤ 1.46, preferably 0.16–1.44, more preferably 0.62–1.38. In this invention, the Sr x Ba (2-x) The preferred method for preparing TiSi2O8 includes the following steps:
[0048] The SrCO3, BaCO3, TiO2 and SiO2 are mixed and then calcined a second time to obtain the Sr x Ba (2-x) TiSi2O8.
[0049] In this invention, the second mixing is preferably wet ball milling; the dispersant used in the wet ball milling is preferably water, and the water is preferably deionized water; the material-to-water ratio in the wet grinding is preferably 0.8–1.2:3, more preferably 1:3; the grinding balls used in the wet ball milling are preferably zirconia balls. This invention has no special requirements for the rotation speed and time of the wet ball milling, as long as the mixing is uniform. In this invention, when x is 0, SrCO3 is not added during the second mixing process. In this invention, the second mixing process preferably further includes: drying and sieving the product sequentially. This invention has no special requirements for the drying, as long as the solvent is removed. In this invention, the aperture of the sieve used for sieving is preferably 60–100 mesh, more preferably 100 mesh. This invention preferably uses the undersize material for a second calcination.
[0050] In this invention, the temperature of the second calcination is preferably 1100-1170°C; the time of the second calcination is preferably 2-4 hours, more preferably 2.5-3.5 hours.
[0051] In this invention, the Sr x Ba (2-x) TiSi2O8, as a by-product, can improve the microstructure, increase density, and broaden the firing temperature range, while also adjusting the capacity temperature coefficient and insulation resistance.
[0052] The microwave ceramic material provided by this invention comprises 1.77–2.82 wt% sintering aid, preferably 2–2.46 wt%, by weight percentage. In this invention, the sintering aid is one or more of B₂O₃, SiO₂, and ZnO, preferably B₂O₃, SiO₂, and ZnO. In this invention, the sintering aid can effectively diffuse to the grain boundary layer, effectively improving the dielectric properties and ceramic body strength of the microwave ceramic material. When the amount of sintering aid added is too low, the ceramic body is under-fired and the insulation resistance decreases; when the amount of sintering aid added is too high, the dielectric loss is too high and the ceramic body strength is low. This invention limits the amount of sintering aid within the above range to ensure the performance of the microwave ceramic material.
[0053] The microwave ceramic material provided by this invention comprises 1.77–9.48 wt% modified additives, preferably 2.27–7.97 wt%, more preferably 3.05–6.88 wt%, by weight percentage. In this invention, the modified additives are one or more of manganese compounds, aluminum compounds, cobalt compounds, niobium compounds, and cerium compounds. In this invention, the manganese compound is preferably manganese oxide and / or manganese carbonate, more preferably manganese oxide; the aluminum compound is preferably one or more of aluminum oxide, aluminum hydroxide, and aluminum carbonate, more preferably aluminum oxide; the cobalt compound is preferably cobalt oxide and / or cobalt carbonate, more preferably cobalt oxide; the niobium compound is preferably niobium oxide and / or niobium hydroxide, more preferably niobium oxide; the cerium compound is preferably cerium oxide and / or cerium carbonate, more preferably cerium oxide. In this invention, the manganese oxide is preferably MnO, the aluminum oxide is preferably Al₂O₃, the cobalt oxide is preferably CoO, the niobium oxide is preferably Nb₂O₅, and the cerium oxide is preferably CeO₂.
[0054] In this invention, when the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, based on the total mass of the microwave ceramic material, the modifying additive preferably includes 0.10–0.34 wt% MnO, more preferably 0.23–0.33 wt%, and even more preferably 0.25–0.29 wt%. In this invention, the additive MnO can ensure low dielectric loss and improve the Q value of the microwave device (capacitor) under microwave conditions. This invention limits the amount of manganese oxide within the above range to maintain the performance of the microwave device well. Too little addition will increase the dielectric loss of the microwave device under microwave conditions, making it prone to overheating and failure; too much addition will result in a porous ceramic structure and poor dielectric properties.
[0055] In this invention, when the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, based on the total mass of the microwave ceramic material, the modifying additive preferably includes 1.52–4.69 wt% Al2O3, more preferably 2.39–3.83 wt%, and even more preferably 2.45–2.5 wt%. In this invention, the additive Al2O3 can improve the sintering characteristics of the ceramic body, enhance its mechanical strength, and improve its dielectric properties. This invention limits the amount of alumina used to maintain the ceramic properties well within the above range; too little alumina results in poor mechanical strength and high dielectric loss, while too much alumina makes sintering the ceramic body difficult.
[0056] In this invention, when the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, based on the total mass of the microwave ceramic material, the modifying additive preferably includes 0.15–0.34 wt% CoO, more preferably 0.23–0.25 wt%. In this invention, the additive CoO can improve and increase the insulation resistance of the capacitor and effectively reduce dielectric loss. Too little CoO will hinder the improvement of the insulation resistance of the microwave device; too much CoO will make the sintering of the microwave device more difficult.
[0057] In this invention, when the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, based on the total mass of the microwave ceramic material, the modifying additive preferably includes 0–3.82 wt% Nb2O5, more preferably 1.23–3.35 wt%, and even more preferably 1.47–2.82 wt%. In this invention, the additive Nb2O5 can increase the lattice activity of the powder, which is beneficial for sintering and improves the reliability of the ceramic capacitor.
[0058] In this invention, when the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, the total mass of the microwave ceramic material is used as the basis. Preferably, the modifying additive includes 0–0.29 wt% CeO2, more preferably 0.1–0.25 wt%. In this invention, the CeO2 additive can prevent capacitor aging, refine grain size, and ensure the dielectric properties of the capacitor.
[0059] The present invention also provides a method for preparing the microwave ceramic material described in the above technical solution, comprising the following steps:
[0060] CaMg(Zr) 0.05 Si 1.95 O6、Sr x Ba (2-x) The microwave ceramic material is obtained by mixing TiSi2O8, sintering aids, and modifying additives.
[0061] In this invention, the process before mixing preferably includes: subjecting the sintering aid to a third calcination. In this invention, the process before the third calcination preferably includes: wet ball milling one or more of B2O3, SiO2, and ZnO, followed by sequential drying and sieving. In this invention, the dispersant used for wet ball milling is preferably water, preferably deionized water; the milling balls used for wet ball milling are preferably zirconia balls; the rotational speed of the wet ball milling is preferably 300–400 r / min, more preferably 350 r / min; the wet ball milling time is preferably 4–6 h, more preferably 5 h. In this invention, the drying temperature is preferably 60–80 °C, more preferably 70 °C. This invention has no special requirements for the drying time, as long as the solvent is removed. In this invention, the mesh size of the sieve used for sieving is preferably 100 mesh. This invention preferably uses the undersize material for the third calcination.
[0062] In this invention, the temperature of the third calcination is preferably 550–650°C, more preferably 600–630°C; the time of the third calcination is preferably 2–4 hours, more preferably 2.5–3.5 hours. The third calcination process removes adsorbed carbon dioxide and / or water of crystallization from the sintering aid components. In this invention, the sintering aid is a low-melting-point substance that promotes the sintering of the ceramic body.
[0063] In this invention, the mixing is preferably wet ball milling; the dispersant used in the wet ball milling is preferably water, and the water is preferably deionized water; the grinding balls used in the wet ball milling are preferably zirconia balls; the wet ball milling time is preferably 5-10 hours, more preferably 6-8 hours. In this invention, the mixing process preferably further includes: drying and sieving the mixed material sequentially. In this invention, the drying temperature is preferably 110-130°C, more preferably 120°C; the drying time is preferably 5-7 hours, more preferably 6 hours. In this invention, the mesh size of the sieve used for sieving is preferably 100 mesh.
[0064] This invention also provides the application of the microwave ceramic materials described in the above-described technical solutions, or the microwave ceramic materials prepared by the methods described in the above-described technical solutions, in the fabrication of microwave devices. In this invention, the microwave device preferably includes a ceramic capacitor or a substrate.
[0065] In this invention, the method for fabricating microwave devices using microwave ceramic materials preferably includes the following steps:
[0066] Microwave ceramic materials and binders are mixed and then granulated and molded sequentially to obtain a green body;
[0067] The blank is sequentially debonded and sintered to obtain the microwave device.
[0068] In this invention, the binder is preferably a polyvinyl butyral solution, and the mass concentration of the polyvinyl butyral solution is preferably 10%. This invention does not impose any particular limitation on the granulation process; conventional methods in the art can be used. In this invention, the molding pressure is preferably 4–6 MPa. In this invention, the shape of the preform is preferably a disc or a cylinder.
[0069] In this invention, the temperature for removing the adhesive is preferably 440–460°C, more preferably 450°C; the holding time for removing the adhesive is preferably 2.5–3.5 h, more preferably 3 h. In this invention, the heating rate to the required temperature for removing the adhesive is preferably 3°C / min. In this invention, the sintering temperature is preferably 1240–1340°C, more preferably 1270–1300°C; the holding time for sintering is preferably 2–5 h, more preferably 3–4 h.
[0070] In this invention, the process after sintering preferably further includes: cooling the sintered product to room temperature in the furnace. In this invention, the room temperature is preferably 20–35°C, more preferably 25–30°C.
[0071] To further illustrate the present invention, the technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.
[0072] Example 1
[0073] CaCO3, Mg(OH)2, ZrO2, and SiO2 with a purity of 99% were mixed in the manner of CaMg(ZrO2) 0.05 Si 1.95 The ingredients were prepared in a molar ratio of O6 and wet-milled in a planetary ball mill at a speed of 350 r / min (using deionized water as the dispersant and zirconium balls as the grinding balls) for 5 h. The wet-milled product was dried at 120 °C and passed through a 60-mesh sieve. The undersize material was then calcined at 1170 °C for 3 h to obtain CaMg(Zr) 0.05 Si 1.95 O6;
[0074] The preferred method for preparing Ba2TiSi2O8 includes the following steps:
[0075] BaCO3, TiO2, and SiO2 with a purity of 99% (molar ratio of BaCO3, TiO2, and SiO2 is 2:1:2) and deionized water were mixed and wet-milled (using zirconia balls as grinding balls) at a total mass ratio of BaCO3, TiO2, and SiO2 to dispersant of 1:3. After wet milling, the product was dried and passed through a 60-mesh sieve. The sieve-filled material was then calcined at 1170℃ for 3 hours to obtain Ba2TiSi2O8.
[0076] B2O3, SiO2 and ZnO with a purity of 99% were ball-milled in a planetary ball mill at a speed of 350 r / min in a molar ratio of 3:2:5 (using deionized water as solvent and zirconium balls as grinding balls) for 5 h. After drying at 70 °C, the mixture was passed through a 100-mesh sieve and then calcined at 600 °C for 4 h to obtain a sintering aid.
[0077] CaMg(Zr) 0.05 Si 1.95 O6, Ba2TiSi2O8, sintering aids and modifying additives according to CaMg(Zr) 0.05 Si 1.95 The microwave ceramic material was prepared by wet ball milling for 5 hours with deionized water as the dispersant and zirconia balls as the grinding balls, followed by drying at 120°C for 6 hours. The mixture contained 83% O6, 12% Ba2TiSi2O8, 2% sintering aid, and 3% modified additives (including 0.25% MnO, 2.5% Al2O3, and 0.25% CoO).
[0078] Examples 2-20
[0079] Microwave ceramic materials were prepared according to the method in Example 1, except that Sr with different x values were prepared as shown in Table 1. x Ba (2-x) TiSi2O8, refer to Table 2 to limit CaMg(Zr 0.05 Si 1.95 O6、Sr x Ba (2-x) The composition and mass percentage of TiSi2O8, sintering aids, and modifying additives.
[0080] Table 1 Sr x Ba (2-x) TiSi2O8 formulation design and calcination temperature
[0081]
[0082]
[0083] Table 2. Formulation design content (mass percentage / wt%) of microwave ceramic materials prepared in Examples 1-20
[0084]
[0085]
[0086] Dielectric property testing: Microwave ceramic material and a 10 wt% PVB (polyvinyl butyral) solution were mixed and granulated, and then pressed into discs and cylindrical blanks under pressures of 4 MPa and 6 MPa, respectively. The blanks were heated to 450℃ at a heating rate of 3℃ / min for 3 hours to remove the binder. The blanks after binder removal were sintered at 1270℃ for 3 hours and then naturally cooled to room temperature (25℃) with the furnace. The two surfaces of the sintered discs were coated with silver paste, silver electrodes were fired, and capacitors were made. The room temperature electrical properties were then tested, and the results are listed in Table 3.
[0087] Table 3 Performance parameters of products prepared from ceramic material formulations
[0088]
[0089]
[0090] Note: The sample capacitance, dielectric loss, and insulation resistivity related to dielectric constant were all tested at room temperature (25℃ ± 3℃).
[0091] As shown in Table 3, the microwave devices prepared using the microwave ceramic materials provided by this invention have a relative permittivity of 6.19–8.25, satisfy the temperature coefficients (CF, CG, AG) of high-frequency capacitor ceramics within the temperature range of -55℃ to 125℃, and an insulation resistivity >1×10⁻⁶. 13 Ω·cm.
[0092] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A microwave ceramic material, characterized by, The components include the following components by mass percentage: Where 0 ≤ x ≤ 1.46; The sintering aid is one or more of B2O3, SiO2 and ZnO; The modified additive is one or more of manganese compounds, aluminum compounds, cobalt compounds, niobium compounds, and cerium compounds.
2. The microwave ceramic material of claim 1, wherein, The CaMg(Zr 0.05 Si 1.95 )O6 preparation method comprises the following steps: CaCO3, Mg(OH)2, ZrO2and SiO2are first mixed to perform first calcination to obtain the CaMg(Zr 0.05 Si 1.95 )O6.
3. The microwave ceramic material of claim 2, wherein, The first mixture is produced by wet ball milling; The first calcination temperature is 1150-1200℃, and the time is 2-5 hours.
4. The microwave ceramic material of claim 1 wherein, The Sr x Ba (2-x) The method for producing TiSi2O8 includes the following steps: SrCO3, BaCO3, TiO2and SiO2are second mixed to be second calcined to obtain the Sr x Ba (2-x) TiSi2O8.
5. The microwave ceramic material of claim 4, wherein, The second mixing process is wet ball milling; The second calcination temperature is 1100-1170℃, and the time is 2-4 hours.
6. The microwave ceramic material of claim 1 wherein, The manganese compound is a manganese oxide and / or manganese carbonate; The aluminum compound is one or more of aluminum oxide, aluminum hydroxide, and aluminum carbonate; The cobalt compound is an oxide of cobalt and / or cobalt carbonate; The niobium compound is an oxide of niobium and / or niobium hydroxide; The cerium compound is an oxide of cerium and / or cerium carbonate.
7. The microwave ceramic material of claim 6 wherein, When the modifying additive is MnO, Al2O3, CoO, Nb2O5, and CeO2, the mass percentage of each component oxide in the microwave ceramic material is as follows: MnO 0.10~0.34wt%; Al2O3 1.52~4.69wt%; CoO 0.15~0.34wt%; Nb₂O₅ 0–3.82 wt%; CeO2 0–0.29 wt%.
8. Process for the production of a microwave ceramic material according to any one of claims 1 to 7, characterized in that, Includes the following steps: CaMg(Zr 0.05 Si 1.95 )O6, Sr x Ba (2-x) TiSi2O8, sintering aids and modifying additives are mixed to obtain the microwave ceramic material.
9. The method of making a microwave ceramic material according to Claim 8, wherein, The process before mixing also includes: subjecting the sintering aid to a third calcination; the third calcination temperature is 550–650°C, and the time is 2–4 hours; The mixing is performed by wet ball milling, and the wet ball milling time is 5 to 10 hours.
10. The application of the microwave ceramic material according to any one of claims 1 to 7 or the microwave ceramic material prepared by the preparation method according to claim 8 or 9 in the preparation of microwave devices.
Citation Information
Patent Citations
C0G microwave dielectric material, preparation method thereof, and preparation method of ceramic material
CN106587987A
Monoclinic phase-based low-dielectric microwave dielectric ceramic material and preparation method thereof
CN111635222A
Dielectric adjustable microwave ceramic dielectric material and method of producing the same
CN101492294A
Low-dielectric constant microwave ceramic dielectric material and preparation method thereof
CN102659396A