CN115594489A - Microwave ceramic material Ca 3-x Li x B 2 O 6 And method for preparing the same - Google Patents
Microwave ceramic material Ca 3-x Li x B 2 O 6 And method for preparing the same Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000012776 electronic material Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 4
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction 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
- C04B35/01—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
- C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/057—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on calcium oxide
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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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
- C04B2235/3203—Lithium oxide or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention belongs to the field of electronic materials and manufacture thereof, and provides a microwave ceramic material Ca 3‑x Li x B 2 O 6 And a method for preparing the same. The chemical formula of the microwave ceramic material provided by the invention is Ca 3‑ x Li x B 2 O 6 (0.5<x<0.8 ) is a single crystal phase Ca 3 B 2 O 6 Has a hexagonal crystal structure. The sintered ceramic material has excellent microwave dielectric property at 850-950 ℃: the dielectric constant is 7.6-7.9, the Q x f value is 32000-40000 GHz, and the temperature coefficient of the resonance frequency is-64-48 ppm/DEG C. The microwave ceramic material has simple preparation process and low production cost, and is beneficial to realizing industrial production.
Description
Technical Field
The invention belongs to the field of electronic materials and manufacturing thereof, and particularly provides a microwave ceramic material Ca 3-x Li x B 2 O 6 And a method for preparing the same.
Background
The fifth generation communication technology greatly stimulates the demand of the industry on microwave components and also puts higher requirements on novel microwave ceramic materials. Borate microwave ceramic materials have been widely studied for their advantages of low cost, low dielectric constant, low dielectric loss, etc., e.g., takada et al, "Synthesiss and Microwave Dielectric Properti es of xRe 2 O 3 -yB 2 O 3 LaBO is reported in (Re = La, nd, sm, dy, ho and Y) Compounds, J.Appl.Phys.42 (2003) 6162-6167 3 The ceramic has better microwave performance when sintered at 1200 ℃: dielectric constant ε r It was 12.5, and Q.times.f. was 53000GHz. However, laBO 3 The ceramics can not meet the requirements of low temperature co-fired ceramics (LTCC)<950 ℃ limit LaBO 3 Industrial application of ceramics.
Based on this background, the present invention provides a microwave ceramic material Ca 3-x Li x B 2 O 6 And a method for preparing the same.
Disclosure of Invention
The invention provides a microwave ceramic material Ca 3-x Li x B 2 O 6 The preparation method comprises the following specific technical scheme:
(1) By means of H 3 BO 3 、Ca(OH) 2 、Li 2 CO 3 As raw material, according to the chemical formula Ca 3-x Li x B 2 O 6 (0.5<x<0.8 ) batching.
(2) Mixing the raw materials with alcohol and zirconium balls, ball-milling for 6 hours, and drying the slurry in an oven at 50-60 ℃ for 12 hours;
(3) Sieving the dried powder, placing the powder in a crucible, covering the crucible, presintering the powder for 3 hours at 750 ℃ to obtain Ca crystal phase 3 B 2 O 6 The pre-sintering material of (2);
(4) Mixing and ball-milling the pre-sintered material, alcohol and zirconium balls for 6 hours, and drying the slurry in an oven at 50-60 ℃ for 12 hours;
(5) Mixing the dry powder with acrylic acid for granulation, and performing dry pressing molding at 20 MPa;
(6) And (3) after the green body is subjected to gel removal for 1 to 2 hours at the temperature of 450 ℃, sintering for 5 hours at the temperature of 850 to 950 ℃ to obtain the microwave ceramic material.
The invention has the beneficial effects that:
1. the invention provides a microwave ceramic material Ca 3-x Li x B 2 O 6 (0.5<x<0.8 Permittivity epsilon) r 7.6 to 7.9, and Q multiplied by f value is 32000 to 40000GHz, temperature coefficient of resonance frequency tau f Is-64 to-48 ppm/DEG C.
2. The invention provides a microwave ceramic material Ca 3-x Li x B 2 O 6 The sintering temperature is 850-950 ℃, the LTCC technical requirement is met, the microstructure is compact, the grain growth is uniform, and no second phase is generated.
Drawings
FIG. 1 shows a microwave ceramic material Ca in example 2 2.1 B 2 O 6 :0.7Li + XRD pattern of (a).
FIG. 2 shows a microwave ceramic material Ca in example 2 2.1 B 2 O 6 :0.7Li + SEM image of (d).
Detailed description of the preferred embodiments
The present invention will be described in further detail with reference to the drawings and examples.
The invention specifically provides 5 embodiments, and the preparation method comprises the following steps:
(1) By means of H 3 BO 3 、Ca(OH) 2 、Li 2 CO 3 As raw material, according to the chemical formula Ca 3-x Li x B 2 O 6 (0.5<x<0.8 ) batching.
(2) Mixing the raw materials with alcohol and zirconium balls, ball-milling for 6 hours, and drying the slurry in an oven at 50-60 ℃ for 12 hours;
(3) Sieving the dried powder, placing in a crucible, covering with a cover, presintering at 750 deg.C for 3 hr to obtain Ca crystal phase 3 B 2 O 6 The pre-sintering material of (2);
(4) Mixing and ball-milling the pre-sintered material, alcohol and zirconium balls for 6 hours, and drying the slurry in an oven at 50-60 ℃ for 12 hours;
(5) Mixing the dry powder with acrylic acid for granulation, and performing dry pressing molding at 20 MPa;
(6) And (3) after the green body is subjected to gel removal for 1 to 2 hours at the temperature of 450 ℃, sintering for 5 hours at the temperature of 850 to 950 ℃ to obtain the microwave ceramic material.
The preparation process parameters and microwave dielectric properties for each example are shown in the following table:
as can be seen from the above table, the present invention provides a microwave ceramic material Ca 3-x Li x B 2 O 6 (0.5<x<0.8 And sintering at 850-950 ℃ has excellent microwave dielectric property: dielectric constant ε r 7.6 to 7.9, Q multiplied by f value of 32000 to 40000GHz, and resonant frequency temperature coefficient tau f Is-64 to-48 ppm/DEG C. As can be seen from FIG. 1, the characteristic peaks of the XRD spectrum are well matched with PDF #70-0868, indicating that the single crystal phase is Ca 3 B 2 O 6 . As can be seen from fig. 2, the microstructure in SEM is dense and the grain growth is uniform, thereby obtaining low dielectric loss.
Any feature disclosed in this specification may be replaced, unless expressly stated otherwise, by other equivalent or similarly purposed alternative features; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (3)
1. The microwave ceramic material is characterized in that the chemical formula of the microwave ceramic material is Ca 3-x Li x B 2 O 6 (0.5<x<0.8)。
2. The microwave ceramic material of claim 1, wherein the microwave ceramic material is a single crystal phase of Ca 3 B 2 O 6 Has a hexagonal crystal structure.
3. The microwave ceramic material and the preparation method thereof according to claim 1, characterized by comprising the following steps:
(1) By means of H 3 BO 3 、Ca(OH) 2 、Li 2 CO 3 As raw material, according to the chemical formula Ca 3-x Li x B 2 O 6 (0.5<x<0.8 ) batching.
(2) Mixing the raw materials with alcohol and zirconium balls, ball-milling for 6 hours, and drying the slurry in an oven at 50-60 ℃ for 12 hours;
(3) Sieving the dried powder, placing in a crucible, covering with a cover, presintering at 750 deg.C for 3 hr to obtain Ca crystal phase 3 B 2 O 6 The pre-sintering material of (1);
(4) Mixing and ball-milling the pre-sintered material, alcohol and zirconium balls for 6 hours, and drying the slurry in an oven at 50-60 ℃ for 12 hours;
(5) Mixing the dry powder with acrylic acid for granulation, and performing dry pressing molding at 20 MPa;
(6) And (3) after the green body is subjected to gel removal for 1 to 2 hours at the temperature of 450 ℃, sintering for 5 hours at the temperature of 850 to 950 ℃ to obtain the microwave ceramic material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211159581.4A CN115594489A (en) | 2022-09-22 | 2022-09-22 | Microwave ceramic material Ca 3-x Li x B 2 O 6 And method for preparing the same |
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| CN202211159581.4A CN115594489A (en) | 2022-09-22 | 2022-09-22 | Microwave ceramic material Ca 3-x Li x B 2 O 6 And method for preparing the same |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050103A (en) * | 2007-04-04 | 2007-10-10 | 华中科技大学 | Microwave medium ceramic material and preparation method |
| US20090270244A1 (en) * | 2008-04-25 | 2009-10-29 | Zhe Jiang University | Low-Loss Microwave Dielectric Ceramic |
| US20160264470A1 (en) * | 2015-03-12 | 2016-09-15 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Low temperature co-fired ceramic material and preparation method therefor |
| CN114702303A (en) * | 2022-03-31 | 2022-07-05 | 电子科技大学 | Microwave dielectric material Ca3B2O6And method for preparing the same |
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2022
- 2022-09-22 CN CN202211159581.4A patent/CN115594489A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050103A (en) * | 2007-04-04 | 2007-10-10 | 华中科技大学 | Microwave medium ceramic material and preparation method |
| US20090270244A1 (en) * | 2008-04-25 | 2009-10-29 | Zhe Jiang University | Low-Loss Microwave Dielectric Ceramic |
| US20160264470A1 (en) * | 2015-03-12 | 2016-09-15 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Low temperature co-fired ceramic material and preparation method therefor |
| CN114702303A (en) * | 2022-03-31 | 2022-07-05 | 电子科技大学 | Microwave dielectric material Ca3B2O6And method for preparing the same |
Non-Patent Citations (1)
| Title |
|---|
| 钟茂锋: "硼酸盐LTCC微波介质陶瓷及其应用研究" * |
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Application publication date: 20230113 |