CN109721340B - High-strength low-loss LTCC material and preparation method thereof - Google Patents
High-strength low-loss LTCC material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
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- 239000000843 powder Substances 0.000 claims abstract description 69
- 239000000919 ceramic Substances 0.000 claims abstract description 34
- 238000000227 grinding Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- 238000010791 quenching Methods 0.000 claims abstract description 6
- 230000000171 quenching effect Effects 0.000 claims abstract description 6
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 229910052593 corundum Inorganic materials 0.000 claims description 13
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 13
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910002637 Pr6O11 Inorganic materials 0.000 claims description 7
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
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- 239000002893 slag Substances 0.000 claims description 6
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- 238000003825 pressing Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 239000006124 glass-ceramic system Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910017970 MgO-SiO2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
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- 238000004031 devitrification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000005355 lead glass Substances 0.000 description 1
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Abstract
The invention discloses a high-strength low-loss LTCC material which is prepared from the following components in percentage by mass: 40-60% of ceramic powder and 40-60% of MSBCZ glass powder, wherein the MSBCZ glass powder at least comprises the following components: MgO, SiO2BaO, CaO and ZnO. The invention also discloses a preparation method of the high-strength low-loss LTCC material, which comprises the following steps: mixing, smelting, water quenching, grinding, drying and sieving raw materials of MSBCZ glass powder in sequence, wherein the raw materials of the MSBCZ glass powder at least comprise MgO and SiO2BaO, CaO and ZnO; weighing 40-60% of ceramic powder and 40-60% of MSBCZ glass powder according to mass percentage, mixing, drying, performing compression molding on the dried powder, and sintering to obtain the high-strength low-loss LTCC material. The high-strength low-loss LTCC material and the preparation method thereof provided by the invention meet the requirements of low dielectric, low loss, high strength and low sintering temperature.
Description
Technical Field
The invention relates to the technical field of electronic ceramic materials, in particular to a high-strength low-loss LTCC material and a preparation method thereof.
Background
Low temperature co-fired ceramic (LTCC) is an advanced passive integration technology, and is the first choice for future electronic component integration. LTCC materials are widely explored and researched at home and abroad, and currently, three major systems, namely a glass ceramic system (microcrystalline glass), a glass/ceramic system and a crystallized ceramic system (pure ceramic), mainly exist.
The low dielectric LTCC (epsilon less than 10) material mainly comprises a glass ceramic system and a glass/ceramic system, wherein the glass ceramic system precipitates crystals through glass preparation and glass heat treatment processes in sequence to finally form polycrystalline ceramic, and the low dielectric constant temperature low temperature ceramic material has the characteristics of low microcrystalline glass crystallization temperature, small microcrystalline dielectric loss, high mechanical strength and the like; the glass/ceramic system is mainly characterized by that it utilizes the characteristics of low melting point of glass (sintering aid) and low dielectric constant and good physical properties of ceramic, and mixes a certain quantity of ceramic into the glass to make the glass and ceramic be sintered together at low temp. (the glass mainly includes crystal glass and amorphous glass), but its strength is generally not higher than 250 MPa.
The above background disclosure is only for the purpose of assisting understanding of the concept and technical solution of the present invention and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-strength low-loss LTCC material and a preparation method thereof, which meet the requirements of low dielectric, low loss, high strength and low sintering temperature.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a high-strength low-loss LTCC material which is prepared from the following components in percentage by mass: 40% -60% of ceramic powder and 40% -60% of MSBCZ glass powder, wherein the MSBCZ glass powder at least comprises the following components: MgO, SiO2BaO, CaO and ZnO.
Preferably, the MSBCZ glass powder also comprises La2O3、Pr6O11、Al2O3、Na2O、TiO2、ZrO2At least one of (1).
Preferably, the MSBCZ glass powder comprises the following components in percentage by mass: MgO 10-20 wt% and SiO240 to 50 percent of BaO, 15 to 30 percent of CaO, 5 to 15 percent of ZnO, and La2O30 to 5% of Pr6O110 to 2% of Al2O30 to 5% of Na20 to 2% of O and TiO20 to 2% of ZrO20 to 2%.
Preferably, the ceramic powder is Al2O3Or AlN.
The invention discloses a preparation method of a high-strength low-loss LTCC material, which comprises the following steps:
s1: mixing, smelting, water quenching, grinding, drying and sieving raw materials of MSBCZ glass powder in sequence, wherein the raw materials of the MSBCZ glass powder at least comprise MgO and SiO2BaO, CaO and ZnO;
s2: weighing 40-60% of ceramic powder and 40-60% of MSBCZ glass powder according to mass percentage, mixing, drying, performing compression molding on the dried powder, and sintering to obtain the high-strength low-loss LTCC material.
Preferably, in step S1, the MSBCZ glass frit comprises the following raw materials by mass percent: 10 to 20 percent of MgO and 40 to 50 percent of SiO215 to 30 percent of BaO, 15 to 20 percent of CaO, 5 to 15 percent of ZnO and 0 to 5 percent of La2O30 to 2% of Pr6O110 to 5% of Al2O30 to 2% of Na2O, 0-2% TiO20 to 2% of ZrO2。
Preferably, step S1 specifically includes: the MSBCZ glass powder is prepared by uniformly mixing raw materials in a dry mode, smelting at 1300-1400 ℃, preserving heat for 2 hours, pouring smelted glass liquid into deionized water for water quenching, adding water quenched glass slag, deionized water and grinding balls into a grinding tank for grinding, drying and sieving.
Preferably, the ceramic powder in step S2 is Al2O3Or AlN.
Preferably, step S2 specifically includes: adding 40-60% of ceramic powder, 40-60% of MSBCZ glass powder, deionized water, a dispersing agent and grinding balls into a grinding tank, mixing, grinding, drying, pressing and molding the dried powder, sintering at 850-900 ℃, and preserving heat for 1-2 hours to obtain the high-strength low-loss LTCC material.
The invention also discloses a high-strength low-loss LTCC material prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that: the invention discloses a high-strength low-loss LTCC material which is prepared from ceramic powder and sintering aid MgO-SiO2The dielectric constant of the finally obtained high-strength low-loss LTCC material is between 6.5 and 8.5(12GHz), the dielectric loss is less than 0.0012(12GHz), the strength is more than 380MPa, the LTCC material can be matched and co-fired with silver below 900 ℃, and the LTCC material can be used as an LTCC substrate, a filter and a coupling jointMicrowave components and parts such as devices.
Furthermore, through the design of the components of the glass powder, the MSBCZ glass with weak crystallization is obtained, compared with non-crystallization type glass, the MSBCZ glass has higher strength, and compared with pure crystallization type glass, the sintering and the influence on the dielectric constant of the MSBCZ glass are easier to control; the ceramic phase is a crystal, the ion arrangement is compact, the corresponding strength is high, the glass is a loose network structure, the binding force between ions is weak, and the corresponding strength is low, so that the sintering densification below 900 ℃ can be realized through mutual adjustment and matching of the proportions of the ceramic phase and the glass phase, the weak crystallization type MSBCZ glass can assist in sintering, the environment cannot be polluted, the dielectric constant of the material can be reduced, and the strength of the material can be improved.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a cross-section of a sintered sample according to an embodiment of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and preferred embodiments.
The invention discloses a high-strength low-loss LTCC material which is prepared from the following components in percentage by mass: 40 to 60 percent of ceramic powder and 40 to 60 percent of MSBCZ glass powder, wherein the ceramic powder is Al2O3Or AlN; the MSBCZ glass powder comprises MgO and SiO2BaO, CaO and ZnO, and may further include La2O3、Pr6O11、Al2O3、Na2O、TiO2、ZrO2. Wherein the prepared MSBCZ glass powder is weak devitrification glass and is mixed with Al2O3Or the AlN ceramic powder has the functions of sintering assistance, cooling and strength increasing in the process of preparing the high-strength low-loss LTCC material. Specifically, the MSBCZ glass powder comprises 10-20% of MgO and 40-50% of SiO in percentage by mass respectively215 to 30 percent of BaO, 15 to 20 percent of CaO, 5 to 15 percent of ZnO and 0 to 5 percent of La2O30 to 2% of Pr6O110 to 5% of Al2O30 to 2% of Na2O, 0-2% TiO20 to 2% of ZrO2。
The invention discloses a preparation method of a high-strength low-loss LTCC material, which comprises the following steps:
s1: preparing MSBCZ glass powder: respectively weighing the raw materials of the MSBCZ glass powder according to the proportion, and sequentially mixing, smelting, water quenching, grinding, drying and sieving;
s2: preparing a high-strength low-loss LTCC material: weighing 40-60% of ceramic powder and 40-60% of MSBCZ glass powder according to mass percentage, mixing, drying, performing compression molding on the dried powder, and sintering to obtain the high-strength low-loss LTCC material.
The following method for preparing the high strength low loss LTCC material of the present invention is further illustrated with reference to the following specific examples.
Example one
S1, preparing MSBCZ glass powder: weighing 13.70 percent of MgO and 40.00 percent of SiO according to the mass percentage2、19.60％BaO、16.80％CaO、7.20％ZnO、1.62％La2O3、0.15％Pr6O11、0.18％Al2O3、0.25％Na2O、0.25％TiO2、0.25％ZrO2Then, after dry-type mixing, smelting at 1300 ℃, preserving heat for 2 hours, then quickly pouring the smelted glass liquid into deionized water, finally adding the water-quenched glass slag, the deionized water and grinding balls into a grinding tank, grinding in a planetary ball mill, drying and sieving;
s2, preparing a high-strength low-loss LTCC material: weighing 40 percent of Al according to mass percentage2O3Ceramic powder and 60% of MSBCZ glass powder are mixed and dried, the dried powder is pressed and molded, then sintered at 850 ℃ and kept warm for 2 hours, and the high-strength low-loss LTCC material is obtained, the properties of the LTCC material are shown in table 1, a Scanning Electron Microscope (SEM) photo of the section of a sintered sample is shown in figure 1, and the LTCC material is obtained from the figure1, the sintered LTCC material has good compactness and no pores, and is a basic microstructure with high strength and high stability.
Example two
S1, preparing MSBCZ glass powder: weighing 13.70 percent of MgO and 42.00 percent of SiO according to weight percentage2、17.60％BaO、16.80％CaO、7.20％ZnO、1.82％La2O3、0.15％Pr6O11、0.18％Al2O3、0.15％Na2O、0.20％TiO2、0.20％ZrO2Then, after dry-type mixing, smelting at 1350 ℃, preserving heat for 2 hours, then quickly pouring the smelted glass liquid into deionized water, finally adding the water-quenched glass slag, the deionized water and grinding balls into a grinding tank, grinding in a planetary ball mill, drying and sieving;
s2, preparing a high-strength low-loss LTCC material: weighing 60 percent of Al according to mass percentage2O3Ceramic powder and 40% of MSBCZ glass powder are mixed and dried, the dried powder is pressed and molded, and then sintered at 900 ℃ and kept warm for 1h, so that the high-strength low-loss LTCC material is obtained, and the properties of the LTCC material are shown in Table 1.
EXAMPLE III
S1, preparing MSBCZ glass powder: weighing 14.70 percent of MgO and 41.00 percent of SiO according to weight percentage2、18.60％BaO、15.80％CaO、7.20％ZnO、1.62％La2O3、0.15％Pr6O11、0.18％Al2O3、0.25％Na2O、0.25％TiO2、0.25％ZrO2Then, after dry-type mixing, smelting at 1350 ℃, preserving heat for 2 hours, then quickly pouring the smelted glass liquid into deionized water, finally adding the water-quenched glass slag, the deionized water and grinding balls into a grinding tank, grinding in a planetary ball mill, drying and sieving;
s2, preparing a high-strength low-loss LTCC material: weighing 48% of AlN ceramic powder and 52% of MSBCZ glass powder according to the mass percentage, mixing, drying, pressing and molding the dried powder, sintering at 880 ℃, and preserving heat for 1.5 hours to obtain the high-strength low-loss LTCC material, wherein the properties are shown in Table 1.
Example four
S1, preparing MSBCZ glass powder: weighing 13.70 percent of MgO and 45.00 percent of SiO according to weight percentage2、16.60％BaO、15.80％CaO、6.20％ZnO、1.62％La2O3、0.15％Pr6O11、0.18％Al2O3、0.25％Na2O、0.25％TiO2、0.25％ZrO2Then, after dry-type mixing, smelting at 1400 ℃, preserving heat for 2 hours, then quickly pouring the smelted glass liquid into deionized water, finally adding the water-quenched glass slag, the deionized water and grinding balls into a grinding tank, grinding in a planetary ball mill, drying and sieving;
s2, preparing a high-strength low-loss LTCC material: weighing 55% of AlN ceramic powder and 45% of MSBCZ glass powder according to the mass percentage, mixing, drying, pressing and molding the dried powder, sintering at 900 ℃ and preserving heat for 1h to obtain the high-strength low-loss LTCC material, wherein the properties are shown in Table 1.
TABLE 1 Properties of sintered samples in examples
As can be seen from Table 1, the LTCC material prepared by the embodiments of the invention has the dielectric constant of 6.5-8.5 (12GHz), the dielectric loss of less than 0.0012(12GHz), the strength of more than 380MPa, and can be matched and co-fired with silver below 900 ℃, and can be applied as microwave components such as LTCC substrates, filters, couplers and the like.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention, and all the properties or uses are considered to be within the scope of the invention.
Claims (5)
1. The high-strength low-loss LTCC material is characterized by being prepared from the following components in percentage by mass: 40% -60% of ceramic powder and 40% -60% of MSBCZ glass powder, wherein the MSBCZ glass powder comprises the following components in percentage by mass: MgO 10-20 wt% and SiO240 to 50 percent of BaO, 15 to 30 percent of CaO, 5 to 15 percent of ZnO, and La2O30 to 5% of Pr6O110 to 2% of Al2O30 to 5% of Na20 to 2% of O and TiO20 to 2% of ZrO20-2% of the ceramic powder, and the ceramic powder is Al2O3Or AlN.
2. A preparation method of a high-strength low-loss LTCC material is characterized by comprising the following steps:
s1: the method comprises the following steps of sequentially mixing, smelting, water quenching, grinding, drying and sieving raw materials of the MSBCZ glass powder, wherein the MSBCZ glass powder comprises the following components in percentage by mass: MgO 10-20 wt% and SiO240 to 50 percent of BaO, 15 to 30 percent of CaO, 5 to 15 percent of ZnO, and La2O30 to 5% of Pr6O110 to 2% of Al2O30 to 5% of Na20 to 2% of O and TiO20 to 2% of ZrO20 to 2 percent;
s2: weighing 40-60% of ceramic powder and 40-60% of MSBCZ glass powder according to mass percentage, mixing, drying, performing compression molding on the dried powder, and sintering to obtain the high-strength low-loss LTCC material, wherein the ceramic powder is Al2O3Or AlN.
3. The method according to claim 2, wherein step S1 specifically includes: the MSBCZ glass powder is prepared by uniformly mixing raw materials in a dry mode, smelting at 1300-1400 ℃, preserving heat for 2 hours, pouring smelted glass liquid into deionized water for water quenching, adding water quenched glass slag, deionized water and grinding balls into a grinding tank for grinding, drying and sieving.
4. The method according to claim 2, wherein step S2 specifically includes: adding 40-60% of ceramic powder, 40-60% of MSBCZ glass powder, deionized water, a dispersing agent and grinding balls into a grinding tank, mixing, grinding, drying, pressing and molding the dried powder, sintering at 850-900 ℃, and preserving heat for 1-2 hours to obtain the high-strength low-loss LTCC material.
5. A high strength low loss LTCC material, produced by the process according to any of claims 2 to 4.
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| CN110436894B (en) * | 2019-06-27 | 2022-10-21 | 深圳顺络电子股份有限公司 | Low-dielectric-constant LTCC material and preparation method thereof |
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| CN115594405B (en) * | 2022-09-28 | 2023-12-26 | 深圳顺络电子股份有限公司 | Low-dielectric high-temperature stability LTCC material and preparation method thereof |
| CN115572049B (en) * | 2022-10-14 | 2024-03-12 | 中国建筑材料科学研究总院有限公司 | Glass water quenching device and preparation method of LTCC glass powder |
| CN116023128B (en) * | 2022-12-15 | 2024-06-21 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-temperature sintered low-dielectric low-loss microwave dielectric ceramic and preparation method thereof |
| CN115849876B (en) * | 2022-12-28 | 2023-11-24 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-temperature sintered medium-low dielectric low-loss microwave dielectric ceramic and preparation method thereof |
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