CN110436894A - A kind of low-k LTCC material and preparation method thereof - Google Patents

A kind of low-k LTCC material and preparation method thereof Download PDF

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CN110436894A
CN110436894A CN201910570612.7A CN201910570612A CN110436894A CN 110436894 A CN110436894 A CN 110436894A CN 201910570612 A CN201910570612 A CN 201910570612A CN 110436894 A CN110436894 A CN 110436894A
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洪国志
聂敏
刘剑
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Shenzhen Shunluo Layered Electronics Co ltd
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Shenzhen Sunlord Electronics Co Ltd
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Abstract

The present invention provides a kind of low-k LTCC material and preparation method thereof, and the low-k LTCC material is prepared after weighing according to the mass percent of following each component: 35%~60% nanometer scale ceramics powder and 40%~65% barium glass powder;Wherein the barium glass powder includes each component of following mass percent: 12%~15% B2O3, 48%~50% SiO2, 7%~15% BaO, 13%~15% CaO, 2%~7% TiO2With 8%~13% SrO.Low-k LTCC material of the invention has the advantages that low-k, low-dielectric loss, high-flexural strength and sintering temperature and low simultaneously, can be used as the microwave devices application such as ltcc substrate, filter, antenna, coupler.

Description

A kind of low-k LTCC material and preparation method thereof
Technical field
The present invention relates to electron ceramic material technology and its manufacturing field more particularly to a kind of low-k LTCC materials Material and preparation method thereof.
Background technique
In recent years, LTCC Technology (Low temperature cofired ceramic, LTCC) is a kind of elder generation Into 3 D stereo assemble integrated technology, be the preferred manner of future electronic component integration.
Low-temperature sintered ceramics material is the most important branch in LTCC Material Field, and main application is in various LTCC bases In plate and integrated device, and dielectric constant has more application and research from 10~100 according to demand, but with microwave communication techniques Raising with the development of radar system, the high frequency and transmission rate of microwave communication frequency promotes the novel of low-k The research and development of LTCC material.
Summary of the invention
The present invention proposes a kind of low-k LTCC material and preparation method thereof, has low-k, low simultaneously The advantages of dielectric loss, high-flexural strength and sintering temperature and low.
In order to achieve the above object, the invention adopts the following technical scheme:
A kind of low-k LTCC material is prepared: 35% after weighing according to the mass percent of following each component ~60% nanometer scale ceramics powder and 40%~65% barium glass powder;Wherein the barium glass powder includes following mass percent Each component: 12%~15% B2O3, 48%~50% SiO2, 7%~15% BaO, 13%~15% CaO, 2% ~7% TiO2With 8%~13% SrO.
It preferably, further include at least one of each component of following mass percent: 0 < K in the barium glass powder2O ≤ 7%, 0 < ZrO2≤ 2%, 0 < Na2O≤2%, 0 < MgO≤2%.
Preferably, the partial size of the nanometer scale ceramics powder is between 100nm~150nm.
Preferably, the nanometer scale ceramics powder is nanometer Al2O3Or Nano-meter SiO_22
A kind of preparation method of the low-k LTCC material, comprising the following steps:
S1: weighing each component is calculated by the mass percent of each component in the barium glass powder, successively mixed, melted Refining, quenching, grinding, drying sieving;
S2: 35%~60% nanometer scale ceramics powder is weighed according to mass percent and is prepared by 40%~65% step S1 Then the obtained barium glass powder is mixed, is dried, and will dry resulting granulation for powders, compression moulding, then sintering obtains Low-k LTCC material.
Preferably, the dry type that is mixed into the step S1 uniformly mixes.
Preferably, the melting in the step S1 is to carry out at 1100 DEG C~1300 DEG C, and keep the temperature 1~3h.
Preferably, the quenching in the step S1 specifically: the glass metal after melting is poured into 20~35 DEG C of deionization Quenching is carried out in water.
Preferably, the grinding in the step S1 and drying sieving specifically: by after quenching glass, deionized water and grind Abrading-ball is added in grinding pot and carries out levigate grinding, and dries 30 mesh or 60 meshes.
Preferably, the step S2 is specifically included: will be made pottery according to the nanoscale of mass percent weighed 35%~60% Porcelain powder and 40%~65% the barium glass powder and deionized water, mill ball be added in grinding pot, carry out mixed grinding extremely 0.5~0.6 μm of partial size, and dry, and resulting powder will be dried and be granulated, after compression moulding, at 830 DEG C~880 DEG C It is sintered and is kept the temperature 0.5~1h, obtains low-k LTCC material.
Compared with prior art, the beneficial effect comprise that material of the invention using nanoscale ceramic powder and Barium glass powder is prepared, it includes with the barium glass powder being specifically formulated have good stability, sintering when glass Glass softening, viscosity decline, reduces the sintering temperature of material, using mass transfer in liquid phase by adjusting nanometer scale ceramics powder and barium glass The ratio of powder, the dielectric constant of finally obtained low-k LTCC material is between 6~10 (11GHz), dielectric loss < 0.0020 (11GHz), bending strength are greater than 130MPa, and sintering temperature is low, can be used as with silver in 900 DEG C or less matching co-firings The microwave devices application such as ltcc substrate, filter, antenna, coupler.
Detailed description of the invention
Fig. 1 is the XRD comparison diagram of the barium glass powder heat treatment front and back of the embodiment of the present invention one.
Fig. 2 is micro- (SEM) photo of surface sweeping Electronic Speculum of the sintered sample section of the embodiment of the present invention one.
Fig. 3 is micro- (SEM) photo of surface sweeping Electronic Speculum of the sintered sample section of comparative example one of the present invention.
Specific embodiment:
Below against attached drawing and in conjunction with preferred embodiment, the invention will be further described.
The low-k LTCC material provided in the specific embodiment of the invention by following mass percent each component Be prepared: 35%~60% nanometer scale ceramics powder and 40%~65% barium glass powder, wherein barium glass powder includes following The each component of mass percent: 12%~15% B2O3, 48%~50% SiO2, 7%~15% BaO, 13%~15% CaO, 2%~7% TiO2With 8%~13% SrO.
Wherein, manufactured barium glass powder is weak crystallization type glass, is preparing low-k LTCC with nanometer scale ceramics powder In materials process, plays and help burning cooling effect.
In a preferred embodiment, further include in barium glass powder following mass percent each component at least one Kind: 0 < K2O≤7%, 0 < ZrO2≤ 2%, 0 < Na2O≤2%, 0 < MgO≤2%.
In a preferred embodiment, the partial size of nanometer scale ceramics powder is between 100nm~150nm;More optimizedly, nanometer Grade ceramic powder can be nanometer Al2O3Or Nano-meter SiO_22
Another embodiment of the invention provides a kind of preparation method of above-mentioned low-k LTCC material, The following steps are included:
S1: the preparation of barium glass powder: weighing each raw material of barium glass powder according to aforementioned ratio respectively, successively mixed, Melting, quenching, grinding, drying sieving;
S2: 35%~60% nanometer scale ceramics the preparation of low-k LTCC material: are weighed according to mass percent Powder and 40%~65% the barium glass powder that is prepared of step S1, then mix, dry, and resulting powder will be dried and carried out It is granulated, compression moulding, then sintering obtains low-k LTCC material.
In some preferred embodiments, the dry type that is mixed into step S1 uniformly mixes;Melting be 1100 DEG C~ It is carried out at 1300 DEG C, and keeps the temperature 1~3h;Quenching specifically: pour into the glass metal after melting in 20~35 DEG C of deionized water Carry out quenching;Grinding and drying sieving specifically: glass, deionized water and the mill ball after quenching are added in grinding pot and carry out Levigate grinding, and dried 30 mesh or 60 meshes.
In some preferred embodiments, the step S2 is specifically included: will be according to mass percent weighed 35% ~60% nanometer scale ceramics powder and 40%~65% the barium glass powder and deionized water, mill ball be added to grinding pot In, mixed grinding is carried out, nanometer scale ceramics powder and barium glass powder are combined with each other, it is ground to 0.5~0.6 μm of partial size, and dry, And resulting powder will be dried and be granulated, after compression moulding, it is sintered and is kept the temperature 0.5~1h at 830 DEG C~880 DEG C, is obtained Low-k LTCC material.
Below by way of some specific embodiments and comparative example to low-k LTCC material of the invention and its preparation Method is further described.
Embodiment one
The preparation of S1, barium glass powder: 13.7%B is weighed by mass percentage2O3, 48.00%SiO2, 8.20%BaO, 13.00%CaO, 4.20%TiO2, 10.90%SrO, 0.4%K2O, 0.4%ZrO2, 0.4%Na2O, then 0.8%MgO is passed through After dry type mixing is uniform, in 1200 DEG C of progress meltings, and keep the temperature 2h, then by the glass metal after melting be quickly poured into room temperature go from In sub- water, finally glass dregs, deionized water, the mill ball after quenching are added in grinding pot, planetary ball mill is placed in and is ground Mill, and dried 60 meshes.In order to analyze the crystal form of barium glass powder, tested as follows: the barium glass powder that will be obtained after sieving Carry out XRD analysis without Overheating Treatment, obtain curve C1 as shown in Figure 1, and by the barium glass powder obtained after sieving 600~ By XRD analysis after being heat-treated at 700 DEG C, curve C2 as shown in Figure 1 is obtained, can be seen that from heat from XRD curve Without apparent peak before reason, and there is more miscellaneous peak after Overheating Treatment, wherein having peak weak at one is CaSiO3, thus illustrate The barium glass powder arrived is weak crystallization type glass, is prepared in low-k LTCC materials process with nanometer scale ceramics powder, energy It plays and helps burning cooling effect.
The preparation of S2, low-k LTCC material: 45% partial size is weighed by mass percentage in 100nm~150nm Between Al2O3Ceramic powder and 55% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μ of partial size M, drying, then by the powder of drying through being granulated, after compression moulding, 0.5h is sintered and kept the temperature at 860 DEG C, obtains low-k LTCC material, performance is as shown in table 1, and micro- (SEM) photo of the surface sweeping Electronic Speculum of sintered sample section is as shown in Fig. 2, can from Fig. 2 To find out, the compactness for the LTCC material being sintered is preferable.
Embodiment two
The preparation of S1, barium glass powder: 13.7%B is weighed by mass percentage2O3, 50.00%SiO2, 6.20%BaO, 13.00%CaO, 4.20%TiO2, 10.90%SrO, 0.4%K2O, 0.4%ZrO2, 0.4%Na2O, then 0.8%MgO is passed through After dry type mixing is uniform, in 1250 DEG C of progress meltings, and keep the temperature 2h, then by the glass metal after melting be quickly poured into room temperature go from In sub- water, finally glass dregs, deionized water, the mill ball after quenching are added in grinding pot, planetary ball mill is placed in and is ground Mill, and dried 30 meshes;
The preparation of S2, low-k LTCC material: the partial size for weighing 50% by mass percentage is 100nm~150nm Al2O3Ceramic powder and 50% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, Drying, then by the powder of drying through being granulated, after compression moulding, 1h is sintered and kept the temperature at 880 DEG C, obtains low-k LTCC Material, performance are as shown in table 1.
Embodiment three
The preparation of S1, barium glass powder: 13.7%B is weighed by mass percentage2O3, 49.00%SiO2, 7.20%BaO, 13.00%CaO, 5.20%TiO2, 9.90%SrO, 0.4%K2O, 0.4%ZrO2, 0.4%Na2O, 0.8%MgO, then through dry Formula after mixing, in 1250 DEG C of progress meltings, and keeps the temperature 2h, the glass metal after melting is then quickly poured into room temperature deionization In water, finally glass dregs, deionized water, the mill ball after quenching are added in grinding pot, planetary ball mill is placed in and is ground, And dried 60 meshes;
The preparation of S2, low-k LTCC material: the partial size for weighing 45% by mass percentage is 100nm~150nm SiO2Ceramic powder and 55% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, Drying, then by the powder of drying through being granulated, after compression moulding, 0.5h is sintered and kept the temperature at 860 DEG C, obtains low-k LTCC material, performance are as shown in table 1.
Example IV
The preparation of S1, barium glass powder: 13.7%B is weighed by weight percentage2O3, 50.00%SiO2, 6.20%BaO, 13.00%CaO, 5.20%TiO2, 9.90%SrO, 0.4%K2O, 0.4%ZrO2, 0.4%Na2O, 0.8%MgO, by dry type After mixing, in 1300 DEG C of progress meltings, and 2h is kept the temperature, then the glass metal after melting is quickly poured into deionized water, Finally glass dregs, deionized water, the mill ball after quenching are added in grinding pot, planetary ball mill is placed in and is ground, and dry Did 60 meshes;
The preparation of S2, low-k LTCC material: the partial size for weighing 50% by mass percentage is 100nm~150nm SiO2Ceramic powder and 50% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, Drying, then by the powder of drying through being granulated, after compression moulding, 1h is sintered and kept the temperature at 880 DEG C, obtains low-k LTCC Material, performance are as shown in table 1.
Comparative example one
The preparation of S1, barium glass powder: 13.7%B is weighed by mass percentage2O3, 50.00%SiO2, 6.20%BaO, 13.00%CaO, 4.20%TiO2, 10.90%SrO, 0.4%K2O, 0.4%ZrO2, 0.4%Na2O, 0.8%MgO is then through dry Formula after mixing, in 1300 DEG C of progress meltings, and keeps the temperature 2h, the glass metal after melting is then quickly poured into room temperature deionization In water, finally glass dregs, deionized water, the mill ball after quenching are added in grinding pot, planetary ball mill is placed in and is ground, And dried 60 meshes;
The preparation of S2, low-k LTCC material: the partial size for weighing 70% by mass percentage is 100nm~150nm Al2O3Ceramic powder and 30% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, Drying, then by the powder of drying through being granulated, after compression moulding, 1h is sintered and kept the temperature at 880 DEG C, obtains low-k LTCC Material, performance is as shown in table 2, and micro- (SEM) photo of the scanning electron microscope of sintered sample section is as shown in figure 3, can from Fig. 3 Out, the compactness for the LTCC material being sintered is poor, there is many holes.
Comparative example two
The preparation of S1, barium glass powder: 13.7%B is weighed by mass percentage2O3, 50.00%SiO2, 6.20%BaO, 13.00%CaO, 4.20%TiO2, 10.90%SrO, 0.4%K2O, 0.8%ZrO2, 0.8%MgO then it is dry mixed uniformly Afterwards, in 1300 DEG C of progress meltings, and 2h is kept the temperature, then the glass metal after melting is quickly poured into deionized water at normal temperature, finally Glass dregs, deionized water, mill ball after quenching is added in grinding pot, planetary ball mill is placed in and is ground, and dried 30 meshes;
The preparation of S2, low-k LTCC material: the partial size for weighing 50% by mass percentage is 100nm~150nm Al2O3Ceramic powder and 50% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, Drying, then by the powder of drying through being granulated, after compression moulding, 1h is sintered and kept the temperature at 950 DEG C, obtains low-k LTCC Material, sintering warpage is serious at such a temperature for sample, is unable to test.
Comparative example three
The preparation of S1, barium glass powder: 13.7%B is weighed by mass percentage2O3, 50.00%SiO2, 6.20%BaO, 13.00%CaO, 5.20%TiO2, 9.90%SrO, 0.4%ZrO2, 0.8%Na2O, 0.8%MgO, it is then dry mixed equal After even, in 1300 DEG C of progress meltings, and 2h kept the temperature, then the glass metal after melting is quickly poured into deionized water, finally will Glass dregs, deionized water, mill ball after quenching are added in grinding pot, are placed in planetary ball mill and are ground, and dry sieving;
The preparation of S2, low-k LTCC material: the partial size for weighing 50% by mass percentage is 1 μm~1.5 μm SiO2Ceramic powder and 50% the barium glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, dry It is dry, then by the powder of drying through being granulated, after compression moulding, 1h is sintered and kept the temperature at 880 DEG C, obtain low-k LTCC material Material, performance are as shown in table 2.
Comparative example four
The preparation of S1, glass powder: 13.7%B is weighed by mass percentage2O3, 50.00%SiO2, 7.30%MgO, 13.00%CaO, 5.20%TiO2, 9.90%SrO, 0.4%K2O, 0.4%ZrO2, 0.1%Na2O, it is then dry mixed equal After even, in 1300 DEG C of progress meltings, and 2h kept the temperature, then the glass metal after melting is quickly poured into deionized water, finally will Glass dregs, deionized water, mill ball after quenching are added in grinding pot, are placed in planetary ball mill and are ground, and dry sieving;
The preparation of S2, low-k LTCC material: the partial size for weighing 50% by mass percentage is 1 μm~1.5 μm SiO2Ceramic powder and 50% the glass powder that is prepared of step S1, then mix, be ground to 0.5~0.6 μm of partial size, drying, Again by the powder of drying through being granulated, after compression moulding, 1h is sintered and kept the temperature at 880 DEG C, obtains low-k LTCC material, Performance is as shown in table 2.
The performance of sintered sample in each embodiment of table 1
The performance of sintered sample in each comparative example of table 2
From table 1 it follows that the dielectric constant for the LTCC material that various embodiments of the present invention are prepared is 6~10 Between (11GHz), dielectric loss≤0.0020 (11GHz), bending strength > 130MPa can be matched with silver at 900 DEG C or less altogether It burns, can be used as the microwave devices application such as ltcc substrate, filter, antenna, coupler.
From Table 2, it can be seen that the higher > 0.0040 of the dielectric loss for the LTCC material being prepared in comparative example (11GHz), low strength < 96MPa, and since sintering temperature is excessively high in comparative example two, cause sample to be sintered severely deformed, nothing Method test.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that Specific implementation of the invention is only limited to these instructions.For those skilled in the art to which the present invention belongs, it is not taking off Under the premise of from present inventive concept, several equivalent substitute or obvious modifications can also be made, and performance or use is identical, all answered When being considered as belonging to protection scope of the present invention.

Claims (10)

1. a kind of low-k LTCC material, it is characterised in that: prepared after being weighed according to the mass percent of following each component Form: 35%~60% nanometer scale ceramics powder and 40%~65% barium glass powder;Wherein the barium glass powder includes following The each component of mass percent: 12%~15% B2O3, 48%~50% SiO2, 7%~15% BaO, 13%~15% CaO, 2%~7% TiO2With 8%~13% SrO.
2. low-k LTCC material according to claim 1, which is characterized in that further include in the barium glass powder as At least one of each component of lower mass percent:
0 < K2O≤7%, 0 < ZrO2≤ 2%, 0 < Na2O≤2%, 0 < MgO≤2%.
3. low-k LTCC material according to claim 1 or 2, which is characterized in that the nanometer scale ceramics powder Partial size is between 100nm~150nm.
4. low-k LTCC material according to claim 3, which is characterized in that the nanometer scale ceramics powder is nanometer Al2O3Or Nano-meter SiO_22
5. the preparation method of low-k LTCC material described in a kind of claim 1-4 any one, which is characterized in that packet Include following steps:
S1: weighing each component is calculated by the mass percent of each component in the barium glass powder, successively mixed, melting, quenched Cold, grinding, drying sieving;
S2: 35%~60% nanometer scale ceramics powder is weighed according to mass percent and 40%~65% step S1 is prepared The barium glass powder, then mix, dry, and resulting granulation for powders will be dried, compression moulding, then sintering obtains low Jie Electric constant LTCC material.
6. preparation method according to claim 5, which is characterized in that the dry type that is mixed into the step S1 is uniformly mixed It closes.
7. preparation method according to claim 5, which is characterized in that the melting in the step S1 be 1100 DEG C~ It is carried out at 1300 DEG C, and keeps the temperature 1~3h.
8. preparation method according to claim 5, which is characterized in that the quenching in the step S1 specifically: by melting Glass metal afterwards pours into 20~35 DEG C of deionized water and carries out quenching.
9. preparation method according to claim 5, which is characterized in that the grinding and drying sieving in the step S1 are specific Are as follows: glass, deionized water and the mill ball after quenching are added in grinding pot and carry out levigate grinding, and dried 30 mesh or 60 mesh Sieve.
10. preparation method according to claim 5, which is characterized in that the step S2 is specifically included:
It will be according to the barium glass powder of the nanometer scale ceramics powder of mass percent weighed 35%~60% and 40%~65% It is added in grinding pot with deionized water, mill ball, carries out mixed grinding to 0.5~0.6 μm of partial size, and dry, and will drying Resulting powder is granulated, after compression moulding, is sintered and is kept the temperature 0.5~1h at 830 DEG C~880 DEG C, it is normal to obtain low dielectric Number LTCC material.
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CN111470776A (en) * 2020-04-28 2020-07-31 山东国瓷功能材料股份有限公司 High-frequency low-loss glass ceramic material and preparation method thereof
CN111470776B (en) * 2020-04-28 2022-04-29 山东国瓷功能材料股份有限公司 High-frequency low-loss glass ceramic material and preparation method thereof
CN113979640A (en) * 2021-10-08 2022-01-28 云南银峰新材料有限公司 High-bending-strength low-temperature co-fired ceramic material for microwave substrate and preparation method thereof
CN113979640B (en) * 2021-10-08 2023-03-24 云南银峰新材料有限公司 High-bending-strength low-temperature co-fired ceramic material for microwave substrate and preparation method thereof
CN115557788A (en) * 2022-03-23 2023-01-03 中国科学院上海硅酸盐研究所 BSZT/BBSMZ/flake Al 2 O 3 Low-temperature co-fired material and preparation method thereof
CN115810438A (en) * 2022-11-23 2023-03-17 中国电子科技集团公司第四十三研究所 Silver-plating-capable slurry for low-temperature co-fired ceramic and preparation method thereof
CN116102340A (en) * 2023-01-03 2023-05-12 北京航天微电科技有限公司 Low-temperature co-fired raw ceramic, preparation method and ceramic substrate

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