CN109721340A - A kind of high intensity low-loss LTCC material and preparation method thereof - Google Patents
A kind of high intensity low-loss LTCC material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000011521 glass Substances 0.000 claims abstract description 74
- 239000000843 powder Substances 0.000 claims abstract description 73
- 239000000919 ceramic Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002844 melting Methods 0.000 claims abstract description 17
- 230000008018 melting Effects 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000010791 quenching Methods 0.000 claims abstract description 12
- 230000000171 quenching effect Effects 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 10
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 229910052593 corundum Inorganic materials 0.000 claims description 18
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 12
- 229910002637 Pr6O11 Inorganic materials 0.000 claims description 12
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 12
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 7
- -1 melting Substances 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002241 glass-ceramic Substances 0.000 description 3
- 238000010344 co-firing Methods 0.000 description 2
- 238000013461 design Methods 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
- 238000010408 sweeping Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a kind of high-intensitive low-loss LTCC materials, are prepared by each component of following mass percent: 40%~60% ceramic powder and 40%~60% MSBCZ glass powder, wherein MSBCZ glass powder includes at least following components: MgO, SiO2, BaO, CaO and ZnO.The invention also discloses a kind of preparation methods of high-intensitive low-loss LTCC material, comprising: is successively mixed the raw material of MSBCZ glass powder, melting, water quenching, grinding, drying sieving, wherein the raw material of MSBCZ glass powder includes at least MgO, SiO2, BaO, CaO and ZnO；40%~60% ceramic powder and 40%~60% MSBCZ glass powder are weighed according to mass percent, then mixes, dry, and resulting powder will be dried and be pressed, be then sintered, obtain high-intensitive low-loss LTCC material.High intensity low-loss LTCC material proposed by the present invention and preparation method thereof, meets low dielectric, low-loss, the requirement of high intensity, sintering temperature and low.
Description
Technical field
The present invention relates to electron ceramic material technical field more particularly to a kind of high-intensitive low-loss LTCC material and its systems
Preparation Method.
Background technique
LTCC Technology (Low temperature cofired ceramic, LTCC) is a kind of advanced nothing
Source integrated technology is the preferred manner of future electronic component integration.Both at home and abroad to LTCC material carried out it is extensive exploration and
Research, mainly there is glass ceramics system (devitrified glass), glass/ceramic system, crystallization ceramics system (pure ceramics) three major controls at present.
Low Jie LTCC (ε < 10) material mainly has two class of glass ceramics system and glass/ceramic system, wherein glass ceramics system
It is successively to be precipitated crystal by glass preparation and glass heat treatment process, eventually becomes polycrystalline ceramics, have ceramics
The features such as temperature is low, crystallite dielectric loss is small, high mechanical strength；If glass/ceramic owner (helps burning using glass low melting point
Agent), low-k the features such as and the good physical property of ceramics, the certain ceramics of blending are by the two low-temperature sintering in glass
It is combined together (glass is broadly divided into crystal form glass and armorphous glass), but intensity is generally not high (general to be no more than
250Mpa)。
The disclosure of background above technology contents is only used for auxiliary and understands design and technical solution of the invention, not necessarily
The prior art for belonging to present patent application, no tangible proof show above content present patent application the applying date
In disclosed situation, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
In order to solve the above technical problems, the present invention proposes a kind of high-intensitive low-loss LTCC material and preparation method thereof, it is full
The low dielectric of foot, low-loss, the requirement of high intensity, sintering temperature and low.
In order to achieve the above object, the invention adopts the following technical scheme:
The invention discloses a kind of high-intensitive low-loss LTCC materials, by each component preparation of following mass percent
At 40%~60% ceramic powder and 40%~60% MSBCZ glass powder, wherein the MSBCZ glass powder include at least with
Lower component: MgO, SiO2, BaO, CaO and ZnO.
Preferably, the MSBCZ glass powder further includes La2O3、Pr6O11、Al2O3、Na2O、TiO2、ZrO2In at least one
Kind.
Preferably, it is 10%~20%, SiO that the mass percent of each component, which is respectively as follows: MgO, in the MSBCZ glass powder2
For 40%~50%, BaO be 15%~30%, CaO is 15%~20%, ZnO is 5%~15%, La2O3For 0~5%,
Pr6O11For 0~2%, Al2O3For 0~5%, Na2O is 0~2%, TiO2For 0~2%, ZrO2It is 0~2%.
Preferably, the ceramic powder is Al2O3Or AlN.
The invention discloses a kind of preparation methods of high-intensitive low-loss LTCC material, comprising the following steps:
S1: the raw material of MSBCZ glass powder is successively mixed, melting, water quenching, grinding, drying sieving, wherein described
The raw material of MSBCZ glass powder includes at least MgO, SiO2, BaO, CaO and ZnO；
S2: weighing 40%~60% ceramic powder and 40%~60% MSBCZ glass powder according to mass percent,
Then it mixes, dry, and resulting powder will be dried and be pressed, be then sintered, obtain high-intensitive low-loss LTCC material
Material.
Preferably, the raw material of MSBCZ glass powder described in step S1 includes that mass percent is respectively as follows: 10%~20%
MgO, 40%~50% SiO2, 15%~30% BaO, 15%~20% CaO, 5%~15% ZnO, 0~5%
La2O3, 0~2% Pr6O11, 0~5% Al2O3, 0~2% Na2O, 0~2% TiO2, 0~2% ZrO2。
Preferably, specifically included in step S1: by the raw material of MSBCZ glass powder it is dry mixed uniformly after, at 1300 DEG C
Melting is carried out at~1400 DEG C, and keeps the temperature 2h, then the glass metal after melting is poured into and carries out water quenching in deionized water, then by water
Glass dregs, deionized water, mill ball after quenching, which are added in grinding pot, carries out levigate grinding, and dries sieving.
Preferably, ceramic powder described in step S2 is Al2O3Or AlN.
Preferably, step S2 is specifically included: will be according to the ceramic powder and 40% of mass percent weighed 40%~60%
~60% MSBCZ glass powder and deionized water, dispersing agent, mill ball is added in grinding pot, carries out mixed grinding, and
Drying, and will dry after resulting powder is pressed, it is sintered and is kept the temperature 1~2h at 850 DEG C~900 DEG C, obtains height
Intensity low-loss LTCC material.
Invention additionally discloses a kind of high-intensitive low-loss LTCC materials, are made according to above-mentioned preparation method.
Compared with prior art, the beneficial effects of the present invention are high intensity low-loss LTCC materials disclosed by the invention
By ceramic powder and sintering aid MgO-SiO2- BaO-CaO-ZnO (MSBCZ) glass powder is prepared, and finally obtained high intensity is low
The dielectric constant of LTCC material is lost between 6.5~8.5 (12GHz), dielectric loss < 0.0012 (12GHz), intensity >
380MPa, and can be used as the microwave devices such as ltcc substrate, filter, coupler with silver in 900 DEG C or less matching co-firings and answer
With.
Further, by the design of glass powder component, a kind of MSBCZ glass of faint crystallization is obtained, compares non-crystallization
The intensity of type glass, MSBCZ glass is higher, relatively pure crystallized glass, and the sintering of MSBCZ glass and influence to dielectric constant are more
It is easy to control；Wherein for ceramic phase compared with the identical or close glass phase of ingredient, the former intensity is generally relatively high, because ceramic
Mutually be crystal, ion arrangement is finer and close, and corresponding intensity is high, and glass is loose network structure, interionic binding force compared with
Weak, corresponding intensity is lower, therefore is matched by ceramics, mutually adjusting for two matched of glass, it can be achieved that 900 DEG C in the present invention
Following densified sintering product will not pollute the environment while faint crystallization type MSBCZ glass helps burning, help to reduce
The dielectric constant of material, the intensity for improving material.
Detailed description of the invention
Fig. 1 is micro- (SEM) photo of surface sweeping Electronic Speculum of one sintered sample section of the embodiment of the present invention.
Specific embodiment
Below against attached drawing and in conjunction with preferred embodiment, the invention will be further described.
A preferred embodiment of the present invention discloses a kind of high-intensitive low-loss LTCC material, by following mass percent
Each component be prepared: 40%~60% ceramic powder and 40%~60% MSBCZ glass powder, wherein ceramic powder be Al2O3
Or AlN；MSBCZ glass powder includes MgO, SiO2, BaO, CaO and ZnO, and may also include La2O3、Pr6O11、Al2O3、Na2O、
TiO2、ZrO2.Wherein manufactured MSBCZ glass powder be faint crystallization type glass, with Al2O3Or AlN ceramic powder meets preparation height
In intensity low-loss LTCC materials process, plays the role of helping burning cooling, increases intensity.Specifically, MSBCZ glass powder includes matter
Measuring percentage is respectively 10%~20% MgO, 40%~50% SiO2, 15%~30% BaO, 15%~20%
CaO, 5%~15% ZnO, 0~5% La2O3, 0~2% Pr6O11, 0~5% Al2O3, 0~2% Na20 O ,~
2% TiO2, 0~2% ZrO2。
Another preferred embodiment of the invention discloses a kind of preparation method of high-intensitive low-loss LTCC material, including
Following steps:
The preparation of S1:MSBCZ glass powder: it weighs the raw material of MSBCZ glass powder respectively according to aforementioned ratio, is successively mixed
Conjunction, melting, water quenching, grinding, drying sieving；
S2: the preparation of high-intensitive low-loss LTCC material: according to mass percent weigh 40%~60% ceramic powder and
Then 40%~60% MSBCZ glass powder is mixed, is dried, and will dry resulting powder and be pressed, then
Sintering, obtains high-intensitive low-loss LTCC material.
It is following that the preparation method of high-intensitive low-loss LTCC material of the invention is carried out further in conjunction with specific embodiments
Explanation.
Embodiment one
The preparation of S1, MSBCZ glass powder: 13.70%MgO, 40.00%SiO are weighed by 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%ZrO2, then it is dry mixed uniformly after, in 1300 DEG C of progress meltings, and keep the temperature 2h, then will be after melting
Glass metal is quickly poured into deionized water, and finally glass dregs, deionized water, the mill ball after water quenching are added in grinding pot, set
It is ground in planetary ball mill, and dries sieving；
The preparation of S2, high-intensitive low-loss LTCC material: 40% Al is weighed by mass percentage2O3Ceramic powder, 60%
Then MSBCZ glass powder is mixed, is dried, then by after the repressed molding of the powder of drying, 2h is sintered and kept the temperature at 850 DEG C, i.e.,
High-intensitive low-loss LTCC material is obtained, performance is as shown in table 1, and micro- (SEM) photo of the surface sweeping Electronic Speculum of sintered sample section is such as
Shown in Fig. 1, from figure 1 it appears that the compactness for the LTCC material that sintering obtains is good, it is that high-intensitive and height is steady without hole
Qualitatively basis microstructure.
Embodiment two
The preparation of S1, MSBCZ glass powder: 13.70%MgO, 42.00%SiO are weighed by 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%ZrO2, then it is dry mixed uniformly after, in 1350 DEG C of progress meltings, and keep the temperature 2h, then will be after melting
Glass metal is quickly poured into deionized water, and finally glass dregs, deionized water, the mill ball after water quenching are added in grinding pot, set
It is ground in planetary ball mill, and dries sieving；
The preparation of S2, high-intensitive low-loss LTCC material: 60% Al is weighed by mass percentage2O3Ceramic powder, 40%
Then MSBCZ glass powder is mixed, is dried, then by after the repressed molding of the powder of drying, 1h is sintered and kept the temperature at 900 DEG C, i.e.,
High-intensitive low-loss LTCC material is obtained, performance is as shown in table 1.
Embodiment three
The preparation of S1, MSBCZ glass powder: 14.70%MgO, 41.00%SiO are weighed by 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%ZrO2, then it is dry mixed uniformly after, in 1350 DEG C of progress meltings, and keep the temperature 2h, then will be after melting
Glass metal is quickly poured into deionized water, and finally glass dregs, deionized water, the mill ball after water quenching are added in grinding pot, set
It is ground in planetary ball mill, and dries sieving；
The preparation of S2, high-intensitive low-loss LTCC material: weigh by mass percentage 48% AlN ceramic powder, 52%
Then MSBCZ glass powder is mixed, is dried, then by after the repressed molding of the powder of drying, 1.5h is sintered and kept the temperature at 880 DEG C,
High-intensitive low-loss LTCC material is obtained, performance is as shown in table 1.
Example IV
The preparation of S1, MSBCZ glass powder: 13.70%MgO, 45.00%SiO are weighed by 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%ZrO2, then it is dry mixed uniformly after, in 1400 DEG C of progress meltings, and keep the temperature 2h, then will be after melting
Glass metal is quickly poured into deionized water, and finally glass dregs, deionized water, the mill ball after water quenching are added in grinding pot, set
It is ground in planetary ball mill, and dries sieving；
The preparation of S2, high-intensitive low-loss LTCC material: weigh by mass percentage 55% AlN ceramic powder, 45%
Then MSBCZ glass powder is mixed, is dried, then by after the repressed molding of the powder of drying, 1h is sintered and kept the temperature at 900 DEG C, i.e.,
High-intensitive low-loss LTCC material is obtained, performance is as shown in table 1.
The performance of sintered sample in each embodiment of table 1
From table 1 it follows that the dielectric constant for the LTCC material that various embodiments of the present invention are prepared is 6.5~8.5
Between (12GHz), dielectric loss < 0.0012 (12GHz), intensity > 380MPa, and can with silver in 900 DEG C or less matching co-firings,
It can be used as the microwave devices application such as ltcc substrate, filter, coupler.
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 high intensity low-loss LTCC material, which is characterized in that be prepared by each component of following mass percent:
40%~60% ceramic powder and 40%~60% MSBCZ glass powder, wherein the MSBCZ glass powder include at least with the following group
Point: MgO, SiO2, BaO, CaO and ZnO.
2. high intensity low-loss LTCC material according to claim 1, which is characterized in that the MSBCZ glass powder also wraps
Include La2O3、Pr6O11、Al2O3、Na2O、TiO2、ZrO2At least one of.
3. high intensity low-loss LTCC material according to claim 1, which is characterized in that each in the MSBCZ glass powder
It is 10%~20%, SiO that the mass percent of component, which is respectively as follows: MgO,2For 40%~50%, BaO be 15%~30%, CaO is
15%~20%, ZnO is 5%~15%, La2O3For 0~5%, Pr6O11For 0~2%, Al2O3For 0~5%, Na2O be 0~
2%, TiO2For 0~2%, ZrO2It is 0~2%.
4. high intensity low-loss LTCC material according to claim 1, which is characterized in that the ceramic powder is Al2O3Or
AlN。
5. a kind of preparation method of high intensity low-loss LTCC material, which comprises the following steps:
S1: the raw material of MSBCZ glass powder is successively mixed, melting, water quenching, grinding, drying sieving, wherein the MSBCZ
The raw material of glass powder includes at least MgO, SiO2, BaO, CaO and ZnO；
S2: 40%~60% ceramic powder and 40%~60% MSBCZ glass powder are weighed according to mass percent, then
Mixing, drying, and resulting powder will be dried and be pressed, it is then sintered, obtains high-intensitive low-loss LTCC material.
6. preparation method according to claim 5, which is characterized in that the raw material packet of MSBCZ glass powder described in step S1
It includes mass percent and is respectively as follows: 10%~20% MgO, 40%~50% SiO2, 15%~30% BaO, 15%~
20% CaO, 5%~15% ZnO, 0~5% La2O3, 0~2% Pr6O11, 0~5% Al2O3, 0~2%
Na2O, 0~2% TiO2, 0~2% ZrO2。
7. preparation method according to claim 5, which is characterized in that specifically included in step S1: by MSBCZ glass powder
Raw material it is dry mixed uniformly after, melting is carried out at 1300 DEG C~1400 DEG C, and keep the temperature 2h, then by the glass metal after melting
Pour into and carry out water quenching in deionized water, then by after water quenching glass dregs, deionized water, mill ball be added grinding pot in carry out it is levigate
Grinding, and dry sieving.
8. preparation method according to claim 5, which is characterized in that ceramic powder described in step S2 is Al2O3Or AlN.
9. preparation method according to claim 5, which is characterized in that step S2 is specifically included: will be according to mass percent
Weighed 40%~60% ceramic powder and 40%~60% the MSBCZ glass powder and deionized water, dispersing agent, mill ball
Be added in grinding pot, carry out mixed grinding, and dry, and will dry after resulting powder is pressed, 850 DEG C~
1~2h is sintered and kept the temperature at 900 DEG C, obtains high-intensitive low-loss LTCC material.
10. a kind of high intensity low-loss LTCC material, which is characterized in that be according to the described in any item preparations of claim 5 to 9
Method is made.
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| CN110357590A (en) * | 2019-07-18 | 2019-10-22 | 成都宏科电子科技有限公司 | Devitrified glass and high-flexural strength low-temperature co-burning ceramic material and preparation method thereof |
| CN110436894A (en) * | 2019-06-27 | 2019-11-12 | 深圳顺络电子股份有限公司 | A kind of low-k LTCC material and preparation method thereof |
| 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 |
| CN111499187A (en) * | 2020-04-28 | 2020-08-07 | 山东国瓷功能材料股份有限公司 | Glass material with low loss and low piezoelectric coefficient d33 in 20-60GHz high-frequency band |
| CN115572049A (en) * | 2022-10-14 | 2023-01-06 | 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 |
| CN115594405A (en) * | 2022-09-28 | 2023-01-13 | 深圳顺络电子股份有限公司（Cn） | Low-dielectric high-temperature-stability LTCC material and preparation method thereof |
| CN115849876A (en) * | 2022-12-28 | 2023-03-28 | 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 |
| CN116023128A (en) * | 2022-12-15 | 2023-04-28 | 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 |
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