CN104108929A - Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof - Google Patents
Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- CN104108929A CN104108929A CN201410226448.5A CN201410226448A CN104108929A CN 104108929 A CN104108929 A CN 104108929A CN 201410226448 A CN201410226448 A CN 201410226448A CN 104108929 A CN104108929 A CN 104108929A
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Abstract
The invention discloses a low-temperature sintered composite microwave dielectric ceramic material and a preparation method thereof, and relates to the electronic material technology. 89.95-96.85wt% of BaO-nZnO-4TiO2 and 3.15-10.05wt% of an ablation-reduction agent undergo a traditional solid phase reaction to produce the low-temperature sintered composite microwave dielectric ceramic material, wherein n is greater than or equal to 0.3 and is less than or equal to 0.6. The microwave dielectric ceramic material has a sintering temperature less than or equal to 900 DEG C, dielectric constant of 20-30, Qxf(GHz) of 10000-15000 and a resonant frequency temperature coefficient of -10 to +10ppm/DEG C. The low-temperature sintered composite microwave dielectric ceramic material can be used for manufacture of microwave devices such as a low-temperature co-fired ceramic system, a multilayer dielectric resonator, a microwave antenna and a filter.
Description
Technical field
The invention belongs to electronic ceramics and manufacture field thereof, relate to a kind of composite microwave medium ceramic material, especially a kind of low-temperature sintering composite microwave medium ceramic material and preparation method thereof.
Background technology
Microwave-medium ceramics refers to and is applied in microwave (300MHz is to 300GHz) band circuitry as dielectric material and completes the pottery of one or more functions, be the key foundation material in modern communication technology, be widely used in the microwave devices such as dielectric resonator, wave filter, dielectric substrate, Medium Wave Guide loop, microwave capacitors, duplexer, antenna.
Be applied to the media ceramic of microwave frequency band, should meet following requirement: (1) suitable specific inductivity is beneficial to miniaturization (size of medium components and parts and the DIELECTRIC CONSTANT ε of device
rsquare root be inversely proportional to); (2) high quality factor q to be to reduce the wastage, general requirement Q * f>=3000GHz (wherein f is resonant frequency).; (3) stable approaching zero frequency-temperature coefficient, to guarantee the temperature stability of device; (4) there is good common burning with silver or copper.In recent years along with electronic information technology is constantly to high frequency and digitizing future development, the miniaturization to components and parts, integrated so that modular requirement is also more and more urgent.LTCC LTCC (Low Temperature Co-fired Ceramics), with its excellent electricity, machinery, calorifics and operational characteristic, has become one of major technique of electronic-component module.The researchist of recent domestic has carried out exploring widely and studying to some low fever's system materials.BaO-ZnO-TiO in microwave-medium ceramics
2system has good microwave dielectric property, with adjustable frequency-temperature coefficient, but conventionally all there is high sintering temperature (1200 ℃ of >), can not be directly and the low melting point metal such as Ag, Cu burn altogether, this has limited its application in LTCC field to a great extent.Therefore the sintering temperature that how to reduce microwave dielectric material has become research emphasis, the method of the sintering temperature of the reduction microwave dielectric material conventionally adopting at present has: (1) improves preparation technology as adopted chemical synthesis process preparation, reduce sintering temperature, but the method complex process, fabrication cycle increases; (2) use superfine powder to make raw material, improve powder active, reduce ceramic sintering temperature, but the method cost is high; (3) add low melting point oxide or low melting glass sintering aid, in sintering process, low melting point oxide or glass sintering auxiliary agent form liquid phase, and cooling-down effect is obvious, and technique is simple, is easy to batch production.Therefore for reducing cost of manufacture, mostly adopt the third method to reduce the sintering temperature of microwave dielectric material.
For BaO-ZnO-TiO
2system microwave-medium ceramics, conventionally adopts and adds low melting point oxide, as B
2o
3and V
2o
5, can reduce BaO-ZnO-TiO
2the sintering temperature of system.But the low melting point oxide adding, B
2o
3and V
2o
5in later stage curtain coating process, easily cause slurry viscosity excessive and unstable, do not mate with industrial casting technique, limited its practical application.And low-temperature sintering affects BaO-ZnO-TiO
2the compactness of system microwave-medium ceramics there will be and oozes silver in LTCC technique, common burning that cannot be good with silver.In view of above narration, how to prepare a kind of stable, low temperature sintering, fine and close composite microwave medium ceramic material can be realized the BaO-ZnO-TiO of industrial application
2system microwave-medium ceramics becomes a study hotspot.
Summary of the invention
The object of the invention is to overcome the problem of above-mentioned existence, provide a kind of can low-temperature sintering (≤900 ℃), system is fine and close, has medium specific inductivity (20～30), low-loss (≤10
-4), Qxf (GHz): 10000～15000, stable nearly zero-10～+ 10ppm/ ℃ of frequency-temperature coefficient, and can in LTCC technique, well burn altogether with silver, be easy to composite microwave medium ceramic material of suitability for industrialized production and preparation method thereof.
The raw material of this stupalith consists of the BaO-nZnO-4TiO of mass percent 89.95%～96.85%
2with mass percent 3.15%～10.05% burning agent, wherein 0.3≤n≤0.6 falls.Described falling burnt agent and consisted of 0% < La
2o
3-B
2o
3-ZnO glass≤50% and 50%≤fall and burn agent A < 100%.Described La
2o
3-B
2o
3-ZnO glass consists of 45%≤La
2o
3≤ 47%, 37%≤B
2o
3≤ 39%, 14%≤ZnO≤16%.The described burning agent A that falls consists of 44.25%≤Li
2cO
3≤ 47.47%, 8.65%≤SiO
2≤ 9.19%, 35.59%≤B
2o
3≤ 38.29%, 0.88% < ZnO≤0.95%, 1.58% < Al
2o
3≤ 9.83% and additive 0.29%≤MnCO
3≤ 0.95% and 0.49%≤CuO≤1.58% and both mass ratioes be 1:1～1:2.
The preparation method of above-mentioned low-temperature sintering composite microwave medium ceramic material is as follows:
Step 1: by starting material BaCO
3, ZnO, TiO
2powder is BaCO:ZnO:TiO in molar ratio
2=1:n:4 batching, wherein 0.3≤n≤0.6, take deionized water as medium wet-milling mixing 3～5 hours, after taking-up, at 100 ℃, dries, and sieves, then 5～8 hours synthetic principal crystalline phase Ba of pre-burning in 800 ℃～1200 ℃ air atmosphere with 60 eye mesh screens
4ti
13o phase and BaZn
2ti
4o
11phase, i.e. BaO-ZnO-TiO
2base-material;
Step 2: starting material La
2o
3, B
2o
3, ZnO by mass percentage: 45%≤La
2o
3≤ 47%, 37%≤B
2o
3≤ 39%, 14%≤ZnO≤16% is prepared burden, take deionized water as medium wet-milling mixes 3～7 hours, after oven dry, with 60 eye mesh screens, sieve, in 500 ℃～800 ℃ pre-burnings 2～8 hours, then at 1100 ℃～1500 ℃ melten glass slags, by the glass dregs of preparation, cracker grinds is standby again;
Step 3: by starting material Li
2cO
3, SiO
2, B
2o
3, ZnO, Al
2o
3by mass percentage: 44.25%≤Li
2cO
3≤ 47.47%, 8.65%≤SiO
2≤ 9.19%, 35.59%≤B
2o
3≤ 38.29%, 0.88%≤ZnO≤0.95%, 1.58%≤Al
2o
3≤ 9.83% prepares burden, and adds additive 0.29%≤MnCO
3≤ 0.95%, 0.49%≤CuO≤1.58% and both mass ratioes are 1:1～1:2, take alcohol as medium wet-milling mixes 3～5 hours, after drying, with 60 eye mesh screens, sieve after taking-up at 80 ℃, make to fall and burn agent A.
Step 4: the La by proportioning being prepared by step 2
2o
3-B
2o
3agent A mixing is burnt in falling of-ZnO glass powder and step 3 preparation, take alcohol as medium wet-milling mixes 3～5 hours, after drying, with 60 eye mesh screens, sieves after taking-up at 80 ℃, makes and falls burning agent.
Step 5: adding the total mass per-cent that accounts for of step 4 preparation in the powder of step 1 preparation is 4.9%～9.52% fall and burn after agent mixes, take alcohol as medium wet-milling mixing 3～5 hours, after drying at 80 ℃ after taking-up, additive capacity accounts for 2～5% acrylic acid solution of raw material total mass as binding agent granulation, compression moulding, finally sintering 1～3 hour in 850 ℃ of-900 ℃ of air atmosphere, makes microwave dielectric ceramic materials.
The present invention has the following advantages in sum: 1, medium specific inductivity (20～30) is beneficial to the miniaturization of device; 2, high quality factor q f value and low loss (≤10
-4); 3, stable nearly temperature coefficient of resonance frequency-10～+ 10ppm/ ℃ of zero; 4, there is good common burning with silver or copper.
Accompanying drawing explanation
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is the BaO:nZnO:4TiO after pre-burning
2and the XRD figure of embodiment 1,2,4,6;
Fig. 2 is the XRD figure of embodiment 2,7,8,9,10, and Si is wherein used as to demarcate;
Fig. 3 (a)～3 (d) is respectively the SEM figure of embodiment 1,2,4,6;
Fig. 3 (e), 3 (f) are respectively the SEM figure of embodiment 7,8;
Fig. 4 is the red experiment comparison diagram of the suction of embodiment 2 and embodiment 7;
Fig. 5 (a), 5 (b) are respectively from different perspectives photo after the sintering of taking;
Fig. 6 is that embodiment 2, embodiment 7 and embodiment 20 inhale red experiment comparison diagram;
Fig. 7 (a), Fig. 7 (b) are that embodiment 20 moulding are schemed 875 ℃ of SEM figure and element branches of burning altogether with silver slurry afterwards.
Embodiment
The BaO-ZnO-TiO that material of the present invention is 89.95%～96.85% by material of the present invention by mass percent
2and mass percent to be 3.15%～10.05% fall burns agent and form, BaO-ZnO-TiO
2based material consist of BaO:nZnO:4TiO
2(0.3≤n≤0.6).Fall burning agent and consist of 0% < La
2o
3-B
2o
3-ZnO glass≤50% and 50%≤fall and burn agent A < 100% composition.Fall burning agent A and consist of 44.25%≤Li
2cO
3≤ 47.47%, 8.65%≤SiO
2≤ 9.19%, 35.59%≤B
2o
3≤ 38.29%, 0.88% < ZnO≤0.95%, 1.58% < Al
2o
3≤ 9.83% and additive 0.29%≤MnCO
3≤ 0.95% and 0.49%≤CuO≤1.58% and both mass ratioes be 1:1～1:2.La
2o
3-B
2o
3-ZnO glass consists of 45%≤La
2o
3≤ 47%, 37%≤B
2o
3≤ 39%, 14%≤ZnO≤16%.By solid phase method, can synthesize this material, concrete steps are with above-mentioned step 1 sample.
Composition and the microwave dielectric property of some specific embodiments are as follows
As can be seen from the above table, by falling, burn adding of agent, make system densified sintering product at low temperatures.And by contrast, do not add the system and the system that adds lanthanum boron zinc glass of lanthanum boron zinc glass, can find out, adding of appropriate lanthanum boron zinc glass, contributes to the finer and close of sintering, obtains medium specific inductivity and good microwave dielectric property.
With the BaO:nZnO:4TiO after pre-burning
2and embodiment 1,2,4,6 is example, by XRD figure (Fig. 1), can find out BaO:nZnO:4TiO after pre-burning
2what exist is mutually: Ba
4ti
13o
30, BaZn
2ti
4o
11, TiO
2.Owing to falling, burn adding of agent, make the Ba in system
4ti
13o
30phase and TiO
2when low fever, generated BaTi
5o
11phase, reaction equation can be expressed as: Ba
4ti
13o
30+ TiO
2→ BaTi
5o
11.And because fall, burn adding of agent, when low fever, also occurred BaTi (BO
3)
2phase.
The embodiment 2,7,8,9,10 of take is example, by contrast, is not added the system of lanthanum boron zinc glass and is added the XRD figure (Fig. 2) of the system of lanthanum boron zinc glass, can find out the phase that form in can change system adding not of lanthanum boron zinc glass.Si in Fig. 2 is used as to demarcate.
The embodiment 1,2,4,6,7,8 of take is example, from SEM figure, can find out, when 875 ℃ of sintering, because fall, burns adding of agent, and pore reduces, and it is fine and close that structure becomes, and illustrates that falling burning agent has promoter action to densified sintering product.By contrast, do not add the system of lanthanum boron zinc glass and add the SEM of the system of lanthanum boron zinc glass to scheme, can find out to add after lanthanum boron zinc glass more to contribute to system fine and close when low-temperature sintering, and can effectively suppress the abnormal growth of crystal grain.Fig. 3 (a)～3 (d) is respectively the SEM figure (not adding lanthanum boron zinc glass) of embodiment 1,2,4,6, and Fig. 3 (e), 3 (f) are respectively the SEM figure (adding lanthanum boron zinc glass) of embodiment 7,8.
By the red experiment of suction of comparative example 2 (not adding lanthanum boron zinc glass) and embodiment 7 (adding lanthanum boron zinc glass), also can find out and more contribute to system densified sintering product at low temperatures adding of lanthanum boron zinc glass.Fig. 4, for inhaling red experiment comparison diagram, puts into red ink by embodiment 2 and embodiment 7 simultaneously, soaks after 8 hours and takes out.Can find not add the embodiment 2 of lanthanum boron zinc glass to occur significantly inhaling red phenomenon, and add the embodiment 7 of lanthanum boron zinc glass to occur hardly inhaling red phenomenon.Illustrate that lanthanum boron zinc glass contributes to system densified sintering product at low temperatures.
By contrast add later the falling of lanthanum boron zinc glass burn agent and lanthanum boron zinc glass respectively with BaO:nZnO:4TiO
2sintering in the time of 875 ℃, can find out that adding falling of lanthanum boron zinc glass to burn agent incorporates BaO:nZnO:4TiO completely
2, and independent lanthanum boron zinc glass and BaO:nZnO:4TiO
2reaction hardly.Effectively acceleration of sintering of lanthanum boron zinc glass is described, but itself can not be as this system burning agent falls.Fig. 5 (a), 5 (b) are respectively from different perspectives photo after the sintering of taking, and wherein cylinder is respectively and adds falling of lanthanum boron zinc glass to burn agent and lanthanum boron zinc glass, and disk is BaO:nZnO:4TiO
2.
Take embodiment 8 as example, by regulating BaO:nZnO:4TiO
2in n and proper extension sintering time, can further improve the densified sintering product of system.Following table is composition and the microwave dielectric property of specific embodiment.
By comparative example 2,7,20 the red experiment of suction, also can find out that system compactness is best when n=0.6.Fig. 6, for inhaling red experiment comparison diagram, puts into red ink by embodiment 2, embodiment 7 and embodiment 20 simultaneously, soaks after 8 hours and takes out.Can find out that embodiment 20 there will not be the red phenomenon of suction completely.
By falling, burn adding of agent, make system densified sintering product at low temperatures, obtain good microwave dielectric property, and frequency-temperature coefficient that can regulation system, make system obtain stable nearly zero frequency-temperature coefficient.
Take embodiment 20 as example, after moulding, burn altogether at 875 ℃ with silver slurry.By SEM, scheme [Fig. 7 (a)] and element branch [Fig. 7 (b)] can find out, this system can be burnt altogether with silver slurry, and can not react with silver slurry.
Claims (3)
1. a low-temperature sintering composite microwave medium ceramic material, is characterized in that: its raw material consists of the BaO-nZnO-4TiO of mass percent 89.95%～96.85%
2burn agent with falling of mass percent 3.15%～10.05% and form, wherein 0.3≤n≤0.6;
Described falling burnt agent and consisted of 0% < La
2o
3-B
2o
3-ZnO glass≤50% and 50%≤fall and burn agent A < 100%;
Described La
2o
3-B
2o
3-ZnO glass consists of 45%≤La
2o
3≤ 47%, 37%≤B
2o
3≤ 39%, 14%≤ZnO≤16%;
The described burning agent A that falls consists of 44.25%≤Li
2cO
3≤ 47.47%, 8.65%≤SiO
2≤ 9.19%, 35.59%≤B
2o
3≤ 38.29%, 0.88% < ZnO≤0.95%, 1.58% < Al
2o
3≤ 9.83% and additive 0.29%≤MnCO
3≤ 0.95% and 0.49%≤CuO≤1.58% and both mass ratioes be 1:1～1:2.
2. low-temperature sintering composite microwave medium ceramic material as claimed in claim 1, is characterized in that: described stupalith sintering temperature is 850 ℃～900 ℃, DIELECTRIC CONSTANT ε
r20～30, Q * f (GHz): 10000～15000, frequency-temperature coefficient τ
ffor-10～+ 10ppm/ ℃.
3. the preparation method of low-temperature sintering composite microwave medium ceramic material as claimed in claim 1, is characterized in that, comprises the following steps:
Step 1: by starting material BaCO
3, ZnO, TiO
2powder is BaCO:ZnO:TiO in molar ratio
2=1:n:4 batching, wherein 0.3≤n≤0.6, take deionized water as medium wet-milling mixing 3～5 hours, after taking-up, at 100 ℃, dries, and sieves, then 5～8 hours synthetic principal crystalline phase Ba of pre-burning in 800 ℃～1200 ℃ air atmosphere with 60 eye mesh screens
4ti
13o phase and BaZn
2ti
4o
11phase, i.e. BaO-ZnO-TiO
2base-material;
Step 2: starting material La
2o
3, B
2o
3, ZnO by mass percentage: 45%≤La
2o
3≤ 47%, 37%≤B
2o
3≤ 39%, 14%≤ZnO≤16% is prepared burden, take deionized water as medium wet-milling mixing 3～7 hours, after oven dry, with 60 eye mesh screens, sieve, in 500 ℃～800 ℃ pre-burnings 2～8 hours, then the pure cold glass dregs that makes immediately after 1100 ℃～1500 ℃ meltings, by the glass dregs of preparation, cracker grinds is standby again;
Step 3: by starting material Li
2cO
3, SiO
2, B
2o
3, ZnO, Al
2o
3by mass percentage: 44.25%≤Li
2cO
3≤ 47.47%, 8.65%≤SiO
2≤ 9.19%, 35.59%≤B
2o
3≤ 38.29%, 0.88%≤ZnO≤0.95%, 1.58%≤Al
2o
3≤ 9.83% prepares burden, and adds additive 0.29%≤MnCO
3≤ 0.95%, 0.49%≤CuO≤1.58% and both mass ratioes are 1:1～1:2, take alcohol as medium wet-milling mixes 3～5 hours, after drying, with 60 eye mesh screens, sieve after taking-up at 80 ℃, make to fall and burn agent A;
Step 4: by the La of step 2 preparation
2o
3-B
2o
3-ZnO glass powder and falling of step 3 preparation are burnt agent A by mass percentage: 0% < La
2o
3-B
2o
3-ZnO glass≤50%, 50%≤fall and burn agent A < 100% mixing, take alcohol as medium wet-milling mixes 3～5 hours, after drying, with 60 eye mesh screens, sieves after taking-up at 80 ℃, makes and falls burning agent;
Step 5: be 3.15%～10.05% fall and burn after agent mixes by adding the total mass per-cent that accounts for of step 4 preparation in the base-material of step 1 preparation, take alcohol as medium wet-milling mixing 3～5 hours, after drying at 80 ℃ after taking-up, additive capacity accounts for 2～5% acrylic acid solution of raw material total mass as binding agent granulation, compression moulding, finally sintering 1～3 hour in 850 ℃ of-900 ℃ of air atmosphere, makes microwave dielectric ceramic materials.
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| CN104108929B CN104108929B (en) | 2015-08-19 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671775A (en) * | 2015-01-26 | 2015-06-03 | 电子科技大学 | LTCC (Low Temperature Co-Fired Ceramic) material having Ba-Nd-Ti system and preparation method |
| CN104944786A (en) * | 2015-06-17 | 2015-09-30 | 电子科技大学 | Low-temperature sintered low-dielectric glass ceramic composite substrate material and preparation method thereof |
| CN105236966A (en) * | 2015-08-31 | 2016-01-13 | 天津大学 | Low-temperature-sintered zinc-titanium-niobium-series microwave dielectric ceramic |
| CN106007703A (en) * | 2016-05-12 | 2016-10-12 | 电子科技大学 | Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof |
| CN106220166A (en) * | 2016-07-12 | 2016-12-14 | 广东国华新材料科技股份有限公司 | A kind of microwave-medium ceramics and preparation method thereof |
| CN106587991A (en) * | 2016-12-06 | 2017-04-26 | 电子科技大学 | Low-temperature-sintered composite microwave dielectric ceramic material and preparation method thereof |
| CN110317057A (en) * | 2019-05-06 | 2019-10-11 | 北京元六鸿远电子科技股份有限公司 | A kind of medium dielectric constant low-temperature co-fired ceramic and preparation method |
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| CN104671775A (en) * | 2015-01-26 | 2015-06-03 | 电子科技大学 | LTCC (Low Temperature Co-Fired Ceramic) material having Ba-Nd-Ti system and preparation method |
| CN104944786A (en) * | 2015-06-17 | 2015-09-30 | 电子科技大学 | Low-temperature sintered low-dielectric glass ceramic composite substrate material and preparation method thereof |
| CN105236966A (en) * | 2015-08-31 | 2016-01-13 | 天津大学 | Low-temperature-sintered zinc-titanium-niobium-series microwave dielectric ceramic |
| CN106007703A (en) * | 2016-05-12 | 2016-10-12 | 电子科技大学 | Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof |
| CN106007703B (en) * | 2016-05-12 | 2019-05-14 | 电子科技大学 | A kind of low-temperature sintering composite microwave medium ceramic material and preparation method thereof |
| CN106220166A (en) * | 2016-07-12 | 2016-12-14 | 广东国华新材料科技股份有限公司 | A kind of microwave-medium ceramics and preparation method thereof |
| CN106220166B (en) * | 2016-07-12 | 2018-04-03 | 广东国华新材料科技股份有限公司 | A kind of microwave-medium ceramics and preparation method thereof |
| CN106587991A (en) * | 2016-12-06 | 2017-04-26 | 电子科技大学 | Low-temperature-sintered composite microwave dielectric ceramic material and preparation method thereof |
| CN110317057A (en) * | 2019-05-06 | 2019-10-11 | 北京元六鸿远电子科技股份有限公司 | A kind of medium dielectric constant low-temperature co-fired ceramic and preparation method |
| CN110317057B (en) * | 2019-05-06 | 2023-03-28 | 北京元六鸿远电子科技股份有限公司 | Medium-dielectric-constant low-temperature co-fired ceramic material and preparation method thereof |
| CN114804897A (en) * | 2022-05-05 | 2022-07-29 | 江苏科技大学 | Sintering aid for ceramic and preparation method thereof, zinc zirconate microwave dielectric ceramic and preparation method thereof |
| CN114804897B (en) * | 2022-05-05 | 2023-02-28 | 江苏科技大学 | Sintering aid for ceramic and preparation method thereof, zinc zirconate microwave dielectric ceramic and preparation method thereof |
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| CN104108929B (en) | 2015-08-19 |
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