CN103693966A - Low temperature co-fired ceramic material and preparation method thereof - Google Patents
Low temperature co-fired ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a low temperature co-fired ceramic material. The low temperature co-fired ceramic material comprises the following components: 79-95wt% of ceramics and 5-21wt% of firing aiding glass. Compared with existing ceramic materials, the low temperature co-fired ceramic material has the beneficial effects that BaO, ZnO and TiO2 components are used as the raw materials of the ceramics; the ceramics formed by BaO and TiO2 have excellent microwave dielectric properties but have higher sintering temperatures; the sintering temperatures of the ceramics can be obviously reduced through addition of ZnO, so that the ceramics with better dielectric properties and lower sintering temperatures are obtained; the firing aiding glass has lower sintering temperature and part of atoms in the firing aiding glass are the same as or similar to part of atoms in a ceramic matrix; and meanwhile, the low temperature co-fired ceramic material with middle dielectric constant is obtained by controlling the contents of the ceramics and the firing aiding glass.
Description
Technical field
The present invention relates to technical field of electronic devices, relate in particular to a kind of low-temperature co-burning ceramic material and preparation method thereof.
Background technology
Modern mobile communication is through the development of 30 years, gradually towards miniaturization, integrated, high reliability and low-cost future development, therefore to take the microwave circuit components and parts that microwave-medium ceramics is base, also has higher requirement.For meeting mobile communication terminal portability and microminiaturized requirement, except reducing the size of tank circuit, the microwave dielectric material of high-k, high Q value and nearly zero-temperature coefficient becomes the focus of research.
LTCC (LTCC) technology is that low-temperature sintered ceramics powder is made to the accurate and fine and close green band of thickness, on green band, utilize the techniques such as laser boring, micropore slip casting, accurate conductor paste printing to make needed circuitous pattern, and a plurality of passive elements are imbedded wherein, then overlap together, at 900 ℃ of sintering, make the passive integration assembly of three-dimensional circuit network, also can be made into the three-dimensional circuit substrate of built-in passive element, on its surface, can mount IC and active part, make passive/active integrated functional module.LTCC has become integrated, the modular preferred manner of mcm with its excellent electronics, machinery, electricity characteristic etc., is widely used in the fields such as substrate, encapsulation and microwave device.Adopt LTCC technique to manufacture microwave device, need microwave dielectric material to burn altogether with metal electrode Au, the Cu of high conductivity, Ag etc.From economy and environmental, consider, use the metals such as Ag, Cu that fusing point is lower ideal as electrode materials.
Due to the requirement of the sintering characteristics such as silver electrode, the sintering temperature of stupalith requires 800～930 ℃ of left and right.Conventionally the method that reduces stupalith sintering temperature has: add oxide compound or low melting glass sintering agent, introduce chemical synthesis process, superfine powder raw material, devitrified glass or amorphous glass etc.Chemosynthesis and superfine powder complex process, yield poorly, cost is high, be difficult for volume production, therefore, adds low melting point oxide or glassy phase and be the method for the reduction stupalith sintering temperature of commonly using, but can cause ceramic performance to worsen.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of low-temperature co-burning ceramic material of medium dielectric constant microwave medium.
In view of this, the invention provides a kind of low-temperature co-burning ceramic material, composed of the following components:
The pottery of 79wt%～95wt%, 5wt%～21wt% helps burning glass;
Described pottery is by BaO, ZnO and TiO
2form;
Describedly help that to burn glass be one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass.
Preferably, described BaO, ZnO and TiO
2mol ratio according to the mol ratio of each element in formula (I), determine;
BaZn
xTi
yO
1+x+2y （I）；
Wherein, 0.15≤x≤0.6,2.5≤y≤4.5.
Preferably, described Zn-B glass is by the ZnO of 20wt%～70wt% and the B of 30wt%～80wt%
2o
3form.
Preferably, described Zn-B-Si glass is by the ZnO of 10wt%～60wt%, the B of 20wt%～75wt%
2o
3siO with 10wt%～40wt%
2form.
Preferably, described Ba-B-Si glass is by the BaO of 20wt%～50wt%, the B of 40wt%～65wt%
2o
3siO with 10wt%～20wt%
2form.
Preferably, described Bi-B-Si glass is by the Bi of 30wt%～70wt%
2o
3, 20wt%～45wt% B
2o
3siO with 10wt%～25wt%
2form.
Preferably, described Ba-Zn-B-Si glass is by the Ba of 10wt%～45wt%
2o
3, the ZnO of 10wt%～50wt% is, the B of 10wt%～45wt%
2o
3siO with 10wt%～25wt%
2form.
Preferably, described Bi-Zn-B-Si glass is by the Bi of 10wt%～40wt%
2o
3, the ZnO of 10wt%～50wt% is, the B of 10wt%～45wt%
2o
3siO with 10wt%～25wt%
2form.
The present invention also provides a kind of preparation method of low-temperature co-burning ceramic material, comprises the following steps:
By BaO, ZnO and TiO
2mix, pre-burning after ball milling, obtains pottery and burns piece, described pottery is burnt to piece and pulverize, and obtains ceramics powder;
By ZnO and B
2o
3mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B and helps burning glass powder;
By ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B-Si and helps burning glass powder;
By BaO, Bi
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Ba-B-Si and helps burning glass powder;
By Bi
2o
3, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Bi-B-Si and helps burning glass powder;
By Ba
2o
3, ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Ba-Zn-B-Si and helps burning glass powder;
By Bi
2o
3, ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Bi-Zn-B-Si and helps burning glass powder;
Described Zn-B is helped and burns glass, Zn-B-Si and help and burn glass, Ba-B-Si and help and burn glass, Bi-B-Si and help and burn glass, Ba-Zn-B-Si and help and burn glass and Bi-Zn-B-Si and help one or more in burning glass to mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
Preferably, in preparing the step of ceramics powder, the time of described ball milling is 6～24h, and the temperature of pre-burning is 950～1200 ℃, and the time is 2～6h.
The invention provides a kind of low-temperature co-burning ceramic material, composed of the following components: the pottery of 79wt%～95wt%, 5wt%～21wt% helps burning glass; Described pottery is by BaO, ZnO and TiO
2form; Describedly help that to burn glass be one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass.Compare with existing stupalith, the present invention is with BaO, ZnO and TiO
2component is ceramic raw material, BaO and TiO
2the pottery forming has excellent microwave dielectric property, but sintering temperature is higher, and adding of ZnO can obviously reduce ceramic sintering temperature., obtain dielectric properties better and the lower pottery of sintering temperature; Help burning glass to there is lower sintering temperature, and help the part of atoms of burning in glass identical or close with the part of atoms in ceramic matrix; Simultaneously by controlling pottery and helping the content that burns glass, thereby obtain having the low-temperature co-burning ceramic material of medium dielectric constant microwave medium.
Experimental result shows, low-temperature co-fired ceramic powder prepared by the present invention can be realized fine and close one-tenth porcelain at 850～930 ℃, and specific inductivity is 30～45, and loss tangent is less than 0.008, be less than ± 50ppm/ ℃ of temperature coefficient of resonance frequency, can realization and the common burning of Cu, Ag electrode.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The embodiment of the invention discloses a kind of low-temperature co-burning ceramic material, composed of the following components:
The pottery of 79wt%～95wt%, 5wt%～21wt% helps burning glass;
Described pottery is by BaO, ZnO and TiO
2form;
Describedly help that to burn glass be one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass.
Low-temperature co-burning ceramic material of the present invention is mainly to burn altogether with silver electrode, and the common burning temperature of described silver electrode is generally 850 ℃ of left and right, so the sintering temperature of low-temperature co-burning ceramic material is 850 ℃～950 ℃.Well known to those skilled in the art: the ceramic sintering temperature that the overwhelming majority has medium dielectric constant microwave medium is higher; And the dielectric properties of glassy phase are poor, be mainly manifested in dielectric loss bigger than normal, so the application adjusts with helping the selection and the content that burn glass by pottery, reach the requirement of LTCC technology to material.
According to the present invention, the content of described pottery is 79wt%～95wt%, is preferably 85wt%～95wt%, more preferably 85wt%～93wt%.If the too high levels of pottery, is difficult to meet the requirement of sintering temperature, if the too low specific inductivity of stupalith that can make of ceramic temperature sharply reduces.Described to help the content that burns glass be 5wt%～21wt%, is preferably 7～20wt%, 7wt%～18wt% more preferably, and more preferably 7wt%～15wt%, most preferably is 10wt%～15wt%.If described in help the too high levels of burning glass, the dielectric properties of severe exacerbation pottery, the content that burns glass if help is too low, causes sintering temperature not reach requirement.
Pottery described in the present invention is by BaO, ZnO and TiO
2form BaO and TiO
2the pottery forming has excellent microwave dielectric property, but sintering temperature is higher, and adding of ZnO can obviously reduce ceramic sintering temperature, and itself and TiO
2the stupalith forming also has good microwave dielectric property, and three adulterates mutually, obtains dielectric properties better and the lower pottery of sintering temperature.Described pottery is the basic phase of low-temperature co-burning ceramic material.As preferred version, described BaO, ZnO and TiO
2mol ratio according to expression formula BaZn
xti
yo
1+x+2ythe mol ratio of each element is determined.
Describedly help that to burn glass be one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass.
Wherein, described Zn-B glass is Zn-B glass well known to those skilled in the art, there is no special restriction, preferred by the ZnO of 20wt%～70wt% and the B of 30wt%～80wt% in the present invention
2o
3form.Described ZnO is preferably 30wt%～60wt%, more preferably 45wt%～55wt%; Described B
2o
3be preferably 40wt%～70wt%, more preferably 45wt%～55wt%.
Described Zn-B-Si glass is preferably by the ZnO of 10wt%～60wt%, the B of 20wt%～75wt%
2o
3siO with 10wt%～40wt%
2form.Described ZnO is preferably 15wt%～50wt%, more preferably 25wt%～40wt%; Described B
2o
3be preferably 30wt%～65wt%, more preferably 50wt%～60wt%; Described SiO
2be preferably 10wt%～30wt%, more preferably 10wt%～20wt%.
Described Ba-B-Si glass is preferably by the BaO of 20wt%～50wt%, the B of 40wt%～65wt%
2o
3siO with 10wt%～20wt%
2form.Wherein, described BaO is preferably 30wt%～50wt%, more preferably 40wt%～50wt%; Described B
2o
3be preferably 40wt%～60wt%, more preferably 40wt%～65wt%; Described SiO
2be preferably 10wt%～15wt%.
Described Bi-B-Si glass is preferably by the Bi of 30wt%～70wt%
2o
3, 20wt%～45wt% B
2o
3siO with 10wt%～25wt%
2form; Described Bi
2o
3content be preferably 35wt%～60wt%, 40wt%～50wt% more preferably; Described B
2o
3be preferably 30wt%～45wt%, more preferably 30wt%～40wt%; Described SiO
2be preferably 15wt%～25wt%, more preferably 20wt%～25wt%.
Described Ba-Zn-B-Si glass is preferably by the Ba of 10wt%～45wt%
2o
3, the ZnO of 10wt%～50wt% is, the B of 10wt%～45wt%
2o
3siO with 10wt%～25wt%
2form; Described Ba
2o
3be preferably 20wt%～40wt%, more preferably 25wt%～35wt%; Described ZnO is preferably 20wt%～40wt%, more preferably 25wt%～35wt%; Described B
2o
3be preferably 20wt%～40wt%, more preferably 20wt%～30wt%; Described SiO
2be preferably 10wt%～20wt%, more preferably 15wt%～20wt%.
Described Bi-Zn-B-Si glass is preferably by the Bi of 10wt%～40wt%
2o
3, the ZnO of 10wt%～50wt% is, the B of 10wt%～45wt%
2o
3siO with 10wt%～25wt%
2form; Described Bi
2o
3be preferably 20wt%～40wt%, more preferably 30wt%～40wt%; Described ZnO is preferably 20wt%～40wt%; 30wt%～40wt% more preferably; Described B
2o
3be preferably 15wt%～40wt%, more preferably 18wt%～30wt%; Described SiO
2be preferably 10wt%～20wt%, more preferably 10wt%～15wt%.
The present invention selects one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass for helping burning glass, because above-mentioned glass has lower sintering temperature on the one hand, on the other hand because the above-mentioned part of atoms of burning in glass that helps is identical or close with the part of atoms in ceramic matrix, help the crystalline structure and the ceramic matrix that burn after glass sintering to there is certain similarity, consistency, the most important thing is, the above-mentioned burning glass that helps has good cooling-down effect to ceramic matrix.
The invention provides a kind of low-temperature co-burning ceramic material, composed of the following components: the pottery of 79wt%～95wt%, 5wt%～21wt% helps burning glass; Described pottery is by BaO, ZnO and TiO
2form; Describedly help that to burn glass be one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass.BaO and TiO
2the pottery forming has excellent microwave dielectric property, but sintering temperature is higher, and adding of ZnO can obviously reduce ceramic sintering temperature, and itself and TiO
2the stupalith forming also has good microwave dielectric property, three adulterates mutually, obtain dielectric properties better and the lower pottery of sintering temperature, and help and burn glass and there is lower sintering temperature, and help the part of atoms of burning in glass identical or close with the part of atoms in ceramic matrix; Simultaneously by controlling pottery and helping the content that burns glass, thereby make low temperature co-fired his stupalith finally obtaining there is medium dielectric constant microwave medium.
The present invention also provides the preparation method of above-mentioned low-temperature co-burning ceramic material, comprises the following steps:
By BaO, ZnO and TiO
2mix, pre-burning after ball milling, obtains pottery and burns piece, described pottery is burnt to piece and pulverize, and obtains ceramics powder;
By ZnO and B
2o
3mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B and helps burning glass powder;
By ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B-Si and helps burning glass powder;
By BaO, Bi
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Ba-B-Si and helps burning glass powder;
By Bi
2o
3, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Bi-B-Si and helps burning glass powder;
By Ba
2o
3, ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Ba-Zn-B-Si and helps burning glass powder;
By Bi
2o
3, ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Bi-Zn-B-Si and helps burning glass powder;
Described Zn-B is helped and burns glass, Zn-B-Si and help and burn glass, Ba-B-Si and help and burn glass, Bi-B-Si and help and burn glass, Ba-Zn-B-Si and help and burn glass and Bi-Zn-B-Si and help one or more in burning glass to mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
According to the present invention, in preparing the process of low-temperature co-burning ceramic material, first prepared ceramics powder and helped burning glass powder, then ceramics powder is mixed with helping burning glass powder, obtain low-temperature co-fired ceramic powder.
In the present invention, above-mentioned ceramics powder has no particular limits with helping the preparation order the present invention who burns glass powder, can first prepare ceramics powder and also can first prepare and help burning glass powder.In preparing the process of ceramics powder, be prepared by the following method:
By BaO, ZnO and TiO
2mix, pre-burning after ball milling, obtains pottery and burns piece, described pottery is burnt to piece and pulverize, and obtains ceramics powder.
In preparing the process of ceramics powder, described BaO, ZnO and TiO
2mol ratio preferably according to the mol ratio of each element in formula (I), determine;
BaZn
xTi
yO
1+x+2y （I）；
Wherein, 0.15≤x≤0.6,2.5≤y≤4.5.
The time of described ball milling is preferably 6～24h, 10～20h more preferably, and after ball milling, the mixed powder that ball milling is obtained is preferably dried, to remove the oil-based solvent in mechanical milling process.Then the powder after drying is carried out to pre-burning, obtain pottery and burn piece.The temperature of described pre-burning is preferably 950～1200 ℃, more preferably 1100～1200 ℃; The time of described pre-burning is preferably 2～6h, more preferably 4～6h.Finally described pottery is burnt to piece and pulverize, obtain ceramics powder.The particle diameter of described ceramics powder is preferably 0.5～3 μ m, more preferably 0.5～2 μ m.
According to the present invention, described Zn-B helps burning glass powder, Zn-B-Si to help burning glass powder, Ba-B-Si to help burning glass powder, Bi-B-Si to help burning glass powder, Ba-Zn-B-Si to help burning glass powder and Bi-Zn-B-Si to help the preparation method of burning glass powder identical, is raw material difference; It is ZnO and B that wherein said Zn-B helps the raw material of burning glass powder
2o
3; It is ZnO, B that described Zn-B-Si helps the raw material of burning glass powder
2o
3with SiO
2; It is BaO, Bi that described Ba-B-Si helps the raw material of burning glass powder
2o
3with SiO
2; It is Bi that described Bi-B-Si helps the raw material of burning glass powder
2o
3, B
2o
3with SiO
2; The raw material of described Ba-Zn-B-Si is Ba
2o
3, ZnO, B
2o
3with SiO
2; It is Bi that described Bi-Zn-B-Si helps the raw material of burning glass powder
2o
3, ZnO, B
2o
3with SiO
2.It is example that the Zn-B of take helps the preparation method of burning glass powder, and its preparation process is:
By ZnO and B
2o
3mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B and helps burning glass powder.
In preparation, Zn-B helps in the process of burning glass powder, and the time of described ball milling is preferably 6～24h, more preferably 10～15h.After mixed powder after ball milling is dried, carry out pre-burning, obtain burning piece, the temperature of described pre-burning is preferably 450～650 ℃, more preferably 500～650 ℃; The time of described pre-burning is preferably 1～6h, more preferably 3～5h.Then will after described burning piece fusing, obtain glass drop; The temperature of described fusing is preferably 1450 ℃～1550 ℃.Finally by obtaining Zn-B after described glass drop cold quenching, pulverizing, help burning glass powder.The described particle diameter that burns glass powder that helps is preferably 0.5～3 μ m, more preferably 0.5～2 μ m.
Preparing respectively ceramics powder and helping after burning glass powder, Zn-B helps and burns glass, Zn-B-Si and help and burn glass, Ba-B-Si and help and burn glass, Bi-B-Si and help and burn glass, Ba-Zn-B-Si and help and burn glass and Bi-Zn-B-Si and help one or more in burning glass to mix with described ceramics powder, obtains low-temperature co-burning ceramic material.
The invention provides a kind of preparation method of low-temperature co-burning ceramic material.In preparing the process of low-temperature co-burning ceramic material, prepared respectively ceramics powder and helped burning glass powder, then described ceramics powder is mixed with helping burning glass powder, obtain low-temperature co-burning ceramic material.Experimental result shows, low-temperature co-fired ceramic powder prepared by the present invention can be realized fine and close one-tenth porcelain at 850～930 ℃, and specific inductivity is 30～45, and loss tangent is less than 0.008, be less than ± 50ppm/ ℃ of temperature coefficient of resonance frequency, can realization and the common burning of Cu, Ag electrode.
In order further to understand the present invention, below in conjunction with embodiment, low-temperature co-burning ceramic material provided by the invention is elaborated, protection scope of the present invention is not limited by the following examples.
Embodiment 1
By the ZnO powder of the BaO powder of 1mol, 0.25mol and the TiO of 2.75mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m;
By the ZnO powder of 50g and the B of 50g
2o
3powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the glass powder of 0.5～2 μ m;
Pack the described glass powder of the described ceramics powder of 87wt% and 13wt% into mixer, after mixing 2h, obtain low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 2
By the ZnO powder of the BaO powder of 1mol, 0.25mol and the TiO of 2.75mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m;
By the Bi of 40g
2o
3the B of powder, 35g
2o
3the SiO of powder and 25g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the glass powder of 0.5～2 μ m.
The described ceramics powder of 89wt% and the described glass powder of 11wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 3
By the ZnO powder of the BaO powder of 1mol, 0.25mol and the TiO of 4mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m;
By the ZnO powder of the BaO powder of 30g, 30g, the B of 25g
2o
3the SiO of powder and 15g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the glass powder of 0.5～2 μ m.
The described ceramics powder of 91wt% and the described glass powder of 9wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 4
By the ZnO powder of the BaO powder of 1mol, 0.5mol and the TiO of 4mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m.
By the BaO powder of 45g, the B of 45g
2o
3the SiO of powder and 10g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the glass powder of 0.5～2 μ m.
The described ceramics powder of 88wt% and the described glass powder of 12wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 5
By the ZnO powder of the BaO powder of 1mol, 0.5mol and the TiO of 4.3mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m.
By the ZnO powder of 30g, the B of 55g
2o
3the SiO of powder and 15g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the glass powder of 0.5～2 μ m.
The described ceramics powder of 93wt% and the described glass powder of 7wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 6
By the ZnO powder of the BaO powder of 1mol, 0.5mol and the TiO of 4.3mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m;
By the ZnO powder of 50g and the B of 50g
2o
3powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Zn-B glass powder of 0.5～2 μ m
By the Bi of 40g
2o
3the B of powder, 35g
2o
3the SiO of powder and 25g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5～2 μ m.
The described Zn-B glass powder of the described ceramics powder of 89wt%, 9wt% and the described Bi-B-Si glass powder of 2wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 7
By the ZnO powder of the BaO powder of 1mol, 0.5mol and the TiO of 4.3mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m;
By the Bi of 40g
2o
3the B of powder, 35g
2o
3the SiO of powder and 25g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5～2 μ m;
By the ZnO powder of the BaO powder of 30g, 30g, the B of 25g
2o
3the SiO of powder and 15g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Ba-Zn-B-Si glass powder of 0.5～2 μ m.
The Bi-B-Si glass powder of the described ceramics powder of 88wt%, 9wt% and the described Ba-Zn-B-Si glass powder of 2wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 8
By the ZnO powder of the BaO powder of 1mol, 0.25mol and the TiO of 2.75mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m;
By the ZnO powder of 50g and the B of 50g
2o
3powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Zn-B glass powder of 0.5～2 μ m;
By the Bi of 40g
2o
3the B of powder, 35g
2o
3the SiO of powder and 25g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5～2 μ m;
By the Bi of 35g
2o
3the ZnO powder of powder, 35g, the B of 20g
2o
3the SiO of powder and 10g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Bi-Zn-B-Si glass powder of 0.5～2 μ m;
The described Bi-B-Si glass powder of the described Zn-B glass powder of the described ceramics powder of 85wt%, 2wt%, 8wt% and the described Bi-Zn-B-Si glass powder of 5wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
Embodiment 9
By the ZnO powder of the BaO powder of 1mol, 0.5mol and the TiO of 4mol
2powder mixes, then adds the deionized water that accounts for above-mentioned powder total mass 80%, mixes laggard row planetary ball mill, and Ball-milling Time is 6h, obtains mixed powder; After being dried, described mixed powder at 1100 ℃ of pre-burning 6h, obtains ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5～3 μ m.
By the Bi of 40g
2o
3the B of powder, 35g
2o
3the SiO of powder and 25g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5～2 μ m;
By the ZnO powder of the BaO powder of 30g, 30g, the B of 25g
2o
3the SiO of powder and 15g
2powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; After frit discharging after ball milling, in 120 ℃ of oven dry, after 650 ℃ of pre-burning 4h, become porcelain; It is that in the crucible of 1500 ℃, rapid melting becomes glass metal to drip on cold roller that described porcelain is added to temperature.After cold quenching, obtaining particle diameter is the amorphous glass porcelain of 15～500 μ m.Described amorphous glass porcelain is pulverized through fluidized bed jet mill, obtained favorable dispersity, particle diameter is the Ba-Zn-B-Si glass powder of 0.5～2 μ m.
The described Bi-B-Si glass powder of the described ceramics powder of 86wt%, 11wt% and the described Ba-Zn-B-Si glass powder of 3wt% are packed into after mixing 2h in mixer and obtains low-temperature co-fired ceramic powder.
Low-temperature co-fired ceramic powder prepared by the present embodiment carries out Performance Detection, and detected result is as shown in table 1, and table 1 is the performance data table of the low-temperature co-burning ceramic material of embodiment 1～9 preparation.
The performance data table of the low-temperature co-burning ceramic material of table 1 embodiment 1～9 preparation
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a low-temperature co-burning ceramic material, composed of the following components:
The pottery of 79wt%～95wt%, 5wt%～21wt% helps burning glass;
Described pottery is by BaO, ZnO and TiO
2form;
Describedly help that to burn glass be one or more in Zn-B glass, Zn-B-Si glass, Ba-B-Si glass, Bi-B-Si glass, Ba-Zn-B-Si glass and Bi-Zn-B-Si glass.
2. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described BaO, ZnO and TiO
2mol ratio according to the mol ratio of each element in formula (I), determine;
BaZn
xTi
yO
1+x+2y （I）；
Wherein, 0.15≤x≤0.6,2.5≤y≤4.5.
3. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Zn-B glass is by the ZnO of 20wt%～70wt% and the B of 30wt%～80wt%
2o
3form.
4. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Zn-B-Si glass is by the ZnO of 10wt%～60wt%, the B of 20wt%～75wt%
2o
3siO with 10wt%～40wt%
2form.
5. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Ba-B-Si glass is by the BaO of 20wt%～50wt%, the B of 40wt%～65wt%
2o
3siO with 10wt%～20wt%
2form.
6. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Bi-B-Si glass is by the Bi of 30wt%～70wt%
2o
3, 20wt%～45wt% B
2o
3siO with 10wt%～25wt%
2form.
7. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Ba-Zn-B-Si glass is by the Ba of 10wt%～45wt%
2o
3, the ZnO of 10wt%～50wt% is, the B of 10wt%～45wt%
2o
3siO with 10wt%～25wt%
2form.
8. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Bi-Zn-B-Si glass is by the Bi of 10wt%～40wt%
2o
3, the ZnO of 10wt%～50wt% is, the B of 10wt%～45wt%
2o
3siO with 10wt%～25wt%
2form.
9. a preparation method for low-temperature co-burning ceramic material, comprises the following steps:
By BaO, ZnO and TiO
2mix, pre-burning after ball milling, obtains pottery and burns piece, described pottery is burnt to piece and pulverize, and obtains ceramics powder;
By ZnO and B
2o
3mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B and helps burning glass powder;
By ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Zn-B-Si and helps burning glass powder;
By BaO, Bi
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Ba-B-Si and helps burning glass powder;
By Bi
2o
3, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Bi-B-Si and helps burning glass powder;
By Ba
2o
3, ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Ba-Zn-B-Si and helps burning glass powder;
By Bi
2o
3, ZnO, B
2o
3with SiO
2mix, pre-burning after ball milling, obtains burning piece, by obtaining glass drop after described burning piece fusing, by pulverizing after described glass drop cold quenching, obtains Bi-Zn-B-Si and helps burning glass powder;
Described Zn-B is helped and burns glass, Zn-B-Si and help and burn glass, Ba-B-Si and help and burn glass, Bi-B-Si and help and burn glass, Ba-Zn-B-Si and help and burn glass and Bi-Zn-B-Si and help one or more in burning glass to mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
10. preparation method according to claim 9, is characterized in that, in preparing the step of ceramics powder, the time of described ball milling is 6～24h, and the temperature of pre-burning is 950～1200 ℃, and the time is 2～6h.
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