CN103693966B - A kind of low-temperature co-burning ceramic material and preparation method thereof - Google Patents
A kind of low-temperature co-burning ceramic material and preparation method thereof Download PDFInfo
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Abstract
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.Compared with existing stupalith, the present invention is with BaO, ZnO and TiO
2component is ceramic raw material, BaO and TiO
2the pottery formed has excellent microwave dielectric property, but sintering temperature is higher, and ZnO adds the sintering temperature that obviously can reduce pottery, obtains dielectric properties better and the lower pottery of sintering temperature; Help burning glass to have lower sintering temperature, and help the part of atoms of burning in glass identical with the part of atoms in ceramic matrix or close; Simultaneously by controlling pottery and helping the content burning glass, thus obtain the low-temperature co-burning ceramic material with medium dielectric constant microwave medium.
Description
Technical field
The present invention relates to technical field of electronic devices, particularly relate to a kind of low-temperature co-burning ceramic material and preparation method thereof.
Background technology
Modern mobile communication, through the development of 30 years, gradually towards miniaturization, integrated, high reliability and low cost future development, therefore it is also proposed higher requirement to the microwave circuit components and parts taking microwave-medium ceramics as base.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-factor and nearly zero-temperature coefficient becomes the focus of research.
LTCC (LTCC) technology low-temperature sintered ceramics powder is made the accurate and fine and close green band of thickness, green band utilize the techniques such as laser boring, micropore slip casting, accurate conductor paste printing make required circuitous pattern, and multiple passive element is imbedded wherein, then overlap together, at 900 DEG C 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, IC and active part can be mounted on its surface, make passive/active integrated functional module.LTCC has become integrated, the modular preferred manner of mcm with the electronics of its excellence, machinery, electricity characteristic etc., is widely used in the fields such as substrate, encapsulation and microwave device.Adopt LTCC manufacture technics microwave device, need microwave dielectric material can burn altogether with metal electrode Au, Cu, Ag etc. of high conductivity.Consider from economy and environmental, 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 at about 800 ~ 930 DEG C.The method of usual reduction 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 be high, not easily volume production, therefore, adds the method that low melting point oxide or glassy phase are conventional reduction stupalith sintering temperatures, but ceramic performance can be caused to worsen.
Summary of the invention
The technical problem that the present invention solves is the low-temperature co-burning ceramic material providing a kind 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
2composition;
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 determine according to the mol ratio of each element in formula (I);
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 B of ZnO and the 30wt% ~ 80wt% of 20wt% ~ 70wt%
2o
3composition.
Preferably, described Zn-B-Si glass is by the B of ZnO, 20wt% ~ 75wt% of 10wt% ~ 60wt%
2o
3with the SiO of 10wt% ~ 40wt%
2composition.
Preferably, described Ba-B-Si glass is by the B of BaO, 40wt% ~ 65wt% of 20wt% ~ 50wt%
2o
3with the SiO of 10wt% ~ 20wt%
2composition.
Preferably, described Bi-B-Si glass is by the Bi of 30wt% ~ 70wt%
2o
3, 20wt% ~ 45wt% B
2o
3with the SiO of 10wt% ~ 25wt%
2composition.
Preferably, described Ba-Zn-B-Si glass is by the Ba of 10wt% ~ 45wt%
2o
3, 10wt% ~ 50wt% the B of ZnO, 10wt% ~ 45wt%
2o
3with the SiO of 10wt% ~ 25wt%
2composition.
Preferably, described Bi-Zn-B-Si glass is by the Bi of 10wt% ~ 40wt%
2o
3, 10wt% ~ 50wt% the B of ZnO, 10wt% ~ 45wt%
2o
3with the SiO of 10wt% ~ 25wt%
2composition.
Present invention also offers a kind of preparation method of low-temperature co-burning ceramic material, comprise the following steps:
By BaO, ZnO and TiO
2mixing, pre-burning after ball milling, obtains pottery and burns block, described pottery is burnt block and pulverizes, obtain ceramics powder;
By ZnO and B
2o
3mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B and help burning glass powder;
By ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B-Si and help burning glass powder;
By BaO, Bi
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Ba-B-Si and help burning glass powder;
By Bi
2o
3, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Bi-B-Si and help burning glass powder;
By Ba
2o
3, ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Ba-Zn-B-Si and help burning glass powder;
By Bi
2o
3, ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Bi-Zn-B-Si and help burning glass powder;
Described Zn-B is helped burn glass, Zn-B-Si help burn glass, Ba-B-Si help burn glass, Bi-B-Si help burn glass, Ba-Zn-B-Si help burn glass and Bi-Zn-B-Si help burn in glass one or more mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
Preferably, in the step preparing ceramics powder, the time of described ball milling is 6 ~ 24h, and the temperature of pre-burning is 950 ~ 1200 DEG C, 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
2composition; 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.Compared with existing stupalith, the present invention is with BaO, ZnO and TiO
2component is ceramic raw material, BaO and TiO
2the pottery formed has excellent microwave dielectric property, but sintering temperature is higher, and ZnO adds the sintering temperature that obviously can reduce pottery, obtains dielectric properties better and the lower pottery of sintering temperature; Help burning glass to have lower sintering temperature, and help the part of atoms of burning in glass identical with the part of atoms in ceramic matrix or close; Simultaneously by controlling pottery and helping the content burning glass, thus obtain the low-temperature co-burning ceramic material with medium dielectric constant microwave medium.
Experimental result shows, low-temperature co-fired ceramic powder prepared by the present invention can realize fine and close one-tenth porcelain at 850 ~ 930 DEG C, and specific inductivity is 30 ~ 45, and loss tangent is less than 0.008, temperature coefficient of resonance frequency is less than ± 50ppm/ DEG C, can realize the common burning with Cu, Ag electrode.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of 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
2composition;
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 mainly burns altogether with silver electrode, and the common burning temperature of described silver electrode is generally at about 850 DEG C, and therefore the sintering temperature of low-temperature co-burning ceramic material is then 850 DEG C ~ 950 DEG C.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, therefore the application is adjusted with helping the selection of burning glass and content by pottery, reaches the requirement of LTCC technology to material.
According to the present invention, the content of described pottery is 79wt% ~ 95wt%, is preferably 85wt% ~ 95wt%, is more preferably 85wt% ~ 93wt%.If the too high levels of pottery, be then difficult to the requirement meeting sintering temperature, if ceramic temperature is too low, the specific inductivity of stupalith can be made sharply to reduce.The described content helping burning glass is 5wt% ~ 21wt%, is preferably 7 ~ 20wt%, is more preferably 7wt% ~ 18wt%, is more preferably 7wt% ~ 15wt%, most preferably be 10wt% ~ 15wt%.If described in help and burn the too high levels of glass, then the dielectric properties of severe exacerbation pottery, if help the content burning glass too low, then cause sintering temperature not reach requirement.
Pottery described in the present invention is by BaO, ZnO and TiO
2composition, BaO and TiO
2the pottery formed has excellent microwave dielectric property, but sintering temperature is higher, and ZnO adds the sintering temperature that obviously can reduce pottery, and itself and TiO
2the stupalith formed 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.Preferably, 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, preferably by the B of ZnO and the 30wt% ~ 80wt% of 20wt% ~ 70wt% in the present invention
2o
3composition.Described ZnO is preferably 30wt% ~ 60wt%, is more preferably 45wt% ~ 55wt%; Described B
2o
3be preferably 40wt% ~ 70wt%, be more preferably 45wt% ~ 55wt%.
Described Zn-B-Si glass is preferably by the B of ZnO, 20wt% ~ 75wt% of 10wt% ~ 60wt%
2o
3with the SiO of 10wt% ~ 40wt%
2composition.Described ZnO is preferably 15wt% ~ 50wt%, is more preferably 25wt% ~ 40wt%; Described B
2o
3be preferably 30wt% ~ 65wt%, be more preferably 50wt% ~ 60wt%; Described SiO
2be preferably 10wt% ~ 30wt%, be more preferably 10wt% ~ 20wt%.
Described Ba-B-Si glass is preferably by the B of BaO, 40wt% ~ 65wt% of 20wt% ~ 50wt%
2o
3with the SiO of 10wt% ~ 20wt%
2composition.Wherein, described BaO is preferably 30wt% ~ 50wt%, is more preferably 40wt% ~ 50wt%; Described B
2o
3be preferably 40wt% ~ 60wt%, be 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
3with the SiO of 10wt% ~ 25wt%
2composition; Described Bi
2o
3content be preferably 35wt% ~ 60wt%, be more preferably 40wt% ~ 50wt%; Described B
2o
3be preferably 30wt% ~ 45wt%, be more preferably 30wt% ~ 40wt%; Described SiO
2be preferably 15wt% ~ 25wt%, be more preferably 20wt% ~ 25wt%.
Described Ba-Zn-B-Si glass is preferably by the Ba of 10wt% ~ 45wt%
2o
3, 10wt% ~ 50wt% the B of ZnO, 10wt% ~ 45wt%
2o
3with the SiO of 10wt% ~ 25wt%
2composition; Described Ba
2o
3be preferably 20wt% ~ 40wt%, be more preferably 25wt% ~ 35wt%; Described ZnO is preferably 20wt% ~ 40wt%, is more preferably 25wt% ~ 35wt%; Described B
2o
3be preferably 20wt% ~ 40wt%, be more preferably 20wt% ~ 30wt%; Described SiO
2be preferably 10wt% ~ 20wt%, be more preferably 15wt% ~ 20wt%.
Described Bi-Zn-B-Si glass is preferably by the Bi of 10wt% ~ 40wt%
2o
3, 10wt% ~ 50wt% the B of ZnO, 10wt% ~ 45wt%
2o
3with the SiO of 10wt% ~ 25wt%
2composition; Described Bi
2o
3be preferably 20wt% ~ 40wt%, be more preferably 30wt% ~ 40wt%; Described ZnO is preferably 20wt% ~ 40wt%; Be more preferably 30wt% ~ 40wt%; Described B
2o
3be preferably 15wt% ~ 40wt%, be more preferably 18wt% ~ 30wt%; Described SiO
2be preferably 10wt% ~ 20wt%, be 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 with the part of atoms in ceramic matrix or close, the crystalline structure after burning glass sintering and ceramic matrix is then helped to have 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
2composition; 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 formed has excellent microwave dielectric property, but sintering temperature is higher, and ZnO adds the sintering temperature that obviously can reduce pottery, and itself and TiO
2the stupalith formed 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 there is lower sintering temperature, and help the part of atoms of burning in glass identical with the part of atoms in ceramic matrix or close; Simultaneously by controlling pottery and helping the content burning glass, thus his stupalith low temperature co-fired finally obtained is made to have medium dielectric constant microwave medium.
Present invention also offers the preparation method of above-mentioned low-temperature co-burning ceramic material, comprise the following steps:
By BaO, ZnO and TiO
2mixing, pre-burning after ball milling, obtains pottery and burns block, described pottery is burnt block and pulverizes, obtain ceramics powder;
By ZnO and B
2o
3mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B and help burning glass powder;
By ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B-Si and help burning glass powder;
By BaO, Bi
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Ba-B-Si and help burning glass powder;
By Bi
2o
3, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Bi-B-Si and help burning glass powder;
By Ba
2o
3, ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Ba-Zn-B-Si and help burning glass powder;
By Bi
2o
3, ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Bi-Zn-B-Si and help burning glass powder;
Described Zn-B is helped burn glass, Zn-B-Si help burn glass, Ba-B-Si help burn glass, Bi-B-Si help burn glass, Ba-Zn-B-Si help burn glass and Bi-Zn-B-Si help burn in glass one or more mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
According to the present invention, in the process preparing low-temperature co-burning ceramic material, first prepare ceramics powder and helped burning glass powder, then ceramics powder having been burnt glass powder and mixes with helping, namely obtain low-temperature co-fired ceramic powder.
In the present invention above-mentioned ceramics powder with help burns glass powder preparation sequentially the present invention have no particular limits, first can prepare ceramics powder and also first can prepare and help burning glass powder.In the process preparing ceramics powder, be prepared by the following method:
By BaO, ZnO and TiO
2mixing, pre-burning after ball milling, obtains pottery and burns block, described pottery is burnt block and pulverizes, obtain ceramics powder.
In the process preparing ceramics powder, described BaO, ZnO and TiO
2mol ratio preferably determine according to the mol ratio of each element in formula (I);
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, is more preferably 10 ~ 20h, and after ball milling, the mixed powder obtained by ball milling is preferably dried, to remove the oil-based solvent in mechanical milling process.Then the powder after oven dry is carried out pre-burning, obtain pottery and burn block.The temperature of described pre-burning is preferably 950 ~ 1200 DEG C, is more preferably 1100 ~ 1200 DEG C; The time of described pre-burning is preferably 2 ~ 6h, is more preferably 4 ~ 6h.Finally described pottery is burnt block to pulverize, namely obtain ceramics powder.The particle diameter of described ceramics powder is preferably 0.5 ~ 3 μm, is more preferably 0.5 ~ 2 μm.
According to the present invention, described Zn-B helps burning glass powder, Zn-B-Si helps burning glass powder, Ba-B-Si helps burning glass powder, Bi-B-Si helps burning glass powder, Ba-Zn-B-Si helps burning glass powder to help the preparation method burning glass powder identical with Bi-Zn-B-Si, is raw material difference; Wherein said Zn-B helps the raw material burning glass powder to be ZnO and B
2o
3; Described Zn-B-Si helps the raw material burning glass powder to be ZnO, B
2o
3with SiO
2; Described Ba-B-Si helps the raw material burning glass powder to be BaO, Bi
2o
3with SiO
2; Described Bi-B-Si helps the raw material burning glass powder to be Bi
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; Described Bi-Zn-B-Si helps the raw material burning glass powder to be Bi
2o
3, ZnO, B
2o
3with SiO
2.Help the preparation method burning glass powder for Zn-B, its preparation process is:
By ZnO and B
2o
3mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B and help burning glass powder.
Help in the process of burning glass powder at preparation Zn-B, the time of described ball milling is preferably 6 ~ 24h, is more preferably 10 ~ 15h.Carry out pre-burning after being dried by mixed powder after ball milling, obtain burning block, the temperature of described pre-burning is preferably 450 ~ 650 DEG C, is more preferably 500 ~ 650 DEG C; The time of described pre-burning is preferably 1 ~ 6h, is more preferably 3 ~ 5h.Then glass drop is obtained by after described burning block fusing; The temperature of described fusing is preferably 1450 DEG C ~ 1550 DEG C.Finally help burning glass powder by namely obtaining Zn-B after described glass drop cold quenching, pulverizing.The described particle diameter burning glass powder that helps is preferably 0.5 ~ 3 μm, is more preferably 0.5 ~ 2 μm.
After preparing ceramics powder respectively and helping and burn glass powder, then Zn-B help burn glass, Zn-B-Si help burn glass, Ba-B-Si help burn glass, Bi-B-Si help burn glass, Ba-Zn-B-Si help burn glass and Bi-Zn-B-Si help burn in glass one or more mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
The invention provides a kind of preparation method of low-temperature co-burning ceramic material.In the process preparing low-temperature co-burning ceramic material, prepare ceramics powder respectively and helped burning glass powder, then described ceramics powder having been burnt glass powder and mixes with helping, namely obtain low-temperature co-burning ceramic material.Experimental result shows, low-temperature co-fired ceramic powder prepared by the present invention can realize fine and close one-tenth porcelain at 850 ~ 930 DEG C, and specific inductivity is 30 ~ 45, and loss tangent is less than 0.008, temperature coefficient of resonance frequency is less than ± 50ppm/ DEG C, can realize the common burning with Cu, Ag electrode.
In order to understand the present invention further, be described in detail to low-temperature co-burning ceramic material provided by the invention below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.25mol and 2.75mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm;
By the ZnO powder of 50g and the B of 50g
2o
3powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the glass powder of 0.5 ~ 2 μm;
The described ceramics powder of 87wt% and the described glass powder of 13wt% are loaded mixer, after mixing 2h, obtains low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 2
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.25mol and 2.75mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the glass powder of 0.5 ~ 2 μm.
The described ceramics powder of 89wt% and the described glass powder of 11wt% are loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 3
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.25mol and 4mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the glass powder of 0.5 ~ 2 μm.
The described ceramics powder of 91wt% and the described glass powder of 9wt% are loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 4
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.5mol and 4mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm.
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the glass powder of 0.5 ~ 2 μm.
The described ceramics powder of 88wt% and the described glass powder of 12wt% are loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 5
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.5mol and 4.3mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm.
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the glass powder of 0.5 ~ 2 μm.
The described ceramics powder of 93wt% and the described glass powder of 7wt% are loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 6
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.5mol and 4.3mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm;
By the ZnO powder of 50g and the B of 50g
2o
3powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Zn-B glass powder of 0.5 ~ 2 μm.
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5 ~ 2 μm.
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 loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 7
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.5mol and 4.3mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5 ~ 2 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Ba-Zn-B-Si glass powder of 0.5 ~ 2 μm.
The described ceramics powder of 88wt%, the Bi-B-Si glass powder of 9wt% and the described Ba-Zn-B-Si glass powder of 2wt% are loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 8
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.25mol and 2.75mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described pottery is broken soon, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm;
By the ZnO powder of 50g and the B of 50g
2o
3powder mixes, and adds Virahol and zirconia ball, wet ball grinding 12h; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Zn-B glass powder of 0.5 ~ 2 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5 ~ 2 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Bi-Zn-B-Si glass powder of 0.5 ~ 2 μm;
The described Zn-B glass powder of the described ceramics powder of 85wt%, 2wt%, the described Bi-B-Si glass powder of 8wt% and the described Bi-Zn-B-Si glass powder of 5wt% are loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
Embodiment 9
By the TiO of the BaO powder of 1mol, the ZnO powder of 0.5mol and 4mol
2powder mixes, then adds the deionized water accounting for above-mentioned powder total mass 80%, and mix laggard row planetary ball mill, Ball-milling Time is 6h, obtains mixed powder; At 1100 DEG C of pre-burning 6h after being dried by described mixed powder, obtain ceramic block.Described ceramic block is broken, and planetary ball mill ball-milling medium is Virahol, obtains the ceramics powder of 0.5 ~ 3 μm.
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Bi-B-Si glass powder of 0.5 ~ 2 μm;
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; In 120 DEG C of oven dry after frit discharging after ball milling, after 650 DEG C of pre-burning 4h, become porcelain; Described porcelain being added temperature is in the crucible of 1500 DEG C, and rapid melting becomes glass metal to drip on cold roller.The amorphous glass porcelain that particle diameter is 15 ~ 500 μm is obtained after cold quenching.Pulverized through fluidized bed jet mill by described amorphous glass porcelain, obtain favorable dispersity, particle diameter is the Ba-Zn-B-Si glass powder of 0.5 ~ 2 μm.
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 loaded after mixing 2h in mixer and obtain low-temperature co-fired ceramic powder.
The 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 low-temperature co-burning ceramic material prepared by embodiment 1 ~ 9.
The performance data table of low-temperature co-burning ceramic material prepared by table 1 embodiment 1 ~ 9
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.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 improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (9)
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
2composition, described BaO, ZnO and TiO
2mol ratio determine according to the mol ratio of each element in formula (I):
BaZn
xTi
yO
1+x+2y(I)；
Wherein, 0.15≤x≤0.6,2.5≤y≤4.5;
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 Zn-B glass is by the B of ZnO and the 30wt% ~ 80wt% of 20wt% ~ 70wt%
2o
3composition.
3. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Zn-B-Si glass is by the B of ZnO, 20wt% ~ 75wt% of 10wt% ~ 60wt%
2o
3with the SiO of 10wt% ~ 40wt%
2composition.
4. low-temperature co-burning ceramic material according to claim 1, is characterized in that, described Ba-B-Si glass is by the B of BaO, 40wt% ~ 65wt% of 20wt% ~ 50wt%
2o
3with the SiO of 10wt% ~ 20wt%
2composition.
5. 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
3with the SiO of 10wt% ~ 25wt%
2composition.
6. 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, 10wt% ~ 50wt% the B of ZnO, 10wt% ~ 45wt%
2o
3with the SiO of 10wt% ~ 25wt%
2composition.
7. 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, 10wt% ~ 50wt% the B of ZnO, 10wt% ~ 45wt%
2o
3with the SiO of 10wt% ~ 25wt%
2composition.
8. the preparation method of low-temperature co-burning ceramic material according to claim 1, comprises the following steps:
By BaO, ZnO and TiO
2mixing, pre-burning after ball milling, obtains pottery and burns block, described pottery is burnt block and pulverizes, obtain ceramics powder;
By ZnO and B
2o
3mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B and help burning glass powder;
By ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Zn-B-Si and help burning glass powder;
By BaO, Bi
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Ba-B-Si and help burning glass powder;
By Bi
2o
3, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Bi-B-Si and help burning glass powder;
By Ba
2o
3, ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Ba-Zn-B-Si and help burning glass powder;
By Bi
2o
3, ZnO, B
2o
3with SiO
2mixing, pre-burning after ball milling, obtains burning block, obtains glass drop, pulverize after described burning block fusing, obtain after described glass drop cold quenching Bi-Zn-B-Si and help burning glass powder;
Described Zn-B is helped burn glass, Zn-B-Si help burn glass, Ba-B-Si help burn glass, Bi-B-Si help burn glass, Ba-Zn-B-Si help burn glass and Bi-Zn-B-Si help burn in glass one or more mix with described ceramics powder, obtain low-temperature co-burning ceramic material.
9. preparation method according to claim 8, is characterized in that, in the step preparing ceramics powder, the time of described ball milling is 6 ~ 24h, and the temperature of pre-burning is 950 ~ 1200 DEG C, and the time is 2 ~ 6h.
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| CN107176793B (en) * | 2016-03-11 | 2020-02-14 | 上海卡翱投资管理合伙企业（有限合伙） | LTCC ceramic material and preparation method thereof |
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| CN110950658A (en) * | 2018-09-27 | 2020-04-03 | 湖南嘉业达电子有限公司 | Preparation method of power type piezoelectric ceramic capable of being sintered at low temperature |
| CN109796202A (en) * | 2019-03-25 | 2019-05-24 | 电子科技大学 | A kind of high-performance low-temperature sintered lamination type piezoresistor material |
| CN110143812A (en) * | 2019-06-09 | 2019-08-20 | 杭州电子科技大学 | A kind of low-k low-temperature co-burning ceramic material and preparation method |
| CN113045314A (en) * | 2019-12-27 | 2021-06-29 | 奇力新电子股份有限公司 | Thin ceramic powder suitable for high-frequency assembly |
| CN112028491A (en) * | 2020-08-11 | 2020-12-04 | 安徽蓝讯新材料科技有限公司 | Linear array image sensor packaging method based on high-temperature co-fired ceramic |
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