CN107555803A - A kind of glass powder, its preparation method and application - Google Patents
A kind of glass powder, its preparation method and application Download PDFInfo
- Publication number
- CN107555803A CN107555803A CN201710856393.XA CN201710856393A CN107555803A CN 107555803 A CN107555803 A CN 107555803A CN 201710856393 A CN201710856393 A CN 201710856393A CN 107555803 A CN107555803 A CN 107555803A
- Authority
- CN
- China
- Prior art keywords
- powder
- glass
- alumina
- glass powder
- oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of glass powder, include the composition of following weight/mass percentage composition：Silica 20~60%, calcium oxide 8~16%, barium monoxide 8~16%, aluminum oxide 14~28%.Glass powder of the present invention can be applied in alumina powder, reduce its sintering temperature, so that it preferably forms common burning with zirconium oxide.The invention also discloses a kind of preparation method and applications of the glass powder simultaneously.Zirconium oxide and aluminum oxide matching co-firing alumina powder prepared by the present invention, due to the mobility of melten glass powder in sintering process, promote the liquid-phase sintering of ceramics, the pricker cooperation of the melten glass compacted zone for helping that there is high-bond in the formation of zirconium aluminium interface, the bending strength of common burning porcelain can be significantly increased.
Description
Technical field
The present invention relates to a kind of powder, its preparation method and application, especially a kind of glass powder, its preparation method and should
With.
Background technology
In multilayer ceramic electronic component field, heterogeneous burn altogether between unlike material material is that research and development prepare high-performance member
The crucial matter of science and technology of device, it is desirable to be tightly combined between dissimilar materials, interface is smooth, mutually expands without significant heterosphere
Phenomena such as dissipating, being layered and ftracture, come off.
Traditional alumina insulating layer and YSZ zirconium oxides (yttrium stable zirconium oxide) matrix high temperature is heterogeneous burn altogether during,
Because the two material sintering shrinkage mismatches, it is easily caused alumina-zirconia ceramics and occurs interface debonding, outer after the completion of common burning
The defects of seeing buckling deformation, product size precision is influenceed, and phenomena such as fracture, defect easily occur in application.
Mismatch phenomenon is burnt altogether in order to improve alumina-zirconia, addition low melting point oxide is often taken in industry, improves production
Product structure design uses the multiple means such as special preparation technique, regulates and controls Al2O3And ZrO2Common burning Shrinkage behavior, realize both
Co-fire match.For example, Zhang Rongrong of Tongji University et al. prepares nanoscale YSZ powders using solvent-thermal method, meanwhile, in Al2O3
Middle addition CaO, MgO and SiO2Deng mixed sintering auxiliary agent, Al is reduced2O3Sintering temperature；On this basis, α phases in powder are adjusted
Change its sintering shrinkage with the ratio of γ phases, finally realize Al2O3With matching co-firing of the YSZ ceramics in the range of 1400 DEG C.China
Methods of the Wang Xiao Die of middle University of Science and Technology et al. by changing green compact useful load and adding sintering aid, increases Al2O3Sintering receive
Shrinkage, while using the means such as increase YSZ transition zones and pressure limit sintering, reduce Al2O3Lost with the sintering of zirconia ceramics
Match somebody with somebody, obtained that buckling deformation is small, the heterogeneous multi-layer ceramics of microcosmic no layering.
At present, existing alumina-zirconia co-fire match solves technological means, and cost is high, complex process, and unfavorable
In realize mass prepare.
The content of the invention
Based on this, a kind of glass powder is provided it is an object of the invention to overcome above-mentioned the deficiencies in the prior art part,
The glass powder can be applied in alumina powder, reduce its sintering temperature, so that it is preferably formed altogether with zirconium oxide
Burn.
To achieve the above object, the technical solution used in the present invention is：A kind of glass powder, including following quality percentage
The composition of content：Silica 20~60%, calcium oxide 8~16%, barium monoxide 8~16%, aluminum oxide 14~28%.
Each composition collective effect in glass powder of the present invention, the effect for preferably reducing sintering temperature can be played, its
In, SiO2It is glass network former oxide, is the main framework composition of glass, there is high-melting-point, high viscosity, low-thermal-expansion
Coefficient and high chemical stability；CaO is glass ectosome ion-oxygen compound, has strong polarizability, can weaken silicon in glass
The intermolecular forces of oxygen key, the high temperature viscosity of glass is reduced, reduce glass melting point, mainly play fluxing action；BaO be glass ectosome from
Sub- oxide, glass melting point can be effectively reduced, mainly plays fluxing action；Al2O3For glass intermediate oxide, help to connect
The network structure of glass, increase glass viscosity and mechanical strength, improve glass melting point.
Preferably, the glass powder also includes magnesia, quality percentage of the magnesia in the glass powder
Content is 8~16%.
MgO introduces frequently as network-modifying ion oxide in glass, can reduce devitrification of glass tendency, reduce glass
Viscosity and fusing point, the temperature flowing of reinforcing glass.
Preferably, the glass powder also includes titanium oxide, quality percentage of the titanium oxide in the glass powder
Content is 1~2%.
TiO2Introduce as nucleator oxide, when adding on a small quantity, can be promoted in the form of heterogeneous nucleation in glass
The crystallization of glass, improve the mechanical strength and insulation characterisitic of glass.
Preferably, the glass powder also includes zirconium oxide, quality percentage of the zirconium oxide in the glass powder
Content is 1~2%.
ZrO2Introduce as nucleator oxide, when adding on a small quantity, can be promoted in the form of heterogeneous nucleation in glass
The crystallization of glass, improve the mechanical strength and insulation characterisitic of glass.
Preferably, the silica, aluminum oxide, calcium oxide, magnesia, barium monoxide, titanium oxide, the particle diameter of zirconium oxide are equal
No more than 15 μm, purity is that analysis is pure；The particle diameter of the titanium oxide is not more than 10 μm, and purity is that analysis is pure；The oxidation
The particle diameter of zirconium is not more than 1 μm, and purity is that analysis is pure.
Meanwhile the present invention also provides a kind of preparation method of the glass powder, comprises the following steps：
(1) by each composition mixing, ball milling, drying, the crushing in glass powder, powder is obtained；
(2) by powder obtained by step (1) in air atmosphere, 1350~1450 DEG C are heated to, is incubated, then be cooled to 1160
~1220 DEG C, the powder after cooling is subjected to water quenching, then the powder after water quenching is sieved, made annealing treatment, that is, obtains this
Invent the glass powder.
Preferably, in the step (2), 1350~1450 DEG C are heated to 2~8 DEG C/min heating rate, insulation 2~
6 hours, then it is cooled to 1160~1220 DEG C with 1~3 DEG C/min speed.
Preferably, in the step (1), the process of ball milling is：Using absolute ethyl alcohol as ball-milling medium, by the glass powder
Each composition is added in ball grinder, ball milling 8~16 hours.
Preferably, in the step (1), the process of drying is：Powder after ball milling is dried 10 hours at 100 DEG C.
Preferably, in the step (2), the process of sieving is：Powder after water quenching is crossed into 200 eye mesh screens.
Preferably, in the step (2), the process of annealing is：By the powder after sieving in 500~600 DEG C of annealing
Processing 6 hours.
In addition, the present invention also provides a kind of alumina powder for including the glass powder.Alumina powder of the present invention, by
In with the addition of frit, making the reduction of its sintering temperature, common burning can be preferably formed with zirconium oxide.
Preferably, in the alumina powder, the weight/mass percentage composition of the alumina powder is 95~98%, the glass
The weight/mass percentage composition of glass powder is 2~5%.
In mixed system, aluminum oxide is function phase, and the electric property, mechanical performance with powder are closely related；Aluminum oxide
Too high levels can cause powder sintering temperature to improve, and alumina content reduces, then can deteriorate material property, for example make the exhausted of material
Edge resistivity reduces, and thermal coefficient of expansion increase, rupture strength reduces, therefore selective oxidation aluminium content is 95~98%；Glass group
Point mainly play a part of it is fluxing, reduce sintering temperature and increase ceramic layer is shown in adhesion, but material can be deteriorated during too high levels
Performance, therefore content is 2~5%.
Preferably, the particle diameter of the alumina powder is not more than 1 μm, and purity is pure to analyze.
Meanwhile the present invention also provides a kind of preparation method of above-mentioned alumina powder, methods described is：By alumina powder and
Glass dust ball milling, drying, sieving, obtain the alumina powder.
Furthermore it is noted that above-mentioned ball milling, drying, the process of sieving can be the process that be described above of the present invention,
Those skilled in the art can also be according to carry out conventional selection be actually needed, and the present invention is not particularly limited to this.
Again, the present invention also provides a kind of alumina slurry for including the alumina powder.The alumina slurry can
Burnt altogether with being realized well with zirconium oxide.
Preferably, the alumina slurry includes the composition of following parts by weight：100 parts of alumina powder, ethanol 30~40
Part, 20~35 parts of triethanolamine, 10~15 parts of polyvinyl butyral resin, 3~6 parts of BBP(Butyl Benzyl Phthalate.
Equally, the present invention also provides a kind of preparation method of above-mentioned alumina slurry, comprises the following steps：In ball mill
Add ethanol, triethanolamine, after 15~30min of ball milling, then add into ball mill alumina powder, polyvinyl butyral resin,
BBP(Butyl Benzyl Phthalate, ball milling 8~16 hours, obtains the alumina slurry.The oxidation aluminium paste prepared by this method, technique
Simply, available for the matching co-firing for realizing zirconium oxide and aluminium oxide ceramics, common burning porcelain is tightly combined, interface is smooth, outward appearance without
Buckling deformation.
The present invention also provides a kind of alumina powder and is preparing zirconium oxide and aluminum oxide altogether in burning alumina slurry
Application.
Relative to prior art, beneficial effects of the present invention are：
Glass powder of the present invention can be applied in alumina powder, reduce its sintering temperature, so that itself and oxidation
Zirconium is preferably formed to be burnt altogether.Zirconium oxide prepared by the present invention and aluminum oxide matching co-firing alumina powder, in sintering process
Due to the mobility of melten glass powder, the liquid-phase sintering of ceramics is promoted, the pricker cooperation of melten glass is with contributing in Gao Lv circle
Face forms the compacted zone with high-bond, can significantly increase the bending strength of common burning porcelain.
Compared with existing zirconium oxide/aluminum oxide altogether burning alumina slurry, alumina slurry of the present invention, which has, substantially to be changed
Kind interface leveling effect, obtains interface cohesion densification, no cracking, the substrate sample without warpage after burning altogether.
Brief description of the drawings
Fig. 1 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 1；
Fig. 2 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 2；
Fig. 3 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 3；
Fig. 4 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 4；
Fig. 5 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 5；
Fig. 6 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 6；
Fig. 7 is the section SEM microstructure figures of zirconium aluminium common burning porcelain sample in embodiment 7.
Embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with the drawings and specific embodiments pair
The present invention is described further.
Embodiment 1
A kind of embodiment of glass powder of the present invention, the composition of glass powder described in the present embodiment and each component content
It is shown in Table 1.
The composition and content of glass powder in the embodiment 1 of table 1
The preparation of glass powder：Glass frit component and its quality proportioning as described in table 1, weigh corresponding oxidation raw material, with
Absolute ethyl alcohol is ball-milling medium, the raw material weighed is added in ball grinder, ball milling 8h；In an oven in 100 DEG C of drying after discharging
10h.Take out drying after powder ground in alms bowl is ground, be put into 99 aluminum crucibles, in Muffle furnace, under air atmosphere with 3 DEG C/
Min heating rate is heated to 1400 DEG C, is incubated 4 hours, then is cooled to 1200 DEG C with 1 DEG C/min speed, is taken at 1200 DEG C
The frit water quenching gone out in crucible.The frit of water quenching is ground, crosses 200 eye mesh screens, 6 hours obtained glass of being annealed at 500 DEG C
Powder.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：285g aluminum oxide and 15g frit are weighed, is mixed
Planetary ball mill ball milling 8h is added with 360mL absolute ethyl alcohol after conjunction and obtain mixed grinding slurry, by mixed grinding slurry in 100
DEG C drying 12h, takes out the powder after drying and is ground in alms bowl is ground, cross 200 eye mesh screens, zirconium oxide and aluminum oxide is made burns altogether and uses oxygen
Change aluminium powder material.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
30wt% ethanol, and alumina powder quality 20wt% triethanolamine is accounted for, 20min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 10wt%, and account for oxidation
Aluminium powder quality 3wt% BBP(Butyl Benzyl Phthalate, after ball milling 8h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, can realize and 5YSZ (addition 5mol%Y2O3ZrO2) between
Matching co-firing, co-fired temperature be 1450 DEG C.Common burning sample is scanned Electronic Micro-Analysis and obtains the amplification 400 of its section
SEM image again, as shown in Figure 1.In Fig. 1, intermediate layer is the Al added with glass ingredient2O3Layer, levels are 5YSZ layers, can
See Al2O3Interface is smooth after being burnt altogether with YSZ and is tightly combined, and sample appearance is without obvious warpage and deformation, and through measurement, sample resists
Roll over intensity >=300MPa.
Embodiment 2
A kind of embodiment of glass powder of the present invention, the composition of glass powder described in the present embodiment and each component content
It is shown in Table 2.
The composition and content of glass powder in the embodiment 2 of table 2
The preparation of glass powder：Glass frit component and its quality proportioning as described in table 2, weigh corresponding oxidation raw material, with
Absolute ethyl alcohol is ball-milling medium, the raw material weighed is added in ball grinder, ball milling 16h；In an oven in 100 DEG C of drying after discharging
10h.Take out drying after powder ground in alms bowl is ground, be put into 99 aluminum crucibles, in Muffle furnace, under air atmosphere with 2 DEG C/
Min heating rate is heated to 1350 DEG C, is incubated 2 hours, then is cooled to 1160 DEG C with 1 DEG C/min speed, is taken at 1160 DEG C
The frit water quenching gone out in crucible.The frit of water quenching is ground, crosses 200 eye mesh screens, 6 hours obtained glass of being annealed at 600 DEG C
Powder.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：285g aluminum oxide and 15g frit are weighed, is mixed
Planetary ball mill ball milling 8h is added with 360mL absolute ethyl alcohol after conjunction and obtain mixed grinding slurry, by mixed grinding slurry in 100
DEG C drying 12h, takes out the powder after drying and is ground in alms bowl is ground, cross 200 eye mesh screens, zirconium oxide and aluminum oxide is made burns altogether and uses oxygen
Change aluminium powder material.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
40wt% ethanol, and alumina powder quality 35wt% triethanolamine is accounted for, 30min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 15wt%, and account for oxidation
Aluminium powder quality 6wt% BBP(Butyl Benzyl Phthalate, after ball milling 16h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, can realize and 5YSZ (addition 5mol%Y2O3ZrO2) between
Matching co-firing, co-fired temperature be 1440 DEG C.Common burning sample is scanned Electronic Micro-Analysis and obtains the amplification 400 of its section
SEM image again, as shown in Figure 2.In Fig. 2, upper strata is the Al added with glass ingredient2O3Layer, lower floor is 5YSZ layers, it is seen that
Al2O3Interface is smooth after being burnt altogether with YSZ and is tightly combined.Sample appearance will measure, the anti-folding of sample without obvious warpage and deformation
Intensity >=290MPa.
Embodiment 3
A kind of embodiment of glass powder of the present invention, the composition of glass powder described in the present embodiment and each component content
It is shown in Table 3.
The composition and content of glass powder in the embodiment 3 of table 3
The preparation of glass powder：Glass frit component and its quality proportioning as described in table 3, weigh corresponding oxidation raw material, with
Absolute ethyl alcohol is ball-milling medium, the raw material weighed is added in ball grinder, ball milling 10h；In an oven in 100 DEG C of drying after discharging
10h.Take out drying after powder ground in alms bowl is ground, be put into 99 aluminum crucibles, in Muffle furnace, under air atmosphere with 8 DEG C/
Min heating rate is heated to 1450 DEG C, is incubated 6 hours, then is cooled to 1220 DEG C with 3 DEG C/min speed, is taken at 1220 DEG C
The frit water quenching gone out in crucible.The frit of water quenching is ground, crosses 200 eye mesh screens, 6 hours obtained glass of being annealed at 500 DEG C
Powder.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：285g aluminum oxide and 15g frit are weighed, is mixed
Planetary ball mill ball milling 8h is added with 360mL absolute ethyl alcohol after conjunction and obtain mixed grinding slurry, by mixed grinding slurry in 100
DEG C drying 12h, takes out the powder after drying and is ground in alms bowl is ground, cross 200 eye mesh screens, zirconium oxide and aluminum oxide is made burns altogether and uses oxygen
Change aluminium powder material.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
35wt% ethanol, and alumina powder quality 30wt% triethanolamine is accounted for, 30min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 12wt%, and account for oxidation
Aluminium powder quality 5wt% BBP(Butyl Benzyl Phthalate, after ball milling 12h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, can realize and 5YSZ (addition 5mol%Y2O3ZrO2) between
Matching co-firing, co-fired temperature be 1420 DEG C.Common burning sample is scanned Electronic Micro-Analysis and obtains the amplification 400 of its section
SEM image again, as shown in Figure 3.In Fig. 3, upper strata is the Al added with glass ingredient2O3Layer, lower floor is 5YSZ layers, it is seen that
Al2O3Interface is smooth after being burnt altogether with YSZ and is tightly combined.Sample appearance is without obvious warpage and deformation, through measurement, the anti-folding of sample
Intensity >=280MPa.
Embodiment 4
A kind of embodiment of glass powder of the present invention, the composition of glass powder and component content are shown in described in the present embodiment
Table 4.
The composition and content of glass powder in the embodiment 4 of table 4
The preparation of glass powder：Glass frit component and its quality proportioning as described in table 4, weigh corresponding oxidation raw material, with
Absolute ethyl alcohol is ball-milling medium, the raw material weighed is added in ball grinder, ball milling 10h；In an oven in 100 DEG C of drying after discharging
10h.Take out drying after powder ground in alms bowl is ground, be put into 99 aluminum crucibles, in Muffle furnace, under air atmosphere with 3 DEG C/
Min heating rate is heated to 1400 DEG C, is incubated 4 hours, then is cooled to 1200 DEG C with 1 DEG C/min speed, is taken at 1200 DEG C
The frit water quenching gone out in crucible.The frit of water quenching is ground, crosses 200 eye mesh screens, 6 hours obtained glass of being annealed at 500 DEG C
Powder.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：288g aluminum oxide and 12g frit are weighed, is mixed
Planetary ball mill ball milling 8h is added with 360mL absolute ethyl alcohol after conjunction and obtain mixed grinding slurry, by mixed grinding slurry in 100
DEG C drying 12h, takes out the powder after drying and is ground in alms bowl is ground, cross 200 eye mesh screens, zirconium oxide and aluminum oxide is made burns altogether and uses oxygen
Change aluminium powder material.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
35wt% ethanol, and alumina powder quality 30wt% triethanolamine is accounted for, 30min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 12wt%, and account for oxidation
Aluminium powder quality 5wt% BBP(Butyl Benzyl Phthalate, after ball milling 12h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, can realize and 5YSZ (addition 5mol%Y2O3ZrO2) between
Matching co-firing, co-fired temperature be 1460 DEG C.Common burning sample is scanned Electronic Micro-Analysis and obtains the amplification 400 of its section
SEM image again, as shown in Figure 4.In Fig. 4, upper strata is the Al added with glass ingredient2O3Layer, lower floor is 5YSZ layers, it is seen that altogether
Al after burning2O3Smooth with YSZ interfaces and be tightly combined, sample appearance is without obvious warpage and deformation, and through measurement, the anti-folding of sample is strong
Degree >=310MPa.
Embodiment 5
A kind of embodiment of glass powder of the present invention, the composition of glass powder described in the present embodiment and each component content
It is shown in Table 5.
The composition and content of glass powder in the embodiment 5 of table 5
The preparation of glass powder：Glass frit component and its quality proportioning as described in table 5, weigh corresponding oxidation raw material, with
Absolute ethyl alcohol is ball-milling medium, the raw material weighed is added in ball grinder, ball milling 10h；In an oven in 100 DEG C of drying after discharging
10h.Take out drying after powder ground in alms bowl is ground, be put into 99 aluminum crucibles, in Muffle furnace, under air atmosphere with 3 DEG C/
Min heating rate is heated to 1400 DEG C, is incubated 4 hours, then is cooled to 1200 DEG C with 1 DEG C/min speed, is taken at 1200 DEG C
The frit water quenching gone out in crucible.The frit of water quenching is ground, crosses 200 eye mesh screens, 6 hours obtained glass of being annealed at 500 DEG C
Powder.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：291g aluminum oxide and 9g frit are weighed, is mixed
Planetary ball mill ball milling 8h is added with 360mL absolute ethyl alcohol after conjunction and obtain mixed grinding slurry, by mixed grinding slurry in 100
DEG C drying 12h, takes out the powder after drying and is ground in alms bowl is ground, cross 200 eye mesh screens, zirconium oxide and aluminum oxide is made burns altogether and uses oxygen
Change aluminium powder material.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
35wt% ethanol, and alumina powder quality 30wt% triethanolamine is accounted for, 30min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 12wt%, and account for oxidation
Aluminium powder quality 5wt% BBP(Butyl Benzyl Phthalate, after ball milling 12h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, can realize and 5YSZ (addition 5mol%Y2O3ZrO2) between
Matching co-firing, co-fired temperature be 1480 DEG C.Common burning sample is scanned Electronic Micro-Analysis and obtains the amplification 400 of its section
SEM image again, as shown in Figure 5.In Fig. 5, intermediate layer is the Al added with glass ingredient2O3Layer, levels are 5YSZ layers, can
See Al after common burning2O3It is smooth with YSZ interfaces, but be slightly layered, this is mainly and Al2O3Amount of glassy phase is relatively low relevant in layer；Sample
Outward appearance is without obvious warpage and deformation, through measurement, sample rupture strength >=335MPa.
Embodiment 6
A kind of embodiment of glass powder of the present invention, the composition of glass powder described in the present embodiment and each component content
It is shown in Table 6.
The composition and content of glass powder in the embodiment 6 of table 6
The preparation of glass powder：Glass frit component and its quality proportioning as described in table 6, weigh corresponding oxidation raw material, with
Absolute ethyl alcohol is ball-milling medium, the raw material weighed is added in ball grinder, ball milling 10h；In an oven in 100 DEG C of drying after discharging
10h.Take out drying after powder ground in alms bowl is ground, be put into 99 aluminum crucibles, in Muffle furnace, under air atmosphere with 3 DEG C/
Min heating rate is heated to 1400 DEG C, is incubated 4 hours, then is cooled to 1200 DEG C with 1 DEG C/min speed, is taken at 1200 DEG C
The frit water quenching gone out in crucible.The frit of water quenching is ground, crosses 200 eye mesh screens, 6 hours obtained glass of being annealed at 500 DEG C
Powder.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：294g aluminum oxide and 6g frit are weighed, is mixed
Planetary ball mill ball milling 8h is added with 360mL absolute ethyl alcohol after conjunction and obtain mixed grinding slurry, by mixed grinding slurry in 100
DEG C drying 12h, takes out the powder after drying and is ground in alms bowl is ground, cross 200 eye mesh screens, zirconium oxide and aluminum oxide is made burns altogether and uses oxygen
Change aluminium powder material.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
35wt% ethanol, and alumina powder quality 30wt% triethanolamine is accounted for, 30min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 12wt%, and account for oxidation
Aluminium powder quality 5wt% BBP(Butyl Benzyl Phthalate, after ball milling 12h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, can realize and 5YSZ (addition 5mol%Y2O3ZrO2) between
Matching co-firing, co-fired temperature be 1500 DEG C.Common burning sample is scanned Electronic Micro-Analysis and obtains the amplification 400 of its section
SEM image again, as shown in Figure 6.In Fig. 6, intermediate layer is the Al added with glass ingredient2O3Layer, levels are 5YSZ layers, can
See Al after common burning2O3Reduced with YSZ interfaces flatness, and have lamination, this is mainly and Al2O3Amount of glassy phase is relatively low in layer
It is relevant；Sample appearance is without obvious warpage and deformation, through measurement, sample rupture strength >=350MPa.
Embodiment 7
A kind of embodiment of glass powder of the present invention is not added with, alumina powder is pure alumina system.
Zirconium oxide burns the preparation with alumina powder with aluminum oxide altogether：300g alumina powder is weighed, the nothing with 360mL
Water-ethanol adds planetary ball mill ball milling 8h and obtains mixed grinding slurry, and mixed grinding slurry is dried into 12h in 100 DEG C, taken out
Powder after drying is ground in alms bowl is ground, and crosses 200 eye mesh screens, and zirconium oxide is made and aluminum oxide burns use alumina powder altogether.
Zirconium oxide burns the preparation with alumina slurry with aluminum oxide altogether：Addition accounts for alumina powder (containing glass powder) quality
35wt% ethanol, and alumina powder quality 30wt% triethanolamine is accounted for, 30min is mixed in ball mill；Add and contain
There is the alumina powder of glass powder, and add the polyvinyl butyral resin for accounting for alumina powder quality 12wt%, and account for oxidation
Aluminium powder quality 5wt% BBP(Butyl Benzyl Phthalate, after ball milling 12h, take out, be made to match with aluminum oxide for zirconium oxide and be total to
The alumina slurry of burning.
Using alumina slurry made from the present embodiment, sintering temperature is 1600 DEG C, it is difficult to is realized and 5YSZ (additions
5mol%Y2O3ZrO2) between matching co-firing.Sample after sintering is scanned Electronic Micro-Analysis and obtains putting for its section
Big 400 times of SEM image, as shown in Figure 7.In Fig. 7, intermediate layer Al2O3Layer, levels are 5YSZ layers, it is seen that after sintering
Al2O3It is bad with YSZ interfaces flatness, and have obvious lamination；Through measurement, sample rupture strength >=230MPa.
Embodiment 8
YSZ green tape surface of the alumina slurry that embodiment 1~7 is prepared after curtain coating through silk-screen printing, lamination,
Isostatic pressed, cutting and altogether burn process zirconium aluminium co-fired ceramic substrate is made.Using the anti-folding of three point bending test method test substrate sample
Intensity, reference standard are that JC/T676-1997 glass material bending strength test methods measure to its rupture strength, specifically
The performance parameter measurement result that the zirconium oxide of embodiment 1~7 burns sample with aluminum oxide altogether is shown in Table 7.
The zirconium oxide of 7 embodiment of table 1~7 burns the performance parameter of sample with aluminum oxide altogether
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Co-fired temperature (DEG C) | 1450 | 1440 | 1420 | 1460 | 1480 | 1500 | 1600 |
| Rupture strength (MPa) | 300 | 290 | 280 | 310 | 335 | 350 | 230 |
It was found from embodiment 1~7, by composition and its glass powder the containing in alumina powder for adjusting glass powder
Amount, the design and preparation of zirconium oxide and aluminum oxide matching co-firing alumina powder and its slurry, the oxidation aluminium paste can be realized
Material can form good matching co-firing with YSZ in 1420~1500 DEG C of temperature ranges.
Meanwhile compared with existing zirconium aluminium burns powder technology altogether, present invention process is simple, it is easy to accomplish, cost is low；And pass through
The zirconium aluminium base sample for burning obtain altogether is crossed, interface is smooth, is tightly combined, and sample appearance is strong without obvious warpage and deformation, anti-folding
Degree >=280MPa, it is well positioned to meet zirconium aluminium base application requirement.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope is protected, although being explained in detail with reference to preferred embodiment to the present invention, one of ordinary skill in the art should
Understand, technical scheme can be modified or equivalent substitution, without departing from the essence of technical solution of the present invention
And scope.
Claims (10)
1. a kind of glass powder, it is characterised in that include the composition of following weight/mass percentage composition：Silica 20~60%, oxygen
Change calcium 8~16%, barium monoxide 8~16%, aluminum oxide 14~28%.
2. glass powder as claimed in claim 1, it is characterised in that also including magnesia, the magnesia is in the glass
Weight/mass percentage composition in powder is 8~16%.
3. glass powder as claimed in claim 1 or 2, it is characterised in that also comprising titanium oxide, the titanium oxide is in the glass
Weight/mass percentage composition in glass powder is 1~2%.
4. glass powder as claimed in claim 1 or 2, it is characterised in that also comprising zirconium oxide, the zirconium oxide is in the glass
Weight/mass percentage composition in glass powder is 1~2%.
5. a kind of preparation method of the glass powder as described in any one of Claims 1 to 4, it is characterised in that comprise the following steps：
(1) by each composition mixing, ball milling, drying, the crushing in glass powder, powder is obtained；
(2) by powder obtained by step (1) in air atmosphere, it is heated to 1350~1450 DEG C, insulation, then it is cooled to 1160~
1220 DEG C, the powder after cooling is subjected to water quenching, then the powder after water quenching is sieved, made annealing treatment, that is, obtains this hair
The bright glass powder.
A kind of 6. alumina powder for including the glass powder as described in any one of Claims 1 to 4.
7. alumina powder as claimed in claim 6, it is characterised in that in the alumina powder, the alumina powder
Weight/mass percentage composition be 95~98%, the weight/mass percentage composition of the glass powder is 2~5%.
A kind of 8. alumina slurry for including alumina powder as claimed in claims 6 or 7.
9. alumina slurry as claimed in claim 8, it is characterised in that include the composition of following parts by weight：Alumina powder
100 parts, 30~40 parts of ethanol, 20~35 parts of triethanolamine, 10~15 parts of polyvinyl butyral resin, BBP(Butyl Benzyl Phthalate 3
~6 parts.
10. a kind of alumina powder as claimed in claims 6 or 7 is preparing zirconium oxide and aluminum oxide burning alumina slurry altogether
In application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710856393.XA CN107555803A (en) | 2017-09-19 | 2017-09-19 | A kind of glass powder, its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710856393.XA CN107555803A (en) | 2017-09-19 | 2017-09-19 | A kind of glass powder, its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107555803A true CN107555803A (en) | 2018-01-09 |
Family
ID=60982300
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710856393.XA Pending CN107555803A (en) | 2017-09-19 | 2017-09-19 | A kind of glass powder, its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107555803A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110304911A (en) * | 2019-05-06 | 2019-10-08 | 北京元六鸿远电子科技股份有限公司 | The continuously adjustable low-temperature co-burning ceramic material of thermal expansion coefficient and preparation method |
| CN111792932A (en) * | 2020-03-30 | 2020-10-20 | 镇江锆源传感科技有限公司 | Preparation method of zirconia and alumina casting green body co-fired sintered sheet layer |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1356288A (en) * | 2000-11-29 | 2002-07-03 | 株式会社村田制作所 | Glass-ceramic composition for ceramic-type electromic element, ceramic-type electronic element and process for preparing malti-layer ceramic-type electronic element |
| US20070281851A1 (en) * | 2006-06-06 | 2007-12-06 | Karine Seneschal-Merz | Sintered glass ceramic and method for producing the same |
| CN102030477A (en) * | 2009-10-07 | 2011-04-27 | 旭硝子株式会社 | Ceramic material composition |
| CN102219386A (en) * | 2011-05-16 | 2011-10-19 | 武汉理工大学 | Preparation method for ultrafine powder body of SiO2-based composite oxide system glass |
| CN102786294A (en) * | 2012-07-16 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Insulating layer slurry of chip-type oxygen sensor and insulating layer preparation method |
| CN103086703A (en) * | 2013-01-30 | 2013-05-08 | 云南云天化股份有限公司 | Material and method for preparing low-temperature co-fired ceramic with high anti-bending strength |
| CN104129920A (en) * | 2014-07-29 | 2014-11-05 | 研创光电科技（赣州）有限公司 | Co-fired glass ceramic material and preparation method thereof, and method for preparing LED package substrate by utilizing co-fired glass ceramic material |
| CN105271758A (en) * | 2015-09-21 | 2016-01-27 | 江苏科技大学 | 3D packaging LTCC substrate material and preparation method |
| CN105732008A (en) * | 2016-02-17 | 2016-07-06 | 同济大学 | Co-firing method and application of laminated type zirconium oxide and aluminium oxide ceramic |
| CN105859144A (en) * | 2016-03-29 | 2016-08-17 | 西安赛尔电子材料科技有限公司 | Sealing glass powder for electric connectors, preparation method for sealing glass powder and sealing process of sealing glass powder |
-
2017
- 2017-09-19 CN CN201710856393.XA patent/CN107555803A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1356288A (en) * | 2000-11-29 | 2002-07-03 | 株式会社村田制作所 | Glass-ceramic composition for ceramic-type electromic element, ceramic-type electronic element and process for preparing malti-layer ceramic-type electronic element |
| US20070281851A1 (en) * | 2006-06-06 | 2007-12-06 | Karine Seneschal-Merz | Sintered glass ceramic and method for producing the same |
| CN102030477A (en) * | 2009-10-07 | 2011-04-27 | 旭硝子株式会社 | Ceramic material composition |
| CN102219386A (en) * | 2011-05-16 | 2011-10-19 | 武汉理工大学 | Preparation method for ultrafine powder body of SiO2-based composite oxide system glass |
| CN102786294A (en) * | 2012-07-16 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Insulating layer slurry of chip-type oxygen sensor and insulating layer preparation method |
| CN103086703A (en) * | 2013-01-30 | 2013-05-08 | 云南云天化股份有限公司 | Material and method for preparing low-temperature co-fired ceramic with high anti-bending strength |
| CN104129920A (en) * | 2014-07-29 | 2014-11-05 | 研创光电科技（赣州）有限公司 | Co-fired glass ceramic material and preparation method thereof, and method for preparing LED package substrate by utilizing co-fired glass ceramic material |
| CN105271758A (en) * | 2015-09-21 | 2016-01-27 | 江苏科技大学 | 3D packaging LTCC substrate material and preparation method |
| CN105732008A (en) * | 2016-02-17 | 2016-07-06 | 同济大学 | Co-firing method and application of laminated type zirconium oxide and aluminium oxide ceramic |
| CN105859144A (en) * | 2016-03-29 | 2016-08-17 | 西安赛尔电子材料科技有限公司 | Sealing glass powder for electric connectors, preparation method for sealing glass powder and sealing process of sealing glass powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110304911A (en) * | 2019-05-06 | 2019-10-08 | 北京元六鸿远电子科技股份有限公司 | The continuously adjustable low-temperature co-burning ceramic material of thermal expansion coefficient and preparation method |
| CN110304911B (en) * | 2019-05-06 | 2022-09-06 | 北京元六鸿远电子科技股份有限公司 | Low-temperature co-fired ceramic material with continuously adjustable thermal expansion coefficient and preparation method thereof |
| CN111792932A (en) * | 2020-03-30 | 2020-10-20 | 镇江锆源传感科技有限公司 | Preparation method of zirconia and alumina casting green body co-fired sintered sheet layer |
| CN111792932B (en) * | 2020-03-30 | 2022-09-27 | 镇江锆源传感科技有限公司 | Preparation method of zirconia and alumina casting green body co-sintered sheet layer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6852198B2 (en) | Boroaluminosilicate mineral material, low temperature co-fired ceramic composite material, low temperature co-fired ceramic, composite substrate and its manufacturing method | |
| JP5468448B2 (en) | High zirconia refractories and melting kilns | |
| CN110790568B (en) | Low-dielectric LTCC green tape and preparation method and application thereof | |
| Biesuz et al. | Liquid phase flash sintering in magnesia silicate glass-containing alumina | |
| CN103803968B (en) | Low-k low-temperature co-burning ceramic material and preparation method thereof in one | |
| Zhu et al. | Sintering behavior and properties of MgTiO3/CaO-B2O3-SiO2 ceramic composites for LTCC applications | |
| CN110372221A (en) | A kind of low-temperature co-fired ceramics green tape material and preparation method thereof | |
| JP6293735B2 (en) | Insulating layer forming material, insulating layer forming paste | |
| CN106966600B (en) | A kind of dentistry nano-sized crystal glass and its production method | |
| CN107555803A (en) | A kind of glass powder, its preparation method and application | |
| CN111116239A (en) | Electronic paste suitable for PZT atomized sheet co-firing process and co-firing method | |
| CN104071985A (en) | Microcrystal glass powder precursor, microcrystal glass powder as well as preparation method and application of microcrystal glass powder precursor and microcrystal glass powder | |
| CN114956821A (en) | High-transmittance yttrium oxide transparent ceramic and preparation method thereof | |
| Wang et al. | Shrinkage and strength characterization of an alumina–glass interpenetrating phase composite for dental use | |
| CN102898027B (en) | Ceramic powder for electronic component packaging material and production method for ceramic powder | |
| CN106747420A (en) | A kind of X5R types multilayer ceramic capacitor thin-medium material and preparation method thereof | |
| JP2004168597A (en) | Lead-free glass and composition for electronic circuit board | |
| JP2018177582A (en) | Glass ceramic composition, and sintered body and dental adjustment material using same | |
| KR100947819B1 (en) | Cinnabar glaze composite for ceramics and manufacturing method thereof | |
| CN102280162A (en) | Isolation medium material for thick film circuit and preparation method of isolation medium material | |
| CN109704763A (en) | A kind of preparation method of low-temperature sintering ceramic dielectric material | |
| CN102354687B (en) | Barrier medium material used for thick film circuit and preparation method thereof | |
| CN101962265A (en) | Glass composition, and preparation method and application thereof | |
| CN102234201A (en) | Metallization process of isostatic pressing porcelain tube for vacuum switch tube | |
| JP2007246297A (en) | Free-cutting glass ceramic and its producing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180109 |
|
| RJ01 | Rejection of invention patent application after publication |