CN105174972B - A kind of preparation method of glass/ceramic nano composite material - Google Patents
A kind of preparation method of glass/ceramic nano composite material Download PDFInfo
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Abstract
A kind of preparation method of glass/ceramic nano composite material, belongs to field of material preparation.After glass powder and nano ceramics medium powder mixing and ball milling and drying, then by " pre-burning, ball milling " process at least one times, to realize that glass uniformly coats nano ceramics medium powder, improve the disruptive field intensity of composite；Wherein, the temperature of the pre-burning is higher than glass softening point temperature, and less than nano ceramics medium powder sintering temperature.Glass can equably coating ceramic particle, and low, disruptive field intensity height is lost in composite, can be used as high pressure high density capacitors in the composite that the inventive method is prepared；Preparation method is simple, pollution-free；Overcome the too high shortcoming of sol-gal process cost, it is adaptable to industrial mass production.
Description
Technical field
The invention belongs to field of material preparation, and in particular to a kind of glass/ceramic for being applied to batch production is nano combined
The preparation method of material.
Background technology
In recent years, glass ceramic composite material causes the extensive concern of domestic and international researcher.Compared to traditional dielectric pottery
Porcelain, glass ceramic composite material due to glass meet insert ceramic particle hole so that improve material consistency, and burn
During knot, the glass of grain boundaries can suppress the growth of crystal grain and play a part of controlling grain size, and it is fine and close to improve material
Degree and crystal grain thinning can increase the disruptive field intensity of material, while improve the frequency-temperature characteristic of material to a certain extent, it is related
The research of aspect has wide practical use in fields such as pulse power energy storage ceramic electric capacity.
(Luo Jun, Du Jun, Tang Qun, Mao ChangHui, the Series multilayer such as Luo Jun
internal electrodes for high energy density glass-ceramic capacitors,Chinese
Sci Bull,2009,54:Na 2688-2693) is prepared for by solid phase method2O–PbO–Nb2O5–SiO2(2:2:3:6) insulate glass
Glass, its dielectric constant is about 170, and high pressure reaches 148kV/mm, and estimation energy storage density is 17J/cc.German Schott AG's research and development
Alkali-free glass (AF45), its dielectric constant is about 6, but pressure-resistant up to 1.2MV/mm, and equivalent energy storage density is up to 35J/cc, is mesh
The preceding insulating glass for possessing highest energy storage density reported.
At present, the domestic ceramic powder as energy storage is mainly barium strontium titanate (BST) powder, but such a porcelain disruptive field intensity
It is relatively low and crystal grain is larger, in Publication No. CN 102531580A patent of invention, nanometer is prepared for using liquid phase alkoxide reaction method
BST powders, then the ceramic material that aluminium Si composite oxide wraps up BST particles is prepared for by collosol and gel, after tested, it punctures
Intensity is raised to more than 100kV/mm, drastically increases the energy storage density of material.
In experiment, in order to allow glass equably coating ceramic particle, glass first often prepared using sol-gal process molten
Glue, then adds ceramic dielectric powder stirring uniformly, last calcination obtains body of powder raw material.Sol-gal process can obtain high
The powder of even property and high-purity, but be due to that cost is high, it is unfavorable for batch and prepares powder, it is contemplated that industrial production, mechanical ball mill
Method is still primary selection, mechanical attrition method be it is a kind of rolled using ball mill, the continuous collision crashing raw material of hard sphere is to reduce it
The method of particle diameter.But the obtained powder size limit of mechanical attrition method can only be to 2 μm or so, and the particle of nano ceramics medium
Diameter it is relatively small (<100nm), both, which are combined obtained powder glass oxide in sintering process, can not coat pottery well
Porcelain particle, reduces the uniformity of material component and then deteriorates the performance of material.
The content of the invention
The purpose of the present invention is to find a kind of preparation side for the glass/ceramic nano composite material for being applied to batch production
Method.Glass can equably coating ceramic particle, and composite loss is low, hits in the composite that the inventive method is prepared
Wear field strength high, can be used as high pressure high density capacitors；Preparation method is simple, pollution-free.
Technical scheme is as follows：
A kind of preparation method of glass/ceramic nano composite material, it is characterised in that glass powder and nano ceramics medium
After powder mixing and ball milling and drying, then by " pre-burning, ball milling " process at least one times, to realize that glass uniformly coats nano ceramics
Medium powder, improves the disruptive field intensity of composite；Wherein, the temperature of the pre-burning is higher than glass softening point temperature, and is less than
Nano ceramics medium powder sintering temperature.
Further, the calcined temperature and the difference of glass softening point temperature are less than and nano ceramics medium powder sintering
The difference of temperature.
Further, described " pre-burning, ball milling " process is 1~8 time.
Preferably, described " pre-burning, ball milling " process is 2~5 times.
A kind of preparation method of glass/ceramic nano composite material, specifically includes following steps：
Step 1：Frit is prepared using smelting process, crushed, ball milling obtains glass powder；
Step 2：The glass powder mixing and ball milling that nano ceramics medium powder and step 1 are obtained, drying；
Step 3：By " pre-burning, ball milling " process at least one times, obtain glass and uniformly coat nano ceramics medium powder
Composite；" pre-burning, the ball milling " process is：The powder pre-burning that upper step is obtained, the temperature of pre-burning is higher than Glass Transition
Point temperature, and less than nano ceramics medium powder sintering temperature, obtain the powder after pre-burning, then ball milling, drying again.
Further, calcined temperature described in step 3 and the difference of glass softening point temperature are less than and nano ceramics medium powder
Expect the difference of sintering temperature.
Further, " pre-burning, ball milling " process described in step 3 is 1~8 time.
Preferably, " pre-burning, ball milling " process described in step 3 is 2~5 times.
A kind of preparation method of glass/ceramic nano composite material, specifically includes following steps：
Step 1：Glass precursor is weighed in proportion, and 18~36h of mixing and ball milling, drying is then charged into crucible, using molten
Refining method high temperature when glass reaches clarifying temp is quenched, and is obtained frit, is crushed, ball milling obtains glass powder；
Step 2：By nano ceramics medium powder (<100nm) and step 1 obtain glass powder (>2 μm) mixing, ball milling
18~36h, drying；
Step 3：By " pre-burning, ball milling " process at least one times, obtain glass and uniformly coat nano ceramics medium powder
Composite；" pre-burning, the ball milling " process is：The powder pre-burning that upper step is obtained, the temperature of pre-burning is higher than Glass Transition
Point temperature, and less than nano ceramics medium powder sintering temperature, the powder obtained after pre-burning 18~36h of ball milling again, to reuniting
Particle crush to reduce its particle diameter again, dry.
Further, glass each component and its content are described in step 1：0~25mol%BaO, 0~40mol%B2O3、0
~20mol%Al2O3, 30~80mol%SiO2。
Preferably, glass each component and its content are described in step 1：10~20mol%BaO, 15~30mol%B2O3、5
~15mol%Al2O3, 40~60mol%SiO2。
Further, " pre-burning, ball milling " process described in step 3 is 1~8 time.
Preferably, " pre-burning, ball milling " process described in step 3 is 2~5 times.
A kind of preparation method of glass/ceramic nano composite material, the glass each component and its content are：0~
25mol%BaO, 0~40mol%B2O3, 0~20mol%Al2O3, 30~80mol%SiO2, the nano ceramics is rutile
Titanic oxide nano material；Preparation process specifically includes following steps：
Step 1：BaO, B are weighed in proportion2O3, Al2O3, SiO2Corresponding soluble-salt, is used as predecessor；Predecessor is mixed
Close 18~36h of ball milling, drying；
Step 2：By upper step dry after powder load smelting furnace crucible in, with 15 ± 1 DEG C/min heating rate by
Room temperature rises to 1200 ± 10 DEG C, then rises to 1500 ± 50 DEG C with 8 ± 1 DEG C/min heating rate, is now the clarification temperature of glass
Degree, high temperature quenching, obtains glass bulk；By obtained glass bulk mechanical crushing, then 24~72h of ball milling, finally cross 300~
The sieve of 400 mesh, obtains glass powder；
Step 3：Glass powder and rutile titanium dioxide nanopowder, 18~36h of mixing and ball milling, drying are weighed in proportion
After obtain powder H0, wherein, the weight/mass percentage composition of glass powder is 0~35wt%；
Step 4：By " pre-burning, ball milling " process at least one times, obtain glass and uniformly coat nano ceramics medium powder
Composite；" pre-burning, the ball milling " process is：The powder that upper step is obtained loads crucible, with 3 ± 1 DEG C/min heating speed
Rate rises to 820 ± 50 DEG C of progress preheatings by room temperature, is incubated 0.5~1h, powder after pre-burning 18~36h of ball milling again, right
The particle of reunion is crushed to reduce its particle diameter again, drying.
Further, " pre-burning, ball milling " process described in step 4 is 1~8 time.
Preferably, " pre-burning, ball milling " process described in step 4 is 2~5 times.
Further, the weight/mass percentage composition of glass powder described in step 3 is 5~30wt%.
Further, the predecessor of glass described in step 1 is followed successively by Ba (NO3) (99.5%), H3BO3(99.5%), Al
(NO3)3·9H2O (99%), glass sand (99.99%).
The glass/ceramic nano composite material that the above method is obtained can be as energy storage material application.
The present invention utilizes low glass transition temperature point, good fluidity and nano ceramics dielectric material sintering temperature higher
Feature, after glass powder and nano ceramics dielectric material mixing and ball milling, then through " pre-burning, ball milling " process at least one times, with reality
Existing glass uniformly wraps up the purpose of ceramic medium material, and improves the disruptive field intensity of material.The selection of calcined temperature of the present invention compared with
For key, glass mobility is small when temperature is relatively low, it is impossible to produce a desired effect, and temperature is too high, and ceramic dielectric may be caused brilliant
Grain length is big, deteriorates material property, and calcined temperature is chosen and is advisable with being slightly above glass softening point temperature, i.e. calcined temperature and glass is soft
Change the difference of point temperature less than the difference with the sintering temperature of nano ceramics medium powder.
Beneficial effects of the present invention are：
1st, the present invention utilizes the difference between glass softening point temperature and nano ceramics medium powder sintering temperature, setting one
Individual rational calcined temperature, glass powder prepared by smelting process (2 μm of particle diameter ＞) and nano ceramics medium powder mixing and ball milling
Afterwards, then through " pre-burning, ball milling " process at least one times, the uniform encapsulated nanoparticles of glass (particle diameter~100nm) are made.The inventive method
Overcome the too high shortcoming of sol-gal process cost, it is adaptable to industrial mass production；Using smelting process, mechanical attrition method etc.
Ripe production technology, at the same it is compatible with ceramic casting technology, and then can be used as high pressure high density capacitors；And prepare
The dielectric material loss of the uniform encapsulated nanoparticles of glass is low, and disruptive field intensity is high；Preparation method is simple, and process is pollution-free.
2nd, in the glass and Nano-Ceramic Composites system provided in the present invention, glass softening point is on 780 ± 50 DEG C of left sides
The right side, and nano rutile-type titanium dioxide sintering temperature is more than 1000 DEG C, therefore the calcined temperature of 820 ± 50 DEG C of selection is appropriate,
But the powder preparation method that the present invention is provided is not limited to such a glass ceramics system, as long as glass softening point and ceramics in system
Sintering temperature all should be in the scope of the present invention in the presence of a rational difference.
Brief description of the drawings
Fig. 1 is the principle schematic of the preparation method of glass/ceramic nano composite material of the present invention；
When Fig. 2 is 25 DEG C of measurement temperature, powder H in embodiment0With powder H4Dielectric constant and loss frequency rely on
Property；
When Fig. 3 is measurement frequency 1kHz, powder H in embodiment0With powder H4Dielectric constant and loss temperature-independent
Property；
Fig. 4 is powder H in embodiment0The SEM figures on surface；
Fig. 5 is powder H in embodiment4The SEM figures on surface.
Embodiment
It is improved present invention is generally directed to the preparation technology of glass and Nano-Ceramic Composites, to adapt it to industry
The need for mass production, and prepare the dielectric properties comparable with sol-gal process.More added with reference to instantiation
Whole elaboration technical scheme.
Embodiment
A kind of preparation method of glass/ceramic nano composite material, specifically includes following steps：
Step 1：According to glass：21mol%BaO, 15mol%B2O3, 5mol%Al2O3, 59mol%SiO2Ratio successively
Weigh predecessor Ba (NO3) (99.5%), H3BO3(99.5%), Al (NO3)3·9H2O (99%) and glass sand
(99.99%) then, above-mentioned predecessor be put into after the ball grinder for filling deionized water, ball milling 24h the drying that discharges；
Step 2：The powder that step 1 is obtained loads in the crucible of smelting furnace, first with 15 DEG C/min heating rate by
Room temperature rises to 1550 DEG C to 1200 DEG C, then with 8 DEG C/min heating rate by 1200 DEG C, is now the clarification temperature of glass
Degree, high temperature quenching, obtains glass bulk；Mechanical crushing first is carried out to bulk, then ball milling 72h, finally cross the sieve of 300 mesh, obtain
To glass powder；
Step 3：Weigh the glass that rutile titanium dioxide nanopowder (~100nm, 99.9999%) and step 2 are obtained
Powder 60g, mixing and ball milling 24h altogether, discharging drying obtain powder H0；Wherein, the weight/mass percentage composition of glass powder is
12wt%, the weight/mass percentage composition of titanic oxide nano material is 88%；
Step 4：By 4 " pre-burning, ball milling " processes, the powder H that glass uniformly coats nano ceramics medium is obtained4；Institute
Stating " pre-burning, ball milling " process is：The powder that upper step is obtained loads crucible, and 820 are risen to by room temperature with 4 DEG C/min heating rate
DEG C preheating is carried out, be incubated 0.5h, powder after pre-burning ball milling 24h again is crushed to reduce it again to the particle of reunion
Particle diameter, discharging drying.
The powder sample H obtained in step 30The powder sample H obtained with step 44In be separately added into 8wt% polyethylene
Butyral (PVB) is granulated as binding agent, and dry method is pressed into diameter phi=15mm ceramic chips under 50MPa pressure,
Handled by 550 DEG C of dumpings；1050 DEG C are risen to 5 DEG C/min heating rate again, and is incubated 1 hour, different pre-burnings time are obtained
Several ceramics samples, is cleaned in sample surfaces, brushes silver, silver ink firing, then carries out dielectric properties and disruptive field intensity test.
After tested, powder sample H0、H4Frequency dependence in 25 DEG C of room temperature of dielectric constant and loss as shown in Fig. 2
Sample H0、H4Dielectric constant and temperature dependency of the loss in frequency 1kHz it is as shown in Figure 3.Through Hi-pot test, sample H0's
Breakdown electric field EB=45.70 (kV/mm), sample H4Breakdown electric field EB=61.56 (kV/mm), show multiple " pre-burning, ball milling "
Process improves the breakdown electric field of material to a certain extent.
Using SEM to sample H0、H4Surface topography is tested, and its result as shown in Figure 4,5, is evident that from figure
Sample H after pre-burning ball milling 4 times4In, the uniformity of glass-coated is obviously improved, and then improves ceramic dense degree, this
It is the main cause that breakdown strength of material is improved.
The present invention is applied to the industrial production application of the high energy storage ceramic of high pressure, simple with principle, inexpensive and pollution-free
The characteristics of, and it is compatible with ceramic casting technology.Example in the present invention is only a kind of application of the present invention, is not intended to limit the present invention
Application, all changes done in the range of the principle of the invention, should be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of glass/ceramic nano composite material, it is characterised in that glass powder and nano ceramics medium powder
After expecting mixing and ball milling and drying, then by " pre-burning, ball milling " process at least one times, it is situated between with realizing that glass uniformly coats nano ceramics
Matter powder, improves the disruptive field intensity of composite；Wherein, the temperature of the pre-burning is higher than glass softening point temperature, and less than receiving
Rice ceramic dielectric powder sintering temperature, and the difference of the calcined temperature and glass softening point temperature is less than and nano ceramics is situated between
The difference of matter powder sintering temperature.
2. a kind of preparation method of glass/ceramic nano composite material, specifically includes following steps：
Step 1：Frit is prepared using smelting process, crushed, ball milling obtains glass powder；
Step 2：The glass powder mixing and ball milling that nano ceramics medium powder and step 1 are obtained, drying；
Step 3：By " pre-burning, ball milling " process at least one times, obtain glass and uniformly coat the compound of nano ceramics medium powder
Material；" pre-burning, the ball milling " process is：The powder pre-burning that upper step is obtained, the temperature of pre-burning is higher than glass softening point temperature
Degree, and less than nano ceramics medium powder sintering temperature, obtain the powder after pre-burning, then ball milling, drying again.
3. a kind of preparation method of glass/ceramic nano composite material, specifically includes following steps：
Step 1：Glass precursor is weighed in proportion, and 18~36h of mixing and ball milling, drying is then charged into crucible, using smelting process
When glass reaches clarifying temp, high temperature is quenched, and obtains frit, is crushed, and ball milling obtains glass powder；
Step 2：The glass powder that nano ceramics medium powder and step 1 are obtained is mixed, 18~36h of ball milling, drying；
Step 3：By " pre-burning, ball milling " process at least one times, obtain glass and uniformly coat the compound of nano ceramics medium powder
Material；" pre-burning, the ball milling " process is：The powder pre-burning that upper step is obtained, the temperature of pre-burning is higher than glass softening point temperature
Degree, and less than nano ceramics medium powder sintering temperature, the powder obtained after pre-burning 18~36h of ball milling again, to of reunion
Grain is crushed to reduce its particle diameter again, dries.
4. the preparation method of the glass/ceramic nano composite material according to claim 1 or 2 or 3, it is characterised in that institute
" pre-burning, ball milling " process is stated for 1~8 time.
5. the preparation method of the glass/ceramic nano composite material according to claim 1 or 2 or 3, it is characterised in that institute
" pre-burning, ball milling " process is stated for 2~5 times.
6. the preparation method of the glass/ceramic nano composite material according to claim 1 or 2 or 3, it is characterised in that institute
State glass each component and its content is：0~25mol%BaO, 0~40mol%B2O3, 0~20mol%Al2O3, 30~
80mol%SiO2。
7. the preparation method of the glass/ceramic nano composite material according to claim 1 or 2 or 3, it is characterised in that institute
State glass each component and its content is：10~20mol%BaO, 15~30mol%B2O3, 5~15mol%Al2O3, 40~
60mol%SiO2。
8. a kind of preparation method of glass/ceramic nano composite material, the glass each component and its content are：0~25mol%
BaO, 0~40mol%B2O3, 0~20mol%Al2O3, 30~80mol%SiO2, the nano ceramics is rutile titanium dioxide
Nanopowder；Preparation process specifically includes following steps：
Step 1：BaO, B are weighed in proportion2O3, Al2O3, SiO2Corresponding soluble-salt, is used as predecessor；By predecessor mixing ball
Grind 18~36h, drying；
Step 2：Powder after upper step is dried loads in the crucible of smelting furnace, with 15 ± 1 DEG C/min heating rate by room temperature
1200 ± 10 DEG C are risen to, then 1500 ± 50 DEG C are risen to 8 ± 1 DEG C/min heating rate, high temperature quenching obtains glass bulk；
By obtained glass bulk mechanical crushing, then 24~72h of ball milling, finally crosses the sieve of 300~400 mesh, obtains glass powder；
Step 3：Glass powder and rutile titanium dioxide nanopowder are weighed in proportion, and 18~36h of mixing and ball milling is obtained after drying
To powder, wherein, the weight/mass percentage composition of glass powder is 0~35wt%；
Step 4：By " pre-burning, ball milling " process at least one times, obtain glass and uniformly coat the compound of nano ceramics medium powder
Material；" pre-burning, the ball milling " process is：The powder that upper step is obtained loads crucible, with 3 ± 1 DEG C/min heating rate by
Room temperature rises to 820 ± 50 DEG C of progress preheatings, is incubated 0.5~1h, powder after pre-burning 18~36h of ball milling again, to reuniting
Particle crush to reduce its particle diameter again, dry.
9. glass and nanometer that the preparation method of the glass/ceramic nano composite material described in claim 1 or 2 or 3 or 8 is obtained
Ceramic composite is used as energy storage material application.
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| CN107021774B (en) * | 2017-04-14 | 2020-06-30 | 常州联德电子有限公司 | Glass-based composite sealing material for flat-plate oxygen sensor and sealing method thereof |
| CN111410528A (en) * | 2020-05-15 | 2020-07-14 | 昆山卡德姆新材料科技有限公司 | Microwave dielectric ceramic and manufacturing method thereof |
| WO2022057518A1 (en) * | 2020-09-15 | 2022-03-24 | 深圳前海发维新材料科技有限公司 | Use of glass composite material with high softening point, low thermal expansion coefficient, high wear resistance and low thermal conductivity in engine gas turbine |
| CN112159112B (en) * | 2020-09-30 | 2021-08-27 | 泗阳群鑫电子有限公司 | High-energy-storage ceramic capacitor dielectric material and preparation process thereof |
| CN113831121A (en) * | 2021-09-25 | 2021-12-24 | 天津理工大学 | Complex phase giant dielectric ceramic material with high breakdown field strength and preparation method thereof |
| CN114671676B (en) * | 2022-04-15 | 2022-11-15 | 安徽宁晶新材料科技有限公司 | Low-dielectric-constant ultralow-loss LTCC powder and preparation method thereof |
| CN115572152B (en) * | 2022-10-20 | 2023-03-21 | 湖南省醴陵市浦口电瓷有限公司 | High-voltage hollow porcelain bushing and preparation process thereof |
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| CN101857375B (en) * | 2010-05-11 | 2011-12-28 | 清华大学 | Low-temperature co-fired glass ceramic composite material with adjustable dielectric constant and preparation method thereof |
| CN102531580B (en) * | 2011-12-14 | 2014-01-29 | 同济大学 | Nanometer barium-strontium titanate medium energy storage material coated by aluminum-silicon composite oxide and preparation method thereof |
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