CN107162573A - A kind of crystal oscillator encapsulation enhanced alumina ceramic composite material of Zirconium oxide fibre samarium oxide and preparation method thereof - Google Patents
A kind of crystal oscillator encapsulation enhanced alumina ceramic composite material of Zirconium oxide fibre samarium oxide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of crystal oscillator encapsulation enhanced alumina ceramic composite material of Zirconium oxide fibre samarium oxide, it is characterised in that adds distilled water into polyvinyl alcohol, and heating stirring dissolves to obtain poly-vinyl alcohol solution；Add distilled water into chitosan, acetic acid, magnetic agitation formation chitosan solution is added dropwise in stirring and dissolving；It will be added to after sericite high-temperature process in chitosan solution, stir to obtain chitosan/sericite solution；After montmorillonite high-temperature process, distilled water is added, magnetic agitation adds tetraethyl orthosilicate and ethanol, and heating stirring is filtered, washed, dries, grinds, sieves, obtain silica montmorillonite heterozygote；Alumina powder, Zirconium oxide fibre, samarium oxide are mixed, ethanol is added, magnetic agitation is uniform, ultrasonic disperse, wet-milling, is dried completely, above resulting material is added, grinding is sealed old；Pour into mould, after pressurized treatments, heating and calcining obtains the composite.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of crystal oscillator encapsulation is enhanced with Zirconium oxide fibre-samarium oxide
The preparation method of alumina ceramic composite material.
Background technology
Quartz oscillator because being widely used in communicating with very high frequency stability, broadcast, radar, navigation
And many measuring instruments.With electronics and information industry develop rapidly with the minimizing of complete electronic set, high performance development trend,
The market demand of quartz crystal oscillator is also by rapid growth.Traditional crystal oscillator can not meet requirement, start to surface attaching type and
Gently, thin, small direction is developed, and ceramic package gradually instead of traditional bare metal shell and cover plastic-metal encapsulation.
The content of the invention
The present invention solves the technical problem of provide a kind of crystal oscillator encapsulation enhanced oxygen of Zirconium oxide fibre-samarium oxide
Change the preparation method of aluminium ceramic composite, the composite prepared according to the technique has good insulating properties and wearability
Energy.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of crystal oscillator encapsulation preparation method of the enhanced alumina ceramic composite material of Zirconium oxide fibre-samarium oxide, its feature
It is, carries out according to the following steps：
A. into 2-3 weight account polyethylene alcohol 1:5-10 adds distilled water, is warming up to 65-75 DEG C of heating, stirring and dissolving obtains poly- second
Enolate solution；
B. into 2-4 parts by weight chitosans 1:40-50 adds distilled water, and 2-3 parts by weight acetic acid is added dropwise in stirring and dissolving, and magnetic force is stirred
Mix 1-2h formation chitosan solutions；1-2 parts by weight sericite is handled into 8-10h at 700-800 DEG C, chitosan solution is added to
In, stirring 1-2h obtains chitosan/sericite solution；
C. the montmorillonite of 2-3 parts by weight is handled into 6-8h, 1 at 750-850 DEG C:10-20 adds distilled water, magnetic agitation 30-
40min, adds 1-2 parts by weight tetraethyl orthosilicate and 1-2 parts by weight of ethanol, plus hydrochloric acid adjusts pH to be 2-3, in 40-50 DEG C of water-bath
Heating stirring 2-3h, filtering, washing 3-5 times, the forced air drying 1-2h in 60-70 DEG C of baking oven grinds, crosses 100-200 mesh
Sieve, obtains silica-montmorillonite heterozygote；
D. 80-90 parts by weight of alumina powder, 5-10 parts by weight Zirconium oxide fibre, 1-2 parts by weight samarium oxide are mixed, 1:5-10
Ethanol is added, magnetic agitation is uniform, and ultrasonic disperse 30-40min pours into wet-milling 2-3h in ball grinder, in 95-105 DEG C of electric heating drum
Complete, resulting material in addition a, b, c is dried in wind drying box, 40-50min is ground, seals old 1-2d；Pour into mould,
After pressurized treatments, 300-400 DEG C of insulation 1-2h is heated to, 550-650 DEG C of insulation 1-2h is warming up to, then be warming up to 1600-1700
DEG C insulation 1-2h, obtain the composite.
Wherein, concentration of hydrochloric acid described in step c is 2-3%.Pressurized treatments refer to be pressurized to 50-100MPa described in step d
Pressurize 2-4min.
The present invention reaction mechanism and have the beneficial effect that：
Chitosan-sericite composite solution is obtained using the method for physical blending, sericite in the base regular is improved
Dispersiveness, with good electrical insulation capability；Montmorillonite is with excellent mechanical property, insulating properties and resistance to elevated temperatures
Layered silicate material, using sol-gal process, tetraethyl orthosilicate hydrolyzes, is condensed into the process of silica in acid condition
In interphase interaction with phyllosilicate, realize silicon dioxide modified montmorillonite, silica dioxide granule cladding and part is shelled
From montmorillonite layer, increase its compatibility between matrix；Rare earth oxide（Samarium oxide）Aluminium oxide ceramics can be improved
Anti-wear performance, strengthens crystal boundary bond strength；Zirconium oxide fibre can improve the thermal shock resistance of aluminium oxide ceramics, bending strength and disconnected
Split toughness.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of preparation method of the crystal oscillator encapsulation enhanced alumina ceramic composite material of Zirconium oxide fibre-samarium oxide, its
It is characterised by, carries out according to the following steps：
A. into 3kg polyvinyl alcohol 1:10 add distilled water, are warming up to 65-75 DEG C of heating, it is molten that stirring and dissolving obtains polyvinyl alcohol
Liquid；
B. into 4kg chitosans 1:40-50 adds distilled water, and 3kg acetic acid is added dropwise in stirring and dissolving, and magnetic agitation 1h formation shells gather
Sugar juice；2kg sericites are handled into 8h at 700-800 DEG C, are added in chitosan solution, stirring 1h obtains chitosan/sericite
Solution；
C. 3kg montmorillonites are handled into 6h, 1 at 750-850 DEG C:15 add distilled water, and magnetic agitation 35min is adding 2kg just
Silester and 2kg ethanol, plus hydrochloric acid adjust pH to be 2-3, the heating stirring 2h in 40-50 DEG C of water-bath, filter, wash 3 times,
Forced air drying 1h in 60-70 DEG C of baking oven, grinds, crosses 100 mesh sieves, obtain silica-montmorillonite heterozygote；
D. 90kg alumina powders, 10kg Zirconium oxide fibres, 2kg samarium oxides are mixed, 1:10 add ethanol, and magnetic agitation is uniform,
Ultrasonic disperse 35min, pours into wet-milling 2h in ball grinder, and complete, addition a, b, c are dried in 95-105 DEG C of electric drying oven with forced convection
Middle resulting material, grinds 45min, seals old 1d；Pour into mould, after pressurized treatments, be heated to 300-400 DEG C of insulation 1h,
550-650 DEG C of insulation 1h is warming up to, then is warming up to 1600-1700 DEG C of insulation 2h, the composite is obtained.
Wherein, concentration of hydrochloric acid described in step c is 2%.Pressurized treatments described in step d refer to be pressurized to 8MPa pressurizes
4min。
Claims (4)
1. a kind of crystal oscillator encapsulation enhanced alumina ceramic composite material of Zirconium oxide fibre-samarium oxide, it is characterised in that：
Add distilled water into polyvinyl alcohol, heating stirring dissolves to obtain poly-vinyl alcohol solution；Add distilled water into chitosan, stir molten
Solution, is added dropwise acetic acid, magnetic agitation formation chitosan solution；It will be added in chitosan solution, stir after sericite high-temperature process
Chitosan/sericite solution；After montmorillonite high-temperature process, distilled water is added, magnetic agitation adds tetraethyl orthosilicate and second
Alcohol, heating stirring, filtering, washing are dried, grind, sieved, obtain silica-montmorillonite heterozygote；By alumina powder,
Zirconium oxide fibre, samarium oxide mixing, add ethanol, and magnetic agitation is uniform, ultrasonic disperse, wet-milling, dry completely, add above institute
Material is obtained, grinding is sealed old；Pour into mould, after pressurized treatments, heating and calcining obtains the composite.
2. a kind of preparation method of the crystal oscillator encapsulation enhanced alumina ceramic composite material of Zirconium oxide fibre-samarium oxide, it is special
Levy and be：
A. into 2-3 weight account polyethylene alcohol 1:5-10 adds distilled water, is warming up to 65-75 DEG C of heating, stirring and dissolving obtains poly- second
Enolate solution；
B. into 2-4 parts by weight chitosans 1:40-50 adds distilled water, and 2-3 parts by weight acetic acid is added dropwise in stirring and dissolving, and magnetic force is stirred
Mix 1-2h formation chitosan solutions；1-2 parts by weight sericite is handled into 8-10h at 700-800 DEG C, chitosan solution is added to
In, stirring 1-2h obtains chitosan/sericite solution；
C. the montmorillonite of 2-3 parts by weight is handled into 6-8h, 1 at 750-850 DEG C:10-20 adds distilled water, magnetic agitation 30-
40min, adds 1-2 parts by weight tetraethyl orthosilicate and 1-2 parts by weight of ethanol, plus hydrochloric acid adjusts pH to be 2-3, in 40-50 DEG C of water-bath
Heating stirring 2-3h, filtering, washing 3-5 times, the forced air drying 1-2h in 60-70 DEG C of baking oven grinds, crosses 100-200 mesh
Sieve, obtains silica-montmorillonite heterozygote；
D. 80-90 parts by weight of alumina powder, 5-10 parts by weight Zirconium oxide fibre, 1-2 parts by weight samarium oxide are mixed, 1:5-10
Ethanol is added, magnetic agitation is uniform, and ultrasonic disperse 30-40min pours into wet-milling 2-3h in ball grinder, in 95-105 DEG C of electric heating drum
Complete, resulting material in addition a, b, c is dried in wind drying box, 40-50min is ground, seals old 1-2d；Pour into mould,
After pressurized treatments, 300-400 DEG C of insulation 1-2h is heated to, 550-650 DEG C of insulation 1-2h is warming up to, then be warming up to 1600-1700
DEG C insulation 1-2h, obtain the composite.
3. a kind of crystal oscillator encapsulation according to claim 2 is combined with the enhanced aluminium oxide ceramics of Zirconium oxide fibre-samarium oxide
The preparation method of material, it is characterised in that concentration of hydrochloric acid described in step c is 2-3%.
4. a kind of crystal oscillator encapsulation according to claim 2 is combined with the enhanced aluminium oxide ceramics of Zirconium oxide fibre-samarium oxide
The preparation method of material, it is characterised in that pressurized treatments described in step d refer to be pressurized to 50-100MPa pressurizes 2-4min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1145346A (en) * | 1996-07-05 | 1997-03-19 | 华南理工大学 | Al2O3-base series composite materials and prepn. thereof |
| CN1996536A (en) * | 2006-12-22 | 2007-07-11 | 邓昱 | A surface paste fuse of nano carborundum-alumina porcelain base and its making method |
| CN102344699A (en) * | 2011-07-05 | 2012-02-08 | 天津大学 | Nano-grade silica modified montmorillonite particle preparation method, and method for applying nano-grade silica modified montmorillonite particles in producing modified aqueous polyurethane resin with in-situ method |
| CN105881700A (en) * | 2016-05-26 | 2016-08-24 | 郑州中瓷科技有限公司 | High-strength ceramic substrate and preparation method and production line thereof |
| CN106699222A (en) * | 2017-02-15 | 2017-05-24 | 山东工业陶瓷研究设计院有限公司 | High-performance flat sheet ceramic membrane support and preparation method thereof |
| CN106810214A (en) * | 2017-01-05 | 2017-06-09 | 中北大学 | A kind of preparation method of high strength and low cost alumina ceramic substrate used for electronic packaging |
-
2017
- 2017-06-29 CN CN201710514288.8A patent/CN107162573A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1145346A (en) * | 1996-07-05 | 1997-03-19 | 华南理工大学 | Al2O3-base series composite materials and prepn. thereof |
| CN1996536A (en) * | 2006-12-22 | 2007-07-11 | 邓昱 | A surface paste fuse of nano carborundum-alumina porcelain base and its making method |
| CN102344699A (en) * | 2011-07-05 | 2012-02-08 | 天津大学 | Nano-grade silica modified montmorillonite particle preparation method, and method for applying nano-grade silica modified montmorillonite particles in producing modified aqueous polyurethane resin with in-situ method |
| CN105881700A (en) * | 2016-05-26 | 2016-08-24 | 郑州中瓷科技有限公司 | High-strength ceramic substrate and preparation method and production line thereof |
| CN106810214A (en) * | 2017-01-05 | 2017-06-09 | 中北大学 | A kind of preparation method of high strength and low cost alumina ceramic substrate used for electronic packaging |
| CN106699222A (en) * | 2017-02-15 | 2017-05-24 | 山东工业陶瓷研究设计院有限公司 | High-performance flat sheet ceramic membrane support and preparation method thereof |
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