CN108821597A - A kind of glass ceramics and preparation method thereof - Google Patents
A kind of glass ceramics and preparation method thereof Download PDFInfo
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- CN108821597A CN108821597A CN201810740285.0A CN201810740285A CN108821597A CN 108821597 A CN108821597 A CN 108821597A CN 201810740285 A CN201810740285 A CN 201810740285A CN 108821597 A CN108821597 A CN 108821597A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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Abstract
The invention belongs to technical field of ceramic material, and in particular to a kind of glass ceramics and preparation method thereof.LaAlO is added in glass ceramics of the invention3, enhance the high temperature resistance of glass ceramics;Silane coupler modified nano silica is added, it is made to have better bending strength, toughness and higher density.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of glass ceramics and preparation method thereof.
Background technique
Ceramic material is natural or synthetic compound through one kind inorganic non-metallic material made of overmolding and high-temperature calcination,
Ceramic material can be divided into two major classes according to its performance and purposes:Structural ceramics and function ceramics, function ceramics, which refers to, to be applied
When mainly utilize the material of its non-mechanical property, this material usually has one or more functions.Such as electricity, magnetic, light, heat, change
The functions such as, biology, function ceramics is many kinds of, and purposes is different.
Glass ceramics (i.e. devitrified glass) has the double grading of glass and ceramics, and the atomic arrangement inside simple glass is
Do not have one of the reason of well-regulated, this is also Glass breadks easily.And glass ceramics is made of as ceramics crystal, that is to say, that
Its atomic arrangement is regular.So glass ceramics is higher than the brightness of ceramics, it is stronger than glass toughness.Glass ceramics, also known as
Devitrified glass, traditional glass ceramics manufacturing method are a kind of crystal phase obtained by high temperature melting, molding and heat treatment and glass
The composite material that glass combines.Glass ceramics has high mechanical strength, and hot expansibility is adjustable, heat shock resistance, resistant to chemical etching,
The superior performance such as low-dielectric loss.In biomedicine field, bioceramic is often used in manufacture dental material, artificial bone
Joint and the filler of bone bonding agent etc..
The method of manufacture glass ceramics generally includes three key steps:Raw material is melted first, such as raw material
Mixture is usually melted at 1500~1700 DEG C;Again by the cooling acquisition melten glass of the slurry of melting and punch forming;Most
Crystallization or ceramic are carried out by suitable heat treatment (including nucleation and crystal growth phase) glass cooling to molding afterwards.
High temperature resistant glass ceramic is the application with new processes such as sintering process, sol-gel methods in glass ceramics preparation
And the new material to grow up.When precipitation such as mullite, spinelle, pollucite crystal resistant to high temperature and content in glass ceramics
When higher, material can be with resistance to very high temperature.In pollucite glass ceramics, this high temperature resistant crystallite is not only precipitated, has also analysed
Some mullite crystals are gone out, and its residual glass phase is wrapped up by crystal, this material can be in 1400 DEG C or so of high temperature
Lower use.
The microstructure of the material glass ceramics of strong mechanical performance has a significant impact to its mechanical property, can use control structure
Improve performance, as intensity and toughness can be improved in pilotaxitic texture;Keep crystal orientation raw using the methods of temperature gradient, hot extrusion
Length can also increase substantially mechanical property, such as with CaO-P2O5For orientation crystallite, flexural strength are precipitated in the glass ceramics of base
Up to 700MPa, and fracture toughness also significantly improves;Composite material is the another effective way for improving glass ceramics mechanical property
Diameter can will have compound therewith different from the fiber of glass-ceramic substrate mechanical property, whisker or particle, it is also possible to metal etc. its
Its material is compound therewith, and the fiber of glass ceramics or spherula can also be combined in other matrixes, such as uses SiC whisker reinforcement
MgO-Al2O3-SiO2The glass ceramics of base, flexural strength and fracture toughness are respectively 500MPa and 4.0MPa, than non-reinforced person
Improve twice or more.The mechanical property of composite material can be with Si3N waits structural ceramics to match in excellence or beauty, and is a kind of promising new structure
Material.
The major advantage of biological glass ceramic biological glass ceramic is can to introduce CaO, P in glass2O5, pass through heat treatment
Hydroxyapatite crystal can be precipitated, with excellent biocompatibility and bioactivation, other components in composition can be analysed
Other types of crystal out guarantees chemical stability, machinability of material etc., more promising than materials such as metal, aluminium oxide.
Many clinical tests have been carried out so far, and some is up to 6 years as long as, and all achieves gratifying achievement.
This kind of material of new function glass ceramics develops with new technology, high-tech demand, it uses glass technology
Forming and the characteristic preparation of crystal needed for being precipitated by dominated crystallization have piezoelectricity, partly lead, is ferroelectricity, electric light, non-linear etc. various
The material of characteristic.Some major function materials of research have glass for infrared rays ceramics, ferroelectricity and ferromagnetism glass ceramics, mix Cr3+
The transparent glass ceramics of plasma, in addition there are the glass ceramics for electronic device and its sealing-in, be used as catalyst carrier with
Porous doped-glass ceramics of sensor etc..But functional crystal amount of precipitation it is inadequate when, performance will lead to " dilution " effect, material
Though having certain functional characteristics, performance indicator is poor, is not able to satisfy application requirement.Therefore, the crystallization of functional crystal how is improved
Rate and makes material as far as possible and be single-phase or be the emphasis in such investigation of materials containing minimum out-phase.
For glass ceramic material, high-temperature stability and impact strength and toughness are always the emphasis studied.
Summary of the invention
The object of the present invention is to provide a kind of novel glass-ceramic, LaAlO is added in glass ceramics of the invention3, enhance
The high temperature resistance of glass ceramics;Silane coupler modified nano silica is added, it is made to have better bending strength, resist
Impact flexibility and higher density.
The technical scheme is that:
A kind of novel glass-ceramic, component is by silane coupler modified nano silica, LaAlO3、MgO、TiO2、
P2O5、B2O3、SrO、CaO、ZnO、Ag2O is constituted.
Preferably, the group of above-mentioned each component becomes:Silane coupler modified nano silica be 30-35 parts by weight,
LaAlO3It is 15-20 parts by weight, TiO for 25-35 parts by weight, MgO2For 10-15 parts by weight, P2O5For 1-3 parts by weight, B2O3For 1-
3 parts by weight, SrO are 2-5 parts by weight, CaO is 3-5 parts by weight, ZnO is 1-3 parts by weight, Ag2O is 1-3 parts by weight.
The preparation method of above-mentioned glass ceramics, includes the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added silane coupling agent, 80-100 DEG C
Lower reaction 5-8 hours, centrifugation, drying, obtains silane coupler modified nano silica;
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、
Ag2Ball milling sieving processing is carried out after O mixing;
(3) mixed material after sieving is warming up to 650-750 DEG C of calcining 1-2 hours;
(4) it is continuously heating to 800-900 DEG C of calcining 3-5 hours, is cooled to room temperature then to get the glass ceramics is arrived.
Preferably, the silane coupling agent is γ-r-chloropropyl trimethoxyl silane, vinyltriethoxysilane, ethylene
Base trimethoxy silane, β-(3,4 epoxycyclohexyl) ethyl trimethoxy silane, γ-(methacryloxy) propyl front three
Oxysilane, γ-dredge propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, γ-ureidopropyltriethoxysilane
One of.
Preferably, the mass ratio of nano silica and silane coupling agent is 2-3 in step (1):1.
Preferably, 200-300 mesh is crossed in step (2) after ball milling.
Preferably, heating rate is 0.5-2 DEG C/min in step (3).
Preferably, heating rate is 1-5 DEG C/min in step (4).
Preferably, rate of temperature fall is 2-5 DEG C/min in step (4).
Beneficial effects of the present invention are as follows:
LaAlO is added in glass ceramics of the invention3, enhance the high temperature resistance of glass ceramics;Silane coupling agent is added
Modified manometer silicon dioxide makes it have better bending strength, toughness and higher density.
Specific embodiment
With reference to embodiment, technical solution of the present invention is described in further detail, but do not constituted pair
Any restrictions of the invention.
Embodiment 1
A kind of novel glass-ceramic, component are configured to:The silane coupler modified nano silica of 32 parts by weight, 28 weights
Measure part LaAlO3, 16 parts by weight MgO, 13 parts by weight TiO2, 2 parts by weight P2O5, 1.5 parts by weight B2O3, 2.5 parts by weight SrO, 3 weights
Measure part CaO, 1 parts by weight ZnO, 1 parts by weight Ag2O is constituted.
The preparation method of above-mentioned glass ceramics, includes the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added and accounts for nano silica weight
1/2 silane coupling agent vinyl triethoxysilane reacts 6 hours at 80 DEG C, centrifugation, dry, obtains silane coupling agent and changes
Property nano silica,
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、
Ag2Ball milling, which is carried out, after O mixing crosses 200 meshes;
(3) mixed material after sieving 650 DEG C are warming up to the rate of 0.5 DEG C/min to calcine 1.5 hours;
(4) continue to be warming up to 850 DEG C of calcinings 3 hours with the rate of 2 DEG C/min, room is then down to the rate of 3 DEG C/min
Temperature to get arrive the glass ceramics.
Embodiment 2
A kind of novel glass-ceramic, component are configured to:The silane coupler modified nano silica of 30 parts by weight, 26 weights
Measure part LaAlO3, 19 parts by weight MgO, 11 parts by weight TiO2, 2.6 parts by weight P2O5, 1.6 parts by weight B2O3, 3.8 parts by weight SrO,
3.2 parts by weight CaO, 1.5 parts by weight ZnO, 1.3 parts by weight Ag2O is constituted.
The preparation method of above-mentioned glass ceramics, includes the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added and accounts for nano silica weight
1/3 silane coupling agent β-(3,4 epoxycyclohexyl) ethyl trimethoxy silane reacts 6 hours at 90 DEG C, centrifugation, dry, obtains
To silane coupler modified nano silica,
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、
Ag2Ball milling, which is carried out, after O mixing crosses 220 meshes;
(3) mixed material after sieving 680 DEG C are warming up to the rate of 1 DEG C/min to calcine 1 hour;
(4) continue to be warming up to 850 DEG C of calcinings 4 hours with the rate of 2 DEG C/min, room is then down to the rate of 3 DEG C/min
Temperature to get arrive the glass ceramics.
Embodiment 3
A kind of novel glass-ceramic, component are configured to:The silane coupler modified nano silica of 32.6 parts by weight,
29.1 parts by weight LaAlO3, 15.3 parts by weight MgO, 11 parts by weight TiO2, 1.9 parts by weight P2O5, 2 parts by weight B2O3, 2.5 parts by weight
SrO, 3 parts by weight CaO, 1.1 parts by weight ZnO, 1.5 parts by weight Ag2O is constituted.
The preparation method of above-mentioned glass ceramics, includes the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added and accounts for nano silica weight
2/5 silane coupling agent γ-(methacryloxy) propyl trimethoxy silicane reacts 8 hours at 95 DEG C, centrifugation, dry,
Silane coupler modified nano silica is obtained,
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、
Ag2Ball milling, which is carried out, after O mixing crosses 260 meshes;
(3) mixed material after sieving 700 DEG C are warming up to the rate of 2 DEG C/min to calcine 1 hour;
(4) continue to be warming up to 850 DEG C of calcinings 5 hours with the rate of 2 DEG C/min, room is then down to the rate of 3 DEG C/min
Temperature to get arrive the glass ceramics.
Embodiment 4
A kind of novel glass-ceramic, component are configured to:The silane coupler modified nano silica of 34.1 parts by weight,
27.3 parts by weight LaAlO3, 15.6 parts by weight MgO, 10.3 parts by weight TiO2, 1 parts by weight P2O5, 2 parts by weight B2O3, 2.2 parts by weight
SrO, 3 parts by weight CaO, 2.5 parts by weight ZnO, 2 parts by weight Ag2O is constituted.
The preparation method of above-mentioned glass ceramics, includes the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added and accounts for nano silica weight
1/3 silane coupling agent γ-ureidopropyltriethoxysilane reacts 5 hours at 90 DEG C, centrifugation, dry, obtains silane coupled
Agent modified manometer silicon dioxide,
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、
Ag2Ball milling, which is carried out, after O mixing crosses 300 meshes;
(3) mixed material after sieving 720 DEG C are warming up to the rate of 1.8 DEG C/min to calcine 1 hour;
(4) continue to be warming up to 900 DEG C of calcinings 4 hours with the rate of 5 DEG C/min, room is then down to the rate of 3 DEG C/min
Temperature to get arrive the glass ceramics.
Embodiment 5
A kind of novel glass-ceramic, component are configured to:The silane coupler modified nano silica of 35 parts by weight, 25.1
Parts by weight LaAlO3, 15.8 parts by weight MgO, 10 parts by weight TiO2, 1.2 parts by weight P2O5, 1.3 parts by weight B2O3, 3 parts by weight SrO,
3.9 parts by weight CaO, 2.3 parts by weight ZnO, 2.4 parts by weight Ag2O is constituted.
The preparation method of above-mentioned glass ceramics, includes the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added and accounts for nano silica weight
1/2 silane coupling agent vinyl trimethoxy silane reacts 8 hours at 80 DEG C, centrifugation, dry, obtains silane coupling agent and changes
Property nano silica,
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、
Ag2Ball milling, which is carried out, after O mixing crosses 300 meshes;
(3) mixed material after sieving 690 DEG C are warming up to the rate of 1.5 DEG C/min to calcine 1 hour;
(4) continue to be warming up to 900 DEG C of calcinings 4 hours with the rate of 4 DEG C/min, room is then down to the rate of 5 DEG C/min
Temperature to get arrive the glass ceramics.
Comparative example
A kind of glass ceramics, component are configured to:35 parts by weight SiO2, 32 parts by weight Al2O3, 19.8 parts by weight MgO, 3 weights
Measure part P2O5, 3 parts by weight B2O3, 4.9 parts by weight CaO, 1 parts by weight ZnO, 1.3 parts by weight Ag2O is constituted.
Performance test
The glass ceramics of the present embodiment 1 to 5 and comparative example is tested to its bending strength, toughness and density respectively,
As a result as shown in table 1 below.
The test of 1 different glass ceramic performance of table
It is found through the foregoing embodiment with the test of comparative example, the glass ceramics in 5 embodiments of the invention is due to adding
Silane coupler modified nano silica and LaAlO are added3, density, bending strength, toughness and high temperature resistant
Characteristic is better than comparative example.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of glass ceramics, which is characterized in that the glass ceramics component by silane coupler modified nano silica,
LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、Ag2O is constituted.
2. a kind of glass ceramics according to claim 1, which is characterized in that the group of each component becomes:It is silane coupled
Agent modified manometer silicon dioxide is 30-35 parts by weight, LaAlO3It is 15-20 parts by weight, TiO for 25-35 parts by weight, MgO2For 10-
15 parts by weight, P2O5For 1-3 parts by weight, B2O3It is 2-5 parts by weight for 1-3 parts by weight, SrO, CaO is 3-5 parts by weight, ZnO 1-
3 parts by weight, Ag2O is 1-3 parts by weight.
3. a kind of preparation method of glass ceramics of any of claims 1 or 2, which is characterized in that include the following steps:
(1) nano silica is added to ultrasonic disperse in ethanol solution, is then added silane coupling agent, it is anti-at 80-100 DEG C
It answers 5-8 hours, centrifugation, drying obtain silane coupler modified nano silica;
(2) by silane coupler modified nano silica, LaAlO3、MgO、TiO2、P2O5、B2O3、SrO、CaO、ZnO、Ag2O is mixed
Ball milling sieving processing is carried out after conjunction;
(3) mixed material after sieving is warming up to 650-750 DEG C of calcining 1-2 hours;
(4) it is continuously heating to 800-900 DEG C of calcining 3-5 hours, is cooled to room temperature then to get the glass ceramics is arrived.
4. a kind of preparation method of glass ceramics according to claim 3, which is characterized in that the silane coupling agent is
γ-r-chloropropyl trimethoxyl silane, vinyltriethoxysilane, vinyltrimethoxysilane, β-(3,4 epoxycyclohexyl)
The thin propyl trimethoxy silicane of ethyl trimethoxy silane, γ-(methacryloxy) propyl trimethoxy silicane, γ-,
One of gamma-aminopropyl-triethoxy-silane, γ-ureidopropyltriethoxysilane.
5. a kind of preparation method of glass ceramics according to claim 3, which is characterized in that nano-silica in step (1)
SiClx and the weight ratio of silane coupling agent are 2-3:1.
6. a kind of preparation method of glass ceramics according to claim 3, which is characterized in that mistake after ball milling in step (2)
200-300 mesh.
7. a kind of preparation method of glass ceramics according to claim 3, which is characterized in that heating rate in step (3)
For 0.5-2 DEG C/min.
8. a kind of preparation method of glass ceramics according to claim 3, which is characterized in that heating rate in step (4)
For 1-5 DEG C/min.
9. a kind of preparation method of glass ceramics according to claim 3, which is characterized in that rate of temperature fall in step (4)
For 2-5 DEG C/min.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111406754A (en) * | 2020-04-28 | 2020-07-14 | 浙江禾本科技股份有限公司 | Hexythiazox water suspending agent and preparation method thereof |
CN112500188A (en) * | 2020-12-21 | 2021-03-16 | 南京工业大学东海先进硅基材料研究院 | Preparation method of porous quartz ceramic filter material |
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CN103619769A (en) * | 2011-06-28 | 2014-03-05 | 3M创新有限公司 | Glass-ceramics and methods of making the same |
CN104140207A (en) * | 2014-07-29 | 2014-11-12 | 青岛祥海电子有限公司 | Industrial waste residue reuse type glass ceramic |
CN107365168A (en) * | 2016-05-11 | 2017-11-21 | 航天特种材料及工艺技术研究所 | A kind of method for improving SiO 2-ceramic based composites tensile strength |
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SU549447A1 (en) * | 1975-09-16 | 1977-03-05 | Предприятие П/Я Г-4816 | Glass ceramic material |
CN103619769A (en) * | 2011-06-28 | 2014-03-05 | 3M创新有限公司 | Glass-ceramics and methods of making the same |
CN104140207A (en) * | 2014-07-29 | 2014-11-12 | 青岛祥海电子有限公司 | Industrial waste residue reuse type glass ceramic |
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Application publication date: 20181116 |