CN109775988A - One kind containing Na9YSi6O18Crystal phase transparent glass ceramics and preparation method thereof - Google Patents
One kind containing Na9YSi6O18Crystal phase transparent glass ceramics and preparation method thereof Download PDFInfo
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- CN109775988A CN109775988A CN201910254365.XA CN201910254365A CN109775988A CN 109775988 A CN109775988 A CN 109775988A CN 201910254365 A CN201910254365 A CN 201910254365A CN 109775988 A CN109775988 A CN 109775988A
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Abstract
The present invention relates to one kind to contain Na9YSi6O18Crystal phase transparent glass ceramics and preparation method thereof, feed molar percentage composition are as follows: Na2CO340~45%, Y2O32~4%, SiO250~55%, P2O51.5~4.5%, Sb2O30.1~0.5%, preparation method obtains transparent glass using first melting, then pass through the method realization of crystallization.The crystal phase of the transparent glass ceramics of invention is Na9YSi6O18, contain Na with a thickness of 1mm9YSi6O18Crystal phase transparent glass ceramics is 82-85% in the transmitance of visible region.
Description
Technical field
The present invention relates to glass ceramics preparation technical fields, relate in particular to Na9YSi6O18For the transparent glass of crystal phase
Ceramics and preparation method thereof.
Background technique
Transparent glass ceramics have function admirable, fabricating technology is simple, manufacturing cost is low and can be with large-scale industry
The advantage that metaplasia produces becomes the wide new material of a kind of high-performance, low price, application market, thus by numerous scientific works
The concern of author.
At present to the research that crystal phase is silicate glass ceramic mainly from four aspects: first, bioceramic aspect,
Wang Fu et al. [The Fourth Military Medical University Ph.D. Dissertation, 2009] prepares high-intensitive dentistry lithium bisilicate glass ceramics, and to this
The hot pressing casting process of glass ceramics carries out preliminary research.Lithium bisilicate crystal phase has suitable thermal expansion coefficient and anaclasis system
Number, can reach good thermodynamics and optical match with glass phase, so that lithium bisilicate glass ceramics is having higher machinery
While performance, it is still able to maintain outstanding semi-transparent light characteristic, high-intensitive and aesthetic effect unification is realized, is repaired in full porcelain aesthetics
Multiple field has broad application prospects；Second, electric conductivity material aspect, such as Toshinori Okura et al. [Solid
State Ionics, 2016,285,143-154] it has synthesized containing Na5YSi4O12The glass ceramics of crystal phase, from structure and conductive machine
Two aspect of reason is discussed.Third, luminescent properties aspect, silicate glass ceramic has moderate phonon energy, excellent
Doping concentration of rare earth ion and good spectral property make rare earth ion doped silicate glass ceramic become one at present and grind
Study carefully hot spot, as Rishideo Kumar et al. [Journal of the European Ceramic Society, 2018,38
(6), 2639-2648] it is prepared for Eu3+Doping transparent lanthanum silicate potassium (KLaSiO4) glass ceramics, and study its luminescent properties.So
And crystal phase Na9YSi6O18Transparent glass ceramics there is not been reported.
Summary of the invention
The purpose of the present invention is to provide one kind to contain Na9YSi6O18Crystal phase transparent glass ceramics and preparation method thereof.
The present invention is achieved by the following technical solutions:
One kind containing Na9YSi6O18Crystal phase transparent glass ceramics, raw material composition and its content (molar percentage) are as follows:
Na2CO340~45%, Y2O32~4%, SiO250~55%, P2O51.5~4.5%, Sb2O30.1~0.5%.This hair
Bright contains Na9YSi6O18Crystal phase transparent glass ceramics is prepared by the following method:
It is calculated by raw material composition and weighs each component, and said components are sufficiently mixed uniformly, be placed in corundum crucible, be put into
In silicon molybdenum furnace, 1200~1400 DEG C are warming up to, raw material is made to be melt into liquid, and at 1200~1400 DEG C after constant temperature 1~3 hour,
Melt in crucible is poured on to curing molding on warmed-up stainless steel mould, is put into rapidly in 450 DEG C of annealing furnaces, heat preservation 1 is small
When, it is down to room temperature with annealing furnace, transparent glass is made；Transparent glass sample is put into chamber type electric resistance furnace, with 2~4 DEG C/min
Heating rate be warming up to 620~650 DEG C, keep the temperature 1~2 hour crystallization, obtain containing Na9YSi6O18Crystal phase transparent glass ceramics；
Obtained it will contain Na9YSi6O18Crystal phase transparent glass ceramics is cut with cutting machine, then uses the abrasive powder of varying particle size
Material carries out two-sided mirror ultrafinish and polishing to glass ceramics, finally obtains transparent glass ceramics with a thickness of 1mm.
X-ray diffraction analysis is used to determine the crystal phase of transparent glass ceramics for Na9YSi6O18；Using scanning electron microscope
Observation contains Na9YSi6O18The microscopic appearance of crystal phase transparent glass ceramics；Using ultraviolet-visible-near infrared spectrometer measurement
Contain Na with a thickness of 1mm9YSi6O18The transmitance in visible region of crystal phase transparent glass ceramics is up to 82~85%.
Detailed description of the invention
Fig. 1 is containing Na9YSi6O18The X-ray diffraction analysis spectrogram of crystal phase transparent glass ceramics, the figure double as Figure of abstract.
Fig. 2 is containing Na9YSi6O18The stereoscan photograph of crystal phase transparent glass ceramics.
Fig. 3 is containing Na9YSi6O18The transmittance curve of crystal phase transparent glass ceramics.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described, but is not limited to these embodiments.
Embodiment 1
The molar percentage 42Na formed according to raw material2CO3-2Y2O3-53SiO2-2.5P2O5-0.5Sb2O3, weigh each group
Point, and said components are sufficiently mixed uniformly, it is placed in corundum crucible, is put into silicon molybdenum furnace, is warming up to 1400 DEG C, keep raw material molten
Melt into liquid the liquid in crucible is poured on to curing molding on warmed-up stainless steel mould, is put into rapidly after constant temperature 1 hour
In 450 DEG C of annealing furnaces, 1 hour is kept the temperature, is down to room temperature with furnace, transparent glass is made；Transparent glass sample is put into box resistance
In furnace, 620 DEG C are warming up to the heating rate of 2 DEG C/min, 2 hours crystallization is kept the temperature, obtains transparent glass ceramics；It will be obtained
Bright glass ceramics is cut with cutting machine, is then carried out two-sided mirror surface to glass ceramics with the diamond dust powder of varying particle size and is ground
Mill and polishing, finally obtaining transparent silicate glass ceramics thickness of sample is 1mm.Transparent glass is determined using X-ray diffraction analysis
The crystal phase of glass ceramics is Na9YSi6O18, see attached drawing 1；Na is contained using scanning electron microscope observation9YSi6O18Crystal phase transparent glass
The microscopic appearance of ceramics, is shown in attached drawing 2；Containing with a thickness of 1mm is measured using ultraviolet-visible-near infrared spectrometer
Na9YSi6O18The light transmission rate of crystal phase transparent glass ceramics, it is seen that light area light transmission rate is shown in attached drawing 3 up to 85%.
Embodiment 2
The molar percentage 45Na formed according to raw material2CO3-2Y2O3-50SiO2-2.6P2O5-0.4Sb2O3, weigh each group
Point, and said components are sufficiently mixed uniformly, it is placed in corundum crucible, is put into silicon molybdenum furnace, is warming up to 1350 DEG C, keep raw material molten
Melt into liquid the melt in crucible is poured on to curing molding on warmed-up stainless steel mould, is put into rapidly after constant temperature 2 hours
In 450 DEG C of batch-type furnaces, 1 hour is kept the temperature, is down to room temperature with furnace, transparent glass is made；Transparent glass sample is put into box resistance
In furnace, 630 DEG C are warming up to 3 DEG C/min of heating rate, 2 hours crystallization is kept the temperature, obtains transparent glass ceramics；It will be obtained
Transparent glass ceramics is cut with cutting machine, is then carried out with the diamond dust powder of varying particle size to transparent glass ceramics two-sided
Mirror ultrafinish and polishing, finally obtaining transparent glass ceramics thickness of sample is 1mm.Transparent glass is determined using X-ray diffraction analysis
The crystal phase of glass ceramics is Na9YSi6O18；Na is contained using scanning electron microscope observation9YSi6O18Crystal phase transparent glass ceramics it is micro-
See pattern；Na is contained with a thickness of 1mm's using ultraviolet-visible-near infrared spectrometer measurement9YSi6O18Crystal phase transparent glass pottery
The light transmission rate of porcelain, it is seen that light area is up to 82%.
Embodiment 3
According to the amount percentage 41Na of substance2CO3-3Y2O3-51SiO2-4.5P2O5-0.5Sb2O3, each component is weighed, and will
Said components are sufficiently mixed uniformly, are placed in corundum crucible, are put into silicon molybdenum furnace, are warming up to 1400 DEG C, raw material is made to be melt into liquid
Melt in crucible is poured on curing molding on warmed-up stainless steel mould after constant temperature 1 hour by state, is put into 450 DEG C rapidly and is moved back
In stove, 1 hour is kept the temperature, is down to room temperature with furnace, transparent glass is made；Transparent glass sample is put into chamber type electric resistance furnace, with 4
DEG C/heating rate of min is warming up to 640 DEG C, 1 hour crystallization is kept the temperature, transparent glass ceramics is obtained；Transparent glass obtained is made pottery
Porcelain is cut with cutting machine, then with the diamond dust powder of varying particle size to transparent glass ceramics carry out two-sided mirror ultrafinish and
Polishing, finally obtaining transparent glass ceramics thickness of sample is 1mm.The crystalline substance of transparent glass ceramics is determined using X-ray diffraction analysis
It is mutually Na9YSi6O18；Na is contained using scanning electron microscope observation9YSi6O18The microscopic appearance of crystal phase transparent glass ceramics；Using
Ultraviolet-visible-near infrared spectrometer measurement contains Na with a thickness of 1mm's9YSi6O18The light of crystal phase transparent glass ceramics penetrates
Rate, it is seen that light area is up to 83%.
Certainly, there are also many embodiments to be familiar with this field without departing substantially from spirit of that invention and essence by the present invention
Technical staff make corresponding changes and modifications in accordance with the present invention, but these corresponding changes and modifications all should belong to this
In invention the attached claims protection scope.
Claims (1)
1. one kind contains Na9YSi6O18Crystal phase transparent glass ceramics, it is characterised in that: the raw material of the transparent glass ceramics forms
And its mole percent level is as follows: Na2CO340~45%, Y2O32~4%, SiO250~55%, P2O51.5~
4.5%, Sb2O30.1~0.5%, the crystal phase of the transparent glass ceramics is Na9YSi6O18, with a thickness of the transparent glass of 1mm
Ceramics are 82~85% in the transmitance of visible region, and the preparation method of the glass ceramics is by following processing step group
At:
1) it is calculated by raw material composition and weighs each component, and said components are sufficiently mixed uniformly, be placed in corundum crucible, be put into silicon
In molybdenum furnace, 1200~1400 DEG C are warming up to, raw material is made to be melt into liquid, and at 1200~1400 DEG C after constant temperature 1~3 hour, it will
Melt in crucible is poured on curing molding on warmed-up stainless steel mould, is put into rapidly in 450 DEG C of annealing furnaces, keeps the temperature 1 hour,
It is down to room temperature with annealing furnace, transparent glass is made；
2) transparent glass sample is put into chamber type electric resistance furnace, is warming up to 620~650 DEG C with the heating rate of 2~4 DEG C/min,
1~2 hour crystallization is kept the temperature, is obtained containing Na9YSi6O18Crystal phase transparent glass ceramics；
3) obtained it will contain Na9YSi6O18Crystal phase transparent glass ceramics is cut with cutting machine, then uses the Buddha's warrior attendant of varying particle size
Emery dust material carries out two-sided mirror ultrafinish and polishing to glass ceramics, finally obtains transparent glass ceramics with a thickness of 1mm.
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| CN1704380A (en) * | 2004-05-25 | 2005-12-07 | 中国科学院福建物质结构研究所 | Preparation of neodymium-doped scandium lanthanum borate nano powder by acid-base titration |
| CN102503139A (en) * | 2011-11-10 | 2012-06-20 | 中国科学院福建物质结构研究所 | Up-conversion luminescence transparent glass ceramics and preparation method thereof |
| CN106986546A (en) * | 2017-05-11 | 2017-07-28 | 长春理工大学 | One kind contains Na3.6Y1.8(PO4)3Transparent phosphate glass ceramics of crystalline phase and preparation method thereof |
| CN108439806A (en) * | 2018-03-28 | 2018-08-24 | 长春理工大学 | One kind containing BaMoO4Crystalline phase transparent glass ceramics and preparation method thereof |
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2019
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| CN1279218A (en) * | 1999-06-24 | 2001-01-10 | 无锡帕克斯装饰制品有限公司 | Process for adhering light-accumulating fluorescent powder onto solid inorganic material |
| CN1704380A (en) * | 2004-05-25 | 2005-12-07 | 中国科学院福建物质结构研究所 | Preparation of neodymium-doped scandium lanthanum borate nano powder by acid-base titration |
| CN102503139A (en) * | 2011-11-10 | 2012-06-20 | 中国科学院福建物质结构研究所 | Up-conversion luminescence transparent glass ceramics and preparation method thereof |
| CN106986546A (en) * | 2017-05-11 | 2017-07-28 | 长春理工大学 | One kind contains Na3.6Y1.8(PO4)3Transparent phosphate glass ceramics of crystalline phase and preparation method thereof |
| CN108439806A (en) * | 2018-03-28 | 2018-08-24 | 长春理工大学 | One kind containing BaMoO4Crystalline phase transparent glass ceramics and preparation method thereof |
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| TOSHINORI OKARA等: ""Na+ superionic conducting silicophosphate glass-ceramics-Review"", 《SOLID STATE IONICS》 * |
| ZHAO MENGJIE等: ""Preparation and Characterization of Na2O-Y2O3-P2O5-SiO2 Transparent Glass Ceramics"", 《SOLID STATE PHENOMENA》 * |
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Application publication date: 20190521 |