CN105837047B - A kind of leucite glass-ceramic, its preparation method and application - Google Patents
A kind of leucite glass-ceramic, its preparation method and application Download PDFInfo
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- 229910052907 leucite Inorganic materials 0.000 title claims abstract description 108
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000002241 glass-ceramic Substances 0.000 title claims description 15
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 35
- 238000001354 calcination Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims description 39
- 238000004321 preservation Methods 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000003814 drug Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims 3
- 238000010298 pulverizing process Methods 0.000 claims 3
- 238000003825 pressing Methods 0.000 claims 2
- 238000007873 sieving Methods 0.000 claims 2
- 238000005303 weighing Methods 0.000 claims 2
- 239000011521 glass Substances 0.000 abstract description 92
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052681 coesite Inorganic materials 0.000 abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 7
- 239000000377 silicon dioxide Substances 0.000 abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 abstract description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000012567 medical material Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- 238000010792 warming Methods 0.000 description 11
- 229940079593 drug Drugs 0.000 description 10
- 239000013583 drug formulation Substances 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000013081 microcrystal Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000003836 solid-state method Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 208000028523 Hereditary Complement Deficiency disease Diseases 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 201000002388 complement deficiency Diseases 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- C03C10/0018—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 monovalent metal oxide as main constituents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention belongs to field of medical materials, in particular to a kind of leucite devitrified glass, preparation method and application.This method is first to SiO2、Al2O3、K2O、B2O3Equal raw materials are calcined for the first time, and leucite porcelain block is obtained after calcining, obtain leucite porcelain powders after broken, wet ball grinding, drying and screening.After leucite porcelain powders tabletting obtained above calcining, leucite devitrified glass is made.For the size of leucite crystal grain at 1 μm or so, lesser crystallite dimension can effectively improve the intensity of leucite devitrified glass in leucite porcelain powders prepared by the present invention.Leucite devitrified glass intensity with higher and preferable translucency after tabletting calcining provide a kind of new method for the preparation of leucite devitrified glass.
Description
Technical field
The invention belongs to field of medical materials, in particular to a kind of leucite devitrified glass, preparation method and application.
Background technique
Microcrystal glass material since be applied to it is clinical since just with its good biocompatibility, extremely strong corrosion resistance and connect
The advantages that being bordering on the color of natural teeth becomes the main material for being applied to treatment injury of teeth.Wherein leucite devitrified glass
With its high thermal expansion coefficient, good mechanical performance and biological property are widely used.Leucite (K2O-Al2O3-
4SiO2) it is used as K2O-Al2O3-SiO2The main phase of system glass ceramics, Dispersed precipitate directly affect matrix in glass matrix
Performance has been applied in external certain dental polishing products with the color of the mechanical strength and beautification dummy that improve dummy.
China's All-ceramic Dental Material relies primarily on external import, but since import All-ceramic material is expensive, largely the upper limit
Made its clinical application, reason be the microcrystal glass material of domestic production mechanical property, thermal expansion coefficient, in terms of
It is unable to reach the standard of imported material.Therefore the domestic dentistry microcrystal glass material of independent research is to reduce cost with important reality
Border meaning.
Leucite (K2O-Al2O3-4SiO2) it is used as K2O-Al2O3-SiO2The main phase of system glass ceramics, Dispersed precipitate is in glass
In glass matrix, the performance of matrix is directly affected.The method that tradition prepares leucite have solid phase method, hydro-thermal method, sol-gel processing,
Coprecipitation etc., it is that original glass is made using water quenching that wherein solid phase method, which prepares leucite devitrified glass, then in sintering process
Middle progress crystallization crystalline substance processing, compared to other methods, solid phase method have many advantages, such as it is easy to operate it is controllable, the period is short, at low cost.
The disadvantages of there are brittleness for domestic leucite devitrified glass greatly, obdurability is not high, leucite crystal is unevenly distributed.Cause
This, it is necessary to reasonable drug formulation is designed, and improves its own disadvantage by improving system of heat treatment process, keeps it strong
Degree, brittleness, translucency and material homogeneity meet clinical use requirement.Leucite devitrified glass mainly passes through original glass at present
It is made, i.e., melts pharmaceutical raw material Hybrid Heating through Overheating Treatment crystallization, original glass is made in water quenching, and original glass is carried out heat
Processing is precipitated crystal and leucite devitrified glass is made.Original glass is usually by SiO2、Al2O3、K2O、Na2O、B2O3、TiO2Deng
Group is grouped as, wherein SiO2、Al2O3And K2O is the main body of glass composition, is mainly used to that leucite crystal, Na is precipitated2O is mainly used
In reduction original glass fusing point, TiO2As nucleating agent.
1442380 A of CN discloses a kind of dentistry devitrified glass, the K including 15-25%2O, the Al of 20-30%2O3、50-
60% SiO2, 1-6% CaO, 0.1-0.8% MgO, 0.04-001% Fe2O3And 0.04-0.1%TiO2's.The Shen
Dentistry devitrified glass please has excellent physicochemical property, but ideal not enough.
Even if it is worth noting that, all including SiO in many patents2、Al2O3、K2O、Na2O and B2O3Etc. components, but this
A little very subtle variations of component will lead to leucite devitrified glass performance and generate very big variation.Griffith micro-crack is theoretical
It points out, micro-crack present in material under the effect of external force, can around generate stress concentration, when stress reaches certain degree
When, crackle will extend until fracture.The mechanism of devitrified glass mechanical property enhancing, is widely considered to be due to leucite disperse point
It being distributed in glass phase, the crackle generated in glass just will receive the obstruction of leucite crystal in extension, and leucite precipitation is more,
This obstruction will be more strong, so that the intensity of devitrified glass is also increased.The size of usual dialogue garnet crystal needs
Strict control is carried out, generally requires its size less than 4 μm, the stress that can be effectively avoided in devitrified glass in this way is concentrated.
Devitrified glass is a kind of translucent product, and translucency directly affects the beauty of tooth, by the index of light transmittance
It may determine that the uniformity that crystal is precipitated in sample.The measurement of light transmittance has important reality to the quality of identification devitrified glass
Meaning.The thickness of material directly affects its optical property, the amount, chemical characteristic, the granular size of crystal and crystalline substance of crystal in material
The uniformity of grain distribution determines the translucency of material.
Summary of the invention
The purpose of the present invention is to provide a kind of leucite devitrified glass, preparation method and application, the leucite is micro-
Crystal glass has good translucency, has taken into account beautiful and mechanical property.
In order to achieve that object of the invention, the invention adopts the following technical scheme:
In a first aspect, the leucite devitrified glass presses quality percentage the present invention provides a kind of leucite devitrified glass
Than including following component:
Wherein, the sum of each component content of the leucite devitrified glass is no more than 100%.
The SiO2Such as it can be 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%.
The K2O for example can be 18%, 19% or 20%.
The Al2O3Such as it can be 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13% or 14%.
The B2O3Such as it can be 0.6%, 0.7%, 0.8%, 0.9% or 1%.
Preferably, the leucite devitrified glass includes following component by mass percentage:
Wherein, the sum of each component content of the dentistry leucite devitrified glass is no more than 100%.
Second aspect, the present invention provide a kind of preparation method of leucite devitrified glass as described in relation to the first aspect, including
Following steps:
(1) SiO is weighed by formula ratio2、Al2O3、K2O and B2O3, ball milling and it is dried after mixing；
(2) drug after being dried step (1) is calcined, and furnace cooling carries out Crystallizing treatment, is cooled to room
Temperature obtains porcelain block；
(3) the porcelain block for obtaining step (2) crushes, and takes slurry to be sieved after dry after ball milling, obtains porcelain powders；
(4) porcelain powders that step (3) obtains are pressed into required size, carry out secondary clacining, leucite crystallite glass is made
Glass.
In the present invention, analysis detection can be carried out to the leucite powder crystallized by secondary clacining, pass through XRD, SEM etc.
Detection means determines optimal heat treatment process parameter, and chooses the best powder of crystallinity and be sintered molding.Conventional solid-state method
Leucite crystal is precipitated during sinter molding, and control is more difficult.The secondary clacining method quasi-complement deficiency of conventional solid-state method,
It can largely save the cost.
Preferably, the time of step (1) described ball milling is 4-8h, such as can be 4h, 5h, 6h, 7h or 8h, preferably 5-
7h, further preferably 6h.
Preferably, step (3) calcination process use temperature programming, described program heating rate be 8-15 DEG C/
Min, for example, can be 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min or
15 DEG C/min, preferably 9-12 DEG C/min, further preferably 10 DEG C/min.
Preferably, the temperature of the calcining be 1300-1550 DEG C, such as can be 1300 DEG C, 1320 DEG C, 1350 DEG C,
1380 DEG C, 1400 DEG C, 1420 DEG C, 1450 DEG C, 1480 DEG C, 1500 DEG C, 1520 DEG C or 1550 DEG C, preferably 1400-1500 DEG C.
Preferably, the time of the calcining be 0.8-3h, such as can be 0.8h, 0.9h, 1h, 1.2h, 1.3h, 1.5h,
1.6h, 1.8h, 2h, 2.2h, 2.3h, 2.5h, 2.8h or 3h, preferably 1-2h, further preferably 1h.
Preferably, the temperature of furnace cooling described in step (2) be 700-850 DEG C, such as can be 700 DEG C, 720 DEG C,
750 DEG C, 760 DEG C, 780 DEG C, 800 DEG C, 820 DEG C, 830 DEG C or 850 DEG C, preferably 750-820 DEG C.
Preferably, the Ball-milling Time is 8-15h, such as can be 8h, 9h, 10h, 11h, 12h, 13h, 14h or 15h,
Preferably 10-13h, further preferably 12h.
Preferably, the sieve of the mistake be 100-400 mesh, such as can be 100 mesh, 120 mesh, 130 mesh, 150 mesh, 180 mesh,
200 mesh, 220 mesh, 230 mesh, 250 mesh, 260 mesh, 280 mesh, 300 mesh, 320 mesh, 350 mesh, 360 mesh or 400 mesh, preferably 150-
300 mesh, further preferably 200 mesh.
Preferably, step (4) the secondary clacining process uses temperature programming, and the rate of described program heating is 8-15
DEG C/min, such as can be 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min
Or 15 DEG C/min, preferably 9-12 DEG C/min, further preferably 10 DEG C/min.
Preferably, the temperature of the secondary clacining is 900-1200 DEG C, such as can be 900 DEG C, 920 DEG C, 950 DEG C, 980
DEG C, 1000 DEG C, 1020 DEG C, 1050 DEG C, 1080 DEG C, 1100 DEG C, 1120 DEG C, 1150 DEG C, 1180 DEG C or 1200 DEG C, preferably
1000-1200 DEG C, further preferably 1150 DEG C.
Preferably, the preparation method of the leucite devitrified glass includes the following steps:
(1) SiO is weighed by formula ratio2、Al2O3、K2O and B2O3, ball milling 6h, which is placed in drying box, after mixing is dried
Processing；
(2) being put into corundum crucible after being dried step (1) is calcined, and is warming up to 1400-1500 with 10 DEG C/min
DEG C, isothermal holding 1h is melted, cools to 800-900 DEG C of progress Crystallizing treatment with the furnace, 2-4h is kept the temperature, is cooled to room temperature and is baked
Porcelain block；
(3) the porcelain block for obtaining step (2) crushes, and the use of dehydrated alcohol is ball-milling medium ball milling 12h, takes slurry after ball milling
200 meshes are crossed after material is dry, obtain porcelain powders；
(4) porcelain powders that step (3) obtains are pressed into required size, carry out secondary clacining, is warming up to 10 DEG C/min
1150 DEG C, 1h is kept the temperature, leucite devitrified glass is made.
The third aspect, the present invention provide a kind of leucite devitrified glass answering in terms of dentistry as described in relation to the first aspect
With.
Compared with prior art, the invention has the following advantages:
(1) present invention just obtains the porcelain powders using leucite as precipitated phase by the adjustment of formula after first calcining,
And the size of leucite crystal is tiny, at 1 μm or so；
(2) present invention is reached by measuring the three-point bending resistance intensity of leucite devitrified glass sample after tabletting and secondary clacining
100-130MPa, microhardness reach 460-520HV, light-transmission coefficient 0.7-0.9cm-1, and sample has good light transmission
Property, take into account beautiful and mechanical property.
Detailed description of the invention
Fig. 1 is the XRD diagram that leucite devitrified glass porcelain powders are made in embodiment 1；
Fig. 2 is the SEM figure that leucite devitrified glass porcelain powders are made in embodiment 1；
Fig. 3 is the XRD diagram that leucite devitrified glass porcelain powders are made in embodiment 2；
Fig. 4 is the SEM figure that leucite devitrified glass porcelain powders are made in embodiment 2；
Fig. 5 is the XRD diagram that leucite devitrified glass porcelain powders are made in embodiment 3；
Fig. 6 is the SEM figure that leucite devitrified glass porcelain powders are made in embodiment 3；
Fig. 7 is the XRD diagram that leucite devitrified glass porcelain powders are made in embodiment 4；
Fig. 8 is the SEM figure that leucite devitrified glass porcelain powders are made in embodiment 4；
Fig. 9 is the XRD diagram that leucite devitrified glass porcelain powders are made in embodiment 5；
Figure 10 is the SEM figure that leucite devitrified glass porcelain powders are made in embodiment 5.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1400 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 1100 DEG C of heat preservation 2h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use is anhydrous
Ethyl alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, tabletting is made after 1150 DEG C of calcinings
Obtain leucite devitrified glass.
XRD the and SEM result of leucite devitrified glass manufactured in the present embodiment is as shown in Figs. 1-2.
Embodiment 2
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1400 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 1000 DEG C of heat preservation 4h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use is anhydrous
Ethyl alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, tabletting is made after 1150 DEG C of calcinings
Obtain leucite devitrified glass.
XRD the and SEM result of leucite devitrified glass manufactured in the present embodiment is as shown in Figure 3-4.
Embodiment 3
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1450 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 900 DEG C of heat preservation 3h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use anhydrous second
Alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, tabletting is made after 1150 DEG C of calcinings
Leucite devitrified glass.
XRD the and SEM result of leucite devitrified glass manufactured in the present embodiment is as seen in figs. 5-6.
Embodiment 4
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1500 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 900 DEG C of heat preservation 3h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use anhydrous second
Alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, tabletting is made after 1150 DEG C of calcinings
Leucite devitrified glass.
XRD the and SEM result of leucite devitrified glass manufactured in the present embodiment is as Figure 7-8.
Embodiment 5
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1500 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 1050 DEG C of heat preservation 2h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use is anhydrous
Ethyl alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, tabletting is made after 1150 DEG C of calcinings
Obtain leucite devitrified glass.
XRD the and SEM result of leucite devitrified glass manufactured in the present embodiment is as shown in figs. 9-10.
Comparative example 1
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1500 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 1050 DEG C of heat preservation 2h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use is anhydrous
Ethyl alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, tabletting is made after 1150 DEG C of calcinings
Obtain leucite devitrified glass.
Comparative example 2
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1500 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 900 DEG C of heat preservation 3h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use anhydrous second
Alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, leucite devitrified glass is made in tabletting.
Comparative example 3
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1500 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But to 900 DEG C of heat preservation 3h, 800 DEG C of heat preservation 2h is cooled to, room temperature is finally cooled to and obtains leucite porcelain block, use anhydrous second
Alcohol is to cross 200 meshes after medium ball milling is dried, and obtains leucite devitrified glass porcelain powders, leucite devitrified glass is made in tabletting.
Comparative example 4
The leucite devitrified glass includes following component by mass percentage:
Drug is weighed by drug formulation, is calcined after ball milling is dry, 1600 DEG C of heat preservation 1h are warming up to 10 DEG C/min, it is cold with furnace
But it to 1100 DEG C of heat preservation 4h, is finally cooled to room temperature and obtains leucite porcelain block, the use of dehydrated alcohol is after medium ball milling is dried
200 meshes are crossed, leucite devitrified glass porcelain powders are obtained, leucite devitrified glass is made in tabletting after 1250 DEG C of calcinings.
Performance test and characterization:
Leucite devitrified glass made from embodiment 1-5 and comparative example 1-5 is tested for the property, test method is as follows:
Test result is as shown in table 1:
Table 1
As it can be seen from table 1 the three-point bending resistance intensity of the garnet devitrified glass sample in embodiment 1-5 has reached 100-
130MPa, microhardness reach 460-520HV, light-transmission coefficient 0.7-0.9cm-1, all it is substantially better than comparative example 1-4, it is seen then that and
Sample has good translucency, has taken into account beautiful and mechanical property.
The Applicant declares that the present invention illustrates the process method of the present invention through the above embodiments, but the present invention not office
It is limited to above-mentioned processing step, that is, does not mean that the present invention must rely on the above process steps to be carried out.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to raw material selected by the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (31)
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Citations (3)
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|---|---|---|---|---|
| US6342302B1 (en) * | 1998-11-13 | 2002-01-29 | Degussa Ag | Ceramic dental restoration |
| US6527846B1 (en) * | 1998-08-17 | 2003-03-04 | Chemichl Ag | Glass-ceramic material for dental restoration and method for producing same |
| CN103910489A (en) * | 2012-12-29 | 2014-07-09 | 中国科学院过程工程研究所 | Glass used as dental veneering porcelain, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2515566A (en) * | 2013-06-28 | 2014-12-31 | Queen Mary & Westfield College | Leucite glass ceramics |
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2016
- 2016-03-23 CN CN201610168992.8A patent/CN105837047B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6527846B1 (en) * | 1998-08-17 | 2003-03-04 | Chemichl Ag | Glass-ceramic material for dental restoration and method for producing same |
| US6342302B1 (en) * | 1998-11-13 | 2002-01-29 | Degussa Ag | Ceramic dental restoration |
| CN103910489A (en) * | 2012-12-29 | 2014-07-09 | 中国科学院过程工程研究所 | Glass used as dental veneering porcelain, preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| 晶化热处理工艺对白榴石微晶玻璃性能影响的研究;包硕等;《硅酸盐通报》;20151130;第34卷(第S1期);第53页第2.2节 |
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