CN104876446B - Enhanced quick treatment devitrified glass of zirconium and combinations thereof, preparation method, purposes - Google Patents
Enhanced quick treatment devitrified glass of zirconium and combinations thereof, preparation method, purposes Download PDFInfo
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- CN104876446B CN104876446B CN201510229156.1A CN201510229156A CN104876446B CN 104876446 B CN104876446 B CN 104876446B CN 201510229156 A CN201510229156 A CN 201510229156A CN 104876446 B CN104876446 B CN 104876446B
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Abstract
The invention discloses enhanced quick treatment devitrified glass of a kind of zirconium and combinations thereof, preparation method, purposes, belong to technical field of oral medicine.Said composition, including following molar fraction than component：Tetraethyl orthosilicate 40 70；Lithium nitrate 10 20；Potassium nitrate 3 12；Zirconium oxychloride 1 20；Aluminum nitrate 0.5 15；Sodium nitrate 0.5 5；Fluorescer 0.5 10；Sensitising agent 0.5 10；Glass modifier 0 10；Colouring agent 0 20.Preparation of the invention is comprised the following steps：Collosol and gel fusion-cast/water quenching die casting crystalline product.The method can include the colouring agent than general devitrified glass higher amount in the case where devitrified glass optics, mechanical property is not changed；Its production temperature is low, energy saving.Devitrified glass of the present invention is used as dental prosthetic material.
Description
Technical field
The invention belongs to technical field of oral medicine, more particularly to a kind of enhanced quick treatment devitrified glass of zirconium and its group
Compound, preparation method, purposes.
Background technology
Ceramics have good biological safety and aesthetic property, become clinically the most commonly used oral restoration material
Material.With the raising that people are required Dental esthetic reparation, traditional ceramics repair materials, because do not possess natural teeth it is translucent, from
The features such as right gloss, will be substituted by new material gradually.
In dental prosthetic new material, this material for obtaining glass part crystallization of devitrified glass possesses ceramics high-strength
Degree, glass translucence, its natural gloss are also very much like with natural teeth.It is relatively low with conventional strength that (bending strength is 120-
Leucite devitrified glass 180MPa) is compared, and the lithium base microcrystal glass with higher-strength (320-420MPa) has turned into market
Main flow dental prosthetic material.
In domestic patent, application publication number is patent " lithium bisilicate glass ceramics, its producer of the A of CN 102741186
Method and application thereof " elaborates that common solid phase fusion prepares the process of lithium bisilicate devitrified glass.In its methods described, glass melting
Temperature is very high, to reach 1500 DEG C or so, and to reduce the porosity, improving material homogeneity, melt temperature will even be raised to
More than 1600 DEG C, and will be in the temperature long-time heat preservation.Furthermore, the A of Chinese patent CN 102741186 due to colouring agent be by
The form of oxide is added in raw material, when colorant content is higher, glass ceramics optical property can be made to change, so as to lead
Cause cannot produce the deeper product of color.In addition, lithium base microcrystal glass when using, final crystallization and thermal treatment process be by with
Family completes, and non-producer completes；So, finished heat treatment process time is reduced, have greatly improved to Consumer's Experience.
Lithium base microcrystal glass in the market has price high, lack of homogeneity, power consumption is high, the porosity is high, Wu Fasheng
The problems such as producing compared with dark colour product.
The content of the invention
It is given below on brief overview of the invention, to provide the basic reason on certain aspects of the invention
Solution.It should be appreciated that this general introduction is not on exhaustive general introduction of the invention.It is not intended to determine key of the invention
Or pith, nor is it intended to limit the scope of the present invention.Its purpose only provides some concepts in simplified form, with
This is used as the preamble in greater detail discussed after a while.
The purpose of the embodiment of the present invention is directed to the defect high that consumes energy of above-mentioned prior art, there is provided one kind production temperature
It is low, enhanced quick treatment devitrified glass of zirconium of energy saving and combinations thereof, preparation method.
To achieve these goals, the present invention is adopted the technical scheme that：
A kind of composition for the enhanced quick treatment devitrified glass of zirconium, including following molar fraction than component：
The present invention also provides a kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, is entered using combinations of the above thing
Prepared by row, specifically include following steps：
Step one：By above-mentioned molar fraction than weighing raw material, by all raw material total mole numbers and the ratio of nitric acid molal quantity
Example is 1:The consumption of 0.5-1.5, adds nitric acid wiring solution-forming, stirs 5-250min, and then ultrasonic vibration 15-120min mixing is equal
It is even to be made colloidal sol；
Step 2：1-24h is incubated during colloidal sol is sealed into water-bath at 50-100 DEG C, gel is formed；Gel is stored at room temperature 12-24
After hour, pour into platinum or platinum-rhodium crucible, when being heated up to 1250 DEG C -1450 DEG C, be incubated 0.5-2h；
Step 3：By the glass metal cooling shaping in step 2 by insulation；
Step 4：By gained mold compound in step 3,800-900 DEG C is heated to, is incubated 0.5-3min.
The present invention provides a kind of zirconium enhanced quick treatment devitrified glass again, is prepared according to above-mentioned preparation method.
The present invention provides a kind of purposes of the enhanced quick treatment devitrified glass of above-mentioned zirconium as dental prosthetic material again.
Compared with prior art, the beneficial effects of the invention are as follows：
Devitrified glass of the invention include high content zirconium compounds, can artificial adjustment devitrified glass mechanical performance and optics
Performance；Can rapidly undergo phase transition at high temperature, and its process stabilization, Newly born phase structure distribution are uniform.It is of the present invention molten
Devitrified glass prepared by sol-gel, it is possible to decrease production temperature, energy saving, and improve material homogeneity.Zirconium of the invention increases
Strong quick treatment devitrified glass can be as dental prosthetic material.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in the embodiment of the present invention
Technical scheme is clearly and completely described, it is clear that described embodiment is a part of embodiment of the invention, rather than complete
The embodiment in portion.The element and feature for describing in one embodiment of the invention can be with one or more other implementations
The element and feature shown in mode are combined.It should be noted that eliminating for purposes of clarity, in explanation unrelated to the invention
, the expression and description of part known to persons of ordinary skill in the art and treatment.Based on the embodiment in the present invention, this area
The every other embodiment that those of ordinary skill is obtained under the premise of creative work is not paid, belongs to protection of the present invention
Scope.
A kind of composition for the enhanced quick treatment devitrified glass of zirconium, including following molar fraction than component：
Zirconium oxychloride mol composition of the invention, by changing zirconium content, can control the machine of devitrified glass between 1-20
Tool performance and optical property.
Preferably, the molar fraction of the potassium nitrate:The molar fraction of lithium nitrate is 1:1-4.
Preferably, the fluorescer is selected from least one of the nitric acid thing of following element：Silver, cerium, bismuth, tin, tellurium, zinc.
Preferably, the sensitising agent is selected from least one of the nitric acid thing of following element：Selenium, strontium, cadmium, titanium, tin, tungsten.
Preferably, the glass modifier is selected from least one of following element acidic materials or its nitric acid thing in itself：Calcium,
Boron, phosphorus, barium, magnesium；
Preferably, the colouring agent is selected from least one of the nitric acid thing of following element：It is iron, cobalt, nickel, selenium, copper, manganese, dilute
Earth elements.
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, is prepared, specifically using combinations of the above thing
Comprise the following steps：
Step one：By above-mentioned molar fraction than weighing raw material, by all raw material total mole numbers and the ratio of nitric acid molal quantity
Example is 1:1 consumption, adds nitric acid wiring solution-forming, stirs 5-250min, and then ultrasonic vibration 15-120min is well mixed is made
Colloidal sol；
Step 2：1-24h is incubated during colloidal sol is sealed into water-bath at 50-100 DEG C, gel is formed；Gel is stored at room temperature 12-24
After hour, pour into platinum or platinum-rhodium crucible, when being heated up to 1250 DEG C -1450 DEG C, be incubated 0.5-2h；
Step 3：By the glass metal cooling shaping in step 2 by insulation；
Step 4：By gained mold compound in step 3,800-900 DEG C is heated to, is incubated 0.5-3min.
Preferably, the cooling shaping of the step 3 includes：By the glass metal of insulation be molded into 450 DEG C -600 DEG C preheating
Die for molding, and anneal 0.5-4 hours；
Or during water will be poured into by the glass metal of insulation in step 2, gained glass dregs are ground into powder, after crossing 300 mesh sieves
It is dry-pressing formed.
Preferably, in the step 3, the dry-pressing formed pressure is：10-100MPa.
Preferably, in the step one, the nitric acid pH value is between 1.5-3.
The sol-gal process that the present invention is used, raw material has been before melting finely dispersed gel state, it is possible to decrease molten
Melt at least 200 DEG C of temperature, and without long-time heat preservation, greatly reduce power consumption.
Before melting, colouring agent is to be mixed in the way of gel in the feed to the present invention so that coloring effect strengthens, and drops
The less colored dose of influence to optical property, so that the colouring agent of higher amount can be added in product, so as to deepen product colour.
The present invention uses specific potassium lithium ratio, using the potassium element polarity principle higher than elemental lithium, is polarized to lithium by potassium
Atom produces influence with the coordination of silicon atom, it is formed chemical bond according to predetermined direction, greatly shortens at final crystallization heat
The reason time, after making user process 0.5-3min at high temperature, you can use.
The present invention provides a kind of zirconium enhanced quick treatment devitrified glass again, is prepared according to above-mentioned preparation method.
The present invention provides a kind of purposes of the enhanced quick treatment devitrified glass of above-mentioned zirconium as dental prosthetic material again.
Below by specific embodiment, the present invention is further illustrated：
Embodiment 1
According to following molar fraction than being equipped with raw material：
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, specifically includes following steps：
Step one：By above-mentioned molar fraction than weighing raw material, by all raw material total mole numbers and the ratio of nitric acid molal quantity
Example is 1:1 consumption, adds nitric acid wiring solution-forming, and nitric acid pH value is 2, stirs 150min, and then ultrasonic vibration 60min mixing is equal
It is even to be made colloidal sol；
Step 2：12h is incubated during colloidal sol is sealed into water-bath at 75 DEG C, gel is formed；After gel is stored at room temperature 16 hours,
Enter in platinum or platinum-rhodium crucible, when being heated up to 1350 DEG C, be incubated 1.5h；
Step 3：During water will be poured into by the glass metal of insulation in step 2, gained glass dregs are ground into powder, cross 300
After mesh sieve, the pressure using 60MPa is dry-pressing formed；
Step 4：By gained mold compound in step 3,850 DEG C are heated to, are incubated 2min.
Embodiment 2
According to following molar fraction than being equipped with raw material：
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, specifically includes following steps：
Step one：By above-mentioned molar fraction than weighing raw material, by all raw material total mole numbers and the ratio of nitric acid molal quantity
Example is 1:0.5 consumption, adds nitric acid wiring solution-forming, and nitric acid pH value is 2.5, stirs 250min, and then ultrasonic vibration 15min is mixed
Conjunction is uniformly made colloidal sol；
Step 2：1h is incubated during colloidal sol is sealed into water-bath at 100 DEG C, gel is formed；After gel is stored at room temperature 12 hours,
Enter in platinum or platinum-rhodium crucible, when being heated up to 1450 DEG C, be incubated 0.5h；
Step 3：550 DEG C of die for molding of preheating will be molded into by the glass metal of insulation in step 2, and annealed
2.5 hours；
Step 4：By gained mold compound in step 3,900 DEG C are heated to, are incubated 0.5min.
Embodiment 3
According to following molar fraction than being equipped with raw material：
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, specifically includes following steps：
Step one：By above-mentioned molar fraction than weighing raw material, by all raw material total mole numbers and the ratio of nitric acid molal quantity
Example is 1:1.5 consumption, adds nitric acid wiring solution-forming, and nitric acid pH value is 1.5, stirs 5min, and then ultrasonic vibration 120min is mixed
Conjunction is uniformly made colloidal sol；
Step 2：24h is incubated during colloidal sol is sealed into water-bath at 50 DEG C, gel is formed；After gel is stored at room temperature 24 hours,
Enter in platinum or platinum-rhodium crucible, when being heated up to 1250 DEG C DEG C, be incubated 2h；
Step 3：During water will be poured into by the glass metal of insulation in step 2, gained glass dregs are ground into powder, cross 400
After mesh sieve, the pressure of 100MPa is dry-pressing formed；
Step 4：By gained mold compound in step 3,800 DEG C are heated to, are incubated 3min.
Embodiment 4
According to following molar fraction than being equipped with raw material：
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, specifically includes following steps：
Step one：By above-mentioned molar fraction than weighing raw material, by all raw material total mole numbers and the ratio of nitric acid molal quantity
Example is 1:1.2 consumption, adds nitric acid wiring solution-forming, and nitric acid pH value is 3, stirs 10min, then ultrasonic vibration 30min mixing
Uniformly it is made colloidal sol；
Step 2：12h is incubated during colloidal sol is sealed into water-bath at 90 DEG C, gel is formed；After gel is stored at room temperature 12 hours,
Enter in platinum or platinum-rhodium crucible, when being heated up to 1300 DEG C, be incubated 1h；
Step 3：In step 2 450 DEG C of die for molding of preheating, and annealing 4 will be molded into by the glass metal of insulation
Hour；
Step 4：By gained mold compound in step 3,800 DEG C are heated to, are incubated 1.5min.
Embodiment 5
According to following molar fraction than being equipped with raw material：
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium is identical with the method for embodiment 1.
Embodiment 6
According to following molar fraction than being equipped with raw material：
A kind of preparation method of the enhanced quick treatment devitrified glass of zirconium is identical with the method for embodiment 1.
In embodiments of the invention 1-3, due to the increase of chromium oxychloride content, degree is raised devitrified glass successively thoroughly；Implement
In example 1 and embodiment 6, because nitric acid cerium content increases, devitrified glass is presented yellow, and color is deepened successively.
Preparation of the invention is comprised the following steps：Sol-gel-melting-casting/water quenching die casting-crystallization-product.The party
Method can include the coloring than general devitrified glass higher amount in the case where devitrified glass optics, mechanical property is not changed
Agent；Its production temperature is low, energy saving.Devitrified glass of the present invention is used as dental prosthetic material.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these modification or
Replace, do not make the spirit and scope of the essence disengaging various embodiments of the present invention technical scheme of appropriate technical solution.
Claims (9)
1. a kind of composition for the enhanced quick treatment devitrified glass of zirconium, it is characterised in that including following molar fraction ratio
Component：
The molar fraction of the potassium nitrate:The molar fraction of lithium nitrate is 1:1-4.
2. the composition for the enhanced quick treatment devitrified glass of zirconium according to claim 1, it is characterised in that described
Fluorescer is selected from least one of the nitric acid thing of following element：Silver, cerium, bismuth, tin, tellurium, zinc.
3. the composition for the enhanced quick treatment devitrified glass of zirconium according to claim 1, it is characterised in that described
Sensitising agent is selected from least one of the nitric acid thing of following element：Selenium, strontium, cadmium, titanium, tin, tungsten.
4. the composition for the enhanced quick treatment devitrified glass of zirconium according to claim 1, it is characterised in that described
Glass modifier is selected from least one in boric acid, phosphoric acid, calcium nitrate, barium nitrate and magnesium nitrate；
And/or；
The colouring agent is selected from least one of the nitric acid thing of following element：Iron, cobalt, nickel, selenium, copper, manganese, rare earth element.
5. a kind of preparation method of the enhanced quick treatment devitrified glass of zirconium, it is characterised in that usage right requirement any one of 1-4
Described composition is prepared, and specifically includes following steps：
Step one：Molar fraction ratio as described in claim any one of 1-4 weighs raw material, by all raw material total mole numbers and nitre
The ratio of sour molal quantity is 1:The consumption of 0.5-1.5, adds nitric acid wiring solution-forming, stirs 5-250min, then ultrasonic vibration 15-
120min is well mixed to be made colloidal sol；
Step 2：1-24h is incubated during colloidal sol is sealed into water-bath at 50-100 DEG C, gel is formed；Gel is stored at room temperature 12-24 hours
Afterwards, pour into platinum or platinum-rhodium crucible, when being heated up to 1250 DEG C -1450 DEG C, be incubated 0.5-2h；
Step 3：By the glass metal cooling shaping in step 2 by insulation；
Step 4：By gained mold compound in step 3,800-900 DEG C is heated to, is incubated 0.5-3min.
6. preparation method according to claim 5, it is characterised in that the cooling shaping of the step 3 includes：Will insulation
Glass metal be molded into 450 DEG C of die for molding of -600 DEG C of preheatings, and anneal 0.5-4 hours；
Or during water will be poured into by the glass metal of insulation in step 2, gained glass dregs are ground into powder, after crossing 200-400 mesh sieves
It is dry-pressing formed.
7. preparation method according to claim 6, in the step 3, the dry-pressing formed pressure is：10-
100MPa；
And/or；
In the step one, the nitric acid pH value is between 1.5-3.
8. the enhanced quick treatment devitrified glass of a kind of zirconium, it is characterised in that according to the preparation described in claim any one of 5-7
Method is prepared.
9. the enhanced quick treatment devitrified glass of zirconium described in a kind of claim 8 is used as the purposes of dental prosthetic material.
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| US3791808A (en) * | 1971-12-23 | 1974-02-12 | Owens Illinois Inc | Method for producing glass ceramics |
| JP3226341B2 (en) * | 1992-07-24 | 2001-11-05 | 三井鉱山株式会社 | Glass ceramic and method for producing the same |
| CN1872753A (en) * | 2005-05-31 | 2006-12-06 | 电子科技大学 | Ceramic material of microcrystalline glass, and preparation method |
| CN103274602B (en) * | 2013-05-20 | 2015-05-13 | 天津大学 | BaO-Al2O3-SiO2 microcrystalline glass prepared by improved sol-gel technology and method |
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Address after: 066004, No. 9, mountain road, Qinhuangdao economic and Technological Development Zone, Hebei Patentee after: Aidit (Qinhuangdao) Polytron Technologies Inc Address before: 066004 West Ring North Road, Qinhuangdao economic and Technological Development Zone, Hebei Province, No. 12 Patentee before: QINHUANGDAO AIDITE HIGH-TECH CERAMIC CO., LTD. |