CN105217959A - A kind of lithium base glass-ceramic preparation method for dental prosthesis - Google Patents
A kind of lithium base glass-ceramic preparation method for dental prosthesis Download PDFInfo
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- CN105217959A CN105217959A CN201410271711.2A CN201410271711A CN105217959A CN 105217959 A CN105217959 A CN 105217959A CN 201410271711 A CN201410271711 A CN 201410271711A CN 105217959 A CN105217959 A CN 105217959A
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Abstract
The embodiment of the invention discloses a kind of lithium base glass-ceramic preparation method for dental prosthesis, comprise: glass powder particle diameter obtained being in advance less than 50 microns loads in mould, be pressed under the condition of 50 ~ 500Mpa, obtain lithium base glass-ceramic base substrate; Described lithium base glass-ceramic base substrate is put into heating unit with the temperature rise rate of 1 DEG C/min ~ 30 DEG C/min, be warming up to 500 DEG C ~ 600 DEG C, carry out first sintering, the soaking time of described first sintering is 10min ~ 120min; Furnace cooling, obtained described lithium base glass-ceramic.Compared with lithium bisilicate glass-ceramic prepared by the lithium base glass-ceramic prepared of technical solution of the present invention and prior art, intensity is less, and hardness is low, and processing characteristics is better, more easily shaping, is applicable to add break and the other repair system of chair.
Description
Technical field
The present invention relates to dental prosthesis technical field, particularly a kind of lithium base glass-ceramic preparation method for dental prosthesis.
Background technology
The other repair system of chair computer aided design and manufacture is incorporated into a kind of dental restoration system formed in dental restorative area.
The feature of the other repair system of chair is convenient and swift, it break grind one's teeth in sleep in the past, traditional artificial tooth manufacturing course such as delivery, quarter are cured, Beijing enamel, after tooth is ground deseaming by dentist, namely with the direct capture of 3D Kamera, import computer into immediately, automatic porcelain block shredder computer auxiliary under, porcelain block is processed into dental prosthesis.
Since the other repair system of chair occurs, the exploitation being suitable for the dental prosthesis material of the other repair system of chair just becomes the research emphasis of domestic and international researchist.
It is found that the dummy that lithium bisilicate glass ceramic material makes both had had outstanding aesthetic effect, and had again good mechanical property, be applicable to very much making dental prosthesis.
But this lithium bisilicate glass ceramic material intensity is all at more than 350Mpa, and because intensity is comparatively large, processing characteristics is poor, is unfavorable for shaping, be difficult to apply in the other repair system of chair.
In order to address this problem, CN102741186 describes a kind of crystallisation step in centre and carries out mechanical workout, and show as high strength, highly translucent and chemically stable lithium bisilicate system glass-ceramic after second step thermal treatment, the method adopted in this patent is that high-temperature melting method is shaping.
But this molding mode is after the first step crystallization, and in product, amount of glassy phase is higher, easily occur collapsing the problems such as limit fracture in the course of processing.
When adopting high-temperature melting method shaping, in order to make glass metal clarification and homogenization, need higher melt temperature, and will be incubated the long period at high operating temperatures, therefore energy consumption is large.
Moreover, long-time high temperature, easily makes the element evaporations such as the phosphorus in lithium bisilicate frit, fluorine, also easily causes the minimizing of Si-OH functional group; Make Ca in the biomaterial obtained
2 +solubility property relatively low; These problems not only cause composition to be difficult to control, and also can reduce the biological activity of material.
Summary of the invention
For solving the problem, the embodiment of the invention discloses a kind of lithium base glass-ceramic preparation side for dental prosthesis; Technical scheme is as follows:
For a lithium base glass-ceramic preparation method for dental prosthesis, comprising:
Glass powder particle diameter obtained being in advance less than 50 microns loads in mould, is pressed, obtains lithium base glass-ceramic base substrate under the condition of 50 ~ 500Mpa; The base starting material of described glass powder is:
SiO
2：60.0wt％～72.0wt％；
Li
2O：10.0wt％～16.0wt％；
K
2O：0.5wt％～4.5wt％；
B
2O
3：0wt％～3.5wt％；
P
2O
5：2.0wt％～5.0wt％；
ZrO
2：0wt％～15.0wt％；
Al
2O
3：2.0wt％～4.0wt％；
ZnO：0wt％～3.0wt％；
MgO：0wt％～1.5％wt％；
La
2O
3：0wt％～2.0wt％；
Na
2O：0wt％～1.5wt％；
CaO：0wt％～2.0％wt％；
Coloring oxide: 0wt% ~ 10.0wt%;
Described lithium base glass-ceramic base substrate is put into heating unit with the temperature rise rate of 1 DEG C/min ~ 30 DEG C/min, be warming up to 500 DEG C ~ 600 DEG C, carry out first sintering, the soaking time of described first sintering is 10min ~ 120min; Furnace cooling, obtained described lithium base glass-ceramic.
In a kind of preferred embodiment of the present invention, after obtained described lithium base glass-ceramic, comprise further:
Described lithium base glass-ceramic is made dummy base substrate;
Described dummy base substrate is put into porcelain oven body, with the temperature rise rate of 10 DEG C/min-60 DEG C/min, be warming up to 800 DEG C ~ 950 DEG C, carry out second time sintering, the soaking time of described second time sintering is 5min ~ 30min, after described second time sintered heat insulating terminates, furnace cooling, obtains dummy.
In a kind of preferred embodiment of the present invention, the preparation method of described glass powder is:
A, take each base starting material by the weight percent of described base starting material, mix after grinding, base starting material particle diameter being less than 400 microns makes admixtion;
B, by described admixtion with the heating rate to 1500 of 10 DEG C/min ~ 15 DEG C/min DEG C ~ 1550 DEG C, and be incubated 0.5h ~ 3h, make it clarify homogenizing, obtained glass metal;
C, described glass metal is carried out shrend, obtain glass fragment, then described glass fragment is dried 1h ~ 2h under the condition of 100 DEG C ~ 150 DEG C;
D, by dry after glass fragment grinding, obtain the glass powder that particle diameter is less than 50 microns.
In a kind of preferred embodiment of the present invention, described coloring oxide is selected from least one in the oxide compound of following element, and described element is iron, titanium, vanadium, manganese, copper, chromium, cobalt, nickel, selenium and rare earth metal.
In a kind of preferred embodiment of the present invention, at least one in described rare earth metal selected from cerium, terbium, erbium, neodymium, praseodymium, samarium, europium.
In a kind of preferred embodiment of the present invention, in step a and d, described grinding is specially uses ball mill ball milling.
In a kind of preferred embodiment of the present invention, the medium of described ball milling is agate or zirconium white.
In a kind of preferred embodiment of the present invention, the weight ratio of described glass fragment and ball-milling medium is 1:2.
In a kind of preferred embodiment of the present invention, in step a, described by particle diameter the base starting material be less than between 400 microns make admixtion, be specially:
Base starting material particle diameter being less than 150 microns makes admixtion.
In a kind of preferred embodiment of the present invention, the particle diameter of described glass powder is specially: be less than 3 microns.
In a kind of preferred embodiment of the present invention, described compression moulding is: dry-pressing formed, isostatic pressing or combination that is dry-pressing formed and isostatic pressing.
In a kind of preferred embodiment of the present invention, described heating unit is vacuum heat treatment furnace or resistance furnace.
In a kind of preferred embodiment of the present invention, the temperature of described second time sintering is 820 DEG C ~ 920 DEG C.
The present invention is by sintering glass powder at 500 DEG C ~ 600 DEG C, obtain lithium base glass-ceramic, its intensity is 40 ~ 120Mpa, compared with the lithium bisilicate glass-ceramic of prior art, this lithium base glass-ceramic intensity is less, and hardness is low, and processing characteristics is better, more easily shaping, be applicable to add break and the other repair system of chair.
The sintering process that the present invention adopts is compared with the high-temperature melting method of prior art, long high temperature homogenizing is not needed in melting process, the insulation short period just can obtain relatively uniform glass metal, glass powder after shrend can carry out further Homogenization Treatments by grinding, greatly saves the energy.
Moreover, shorter soaking time makes the element evaporation degree such as phosphorus, fluorine in lithium bisilicate frit reduce; Not easily cause the minimizing of Si-OH functional group; And make Ca in the biomaterial that obtains
2 +solubility property also relatively high; Therefore, make the control of its composition more accurate; Also the product finally obtained is made to have good biological activity.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below.Obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
In the inventive solutions, after host glass powder being made lithium base glass-ceramic base substrate, first lithium base glass-ceramic base substrate is carried out first sintering at 500 DEG C ~ 600 DEG C, in sintering process, because temperature is lower, not there is chemical transformation in each component, just relies on physical action to be mutually bonded together.Therefore, compactness is poor, and intensity is low, and usually at 40 ~ 120Mpa, processing characteristics is better.
After shaping, crystallization again under 800 ~ 950 DEG C of conditions, lithium metasilicate changes into lithium bisilicate to glass-ceramic, and hardness increases substantially, and can reach more than 350Mpa, reaches the requirement of dental restoration.
The equipment adopted in the embodiment of the present invention, the agate jar of the ball mill such as grinding base starting material, the sintering oven preparing glass metal, abrading glass fragment, the hydraulic single column press of compression moulding, isostatic pressing machine and to lithium base glass-ceramic base substrate carry out sintering sintering oven used or vacuum heat treatment furnace all belong to the state of the art, those skilled in the art can carry out choice for use according to practical situation, and the present invention does not do concrete restriction at this.
Below for each embodiment, a kind of preparation method of the lithium base glass-ceramic for dental prosthesis is described in detail.
Embodiment one
For the preparation of the lithium base glass-ceramic of dental prosthesis, its preparation method is as follows:
A, take each base starting material by the quality of each component of embodiment in table 11, then each base starting material is used ball mill ball milling 2.5 hours respectively, obtain the admixtion that particle diameter is less than 150 microns;
B, obtained admixtion is put into platinum crucible, with the heating rate to 1550 DEG C of 10 DEG C/min in sintering oven, and be incubated 1h and clarify homogenizing, obtained glass metal;
C, obtained glass metal is carried out shrend, obtain glass fragment, then described glass fragment is dried 1h under the condition of 120 DEG C;
D, to put into the glass fragment after drying with agate be that the ball grinder of ball-milling medium carries out ball mill pulverizing, and the amount of the agate ball added is 200g, and ball milling 50 hours, obtains the glass powder that particle diameter is less than 10 microns;
E, obtained glass powder to be loaded in mould, carry out dry-pressing formed with hydraulic single column press under the condition of 160Mpa, obtain lithium base glass-ceramic base substrate;
F, obtained glass-ceramic base substrate is put into resistance furnace with the temperature rise rate of 5 DEG C/min, be warming up to 500 DEG C, sinter, the soaking time of sintering is 80min; Furnace cooling, obtained described lithium base glass-ceramic.
According to the method such as described in embodiment 1, adopt the quality of each base starting material of embodiment 2-7 in table 1, and the processing parameter of each step in table 2, prepare the lithium base glass-ceramic for dental prosthesis of embodiment 2-7 respectively.
It should be noted that, in table 1, each oxide compound can obtain with its corresponding carbonate, nitrate, vitriol or oxide compound.
Each component and quality thereof in table 1 embodiment 1-7
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | |
| SiO 2 | 65.0 | 67.0 | 68.0 | 70.5 | 60 | 63 | 63 |
| Li 2O | 13.5 | 14.0 | 14.5 | 13.0 | 13 | 12 | 11 |
| K 2O | 3.2 | 3.3 | 3.5 | 3.8 | 2.2 | 2.1 | 4 |
| B 2O 3 | 2.8 | 2.8 | 2.7 | 2.9 | 0.3 | 2.5 | 3.4 |
| P 2O 5 | 3.0 | 3.1 | 3.3 | 3.4 | 2.1 | 4.8 | 2.8 |
| ZrO 2 | 1.5 | 3.5 | 2.5 | —— | 9.5 | 5.3 | 0.8 |
| Al 2O 3 | 2.4 | 2.6 | 2.1 | 2.0 | 2.2 | 2.8 | 3 |
| ZnO | 1.5 | —— | 2.0 | 1.5 | 3 | 1 | 0.8 |
| MgO | 0.6 | 0.5 | 0.6 | 0.6 | 1.5 | —— | 1 |
| La 2O 3 | 0.1 | 0.1 | —— | —— | 0.5 | 0.9 | 1.5 |
| Na 2O | 0.6 | 0.3 | 0.4 | 0.5 | 1.4 | —— | 0 |
| CaO | —— | —— | —— | —— | 0.5 | 1.5 | 2 |
| CeO 2 | 2.8 | 1.5 | —— | 1.2 | 0.7 | 2.5 | 1.3 |
| V 2O 5 | 0.8 | 0.2 | 0.4 | 0.5 | 1 | —— | 1.2 |
| Er 2O 3 | 1.2 | 0.1 | —— | 0.1 | 1.4 | 0.7 | 1.8 |
| Tb 2O 3 | 1.0 | 1.0 | —— | —— | 0.7 | 0.9 | 2.4 |
* in upper table, the mass unit of each component is g.
The processing parameter of each step of table 2 embodiment 2-7
Lithium base glass-ceramic for dental prosthesis prepared by the preparation method applying the various embodiments described above, hardness is lower.The lithium base glass-ceramic obtained by above-described embodiment is processed into the size of rule, intensity, the density of the lithium base glass-ceramic obtained by test.The mode of CAD/CAM is adopted to be processed into dental restoration after bonding caudal peduncle.The processing characteristics of the lithium base glass-ceramic obtained by test.Result is as shown in table 3.
The performance test results of lithium base glass-ceramic prepared by table 3 embodiment 1-7
As can be seen from the data in upper table, the intensity of prepared lithium base glass-ceramic is all at 40-120Mpa, intensity is less, relatively be conducive to processing, but be through the dummy base substrate be processed into, no matter from terms of mechanics or aesthstic aspect, also do not reach the requirement of dental prosthesis, so need further to heat up crystallization, namely carry out second time sintering, gain in strength.
For embodiment 1, its intensification crystallisation process is described in detail.
Complex base substrate embodiment 1 prepared puts into porcelain oven body, with the temperature rise rate of 30 DEG C/min, is warming up to 850 DEG C, carries out second time sintering, and the soaking time of second time sintering is 10min, and after insulation terminates, furnace cooling, obtains dummy.
According to the method that the second time of embodiment 1 sinters, adopt each processing parameter in table 4, the dummy base substrate prepared embodiment 2-7 respectively carries out second time sintering, the results are shown in Table 5.
The second time sintering process parameter of dummy base substrate prepared by table 4 embodiment 2-7
The second time sintering result of dummy base substrate prepared by table 5 embodiment 1-7
As can be seen from Table 5, after the dummy base substrate that lithium base glass-ceramic is made being carried out second time sintering, can obtain the dummy that principal crystalline phase is lithium bisilicate, its intensity is greater than 320Mpa, and has light transmission in various degree.
It should be noted that, the foregoing is only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention.All any amendments done within the spirit and principles in the present invention, equivalent replacement, improvement etc., be all included in protection scope of the present invention.
Claims (13)
1., for a lithium base glass-ceramic preparation method for dental prosthesis, it is characterized in that, comprising:
Glass powder particle diameter obtained being in advance less than 50 microns loads in mould, is pressed, obtains lithium base glass-ceramic base substrate under the condition of 50 ~ 500Mpa; The base starting material of described glass powder is:
SiO
2：60.0wt％～72.0wt％；
Li
2O：10.0wt％～16.0wt％；
K
2O：0.5wt％～4.5wt％；
B
2O
3：0wt％～3.5wt％；
P
2O
5：2.0wt％～5.0wt％；
ZrO
2：0wt％～15.0wt％；
Al
2O
3：2.0wt％～4.0wt％；
ZnO：0wt％～3.0wt％；
MgO：0wt％～1.5％wt％；
La
2O
3：0wt％～2.0wt％；
Na
2O：0wt％～1.5wt％；
CaO：0wt％～2.0％wt％；
Coloring oxide: 0wt% ~ 10.0wt%;
Described lithium base glass-ceramic base substrate is put into heating unit with the temperature rise rate of 1 DEG C/min ~ 30 DEG C/min, be warming up to 500 DEG C ~ 600 DEG C, carry out first sintering, the soaking time of described first sintering is 10min ~ 120min; Furnace cooling, obtained described lithium base glass-ceramic.
2. preparation method as claimed in claim 1, is characterized in that, after obtained described lithium base glass-ceramic, comprises further:
Described lithium base glass-ceramic is made dummy base substrate;
Described dummy base substrate is put into porcelain oven body, with the temperature rise rate of 10 DEG C/min-60 DEG C/min, be warming up to 800 DEG C ~ 950 DEG C, carry out second time sintering, the soaking time of described second time sintering is 5min ~ 30min, after described second time sintered heat insulating terminates, furnace cooling, obtains dummy.
3. preparation method as claimed in claim 1, it is characterized in that, the preparation method of described glass powder is:
A, take each base starting material by the weight percent of described base starting material, mix after grinding, base starting material particle diameter being less than 400 microns makes admixtion;
B, by described admixtion with the heating rate to 1500 of 10 DEG C/min ~ 15 DEG C/min DEG C ~ 1550 DEG C, and be incubated 0.5h ~ 3h, make it clarify homogenizing, obtained glass metal;
C, described glass metal is carried out shrend, obtain glass fragment, then described glass fragment is dried 1h ~ 2h under the condition of 100 DEG C ~ 150 DEG C;
D, by dry after glass fragment grinding, obtain the glass powder that particle diameter is less than 50 microns.
4. preparation method as claimed in claim 1, it is characterized in that, described coloring oxide is selected from least one in the oxide compound of following element, and described element is iron, titanium, vanadium, manganese, copper, chromium, cobalt, nickel, selenium and rare earth metal.
5. preparation method as claimed in claim 4, is characterized in that, at least one in described rare earth metal selected from cerium, terbium, erbium, neodymium, praseodymium, samarium, europium.
6. preparation method as claimed in claim 3, is characterized in that, in step
awith in d, described grinding is specially uses ball mill ball milling.
7. preparation method as claimed in claim 6, it is characterized in that, the medium of described ball milling is agate or zirconium white.
8. preparation method as claimed in claim 6, it is characterized in that, the weight ratio of described glass fragment and ball-milling medium is 1:2.
9. preparation method as claimed in claim 3, is characterized in that, in step a, described by particle diameter the base starting material be less than between 400 microns make admixtion, be specially:
Base starting material particle diameter being less than 150 microns makes admixtion.
10. preparation method as claimed in claim 1, it is characterized in that, the particle diameter of described glass powder is specially: be less than 3 microns.
11. preparation methods as claimed in claim 1, it is characterized in that, described compression moulding is: dry-pressing formed, isostatic pressing or combination that is dry-pressing formed and isostatic pressing.
12. preparation methods as claimed in claim 1, it is characterized in that, described heating unit is vacuum heat treatment furnace or resistance furnace.
13. preparation methods as claimed in claim 2, is characterized in that, the temperature of described second time sintering is 820 DEG C ~ 920 DEG C.
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| CN107265867A (en) * | 2017-06-16 | 2017-10-20 | 有研医疗器械（北京）有限公司 | It is a kind of for lithium base glass ceramic powder of dental prosthetic and preparation method thereof |
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| CN109592904A (en) * | 2017-10-02 | 2019-04-09 | 株式会社松风 | High-intensitive lithium metasilicate glass composition with high shielding |
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| CN109592904A (en) * | 2017-10-02 | 2019-04-09 | 株式会社松风 | High-intensitive lithium metasilicate glass composition with high shielding |
| CN109592904B (en) * | 2017-10-02 | 2023-08-04 | 株式会社松风 | High strength lithium silicate glass composition with high shielding property |
| CN109231840A (en) * | 2018-11-29 | 2019-01-18 | 成都贝施美生物科技有限公司 | A kind of glass ceramics and preparation method thereof |
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| EP3957614A4 (en) * | 2019-04-15 | 2022-04-20 | Shenzhen Upcera Dental Technology Co., Ltd | Pre-sintered ceramic block for dental restoration, preparation method therefor and use thereof |
| WO2020210956A1 (en) * | 2019-04-15 | 2020-10-22 | 深圳爱尔创口腔技术有限公司 | Pre-sintered porcelain block for dental restoration, preparation method therefor and application thereof |
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| CN113574026A (en) * | 2019-04-15 | 2021-10-29 | 深圳爱尔创口腔技术有限公司 | Pre-sintered ceramic block for dental prosthesis, preparation method and application thereof |
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| RU2785730C1 (en) * | 2019-04-15 | 2022-12-12 | Шэньчжэнь Упцера Дентал Текнолоджи Ко., Лтд | Ceramic block for teeth restoration, subjected to pre-sintering, its manufacturing method and its use |
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Application publication date: 20160106 |