CN109534681B - Preparation method of lithium disilicate composite bioglass ceramic - Google Patents
Preparation method of lithium disilicate composite bioglass ceramic Download PDFInfo
- Publication number
- CN109534681B CN109534681B CN201910018657.3A CN201910018657A CN109534681B CN 109534681 B CN109534681 B CN 109534681B CN 201910018657 A CN201910018657 A CN 201910018657A CN 109534681 B CN109534681 B CN 109534681B
- Authority
- CN
- China
- Prior art keywords
- composite
- lithium disilicate
- glass
- bioglass
- grinding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
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
- C03C10/0009—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 silica as main constituent
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
Abstract
The invention belongs to the field of biological functional materials, and discloses a preparation method of lithium disilicate composite bioglass ceramic. The method comprises the following steps: firstly, preparing bioglass powder by a sol-gel method and a melting method, mixing according to a certain proportion, grinding, sieving, molding and calcining to prepare the lithium disilicate composite bioglass ceramic. The method has the advantages of simple process, low price of used raw materials, easy operation and the like, and the prepared lithium disilicate composite bioglass ceramic has good mechanical property and bioactivity, can be applied to repair of wound defects, drug controlled release, cell culture and the like in the dental field, and has good application prospect.
Description
Technical Field
The invention relates to the field of biological functional materials, in particular to a preparation method of lithium disilicate composite bioglass ceramic.
Background
Dental caries is always a global oral disease with high incidence rate and wide distribution. At present, the treatment of dental caries mainly adopts mechanical removal of carious lesion parts, and amalgam materials, novel metal alloys, composite resins, dental ceramics and other materials are filled in the carious lesion parts. In the mouth rehabilitation operation, the affinity of metal and medical polymer materials with human tissues is poor. If implanted into the human body for a long time, metal ions are eluted from the metal material, and unreacted monomers remaining during production are eluted from the polymer material, thereby causing a certain risk to the human body tissue. Therefore, the biological ceramic material is more and more favored by people and becomes a hot point of research in recent years.
Bioglass (BG) is an important branch of biomedical materials, mainly composed of silicate glass materials, the main component of which is SiO2And CaO. After the bioactive glass is implanted into a body, the bioactive glass surface reacts with body fluid in an ion mode, and finally a low-crystallinity hydroxyapatite carbonate layer HCA similar to inorganic minerals in bones is formed on the glass surface. The chemical composition of BG is similar to the skeleton of an organism, and has excellent osteoinductivity, osteoconductivity and biocompatibility. In addition, BG allows cells to rapidly proliferate and differentiate on its surface, eventually fusing with surrounding tissues. However, some reactive glasses currently used for preparing dental materials have relatively low strength, which limits their use in the posterior dental area, especially the molar area, where the amount of occlusal forces is large.
The lithium disilicate glass ceramics can generate a rod-shaped lithium disilicate main crystal phase by controlled crystallization. The lithium disilicate crystal belongs to a cubic structure, and the vertex of the Si-O tetrahedron is formed by Li+And (4) occupying, and modifying the network. According to the research of the oral medical college of Wuhan university, the main reason for the improvement of the mechanical properties of the lithium disilicate glass ceramics is that a small amount of lithium phosphate exists in the glass matrix and is distributed on the surface of lithium disilicate crystals. These phosphate crystals generate radial compressive stress, and when cracks occur on the surface or inside of the ceramic, the cracks can be prevented from further propagation, thereby improving mechanical properties. Although the lithium disilicate glass ceramics is an oral cavity repairing material with outstanding performance, and the mechanical property of the lithium disilicate glass ceramics can basically meet the requirement of dental medical materials, the lithium disilicate glass ceramics has poor biological activity, thereby influencing the practical application and becoming a research hotspot of the oral cavity repairing material.
Currently, there are two general methods for making bioglass. Wherein, the melting method is to directly mix glass raw materials, rapidly cool and anneal the glass raw materials after high-temperature melting to obtain glass; then, the bioactive glass ceramic is formed through nucleation and crystallization, and has high density and no air holes. Compared with glass prepared by a melting method, the sol-gel method is a process for synthesizing materials at low temperature, chemical components around alkali metal ions in the sol-gel bioactive glass are more uniform, and phase separation is more favorable to be generated thermodynamically, but the sol-gel bioactive glass is generally in a porous structure, has good bioactivity, and is generally poor in mechanical property. The invention mixes the bioglass powder prepared by the sol-gel method and the melting method together according to a certain proportion, and can obtain the lithium disilicate composite bioglass ceramic with high mechanical property and good bioactivity. The method is simple and efficient, and the used raw materials are cheap and easy to obtain, so that the method has a good industrialization prospect.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a lithium disilicate composite bioglass ceramic material which is simple to operate and can obtain good mechanical property and bioactivity by combining the advantages of a sol-gel method and a melting method for preparing bioglass, and can be applied to the field of dental biomedicine.
The technical scheme of the invention is as follows:
a preparation method of lithium disilicate composite bioglass ceramic comprises the following steps:
(1) preparing glass by a sol-gel method:
adding a nitric acid solution with the concentration of 1 mol/L into deionized water, fully stirring, adjusting the pH value to 2-4, adding a proper amount of tetraethyl orthosilicate aqueous solution into the nitric acid solution, and stirring by adopting magnetic force until the solution becomes clear; other raw materials are SiO according to the molar ratio of (50-60)2-(26~36)Li2O-8ZrO2-3K2O-2P2O5-Al2O3Adding triethyl phosphate, lithium nitrate, zirconium nitrate pentahydrate, potassium nitrate and aluminum nitrate nonahydrate in sequence, ensuring that the mixture is magnetically stirred for 30 minutes before adding each substance, and finally magnetically stirred for 1 hour and kept stand to form the compoundTransparent sol; aging the obtained sol at 60-80 ℃ for 10-48 h, and then heating to 100-180 ℃ for drying for 12-72 h; and grinding the xerogel to obtain gel particles, then calcining the gel particles in a muffle furnace at 400-600 ℃ for 2-24 h, cooling at room temperature, and grinding to obtain glass powder prepared by a sol-gel method, wherein the glass powder is marked as SBG.
(2) Preparing glass by a melting method:
according to the molar ratio of (50-60) SiO2-(26~36)Li2O-8ZrO2-3K2O-2P2O5-Al2O3Weighing silicon dioxide, lithium carbonate, zirconium oxide, potassium carbonate, phosphorus pentoxide and aluminum oxide according to the proportion, fully mixing the raw materials, and putting the mixture into crucibles, wherein the loading height of each crucible is not more than 2/3 of the total height of the crucible. And (3) placing the material-loading crucible into a muffle furnace, preserving heat at 330 ℃ for 30 min, preserving heat at 840 ℃ for 30 min, and then preserving heat at 1500 ℃ for 0.5-3 h. And finally, quickly pouring the liquid in the crucible into normal-temperature water in a molten state for cold quenching to obtain glass particles, drying the glass particles at 100 ℃ for 3 hours, and mechanically grinding the glass particles to obtain glass powder prepared by a melting method, wherein the glass powder is marked as MBG.
(3) Mixing the SBG obtained in the step (1) and the MBG glass powder obtained in the step (2) according to a mass ratio of 1: 9-9: 1, fully grinding the mixed powder, drying the ground mixed powder in a drying oven at 100 ℃ for 3 hours, grinding and sieving the ground mixed powder again to obtain mixed glass powder with the particle size of less than 45 mu m, pressing the mixed glass powder by adopting a mold to obtain a block in a required shape, and finally transferring the block to a muffle furnace to calcine the block for 1 to 24 hours at 750 to 900 ℃ to obtain the lithium disilicate composite bioglass ceramic.
In the tetraethyl orthosilicate aqueous solution in the step (1), the molar ratio of tetraethyl orthosilicate to water is 1: 4.
And (2) in the step (1), the temperature rising speed of the gel particle calcination is 2-5 ℃/min.
And (3) the temperature rising speed of the loading crucible calcination in the step (2) is 2-10 ℃/min.
And (4) in the step (3), the temperature rising speed of the mixed powder block body calcination is 2-10 ℃/min.
Compared with the prior art, the invention has the following advantages:
1. the method has the advantages of simple process, easy operation, simple and easily obtained raw materials and good industrialization prospect.
2. The bioglass prepared by the melting method has the characteristics of good mechanical property but poor biological activity, and the bioglass prepared by combining the sol-gel method has large specific surface area and good biological activity but poor mechanical property; the advantages of the two methods are combined by a method of mixing the two powders in a specific ratio, so that the lithium disilicate bioglass ceramic with good mechanical property and bioactivity can be obtained and can be applied to the repair of wound defects, drug controlled release, cell culture and the like in the dental field.
Drawings
FIG. 1 is a flow chart of a lithium disilicate composite bioglass ceramic prepared according to the present invention;
FIG. 2 is an XRD pattern of bioglass prepared by the sol-gel process and the fusion process as prepared in example 1;
FIG. 3 is an XRD pattern of a lithium disilicate composite bioglass ceramic prepared in example 1;
FIG. 4 is a scanned topography of the lithium disilicate composite bioglass ceramic prepared in example 1;
FIG. 5 shows the results obtained with different SBGs under the conditions of example 1: preparing the bending strength of the lithium disilicate composite bioglass ceramic according to the MBG ratio;
FIG. 6 shows the results obtained under the conditions of example 1 with (a) SBG: MBG =8:2 and (b) pure MBG preparation of lithium disilicate composite bioglass ceramics scanning morphology after 7 days immersion in simulated body fluid.
Detailed description of the invention
The technical solution of the present invention will be described in detail by examples, but the present invention is not limited thereto.
Example 1
A preparation method of lithium disilicate composite bioglass ceramic comprises the following steps:
(1) preparing glass by a sol-gel method:
adding 1 mol/L nitric acid solution into deionized water, stirring, adjusting pH to 3, and adding appropriate amount of silicic acidAdding ethyl ester water solution (the molar ratio of tetraethyl orthosilicate to water is 1: 4) into nitric acid solution, and stirring by magnetic force until the solution becomes clear; other raw materials are mixed according to the molar ratio of 50SiO2-36Li2O-8ZrO2-3K2O-2P2O5-Al2O3Sequentially adding triethyl phosphate, lithium nitrate, zirconium nitrate pentahydrate, potassium nitrate and aluminum nitrate nonahydrate according to the proportion, ensuring that magnetic stirring is carried out for 30 minutes before adding each substance, finally carrying out magnetic stirring for 1 hour, and standing to form transparent sol; aging the obtained sol at 70 ℃ for 24h, heating to 140 ℃, and drying for 42 h; and grinding the xerogel to obtain gel particles, then calcining at 500 ℃ for 12 h in a muffle furnace, wherein the temperature rise rate of the calcination is 4 ℃ per min, cooling to room temperature along with the furnace, and grinding to obtain glass powder prepared by a sol-gel method, wherein the glass powder is marked as SBG.
(2) Preparing glass by a melting method:
according to the molar ratio of 50SiO2-36Li2O-8ZrO2-3K2O-2P2O5-Al2O3Weighing silicon dioxide, lithium carbonate, zirconium oxide, potassium carbonate, phosphorus pentoxide and aluminum oxide according to the proportion, fully mixing the raw materials, and putting the mixture into crucibles, wherein the loading height of each crucible is not more than 2/3 of the total height of the crucible. And (3) placing the loading crucible into a muffle furnace, wherein the temperature rise rate of calcination is 7 ℃ per minute, the temperature is firstly preserved at 330 ℃ for 30 minutes, then preserved at 840 ℃ for 30 minutes, and then preserved at 1500 ℃ for 1.5 hours. And finally, quickly pouring the liquid in the crucible into normal-temperature water in a molten state for cold quenching to obtain glass particles, drying the glass particles at 100 ℃ for 3 hours, and mechanically grinding the glass particles to obtain glass powder prepared by a melting method, wherein the glass powder is marked as MBG.
(3) Respectively mixing the SBG obtained in the step (1) and the MBG glass powder obtained in the step (2) according to a mass ratio of 2: 8. 5: 5 and 8:2, adding a small amount of PVA, fully grinding the mixed powder, drying the ground mixed powder in a drying box at 100 ℃ for 3 hours, grinding and sieving the ground mixed powder again to obtain mixed glass powder with the particle size of less than 45 mu m, pressing the mixed glass powder by adopting a mould to obtain a block body with a required shape, and finally transferring the mixed glass powder to a muffle furnace to be calcined at 820 ℃ for 12 hours, wherein the temperature rise rate of the calcination is 2 ℃ per minute, so that the lithium disilicate composite biological glass ceramics with different mixing ratios are obtained.
Fig. 2 is an XRD pattern of bioglass prepared by sol-gel process and melting process as in example 1, which illustrates that SBG and MBG samples prepared by sol-gel process and melting process are mainly in glass state, and SBG samples prepared by sol-gel process have very small amount of lithium metasilicate in crystallite form.
Fig. 3 is an XRD pattern of the lithium disilicate composite bioglass ceramic prepared in example 1, and the result shows that bioglass ceramic having a large amount of lithium disilicate phase can be obtained by calcination. FIG. 4 is a scanned morphology of the lithium disilicate composite bioglass ceramic prepared in example 1, and the result shows that the generated lithium disilicate crystal grains grow into a rod-like interlocking structure, which is beneficial to improving the mechanical properties of the material.
FIG. 5 shows the results obtained with different SBGs under the conditions of example 1: the bending strength of the lithium disilicate composite bioglass ceramic prepared by MBG proportion shows that the MBG powder is compounded in the SBG sample and is sintered together, and compared with a pure SBG or MBG powder sintered sample, the MBG composite bioglass ceramic has better three-point bending strength and better mechanical property.
FIG. 6 shows the results obtained under the conditions of example 1 with (a) SBG: MBG =8:2 and (b) pure MBG preparation of lithium disilicate composite bioglass ceramics scanning morphology after 7 days immersion in simulated body fluid. The results show that the surface of the glass ceramic sample after sintering of pure MBG powder induces little deposit whereas the surface of the glass ceramic sample after sintering of pure MBG powder is free of deposits induced by SBG: MBG =8:2 the surface of the sample after mixed sintering is soaked in simulated body fluid for 7 days to deposit a large amount of small flower-like substances, which shows that the biological activity of the material can be improved by mixing two different powders.
Example 2
A preparation method of lithium disilicate composite bioglass ceramic comprises the following steps:
(1) preparing glass by a sol-gel method:
adding 1 mol/L nitric acid solution into deionized water, stirring, adjusting pH to 2, adding appropriate amount of tetraethyl orthosilicate water solution (the molar ratio of tetraethyl orthosilicate to water is 1: 4) into nitric acid solutionMagnetically stirring until the solution becomes clear; other raw materials are mixed according to the molar ratio of 50SiO2-36Li2O-8ZrO2-3K2O-2P2O5-Al2O3Sequentially adding triethyl phosphate, lithium nitrate, zirconium nitrate pentahydrate, potassium nitrate and aluminum nitrate nonahydrate according to the proportion, ensuring that magnetic stirring is carried out for 30 minutes before adding each substance, finally carrying out magnetic stirring for 1 hour, and standing to form transparent sol; aging the obtained sol at 80 ℃ for 10 h, heating to 180 ℃, and drying for 12 h; and grinding the xerogel to obtain gel particles, then calcining for 24 hours at 600 ℃ in a muffle furnace, wherein the temperature rise rate of the calcination is 5 ℃ per minute, cooling to room temperature along with the furnace, and grinding to obtain glass powder prepared by a sol-gel method, wherein the glass powder is marked as SBG.
(2) Preparing glass by a melting method:
according to the molar ratio of 55SiO2-31Li2O-8ZrO2-3K2O-2P2O5-Al2O3Weighing silicon dioxide, lithium carbonate, zirconium oxide, potassium carbonate, phosphorus pentoxide and aluminum oxide according to the proportion, fully mixing the raw materials, and putting the mixture into crucibles, wherein the loading height of each crucible is not more than 2/3 of the total height of the crucible. And (3) placing the loading crucible into a muffle furnace, wherein the temperature rise rate of calcination is 2 ℃ per minute, the temperature is firstly preserved at 330 ℃ for 30 min, then preserved at 840 ℃ for 30 min, and then preserved at 1500 ℃ for 3 h. And finally, quickly pouring the liquid in the crucible into normal-temperature water in a molten state for cold quenching to obtain glass particles, drying the glass particles at 100 ℃ for 3 hours, and mechanically grinding the glass particles to obtain glass powder prepared by a melting method, wherein the glass powder is marked as MBG.
(3) Mixing the SBG obtained in the step (1) and the MBG glass powder obtained in the step (2) according to a mass ratio of 8:2, adding a small amount of PVA, fully grinding the mixed powder, drying the ground mixed powder in a drying box at 100 ℃ for 3 hours, grinding and sieving the ground mixed powder again to obtain mixed glass powder with the particle size of less than 45 mu m, pressing the mixed glass powder by adopting a mould to obtain a block body with a required shape, and finally transferring the mixed glass powder to a muffle furnace to calcine the mixed glass powder at 900 ℃ for 24 hours, wherein the temperature rise rate of the calcination is 10 ℃ per minute, so that the lithium disilicate composite biological glass ceramic is obtained.
Example 3
A rapid preparation method of lithium disilicate composite bioglass ceramic comprises the following steps:
(1) preparing glass by a sol-gel method:
adding a nitric acid solution with the concentration of 1 mol/L into deionized water, fully stirring, adjusting the pH value to be 4, adding a proper amount of tetraethyl orthosilicate aqueous solution (the molar ratio of tetraethyl orthosilicate to water is 1: 4) into the nitric acid solution, and stirring by adopting magnetic force until the solution becomes clear; other raw materials are mixed according to the molar ratio of 60SiO2-26Li2O-8ZrO2-3K2O-2P2O5-Al2O3Sequentially adding triethyl phosphate, lithium nitrate, zirconium nitrate pentahydrate, potassium nitrate and aluminum nitrate nonahydrate according to the proportion, ensuring that magnetic stirring is carried out for 30 minutes before adding each substance, finally carrying out magnetic stirring for 1 hour, and standing to form transparent sol; aging the obtained sol at 60 ℃ for 48 h, heating to 100 ℃, and drying for 72 h; and grinding the xerogel to obtain gel particles, then calcining at 400 ℃ in a muffle furnace for 24h, wherein the temperature rise rate of the calcination is 2 ℃ per min, cooling to room temperature along with the furnace, and grinding to obtain glass powder prepared by a sol-gel method, wherein the glass powder is marked as SBG.
(2) Preparing glass by a melting method:
according to the molar ratio of 60SiO2-26Li2O-8ZrO2-3K2O-2P2O5-Al2O3Weighing silicon dioxide, lithium carbonate, zirconium oxide, potassium carbonate, phosphorus pentoxide and aluminum oxide according to the proportion, fully mixing the raw materials, and putting the mixture into crucibles, wherein the loading height of each crucible is not more than 2/3 of the total height of the crucible. And (3) placing the loading crucible into a muffle furnace, wherein the temperature rise rate of calcination is 10 ℃, the temperature is firstly preserved at 330 ℃ for 30 min, then preserved at 840 ℃ for 30 min, and then preserved at 1500 ℃ for 0.5 h. And finally, quickly pouring the liquid in the crucible into normal-temperature water in a molten state for cold quenching to obtain glass particles, drying the glass particles at 100 ℃ for 3 hours, and mechanically grinding the glass particles to obtain glass powder prepared by a melting method, wherein the glass powder is marked as MBG.
(3) Mixing the SBG obtained in the step (1) and the MBG glass powder obtained in the step (2) according to a mass ratio of 2: 8, adding a small amount of PVA, fully grinding the mixed powder, drying the ground mixed powder in a drying oven at 100 ℃ for 3 hours, grinding and sieving the ground mixed powder again to obtain mixed glass powder with the particle size of less than 45 mu m, pressing the mixed glass powder by adopting a mold to obtain a block body with a required shape, transferring the block body to a muffle furnace for calcining at 750 ℃ for 24 hours, wherein the temperature rise rate of the calcining is 4 ℃ per minute, and obtaining the lithium disilicate composite biological glass ceramic.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (5)
1. A preparation method of lithium disilicate composite bioglass ceramic is characterized by comprising the following steps: the method comprises the following steps:
(1) adding a nitric acid solution with the concentration of 1 mol/L into deionized water, fully stirring, adjusting the pH value to 2-4, adding a proper amount of tetraethyl orthosilicate aqueous solution, and stirring by magnetic force until the solution becomes clear; according to the molar ratio of SiO2：Li2O：ZrO2：K2O：P2O5：Al2O3= (50-60): (26-36): 8: 3: 2: 1, sequentially adding triethyl phosphate, lithium nitrate, zirconium nitrate pentahydrate, potassium nitrate and aluminum nitrate nonahydrate, ensuring that magnetic stirring is carried out for 30 minutes before adding each substance, and finally, carrying out magnetic stirring for 1 hour, and standing to form transparent sol; aging the obtained sol at 60-80 ℃ for 10-48 h, and then heating to 100-180 ℃ for drying for 12-72 h; grinding the xerogel to obtain gel particles, then calcining the gel particles in a muffle furnace at 400-600 ℃ for 2-24 hours, cooling the calcined gel particles at room temperature, and grinding the calcined gel particles to obtain glass powder prepared by a sol-gel method, wherein the glass powder is marked as SBG;
(2) SiO in molar ratio2：Li2O：ZrO2：K2O：P2O5：Al2O3= (50-60): (26-36): 8: 3: 2: 1, fully mixing the raw materials, putting the mixture into a crucible, wherein the loading height does not exceed 2/3 of the total height of the crucible, putting the loaded crucible into a muffle furnace, preserving heat at 330 ℃ for 30 min, preserving heat at 840 ℃ for 30 min, and then preserving heat at 1500 DEG CPreserving heat for 0.5-3 h, finally, quickly pouring liquid in a crucible into normal-temperature water in a molten state for cold quenching to obtain glass particles, drying the glass particles for 3h at 100 ℃, and mechanically grinding the glass particles to obtain glass powder prepared by a melting method, wherein the glass powder is marked as MBG;
(3) mixing the SBG obtained in the step (1) and the MBG glass powder obtained in the step (2) according to a mass ratio of 1: 9-9: 1, fully grinding the mixed powder, drying the ground mixed powder in a drying oven at 100 ℃ for 3 hours, grinding and sieving the ground mixed powder again to obtain mixed glass powder with the particle size of less than 45 mu m, pressing the mixed glass powder by adopting a mold to obtain a block in a required shape, and finally transferring the block to a muffle furnace to calcine the block for 1 to 24 hours at 750 to 900 ℃ to obtain the lithium disilicate composite bioglass ceramic.
2. The method of claim 1, wherein the lithium disilicate composite bioglass ceramic comprises: in the tetraethyl orthosilicate aqueous solution in the step (1), the molar ratio of tetraethyl orthosilicate to water is 1: 4.
3. The method of claim 1, wherein the lithium disilicate composite bioglass ceramic comprises: and (2) in the step (1), the temperature rising speed of the gel particle calcination is 2-5 ℃/min.
4. The method of claim 1, wherein the lithium disilicate composite bioglass ceramic comprises: and (3) the temperature rising speed of the loading crucible calcination in the step (2) is 2-10 ℃/min.
5. The method of claim 1, wherein the lithium disilicate composite bioglass ceramic comprises: and (4) in the step (3), the temperature rising speed of the mixed powder block body calcination is 2-10 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910018657.3A CN109534681B (en) | 2019-01-09 | 2019-01-09 | Preparation method of lithium disilicate composite bioglass ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910018657.3A CN109534681B (en) | 2019-01-09 | 2019-01-09 | Preparation method of lithium disilicate composite bioglass ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109534681A CN109534681A (en) | 2019-03-29 |
| CN109534681B true CN109534681B (en) | 2021-04-27 |
Family
ID=65834618
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910018657.3A Expired - Fee Related CN109534681B (en) | 2019-01-09 | 2019-01-09 | Preparation method of lithium disilicate composite bioglass ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109534681B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981203A (en) * | 2019-11-26 | 2020-04-10 | 中国科学院上海硅酸盐研究所 | High-strength lithium disilicate glass ceramic and preparation method and application thereof |
| CN114790083B (en) * | 2022-05-05 | 2023-09-05 | 山东国瓷功能材料股份有限公司 | Glass ceramic and preparation method and application thereof |
| CN115417600A (en) * | 2022-08-16 | 2022-12-02 | 深圳奇遇科技有限公司 | Lithium disilicate glass ceramic bracket and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923752A (en) * | 2005-08-30 | 2007-03-07 | 四川大学 | Composite organism ceramic material composed of apatite-wollastonite/beta-tricalcium phosphate |
| CN102223853A (en) * | 2008-10-01 | 2011-10-19 | 3M创新有限公司 | Dental appliance, process for producing a dental appliance and use thereof |
| CN102741186A (en) * | 2009-12-23 | 2012-10-17 | 弗劳恩霍弗实用研究促进协会 | Lithium disilicate glass ceramics, method for the production thereof and use thereof |
| CN103553339A (en) * | 2013-09-30 | 2014-02-05 | 西安交通大学 | Lithium disilicate microcrystalline glass material prepared by using hybrid reaction sintering method and method |
| CN107746268A (en) * | 2017-11-07 | 2018-03-02 | 聊城大学 | A kind of hardystonite/calcium silicates composite bioceramic material and preparation method thereof |
-
2019
- 2019-01-09 CN CN201910018657.3A patent/CN109534681B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1923752A (en) * | 2005-08-30 | 2007-03-07 | 四川大学 | Composite organism ceramic material composed of apatite-wollastonite/beta-tricalcium phosphate |
| CN102223853A (en) * | 2008-10-01 | 2011-10-19 | 3M创新有限公司 | Dental appliance, process for producing a dental appliance and use thereof |
| CN102741186A (en) * | 2009-12-23 | 2012-10-17 | 弗劳恩霍弗实用研究促进协会 | Lithium disilicate glass ceramics, method for the production thereof and use thereof |
| CN103553339A (en) * | 2013-09-30 | 2014-02-05 | 西安交通大学 | Lithium disilicate microcrystalline glass material prepared by using hybrid reaction sintering method and method |
| CN107746268A (en) * | 2017-11-07 | 2018-03-02 | 聊城大学 | A kind of hardystonite/calcium silicates composite bioceramic material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Characterization of the bioactive and mechanical behavior of dental ceramic/sol–gel derived bioactive glass mixtures;Zahra Abbasi 等;《Journal of the mechaincal behavior of biomedical materials》;20150930;第54卷;第115-122页 * |
| Sintering of dental ceramic/sol– gel-derived bioactive glass mixtures for dental applications: the study of microstructural, biological, and thermal properties;Zahra Abbasi 等;《J Sol-Gel Technol》;20161011;第81卷;第523-533页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109534681A (en) | 2019-03-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109534681B (en) | Preparation method of lithium disilicate composite bioglass ceramic | |
| US4652534A (en) | High-strength glass ceramic containing apatite crystals and a large quantity of wollastonite crystals and process for producing same | |
| Laczka et al. | Gel‐derived materials of a CaO‐P2O5‐SiO2 system modified by boron, sodium, magnesium, aluminum, and fluorine compounds | |
| CN110981203A (en) | High-strength lithium disilicate glass ceramic and preparation method and application thereof | |
| US7074730B2 (en) | Bioactive rhenanite glass ceramic | |
| WO2019179194A1 (en) | Calcium polyphosphate/wollastonite bio-composite ceramic material and preparation method therefor | |
| CN108328932A (en) | A kind of gear division devitrified glass that Ce, Er, Tb, Y are co-doped with and its preparation and application | |
| CN106007700A (en) | Method for manufacturing porous hydroxyapatite orbital implant | |
| CN114349348B (en) | Lithium disilicate glass ceramic for all-ceramic denture and preparation method thereof | |
| CN103979945B (en) | A kind of preparation method of biological active tabular spar ceramics | |
| CN109721040A (en) | A kind of preparation method of high-performance biomedicine type alpha tricalcium phosphate | |
| TW201604169A (en) | A degradable magnesium-calcium silicate bone cement and producing method thereof | |
| CN105079872A (en) | Fine repairing artificial material and method for preparing same | |
| CN107746268B (en) | Anorthite/calcium silicate composite biological ceramic material and preparation method thereof | |
| CN107586041B (en) | Microcrystalline glass for dentistry and preparation method thereof | |
| CN114455953B (en) | Porcelain powder for full-ceramic false tooth and preparation method thereof | |
| CN113979729B (en) | Lithium-silicon compound enhanced bioactive ceramic material and preparation method thereof | |
| CN113698101B (en) | Glass ceramic finished product with gradually changed color, preparation method and application thereof | |
| CN111825337B (en) | Biological microcrystalline glass and preparation method and application thereof | |
| CN112174152B (en) | Polyion co-doped tetracalcium phosphate powder, synthesis method and application | |
| CN114074932B (en) | Preparation method of high-biodegradability alpha-tricalcium phosphate nano powder for 3D printing | |
| RU2765471C1 (en) | Method for producing bioglass doped with zirconium dioxide | |
| CN110255938B (en) | Calcium silicophosphate matrix powder and preparation method thereof, bone repair material and preparation method thereof | |
| Goudouri et al. | Magnesium based sol-gel derived bioactive glass ceramics for dental tissue regeneration | |
| JPH01115360A (en) | Inorganic living body material and preparation thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210427 Termination date: 20220109 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |