Resin-infiltrated porous ceramic composite material, method for preparing the same, and use thereof
By employing low-temperature sintering technology of lead-free low-melting-point glass powder and silicate powder, the problems of high defect rate and insufficient interfacial bonding in resin ceramic composite materials have been solved, realizing high-strength, low-temperature prepared porous ceramic composite materials suitable for dental restoration.
Patent Information
- Application Number
- CN202311189362.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-15
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2043-09-15
AI Technical Summary
Existing resin-ceramic composite materials have insufficient mechanical properties and a high defect rate during low-temperature sintering. Furthermore, the interfacial bonding between ceramics and resin is poor, resulting in a short material service life.
Porous ceramic composite materials are prepared by mixing lead-free low-melting-point glass powder and silicate powder in a certain proportion and sintering at low temperature (500-650℃). The glass powder is used as a binder in the molten state to enhance the interfacial bonding and provide interconnected pores to reduce the defect rate.
It significantly reduced the defect rate (approximately 50%), improved the mechanical properties of the material, and ensured the strength and toughness of the material under low-temperature sintering conditions, meeting the clinical requirements for dental restorative materials.
Smart Images

Figure BDA0004450021830000071 
Figure BDA0004450021830000081 
Figure BDA0004450021830000082
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of dental restoration materials, and more particularly relates to a resin-infiltrated porous ceramic composite material and a preparation method and application thereof. BACKGROUND
[0002] The transformation of dental restoration materials from the initial gold-silver-copper noble metal to resin restoration materials is a major change in the development of dental restoration materials. Composite resin restoration materials are widely used due to their aesthetic color, good physical and chemical properties, and easy processing performance. Among them, the Bis-GMA resin matrix material has more than 50 years of clinical experience, but according to clinical statistical data, the service life of the Bis-GMA resin matrix material is usually short (6-8 years), and it has problems such as large polymerization shrinkage, low mechanical strength, and low curing degree. In order to solve these problems, resin-ceramic composite materials are applied.
[0003] In resin-ceramic composite materials, ceramic is used as a reinforcing body, which can not only improve the mechanical properties of resin composite materials such as strength and modulus, but also improve the wear resistance and prolong the service life of the material. However, if the ceramic is too dense, it will not provide enough connected pore diameter for resin infiltration, and reducing the sintering temperature will lead to a decrease in shrinkage and a decrease in mechanical properties. Although the mechanical properties of resin-ceramic composite materials are improved, the improvement is limited. Moreover, the modulus of ceramic is generally much greater than that of the resin system, which can easily lead to insufficient interfacial bonding between the two and cause cracks or fractures, resulting in a high rate of defective products. Therefore, it is necessary to study a resin-ceramic composite material with a high yield, especially a resin-ceramic composite material that can meet the requirements of mechanical properties at a low sintering temperature, which is more conducive to its popularization and application. SUMMARY
[0004] In view of the above defects or improvement needs of the prior art, the present application provides a resin-infiltrated porous ceramic composite material and a preparation method and application thereof, which aims to find that the ceramic resin composite material prepared by mixing lead-free low-melting point glass powder and silicate powder in a mass ratio of 1-20:80-99 and then granulating can reduce the defective rate of the material and prepare a composite material meeting the requirements of mechanical properties at 500-650 DEG C, thereby solving the technical problem of a high defective rate of dental restoration materials prepared by using a single silicate powder.
[0005] To achieve the above-mentioned purpose, according to one aspect of the present application, a preparation method of a resin-infiltrated porous ceramic composite material is provided, which comprises the following steps:
[0006] (1) mixing lead-free low-melting point glass powder with a particle size of 50-500 nm and silicate powder with a particle size of 50-500 nm in a predetermined ratio, granulating to obtain a mixed powder, and twice-pressing to prepare a porous glass ceramic green body;
[0007] The mass ratio of the low-melting point lead-free glass powder to the silicate powder is 1-20:80-99; the low-melting point lead-free glass powder mainly comprises Bi2O3, ZnO, B2O3, SiO2, Al2O3, Na2O, ZrO2, SnCl2, Sb2O3, Li2O, BaO, K2O, and the melting temperature is less than or equal to 500 DEG C.
[0008] (2) low-temperature sintering: sintering the porous glass ceramic green body obtained in (1) at a low temperature of 500 DEG C-650 DEG C to obtain a porous glass ceramic body; and resin-infiltrated porous ceramic composite material is obtained after resin infiltration and solidification.
[0009] Preferably, the resin-infiltrated porous ceramic composite material is prepared by the method, and the low-melting point lead-free glass powder mainly comprises Bi2O3, ZnO, B2O3, SiO2, Al2O3, Na2O, and the mass ratio of Bi2O3:ZnO:B2O3:SiO2:Al2O3:Na2O is 49:20.5:(25.5-26.5):3.5:(0.5-1.5).
[0010] Preferably, the resin-infiltrated porous ceramic composite material is prepared by the method, and the mass ratio of the low-melting point lead-free glass powder to the silicate powder is 5-15:85-95.
[0011] Preferably, the resin-infiltrated porous ceramic composite material is prepared by the method, and the sintering temperature of the low-temperature sintering in step (2) is 550-600 DEG C, and the holding time is 2-3h.
[0012] Preferably, the resin-infiltrated porous ceramic composite material is prepared by the method, and the twice pressing in step (1) comprises pre-pressing and cold isostatic pressing, wherein the pressure of the pre-pressing is 4-6t, and the pressing time is 15-40s; the pressure of the cold isostatic pressing is 200-400MPa, and the pressing time is 1-5min.
[0013] According to another aspect of the present application, a resin-infiltrated porous ceramic composite material is also provided, which is prepared by the method as described in the present application.
[0014] Preferably, the resin-infiltrated porous ceramic composite material has a Vickers hardness average value of more than 1.6GPa, an elastic modulus average value of more than 25GPa, and a fracture toughness average value of more than 1.5MPa.m 1 / 2 The above.
[0015] Preferably, the resin-infiltrated porous ceramic composite material has a mean Vickers hardness of greater than 2.0 GPa, a mean elastic modulus of greater than 34 GPa, and a mean fracture toughness of greater than 2.0 MPa.m 1 / 2 , and a bending strength of greater than 160 MPa.
[0016] According to another aspect of the present application, there is also provided use of the resin-infiltrated porous ceramic composite material as described in the present application in dental restoration.
[0017] Preferably, the use of the resin-infiltrated porous ceramic composite material in dental restoration includes artificial teeth, veneers, inlays, and crowns; and the crown restoration includes full crown, single crown, and bridge crown restoration.
[0018] Overall, compared with the prior art, the above technical solutions conceived by the present application can achieve the following technical effects because the silicate powder and the low-melting point glass powder mixed powder are used as raw materials, and the mass ratio of the lead-free low-melting point glass powder to the silicate powder is 1-20:80-99.
[0019] The preparation method of the resin-infiltrated porous ceramic composite material provided by the present application can make the ceramic matrix and the resin network in the resin-infiltrated ceramic have better bonding performance due to the low-melting point glass powder in the raw material, prevent cracking, effectively reduce the scrap rate, and reduce the scrap rate to 2.3% compared with the existing scrap rate (5-6%), which is about 50% lower. Moreover, the sintering temperature is reduced to 500-650°C, the mechanical properties of the material are equivalent to or even better than the mechanical properties of the existing sintering temperature of 700-800°C, the sintering temperature of the ceramic matrix can be reduced while the overall mechanical properties are ensured, and the effect of energy saving and emission reduction can be achieved. DETAILED DESCRIPTION
[0020] In order to make the purpose, technical solutions and advantages of the present application clearer and more apparent, the present application will be further described in detail below with reference to examples. It should be understood that the specific examples described herein are only used to explain the present application and do not limit the present application. In addition, the technical features involved in each embodiment of the present application described below can be combined with each other as long as they do not conflict with each other.
[0021] The mechanical properties of dental restoration materials in clinical application should meet the following requirements: bending strength of 150 MPa or more, elastic modulus of about 20 GPa, and Vickers hardness of about 2.00 GPa. At present, the sintering temperature of silicate powder ceramic block is about 800℃, although the mechanical properties of existing materials can meet the requirements of clinical application, but further improvement is needed, and the existing defective rate is high (defective rate is 5-6%). In order to further improve the mechanical properties of the material, the existing research usually adopts sintering at a temperature of 1000℃ or more, although the patent CN201910597419.2 a low temperature sintering alumina black ceramic and its preparation method adopts low temperature and long time gradual heating method for sintering, but its sintering process is first heated to 500-500℃, and then heated to 700-950℃, and then heated to 1100-1250℃, and then heated to 5-15h, the sintering time is long, the sintering process is complex, and the final sintering temperature is still above 1000℃, and the sintering temperature is high, the ceramic block is easy to be too dense, the resin is difficult to penetrate, and it is not conducive to continuous production, and the efficiency is low.
[0022] The present application finds that the lead-free low-melting point glass powder and the silicate powder are mixed in a mass ratio of 1-20:80-99 to prepare a ceramic resin composite material, and it is found that the dental restoration material meeting the mechanical property requirements can be obtained by sintering at a low temperature of 500-650℃, and the defective rate of the restoration material is obviously reduced.
[0023] The present application provides a preparation method of resin-permeated porous ceramic composite material, which comprises the following steps:
[0024] (1) The lead-free low-melting point glass powder of 50-500nm and the silicate powder of 50-500nm are mixed in a mass ratio of (1-20):(80-99), granulated to obtain a mixed powder; the main components of the lead-free low-melting point glass powder are not limited to Bi2O3, ZnO, B2O3, SiO2, Al2O3, Na2O, ZrO2, SnCl2, Sb2O3, Li2O, BaO, K2O, two or more components, preferably Bi2O3-ZnO-B2O3-SiO2-Al2O3-Na2O, and the mass ratio of each component is 49:20.5:(25.5-26.5):3.5:(0.5-1.5); the melting temperature is ≤500℃.
[0025] (2) twice pressing, specifically as follows:
[0026] Once pre-pressing: the mixed powder is pressed at a pressure of 4-6t for 15-40s;
[0027] Cold isostatic pressing secondary pressing: the cold isostatic pressing pressure is 200-400 MPa, and the pressing time is 1-5 min, so as to obtain a porous glass ceramic green body;
[0028] (3) Low temperature sintering: the porous glass ceramic green body obtained in (2) is sintered at 500-650 ℃, so as to obtain a porous glass ceramic body;
[0029] It is found in the experiment that the addition of 1-20% of the lead-free low-melting glass powder in the mixed powder can significantly improve the mechanical properties of the material, mainly because the lead-free low-melting glass powder can enhance the interfacial bonding force of the resin and the ceramic, which is beneficial to reduce the defective rate; although the reduction of the sintering temperature will lead to the decrease of the shrinkage rate and the mechanical properties, the glass powder is in a molten state at 500-650 ℃, and the glass powder in the molten state can form "welding points" between the silicate powder particles, thereby playing the role of a binder, which can improve the bonding between the silicate grains, and it is unexpectedly found that although the sintering temperature is reduced, the mechanical properties of the material remain unchanged, and the mechanical properties of the material meet the requirements of clinical application.
[0030] (4) The porous glass ceramic body obtained in (3) is subjected to resin infiltration and solidification, so as to obtain a resin-infiltrated porous ceramic composite material.
[0031] Since the porous glass ceramic body is sintered at a relatively low sintering temperature, the internal voids can provide sufficient connected pore diameters for resin infiltration, and the addition of the lead-free low-melting glass powder in the silicate can reduce the exothermic peak temperature of the resin solidification reaction, which can reduce the linear expansion coefficient and the shrinkage rate of the solidified material, thereby eliminating the internal stress of the solidified material, further preventing cracking, and reducing the defective rate.
[0032] Preferably, the mixed powder is mixed according to the mass ratio of the lead-free low-melting glass powder to the silicate powder being (5-15):(85-95); more preferably, the low-temperature sintering temperature is 550-600 ℃, and the average Vickers hardness of the obtained material is greater than 1.6 GPa, the average elastic modulus is greater than 25 GPa, and the average fracture toughness is greater than 1.5 MPa.m 1 / 2 Above.
[0033] In some embodiments, the mixed powder is mixed according to the mass ratio of the lead-free low-melting glass powder to the silicate powder being 8:92, and the obtained composite material has good mechanical properties after sintering at 600 ℃ for 2 h, the average Vickers hardness is greater than 2.0 GPa, the average elastic modulus is greater than 34 GPa, the average fracture toughness is greater than 2.0 MPa.m 1 / 2 , the bending strength is greater than 160 Mpa, and the defective rate of the finished product is as low as 2.3%.
[0034] In addition, the present application also provides a resin-infiltrated porous ceramic composite material prepared according to the preparation method of the present application.
[0035] The composite material has a mean Vickers hardness of 1.6 GPa or more, a mean modulus of elasticity of 25 GPa or more, and a mean fracture toughness of 1.5 MPa.m 1 / 2 The above; preferably the mean Vickers hardness is greater than 2.15 GPa, the mean modulus of elasticity is greater than 34 GPa, and the mean fracture toughness is greater than 2.0 MPa.m 1 / 2 The bending strength is greater than 160 MPa.
[0036] The application also provides a use of the resin-infiltrated porous ceramic composite material in dental restoration, which includes artificial teeth, veneers, inlays, and crowns; wherein the crown restoration includes full crown, single crown, and connected crown restoration.
[0037] The following is an example:
[0038] The main components of the lead-free low-melting point glass powder in the embodiment of the application are Bi2O3-ZnO-B2O3-SiO2-Al2O3-Na2O, wherein the mass ratio of Bi2O3:ZnO:B2O3:SiO2:Al2O3:Na2O is 49:20.5:(25.5-26.5):3.5:(0.5-1.5). The 50-500 nm lead-free low-melting point glass powder and the 50-500 nm sodium aluminosilicate powder are mixed in a mixing powder machine at a mass ratio of (1-20):(80-99) to obtain a mixed powder, which is denoted as AX, wherein X is the mass content of the lead-free low-melting point glass powder, i.e., the mass percentage of the lead-free low-melting point glass powder in the mixed powder. For example, A1 represents that the mass content of the lead-free low-melting point glass powder is 1%, and the mixed powder is granulated with a binder solution such as PVA liquid to obtain glass powders A1-A20.
[0039] Example 1
[0040] (1) The 50-500 nm lead-free low-melting point glass powder and the 50-500 nm sodium aluminosilicate powder are mixed at a mass ratio of 1:99 to obtain a mixed powder, which is denoted as A1.
[0041] (2) The mixed powder is pressed twice:
[0042] Once pre-pressing: the A1 powder prepared in (1) is transferred to a mold, and a porous ceramic body is formed by a hydraulic machine, and the pressure of the hydraulic machine is set to 6 t, and the pressure is maintained for 30 s.
[0043] Cold isostatic pressing: the porous ceramic body is placed in a sealed protective film, and then cold isostatic pressing is performed, wherein the pressure increasing rate of the cold isostatic pressing is 200 MPa / min, the pressure is maintained at 200 MPa for 3 min, and then the pressure is reduced to obtain a porous glass ceramic body.
[0044] (3) Sintering of the porous ceramic green body at low temperature: the porous glass-ceramic green body obtained in (2) is sintered at 500℃, 550℃, 600℃, 650℃, respectively, with a heating rate of 5℃ / min, and is kept for 2h; after sintering, the sintered body is dried in a vacuum drying oven at 110℃ for 2h, or is modified with a silane coupling agent and then dried in a vacuum.
[0045] (4) Resin infiltration and curing: the resin mixture is injected into a mold, and the porous glass-ceramic obtained in (3) is placed in the mold, and a pressure of 0.6MPa is applied, and the resin is allowed to infiltrate into the pores of the ceramic under vacuum for 4h; after resin infiltration, the porous glass-ceramic is packaged with a high-temperature vacuum film, and then is placed in a high-pressure chamber, and the hydraulic oil in the high-pressure chamber is heated to 70℃, and the pressure is increased to 120MPa, and is kept for 2h, and then the temperature is increased to 120℃, and the pressure is adjusted to 180MPa, and is kept for 3h, and then is taken out.
[0046] The resin mixture is prepared according to the following method:
[0047] Bis-GMA and TEGDMA are mixed in a mass ratio of 1:1, stirred for 2h, 1wt% of a curing agent (based on the mass of Bis-GMA and TEGDMA) is added, and stirring is continued for 2h to obtain the resin mixture; in this embodiment, the curing agent is benzoyl peroxide (BPO).
[0048] When used, the resin-infiltrated porous glass-ceramic composite material obtained in (4) is polished, such as using sandpaper to polish the excess resin layer after curing, and using animal hair or nut shells mixed with a polishing agent to polish.
[0049] The resin-infiltrated porous ceramic composite material prepared using mixed powder A1 is tested, and the results are shown in the following table:
[0050] Table 1 Mechanical properties and rejection rate of resin-infiltrated porous ceramic composite material
[0051]
[0052]
[0053] In Table 1, "150.27(11.30)" means "150.27±11.30", and the same applies to the others.
[0054] As can be seen from Table 1, by adding 1% of lead-free low-melting point glass powder and sintering at 500℃, a ceramic composite material with a mean Vickers hardness of 1.41GPa and a mean elastic modulus of more than 25GPa can be obtained, and the mean fracture toughness of the material can reach 1.5MPa.m 1 / 2The defective rate is 5.3%, and the defective rate decreases with the increase of the sintering temperature, while the mechanical property increases first and then decreases.
[0055] Example 2
[0056] The 50-500nm lead-free low-melting point glass powder and the 50-500nm sodium aluminosilicate powder are mixed uniformly at a mass ratio of 3:97 to obtain a mixed powder, denoted as A3; other conditions are the same as in Example 1, and a resin-infiltrated porous ceramic composite material is prepared.
[0057] The resin-infiltrated porous ceramic composite material prepared by using the mixed powder A3 is tested, and the results are shown in the following table:
[0058] Table 2 Mechanical properties of resin-infiltrated porous ceramic composite material
[0059]
[0060] Example 3
[0061] The 50-500nm lead-free low-melting point glass powder and the 50-500nm sodium aluminosilicate powder are mixed uniformly at a mass ratio of 5:95 to obtain a mixed powder, denoted as A5; other conditions are the same as in Example 1, and a resin-infiltrated porous ceramic composite material is prepared.
[0062] The resin-infiltrated porous ceramic composite material prepared by using the mixed powder A5 is tested, and the results are shown in the following table:
[0063] Table 3 Mechanical properties of resin-infiltrated porous ceramic composite material
[0064]
[0065] Example 4
[0066] The 50-500nm lead-free low-melting point glass powder and the 50-500nm sodium aluminosilicate powder are mixed uniformly at a mass ratio of 8:92 to obtain a mixed powder, denoted as A8; other conditions are the same as in Example 1, and a resin-infiltrated porous ceramic composite material is prepared.
[0067] The resin-infiltrated porous ceramic composite material prepared by using the mixed powder A8 is tested, and the results are shown in the following table:
[0068] Table 4 Mechanical properties of resin-infiltrated porous ceramic composite material
[0069]
[0070] Example 5
[0071] The 50-500nm lead-free low-melting point glass powder and the 50-500nm sodium aluminosilicate powder are mixed uniformly at a mass ratio of 12:88 to obtain a mixed powder, denoted as A12; other steps are the same as in Example 1 to obtain the resin-infiltrated porous ceramic composite material.
[0072] The resin-infiltrated porous ceramic composite material prepared using the mixed powder A12 is tested, and the results are shown in the following table:
[0073] Table 5 Mechanical properties of resin-infiltrated porous ceramic composite material
[0074]
[0075]
[0076] Example 6
[0077] The 50-500nm lead-free low-melting point glass powder and the 50-500nm sodium aluminosilicate powder are mixed uniformly at a mass ratio of 15:85 to obtain a mixed powder, denoted as A15; other steps are the same as in Example 1 to obtain the resin-infiltrated porous ceramic composite material.
[0078] The resin-infiltrated porous ceramic composite material prepared using the mixed powder A15 is tested, and the results are shown in the following table:
[0079] Table 6 Mechanical properties of resin-infiltrated porous ceramic composite material
[0080]
[0081] Example 7
[0082] The 50-500nm lead-free low-melting point glass powder and the 50-500nm sodium aluminosilicate powder are mixed uniformly at a mass ratio of 20:80 to obtain a mixed powder, denoted as A20; other steps are the same as in Example 1 to obtain the resin-infiltrated porous ceramic composite material.
[0083] The resin-infiltrated porous ceramic composite material prepared using the mixed powder A20 is tested, and the results are shown in the following table:
[0084] Table 7 Mechanical properties of resin-infiltrated porous ceramic composite material
[0085]
[0086]
[0087] Resin-infiltrated porous ceramic composites are prepared by using mixed powders A1-A20 respectively. Test results show that adding lead-free low-melting glass powder can significantly improve the mechanical properties and fracture toughness of the composite material, and can reduce the defective rate and increase the yield. When the content of lead-free low-melting glass powder in the mixed powder is 8%, and the sintering temperature is 600°C, the mechanical properties of the prepared composite material are optimal, and the defective rate is lowest.
[0088] Comparative Example 1
[0089] Resin-infiltrated porous ceramic composites are prepared by using 50-500nm sodium aluminosilicate powder, wherein the sodium aluminosilicate powder is first mixed with a binder PVA liquid to prepare granules, and then the green body is prepared by rough compression and cold isostatic pressing, and sintering at a high temperature of 700-850°C for 2h, which is denoted as A0. Other conditions are the same as in Example 1 to prepare resin-infiltrated porous ceramic composites. The obtained resin-infiltrated porous ceramic composites are tested, and the results are shown in the following table:
[0090] Table 8 Mechanical properties of resin-infiltrated porous ceramic composites
[0091]
[0092] Comparative Example 1 is the common sintering temperature for preparing ceramic composites from existing single silicate powders. Although the mechanical properties of the material meet the clinical use requirements, the defective rate is high, and the Vickers hardness of the material is 1.6-1.65GPa, which is still lower than that of natural teeth.
[0093] Comparative Example 2
[0094] Resin-infiltrated porous ceramic composites are prepared by using 50-500nm sodium aluminosilicate powder, wherein the sodium aluminosilicate powder is first mixed with a binder PVA liquid to prepare granules, and then the green body is prepared by rough compression and cold isostatic pressing, and sintering at a high temperature of 500-650°C for 2h, and other conditions are the same as in Example 1 to prepare resin-infiltrated porous ceramic composites.
[0095] The obtained resin-infiltrated porous ceramic composites are tested, and the results are shown in the following table:
[0096] Table 9 Mechanical properties of resin-infiltrated porous ceramic composites
[0097]
[0098] Comparative Example 2 is the common process for preparing ceramic composites from existing single silicate powders, but the sintering temperature is reduced, the shrinkage of the ceramic matrix is reduced, the porosity is increased, and thus the mechanical properties are reduced, and the defective rate is higher.
[0099] Comparative Example 3
[0100] Resin-infiltrated porous ceramic composite material was prepared by using mixed powders of 50-500 nm sodium aluminosilicate powder and low-melting-point glass powder, wherein the low-melting-point glass powder accounts for 8% of the mass of the mixed powders, the particle size is 50-500 nm, the sintering temperature is 700-850℃, and the other conditions are the same as those in Example 1. Resin-infiltrated porous ceramic composite material was prepared.
[0101] The obtained resin-infiltrated porous ceramic composite material was tested, and the results are shown in the following table:
[0102] Table 10 Mechanical properties of resin-infiltrated porous ceramic composite material
[0103]
[0104] In Comparative Example 3, when the sintering temperature is 700-850℃, the ceramic matrix is as dense as possible, and the internal pore size is connected. However, the addition of low-melting-point glass powder at this sintering temperature will affect the connectivity of the pore size to some extent, which will prevent the resin from completely infiltrating and produce certain voids, thereby leading to a decrease in the strength of the material.
[0105] Those skilled in the art will readily understand that the above description is only the preferred embodiment of the present application, and is not intended to limit the present application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present application shall be included in the protection scope of the present application.
Claims
1. A method for preparing a resin-infiltrated porous ceramic composite material, characterized in that, Includes the following steps: (1) Mix lead-free low-melting-point glass powder of 50-500nm with silicate powder of 50-500nm in a preset ratio to obtain mixed powder, and press twice to prepare porous glass ceramic green body; the silicate powder is sodium aluminosilicate powder. The preset ratio is as follows: the mass ratio of lead-free low-melting-point glass powder to silicate powder is 1~20:80~99; the lead-free low-melting-point glass powder mainly consists of two or more components, including but not limited to Bi2O3, ZnO, B2O3, SiO2, Al2O3, Na2O, ZrO2, SnCl2, Sb2O3, Li2O, BaO, and K2O, with a melting point ≤500℃; (2) Low temperature sintering: The porous glass ceramic green body obtained in (1) is sintered at a low temperature of 500℃~650℃ to obtain a porous glass ceramic green body; after resin infiltration and curing, a resin-infiltrated porous ceramic composite material is obtained.
2. The method for preparing the resin-infiltrated porous ceramic composite material as described in claim 1, characterized in that, The mass ratio of the lead-free low-melting-point glass powder to the silicate powder is 5~15:85~95.
3. The method for preparing the resin-infiltrated porous ceramic composite material as described in claim 2, characterized in that, The low-temperature sintering in step (2) has a sintering temperature of 550~600℃ and a holding time of 2~3h.
4. The method for preparing the resin-infiltrated porous ceramic composite material as described in claim 3, characterized in that, The two pressing steps in step (1) include pre-pressing and cold isostatic pressing. The pressure of pre-pressing is 4-6t and the pressing time is 15-40s. The pressure of cold isostatic pressing is 200-400MPa and the pressing time is 1-5min.
5. A resin-infiltrated porous ceramic composite material, characterized in that, Prepared according to the preparation method described in any one of claims 1 to 4.
6. The resin-infiltrated porous ceramic composite material as described in claim 5, characterized in that, The composite material has an average Vickers hardness of over 1.6 GPa, an average elastic modulus of over 25 GPa, and an average fracture toughness of over 1.5 MPa.m. 1 / 2 above.
7. The resin-infiltrated porous ceramic composite material as described in claim 6, characterized in that, The composite material has an average Vickers hardness greater than 2.0 GPa, an average elastic modulus greater than 34 GPa, and an average fracture toughness greater than 2.0 MPa.m. 1 / 2 The bending strength is greater than 160 MPa.
8. The application of a resin-infiltrated porous ceramic composite material as described in any one of claims 5 to 7 in dental restoration.
9. The application of the resin-infiltrated porous ceramic composite material as described in claim 8 in dental restoration, characterized in that, The dental restorations mentioned include artificial teeth, veneers, inlays, and crowns; among which crown restorations include full crowns, single crowns, and multi-crown restorations.
Citation Information
Patent Citations
A low-temperature sintered alumina black ceramic and its preparation method
CN110330315B
Glass ceramic matrix as well as preparation method and application thereof
CN116177884A