CN109180022B - Molten salt for chemical toughening of dental microcrystalline glass and use method thereof - Google Patents

Molten salt for chemical toughening of dental microcrystalline glass and use method thereof Download PDF

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CN109180022B
CN109180022B CN201811353536.6A CN201811353536A CN109180022B CN 109180022 B CN109180022 B CN 109180022B CN 201811353536 A CN201811353536 A CN 201811353536A CN 109180022 B CN109180022 B CN 109180022B
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molten salt
microcrystalline glass
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CN109180022A (en
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陈孔发
纪锦仲
彭兵
张腾
林燕喃
刘鸿琳
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Fuzhou University
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    • 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
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions

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Abstract

The invention discloses a molten salt for chemical toughening of dental microcrystalline glass and a use method thereof, wherein the molten salt comprises the following components in percentage by mass: 85% -95% KNO3、3%～11%CH3COOK、1%～6%KCl、0.5%～2%Al2O3The sum of the mass percentages of the components is 100 percent. A mode that a sample is embedded into molten salt in advance and is heated along with a furnace is adopted, the heating rate of the heating furnace is 1-10 ℃/min, the heat preservation temperature is 420-500 ℃, and the heat preservation time is 0.5-4 h. The fused salt using the formula can protect the surface of dental microcrystalline glass, greatly shorten the ion exchange time, has excellent mechanical properties such as bending strength, fracture toughness and hardness after chemical toughening, also has good chemical stability and biocompatibility, and can be used for dental all-ceramic repair materials.

Description

Molten salt for chemical toughening of dental microcrystalline glass and use method thereof
Technical Field
The invention belongs to the field of microcrystalline glass, and particularly relates to a molten salt for chemical toughening of dental microcrystalline glass and a use method thereof.
Background
Teeth not only can chew food and help pronunciation, but also has great influence on the face beauty. Teeth are important components of human bodies, and dental restoration problems are prominent in the current society. Therefore, the dental restoration problem is prominent day by day, and the artificial tooth (commonly called as 'false tooth') which has higher strength and more beautiful appearance and is prepared by selecting proper restoration materials is used for restoring and decorating the tooth so as to restore the biological function and beautiful appearance of the tooth, thus becoming a research hotspot.
Microcrystalline glass material of the dental silicate type (e.g. lithium disilicate Li)2Si2O5，Li2O·2SiO2) Because the mechanical index and the semi-permeability are closer to the advantages of natural teeth, easy machining and the like, the dental implant is favored by people. However, the brittleness, bending strength and the like of the restoration limit the development of the restoration, and the strength which can be achieved by the lithium disilicate glass ceramics at present cannot meet the requirement of manufacturing a single crown of a posterior tooth. Therefore, the dental fused salt for chemical tempering of the microcrystalline glass provided by the patent has important significance for meeting market requirements.
In the prior achievement aspect, the domestic applied patent (application number CN 106986556A, CN 101921054A and the like) adds K2CO3KCl and KOH are auxiliary reagents, which can improve the surface stress and the depth of a stress layer of the chemically strengthened glass, but are mainly applied to industrial glass; moreover, the KOH auxiliary reagent has a certain toxicity, and cannot be strengthened by the dental glass ceramics from the safety point of view; in addition, the KOH auxiliary reagent is added, the process is complex, the ion exchange time is too long, and the method is not suitable for the requirements of high efficiency and rapidness of dental restoration.
Disclosure of Invention
The invention aims to provide a molten salt for chemical toughening of dental microcrystalline glass and a use method thereof. The method can be used for surface treatment of dental all-ceramic repair materials.
The invention is implemented by the following technical scheme:
a molten salt for chemically toughening the microcrystal glass in dentistry is composed of KNO as main component and auxiliary component3The auxiliary component is Al2O3KCl and CH3And COOK (cooling). The weight percentages are as follows: KNO3 85%～95%、CH3COOK 3%～11%、KCl 1%～6%、Al2O3 0.5 to 2 percent, and the sum of the mass percent of the components is 100 percent.
The use method of the molten salt for chemically toughening the dental microcrystalline glass specifically comprises the following steps:
(1) cutting, grinding and polishing the glass block to enable the sample to be in a shape required by tests such as hardness, breaking strength and the like, cleaning, drying and then carrying out heat treatment to obtain a dental microcrystalline glass sample;
(2) weighing reagents according to the proportion of each component of the molten salt, mixing and then putting into alumina or other high-temperature stable crucibles for standby;
(3) fixing the sample obtained in the step (1) by using a stainless steel bracket and then embedding the sample into molten salt so that the sample can be buried by the molten salt;
(4) and (3) placing the alumina crucible into which the sample is placed in a heating furnace, heating to melt the molten salt, and preserving heat for a period of time to ensure smooth ion exchange. The mode that the sample is embedded into the molten salt in advance and is heated along with the furnace is adopted, so that the sample is prevented from being placed at high temperature, the sample is damaged due to rapid temperature change, and the steps are reduced, and the introduction of additional variables is also avoided;
(5) and after the ion exchange is finished, rapidly taking out the sample in the molten salt, cooling the sample, taking deionized water to clean the cooled sample, and drying to finish the chemical toughening of the dental microcrystalline glass.
The dental microcrystalline glass comprises SiO as a main component2、Li2CO3、K2CO3、Na2CO3、Al2O3、P2O5And ZrO2。
The sample size in the step (1) is the final size, no obvious defect exists, deionized water is used for cleaning, and the heat treatment method of the microcrystalline glass is determined according to specific glass components and the thermal property of the microcrystalline glass.
In the step (4), the heating rate of the heating furnace is 1-10 ℃/min, and preferably 4-8 ℃/min; the heat preservation temperature is 420-500 ℃, and preferably 450-480 ℃; the heat preservation time is 0.5-4 h, preferably 1-2 h.
And (4) in the step (4), the bracket is made of stainless steel and cannot be corroded by molten salt, and the molten salt is required to completely cover the surface of the sample after being melted, so that the upper surface and the lower surface can be subjected to ion exchange.
The cooling in the step (5) can adopt cooling methods with different rates such as furnace cooling, air cooling, water cooling and the like, and a method with a higher cooling speed is selected on the premise of ensuring that the sample does not have the defects of cracking, collapse and the like.
The invention has the following remarkable advantages:
(1) the auxiliary reagent is added into the molten salt, so that the surface of the sample is protected from being corroded while the ion exchange is accelerated, the surface of the glass ceramics is not damaged, and the influence on the optical properties of the sample such as light transmittance and fluorescence is small.
(2) Using CH3COOK as an adjuvant, CH during the strengthening process3COOK absorbing CO in air2Gradually precipitating K2CO3And excessive divalent cations in the molten salt are inhibited from exchanging with sodium ions in the molten salt to influence the exchange of potassium ions and sodium ions, the divalent ions have smaller radius than the potassium ions, the exchange effect is reduced, and the continuous control of the ion exchange rate is realized.
（3）CH3COOK is slowly converted into K in the using process2CO3Long service life, low cost, KCl and Al2O3The continuous control of sodium ions is matched with the use, so that the ion exchange quality of potassium ions and sodium ions is ensured.
(4) The formula can be applied to the field of dental restoration, so that the strength after exchange is improved, the restoration range of the dental glass ceramics is expanded, and the formula can be applied to restoration of parts with lower strength requirements such as the front dental crown and the like and can also meet the requirements of parts with higher strength requirements such as the back dental crown and the like.
(5) The molten salt auxiliary reagent is simple and easy to obtain, the process is stable, and the practical and industrial conditions are achieved.
Detailed Description
A molten salt for chemically toughening the microcrystal glass in dentistry is composed of KNO as main component and auxiliary component3The auxiliary component is Al2O3KCl and CH3And COOK (cooling). The weight percentages are as follows: KNO3 85%～95%、CH3COOK 3%～11%、KCl 1%～6%、Al2O3 0.5 to 2 percent, and the sum of the mass percent of the components is 100 percent.
The use method of the molten salt for chemically toughening the dental microcrystalline glass specifically comprises the following steps:
(1) cutting, grinding and polishing the glass block to enable the sample to be in a shape required by tests such as hardness, breaking strength and the like, cleaning, drying and then carrying out heat treatment to obtain a dental microcrystalline glass sample;
(2) weighing reagents according to the proportion of each component of the molten salt, mixing and then putting into alumina or other high-temperature stable crucibles for standby;
(3) fixing the sample obtained in the step (1) by using a stainless steel bracket and then embedding the sample into molten salt so that the sample can be buried by the molten salt;
(4) and (3) placing the alumina crucible into which the sample is placed in a heating furnace, heating to melt the molten salt, and preserving heat for a period of time to ensure smooth ion exchange. The mode that the sample is embedded into the molten salt in advance and is heated along with the furnace is adopted, so that the sample is prevented from being placed at high temperature, the sample is damaged due to rapid temperature change, and the steps are reduced, and the introduction of additional variables is also avoided;
(5) and after the ion exchange is finished, rapidly taking out the sample in the molten salt, cooling the sample, taking deionized water to clean the cooled sample, and drying to finish the chemical toughening of the dental microcrystalline glass.
The dental microcrystalline glass comprises SiO as a main component2、Li2CO3、K2CO3、Na2CO3、Al2O3、P2O5And ZrO2。
The sample size in the step (1) is the final size, no obvious defect exists, deionized water is used for cleaning, and the heat treatment method of the microcrystalline glass is determined according to specific glass components and the thermal property of the microcrystalline glass.
In the step (4), the heating rate of the heating furnace is 1-10 ℃/min, and preferably 4-8 ℃/min; the heat preservation temperature is 420-500 ℃, and preferably 450-480 ℃; the heat preservation time is 0.5-4 h, preferably 1-2 h.
And (4) in the step (4), the bracket is made of stainless steel and cannot be corroded by molten salt, and the molten salt is required to completely cover the surface of the sample after being melted, so that the upper surface and the lower surface can be subjected to ion exchange.
The cooling in the step (5) can adopt cooling methods with different rates such as furnace cooling, air cooling, water cooling and the like, and a method with a higher cooling speed is selected on the premise of ensuring that the sample does not have the defects of cracking, collapse and the like.
Table 1 shows the selection of the reagent (molten salt for chemical tempering of dental glass ceramics) for ion exchange and the contents thereof in examples 1 to 4
Figure DEST_PATH_IMAGE002
Example 1
According to the proportion of each exchange reagent component in the table 1, a certain amount of analytically pure raw materials are weighed, mixed uniformly, put into an alumina crucible and covered with a dental microcrystalline glass sample. According to the steps, the crucible is placed into a heating furnace, heated to 450 ℃ at the speed of 8 ℃/min, kept warm for 1h, taken out, and the sample is cooled in the air. The samples were cleaned and subjected to various performance tests, and the results are shown in table 2. The three-point bending strength value is 639MPa, and the fracture toughness is 4.6MPa x m0.5HV1 vickers hardness number 684. Compared with an untreated sample, the mechanical property is greatly enhanced, and the repair requirements of parts with higher strength requirements such as the back dental crown can be met. Meanwhile, the time required for ion exchange is 1 hour, which is greatly shortened compared with other patents.
Example 2
According to the proportion of each exchange reagent component in the table 1, a certain amount of analytically pure raw materials are weighed, mixed uniformly, put into an alumina crucible and covered with a dental microcrystalline glass sample. According to the steps, the crucible is placed into a heating furnace, heated to 450 ℃ at the speed of 8 ℃/min, kept warm for 1h, taken out, and the sample is cooled in the air. The samples were cleaned and subjected to various performance tests, and the results are shown in table 2. The three-point bending strength value is 620MPa, and the fracture toughness is 4.5MPa multiplied by m0.5HV1 vickers hardness number 676. The mechanical properties were reduced compared to example 1.
Example 3
Exchange reagent groups according to Table 1Proportioning, weighing a certain amount of analytically pure raw materials, uniformly mixing, putting into an alumina crucible, and covering a dental microcrystalline glass sample. According to the steps, the crucible is placed into a heating furnace, heated to 450 ℃ at the speed of 8 ℃/min, kept warm for 1h, taken out, and the sample is cooled in the air. The samples were cleaned and subjected to various performance tests, and the results are shown in table 2. The three-point bending strength value is 626MPa, and the fracture toughness is 4.5MPa multiplied by m0.5The HV1 Vickers hardness number is 681.
Example 4
According to the proportion of each exchange reagent component in the table 1, a certain amount of analytically pure raw materials are weighed, mixed uniformly, put into an alumina crucible and covered with a dental microcrystalline glass sample. According to the steps, the crucible is placed into a heating furnace, heated to 450 ℃ at the speed of 8 ℃/min, kept warm for 1h, taken out, and the sample is cooled in the air. The samples were cleaned and subjected to various performance tests, and the results are shown in table 2. The three-point bending strength value is 647MPa, and the fracture toughness is 4.8MPa multiplied by m0.5HV1 vickers hardness number 693 is the most preferred embodiment.
Example 5
According to the proportion of each exchange reagent component in the table 1, a certain amount of analytically pure raw materials are weighed, mixed uniformly, put into an alumina crucible and covered with a dental microcrystalline glass sample. According to the steps, the crucible is placed into a heating furnace, heated to 450 ℃ at the speed of 8 ℃/min, kept warm for 1h, taken out, and the sample is cooled in the air. The samples were cleaned and subjected to various performance tests, and the results are shown in table 2. The three-point bending strength value is 634MPa, and the fracture toughness is 4.6MPa multiplied by m0.5The HV1 vickers hardness number is 678.
The invention realizes the fused salt for chemically toughening the dental microcrystalline glass through the implementation. The remarkable effects are concentrated on excellent fracture toughness, bending strength, short chemical toughening time and the like.
TABLE 2 comparison of mechanical Properties of chemically tempered dental glass-ceramics
Figure DEST_PATH_IMAGE004
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 (4)

1. A use method of molten salt for chemical toughening of dental microcrystalline glass is characterized by comprising the following steps: the molten salt comprises a main component and an auxiliary component, wherein the main component is KNO3The auxiliary component is Al2O3KCl and CH3COOK；
The molten salt comprises the following components in percentage by mass: KNO3 86.5%、CH3COOK 8%、KCl 4%、Al2O3 1.5%；
The use method of the molten salt for chemically toughening the dental microcrystalline glass specifically comprises the following steps:
(1) cutting, grinding and polishing the dental microcrystalline glass block into a required shape, cleaning, drying and then carrying out heat treatment;
(2) mixing all components of the molten salt and then putting the mixture into an alumina crucible for later use;
(3) fixing the dental glass ceramics obtained in the step (1) by using a stainless steel bracket, and then embedding the dental glass ceramics into the molten salt obtained in the step (2);
(4) placing the crucible filled with the dental microcrystalline glass in the step (3) in a heating furnace, heating to melt the molten salt, and preserving heat for a period of time;
(5) after the heat preservation is finished, quickly taking out the dental microcrystalline glass sample in the molten salt, cooling the dental microcrystalline glass sample, cleaning the dental microcrystalline glass sample by using deionized water, and drying the dental microcrystalline glass sample to finish the chemical toughening of the dental microcrystalline glass;
in the step (4), the heating rate of the heating furnace is 4-8 ℃/min; the heat preservation temperature is 450 ℃; the heat preservation time is 1 h.
2. The use method of the molten salt for chemical tempering of dental glass-ceramic according to claim 1, characterized in that: the dental microcrystalline glass comprises SiO as a main component2、Li2CO3、K2CO3、Na2CO3、Al2O3、P2O5And ZrO2。
3. The use method of the molten salt for chemical tempering of dental glass-ceramic according to claim 1, characterized in that: in the step (4), the surface of the dental microcrystalline glass sample needs to be completely covered after the molten salt is melted, so that the upper surface and the lower surface of the glass can be subjected to ion exchange.
4. The use method of the molten salt for chemical tempering of dental glass-ceramic according to claim 1, characterized in that: the cooling method in the step (5) comprises one of furnace cooling, air cooling and water cooling.
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CN110342800A (en) * 2019-07-29 2019-10-18 中国建筑材料科学研究总院有限公司 Glass strengthening method and high strength glass
CN111620555B (en) * 2020-05-27 2022-07-29 维达力实业（赤壁）有限公司 Microcrystalline glass and tempering method and application thereof
CN114031311B (en) * 2021-09-08 2024-04-26 中山大学附属口腔医院 Molten salt for ion exchange and ion exchange enhancement method for enhancing mechanical property of lithium disilicate glass ceramic for dentistry
CN113716871B (en) * 2021-09-08 2023-06-06 深圳爱尔创口腔技术有限公司 Fluorescent lithium silicate glass ceramic enhanced by ion exchange and preparation method thereof
CN115594418B (en) * 2022-09-09 2024-01-30 福州瑞克布朗医药科技有限公司 Microcrystalline glass dental prosthesis and preparation method thereof

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