阅读说明：本技术 一种可快速着色的微晶玻璃制备方法及制得的产品及应用 (Preparation method of microcrystalline glass capable of being rapidly colored, prepared product and application ) 是由 张琪 吴宇鑫 仲文 余任飞 彭媛媛 吉昊 彭兵 刘鸿琳 林燕喃 李�泳 于 2020-07-09 设计创作，主要内容包括：本发明提供了一种可快速着色的微晶玻璃制备方法及制得的成品及应用,本发明以基质玻璃粉和色料为原料,经高温煅烧,除碳除氮,再经熔融制得玻璃液,浇铸到提前预热的模具中进行有色玻璃块的成型,并将有色玻璃块迅速放入退火炉中,去应力退火后冷却,得到着色的微晶玻璃。本发明提供的可快速着色的微晶玻璃制备方法,着色时间短,成本低,适用于大规模生产。(The invention provides a preparation method of microcrystalline glass capable of being rapidly colored, a finished product prepared by the preparation method and application of the microcrystalline glass. The preparation method of the microcrystalline glass capable of being rapidly colored, provided by the invention, has the advantages of short coloring time and low cost, and is suitable for large-scale production.)

1. A preparation method of microcrystalline glass capable of being rapidly colored is characterized by comprising the following steps: the method comprises the following steps:

a, weighing: weighing matrix glass powder and a pigment, then placing the matrix glass powder and the pigment into a ball milling tank for ball milling, and fully and uniformly mixing to obtain a matrix glass powder and pigment mixture; wherein, the mol percentage of the matrix glass powder and the pigment is (95-98): (2-5);

b, melting: b, placing the mixture of the matrix glass powder and the pigment weighed in the step a into a muffle furnace for calcination, setting calcination temperature and calcination time, removing carbon and nitrogen in the mixture of the matrix glass powder and the pigment, placing the calcined mixture of the matrix glass powder and the pigment into a high-temperature program control furnace for melting, and setting melting temperature and melting time to obtain fully-melted glass liquid for later use;

c, forming: b, casting the molten glass prepared in the step b into a mold preheated in advance to mold a colored glass block to prepare the colored glass block for later use;

d, annealing: and c, putting the colored glass block prepared in the step c into an annealing furnace, setting the annealing temperature and the annealing time for stress relief annealing, and cooling along with the annealing furnace after the annealing is finished to obtain the colored microcrystalline glass.

2. The method for preparing the microcrystalline glass capable of being rapidly colored according to claim 1, wherein the method comprises the following steps: in the step a, the matrix glass powder consists of potassium oxide, silicon dioxide, lithium oxide, aluminum oxide, phosphorus oxide, zirconium oxide and sodium oxide.

3. The method for preparing the microcrystalline glass capable of being rapidly colored according to claim 1, wherein the method comprises the following steps: the matrix glass powder comprises 1-3.2 mol% of potassium oxide, 40-75 mol% of silicon dioxide, 20-40 mol% of lithium oxide, 0.1-5 mol% of aluminum oxide, 0.1-4.5 mol% of phosphorus oxide, 1-6 mol% of zirconium oxide and 0.1-5 mol% of sodium oxide.

4. The method for preparing the microcrystalline glass capable of being rapidly colored according to claim 1, wherein the method comprises the following steps: in the step a, the pigment consists of erbium oxide, cerium oxide, vanadium pentoxide and tetraterbium heptaoxide, and the molar ratio of the erbium oxide to the cerium oxide to the vanadium pentoxide to the tetraterbium heptaoxide is (0.1-1): (0.1-1): (0.1-1): (0.1-1).

5. The method for preparing the microcrystalline glass capable of being rapidly colored according to claim 1, wherein the method comprises the following steps: in the step b, the calcining temperature is 800 ℃, and the calcining time is 30-60 min.

6. The method for preparing the microcrystalline glass capable of being rapidly colored according to claim 1, wherein the method comprises the following steps: the melting temperature in the step b is 1300-1600 ℃, and the melting time is 30-90 min.

7. The method for preparing the microcrystalline glass capable of being rapidly colored according to claim 1, wherein the method comprises the following steps: the annealing temperature in the step d is 500-580 ℃, and the annealing time is 30-150 min.

8. A colored glass-ceramic produced by the production method according to claim 1.

9. Use of the colored glass ceramic according to claim 8 for the preparation of dental porcelain.

10. Use of a coloured glass ceramic according to claim 9 for the preparation of a dental porcelain, characterized in that: the colored glass ceramics need to be nucleated and crystallized, and the method specifically comprises the following steps,

1) and (3) nucleation: putting the cooled colored glass ceramics into a program control furnace, and carrying out nucleation treatment at the temperature of 500-;

2) and (3) crystallization: crystallizing the colored glass ceramics after nucleation treatment obtained in the step 1) at the temperature of 700-800 ℃;

3) molding: cooling the colored glass ceramics obtained in the step 2) along with the furnace, and placing the colored glass ceramics in a dental porcelain furnace to increase the temperature to 670-900 ℃ at the heating rate of 47-66 ℃/min, and keeping the temperature for 10-80 min to obtain the colored glass ceramics.

Technical Field

The invention relates to the technical field of dental materials, in particular to a preparation method of microcrystalline glass capable of being rapidly colored, a prepared product and application.

Background

With the improvement of living standard of people and the coming of aging society, how to treat or repair the physiological function deficiency of human body caused by various reasons promotes the increasingly prominent demand of people for high-quality biological materials. Modern biomaterials are expected to have remarkable functions, stable chemical properties and more importantly, good biocompatibility.

Teeth are important components of human bodies, play roles in chewing, sounding, decoration and the like, and keep normal physiological functions of the teeth, which is very important for the health and the spiritual features of people. Under the combined action of various foods, which are increasingly abundant, and factors such as people's daily poor eating habits and the surrounding environment, natural teeth of a human body are damaged to a greater or lesser extent, such as tooth defects, loss or yellowing and blackening. Therefore, the dental restoration problem is obvious day by day, and the selection of proper restoration materials to prepare the denture (commonly called as the 'denture') with higher strength and more beautiful appearance for restoring and decorating the teeth so as to restore the biological function and beautiful appearance of the teeth becomes a hot point of research.

The demand determines the market, and there are a large number of dental restorative materials available on the market today. Wherein, the all-ceramic tooth material comprises zirconia and alumina which are relatively high-end all-ceramic tooth products in the market. However, the defects of opacity, too high hardness, difficult processing and the like of the material do not meet aesthetic requirements, and the time and cost are consumed in the processing process, while the coloring process of a few lithium silicate dental materials in the current market is complex, the cost is higher and the period is long.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provide a method for preparing microcrystalline glass capable of being rapidly colored, which comprises the steps of adding a proper pigment into matrix glass powder for coloring, adding sodium oxide to reduce the viscosity of the glass and improve the chemical stability, and developing the colored microcrystalline glass for dentistry through a one-step coloring process by a melting method.

The invention also aims to provide the colored microcrystalline glass prepared by the method and application thereof, and the microcrystalline glass can be further applied to dental porcelain through nucleation and crystallization treatment.

A preparation method of microcrystalline glass capable of being rapidly colored comprises the following steps:

a, weighing: weighing matrix glass powder and a pigment, then placing the matrix glass powder and the pigment into a ball milling tank for ball milling, and fully and uniformly mixing to obtain a matrix glass powder and pigment mixture; wherein, the mol percentage of the matrix glass powder and the pigment is (95-98): (2-5);

b, melting: b, placing the mixture of the matrix glass powder and the pigment weighed in the step a into a muffle furnace for calcination, setting calcination temperature and calcination time, removing carbon and nitrogen in the mixture of the matrix glass powder and the pigment, placing the calcined mixture of the matrix glass powder and the pigment into a high-temperature program control furnace for melting, and setting melting temperature and melting time to obtain fully-melted glass liquid for later use;

c, forming: b, casting the molten glass prepared in the step b into a mold preheated in advance to mold a colored glass block to prepare the colored glass block for later use;

d, annealing: and c, putting the colored glass block prepared in the step c into an annealing furnace, setting the annealing temperature and the annealing time for stress relief annealing, and cooling along with the annealing furnace after the annealing is finished to obtain the colored microcrystalline glass.

Wherein the die in the step c is a graphite die or a copper die.

Preferably, the base glass frit in step a is composed of potassium oxide, silicon dioxide, lithium oxide, aluminum oxide, phosphorus oxide, zirconium oxide, and sodium oxide.

Preferably, the molar percentages of the components in the matrix glass powder are respectively 1-3.2% of potassium oxide, 40-75% of silicon dioxide, 20-40% of lithium oxide, 0.1-5% of aluminum oxide, 0.1-4.5% of phosphorus oxide, 1-6% of zirconium oxide and 0.1-5% of sodium oxide.

Preferably, the pigment in the step a is composed of erbium oxide, cerium oxide, vanadium pentoxide and tetraterbium heptaoxide, and the molar ratio of erbium oxide, cerium oxide, vanadium pentoxide and tetraterbium heptaoxide is (0.1-1): (0.1-1): (0.1-1): (0.1-1).

Preferably, the calcination temperature in the step b is 800 ℃, and the calcination time is 30-60 min.

Preferably, the melting temperature in the step b is 1300-1600 ℃, and the melting time is 30-90 min.

Preferably, the annealing temperature in the step d is 500-580 ℃, and the annealing time is 30-150 min.

The invention relates to the colored glass ceramics prepared by the preparation method.

The invention also relates to the use of a coloured glass ceramic according to the invention for producing a dental porcelain.

Preferably, the colored glass-ceramic is subjected to nucleation and crystallization, and specifically comprises the following steps,

1) and (3) nucleation: placing the cooled colored glass-ceramic block into a program control furnace, and carrying out nucleation treatment at the temperature of 500-;

2) and (3) crystallization: crystallizing the colored glass ceramics after nucleation treatment obtained in the step 1) at the temperature of 700-800 ℃;

3) molding: cooling the colored glass ceramics obtained in the step 2) along with the furnace, and placing the colored glass ceramics in a dental porcelain furnace to increase the temperature to 670-900 ℃ at the heating rate of 47-66 ℃/min, and keeping the temperature for 10-80 min to obtain the colored glass ceramics.

The invention uses matrix glass powder and pigment as raw materials, and the raw materials are calcined at high temperature, decarbonized and denitrated, and then melted to prepare glass liquid, and the glass liquid is cast into a mold preheated in advance to form a colored glass block, and the colored glass block is rapidly placed into an annealing furnace, and cooled after stress relief annealing to obtain the colored microcrystalline glass.

Compared with the prior art, the invention has the following beneficial effects:

1. the preparation method of the microcrystalline glass capable of being rapidly colored, provided by the invention, has the advantages of short coloring time and low cost, and is suitable for large-scale production.

2. The microcrystalline glass prepared by the invention has moderate hardness, and can be applied to cutting processing after CAD/CAM digital modeling.

3. The microcrystalline glass capable of being rapidly colored provided by the invention has the advantages of low manufacturing cost, rich color, luster and proper transparency, and meets the requirement standard of dental materials.

The foregoing is only an overview of the technical solutions of the present invention, and in order to more clearly understand the technical solutions of the present invention, the present invention is further described below with reference to the accompanying drawings.

Drawings

FIG. 1 is a flow chart of the preparation process of the present invention.

Detailed Description

In order to understand the present invention, the following examples are given to further illustrate the present invention.