1. A dyeing material is characterized in that the dyeing material is prepared by mixing glaze powder, liquid dyeing material and anti-drying agent according to the weight ratio of 1 (5-100) to 0.5-8;

the fineness of the dyeing material is 5-20 μm.

2. The dyeing material as claimed in claim 1, wherein the dyeing material is prepared by mixing glaze powder, liquid dyeing material and anti-drying agent in a weight ratio of 1 (10-80) to (1-7).

3. Dyeing material according to claim 1, characterized in that the fineness of the dyeing material is 5-10 μ ι η.

4. The dyed material of claim 1 wherein said anti-drying agent is one or more of propylene glycol, sorbitol, glycerin, glucose.

5. A process for the preparation of a dyed material according to any one of claims 1 to 4 comprising the steps of:

a1, preparing a liquid dyeing material according to colorimetric requirements;

a2, mixing glaze powder with liquid dyeing material, adding anti-drying agent, and performing ultrasonic treatment to obtain mixed solution;

a3, grinding the mixed solution in A2 to obtain the product.

6. The method for preparing a dyeing material according to claim 5, characterized in that in A2, the temperature of ultrasonic treatment is 40-50 ℃, the frequency is 25-28kHz, and the time is 6-8 min.

7. The use of the dyeing material of any one of claims 1 to 4 on a zirconium dioxide full-porcelain tooth, characterized in that the dyeing material is coated on the surface of a semi-finished zirconium dioxide full-porcelain tooth product and sintered to obtain a finished zirconium dioxide full-porcelain tooth product.

8. Use of the dyed material according to claim 7 on zirconium dioxide all-ceramic teeth, characterized in that the sintering process is: sintering the zirconium dioxide full porcelain tooth semi-finished product coated with the dyeing material at 850-950 ℃ for 1-2min, naturally cooling to 280-320 ℃, immediately heating to 850-950 ℃ for continuous sintering for 1-2min, naturally cooling to 280-320 ℃, heating again to 850-950 ℃ for sintering for 1-2min, and naturally cooling to 280-320 ℃ to obtain the zirconium dioxide full porcelain tooth semi-finished product.

9. Use of the dyed material according to claim 8 on zirconium dioxide all-ceramic teeth, wherein the rate of temperature rise is 25-35 ℃/min.

10. The use of the dyeing material on zirconium dioxide all-ceramic teeth as claimed in claim 8, wherein the sintering temperature is 880-.

Background

The full-ceramic tooth is characterized in that an inner crown is made on a tooth root to be treated, the inner crown is a layer of full-ceramic transparent supporting framework, then a layer of ceramic powder with color similar to that of a natural tooth is baked on the outer crown surface of the inner crown, and finally the ceramic powder is bonded on the tooth, so that the high-tech tooth inlaying method is developed in recent years. There are various kinds of full-ceramic teeth, and among them, the zirconium dioxide full-ceramic tooth is the firmest one of the dental restorations. At present, zirconium dioxide full-ceramic teeth are generally formed by computer aided design, laser scanning, cutting by computer program control to form an inner crown, baking a layer of ceramic powder with color close to that of natural teeth on the outer layer of the inner crown after sintering, polishing and trying on, and finally adhering the ceramic powder on the teeth.

Although the zirconium dioxide full-ceramic tooth has a flexural strength of over 1000MPa by itself, the strength of the modified ceramic layer on the surface thereof is only about 100 MPa. Because zirconium dioxide and its surface porcelain layer have different thermal expansion coefficient, can lead to zirconium dioxide full porcelain tooth surface porcelain layer to break apart, simultaneously, if the patient who uses zirconium dioxide full porcelain tooth has the habit of grinding one's teeth in sleep, or gnaws at ordinary times and stings hard thing more, also can lead to full porcelain tooth surface to break apart porcelain. If the zirconium dioxide full-ceramic tooth surface has a ceramic collapse phenomenon, the appearance is affected if the zirconium dioxide full-ceramic tooth surface is light, the full-ceramic tooth is damaged if the zirconium dioxide full-ceramic tooth surface is heavy, the repair is also complex, and the cost is high.

Therefore, in order to prevent the porcelain collapse phenomenon of the teeth and prolong the service life of the zirconium dioxide all-ceramic teeth, the zirconium dioxide all-ceramic teeth which are not applied with porcelain and have the same transparent effect and beautiful appearance as the applied ceramic teeth are developed, and the method has very important significance.

Disclosure of Invention

In order to overcome the defect that the zirconium dioxide full-porcelain tooth is easy to break, the zirconium dioxide full-porcelain tooth which is not applied with porcelain and has the same transparent effect and attractive appearance as the applied porcelain tooth is produced, and the application provides a dyeing material, a preparation method thereof, application on the zirconium dioxide full-porcelain tooth and a use method thereof.

In a first aspect, the present application provides a dyeing material, which adopts the following technical scheme:

a dyeing material is prepared by mixing glaze powder, liquid dyeing material and anti-drying agent according to the weight ratio of 1 (5-100) to 0.5-8;

the fineness of the dyeing material is 5-20 μm.

The liquid dyeing material is 16-color or 26-color dyeing liquid.

The anti-drying agent is one or more of propylene glycol, sorbitol, glycerol and glucose.

By adopting the technical scheme, the liquid dyeing material is used as a main dyeing substance and a solvent, and the added glaze powder mainly generates a transparent effect, so that the transparency and the naturalness of the dyeing material are improved. The dyeing material can endow the coated object with better transparent effect and beautiful appearance after being coated on the surface of the coated object. Such as: the coating is coated on the surface of the zirconium dioxide full-ceramic tooth to replace a zirconium dioxide full-ceramic tooth surface modified ceramic layer, so that the transparency and the attractiveness of the zirconium dioxide full-ceramic tooth can be improved, the zirconium dioxide full-ceramic tooth has the same appearance effect as a natural tooth, the ceramic collapse phenomenon cannot occur, and the service life of the zirconium dioxide full-ceramic tooth is prolonged.

Preferably, the dyeing material is formed by mixing glaze powder, liquid dyeing material and anti-drying agent according to the weight ratio of 1 (10-80) to 1-7.

By adopting the technical scheme, the dyeing material has the color effect closer to that of a natural tooth after being fixed by further optimizing the proportion of the raw materials, and the transparency and the attractiveness of the surface of the zirconium dioxide all-ceramic tooth are improved.

Preferably, the dyeing material has a fineness of 5 to 10 μm.

Through adopting above-mentioned technical scheme, through the further optimization to dyeing material fineness, improved the planarization of dyeing material when coating, reduce the condition emergence of coating surface unevenness or production great caking, simultaneously, still can fully with coated object surface adhesion fixed, improve the fastness of coating.

In a second aspect, the present application provides a method for preparing a dyed material, which adopts the following technical scheme:

a method for preparing a dyed material, comprising the steps of:

a1, preparing a liquid dyeing material according to colorimetric requirements;

a2, mixing glaze powder with liquid dyeing material, adding anti-drying agent, and performing ultrasonic treatment to obtain mixed solution;

a3, grinding the mixed solution in A2 to obtain the product.

By adopting the technical scheme, the preparation process is simple, the raw materials are easy to obtain, the liquid dyeing liquid with different color effects can be prepared according to different use conditions, and then the prepared liquid dyeing material is ultrasonically mixed with the glaze powder and the anti-drying agent, so that the raw materials can be fully dispersed in a mixed system, and the dyeing material with better dyeing effect and dyeing adhesive force is prepared.

Preferably, in the A2, the ultrasonic treatment temperature is 40-50 ℃, the frequency is 25-28kHz, and the time is 6-8 min.

By adopting the technical scheme, under the above conditions, the liquid dyeing material, the glaze powder and the anti-drying agent can be fully mixed, the dispersibility of each component in a mixed system is improved, the prepared dyeing material has more uniform texture, and the phenomena of caking, unevenness and the like when the dyeing material is coated on the surface of the zirconium dioxide all-ceramic tooth are reduced.

In a third aspect, the application provides an application of a dyeing material on a zirconium dioxide all-ceramic tooth, and adopts the following technical scheme:

the application of the dyeing material on the zirconium dioxide full-porcelain tooth is characterized in that the dyeing material is coated on the surface of a semi-finished product of the zirconium dioxide full-porcelain tooth and sintered to obtain a finished product of the zirconium dioxide full-porcelain tooth.

Through adopting above-mentioned technical scheme, use the dyeing material of this application to replace surface modification porcelain layer, avoided the porcelain collapse phenomenon on zirconium dioxide all-ceramic tooth surface, prolonged the life of all-ceramic tooth. Meanwhile, although the surface of the all-ceramic tooth is not provided with the ceramic, the all-ceramic tooth has the same transparent effect and beautiful appearance as the ceramic, so that the finished product of the zirconium dioxide all-ceramic tooth is closer to a natural tooth.

Preferably, the sintering process is as follows: sintering the zirconium dioxide full porcelain tooth semi-finished product coated with the dyeing material at 850-950 ℃ for 1-2min, naturally cooling to 280-320 ℃, immediately heating to 850-950 ℃ for continuous sintering for 1-2min, naturally cooling to 280-320 ℃, heating again to 850-950 ℃ for sintering for 1-2min, and naturally cooling to 280-320 ℃ to obtain the zirconium dioxide full porcelain tooth semi-finished product.

Through adopting above-mentioned technical scheme, the zirconium dioxide full porcelain tooth that has the coating dyeing material according to above-mentioned parameter condition sinters, can obviously reduce the production of coating bubble, makes the dyeing material coating on the full porcelain tooth surface of zirconium dioxide more level and smooth, simultaneously, through the processing of cooling down of natural cooling after the sintering of heating up many times, can make the more firm attached to in the full porcelain tooth surface of zirconium dioxide of dyeing material, reduces follow-up when using, and the condition that full porcelain tooth surface dyeing material coating drops takes place.

Preferably, the heating rate is 25-35 ℃/min.

By adopting the technical scheme, the temperature is raised within the temperature-raising rate range, so that the generation of bubbles in the coating layer of the dyeing material can be further reduced, the smoothness of the coating layer is ensured, and the zirconium dioxide full-ceramic tooth is closer to a natural tooth.

Preferably, in the sintering process, the sintering temperature is 880-900 ℃, the sintering time is 1.4-1.6min, and the cooling temperature is 295-305 ℃.

By adopting the technical scheme, the fastness and the flatness of the adhesion of the dyeing material on the surface of the zirconium dioxide all-ceramic tooth are further improved by further optimizing the sintering conditions.

In summary, the present application has the following beneficial effects:

1. the dyeing material of this application coats in the all-ceramic tooth surface of zirconium dioxide, replaces the modification porcelain layer on all-ceramic tooth surface, and not only the cost is reduced, can also make all-ceramic tooth have the outward appearance the same with natural tooth, simultaneously, still can not take place to collapse porcelain phenomenon, prolongs the life of the all-ceramic tooth of zirconium dioxide.

2. This application is through sintering the zirconium dioxide full porcelain tooth who has coated the dyeing paint with specific step, through control sintering temperature, sintering time and rate of rise of temperature, has effectively reduced the production of the interior bubble of coating layer, has reduced the condition emergence of coating layer surface unevenness, simultaneously, has improved the fastness of dyeing material coating at the zirconium dioxide full porcelain tooth surface adhesion.

Detailed Description

The present application will be described in further detail with reference to examples.

The raw materials used in the examples of the present application are commercially available, except for the following specific descriptions:

the glaze powder is prepared from Vita corporation, Dengshi Berjin diamond glaze powder;

the liquid dyeing material is collected from Vita company, 16-color dyeing liquor;

the propylene glycol is obtained from Shanghai Aladdin Biotechnology, Inc., and is numbered as follows: p103434, the purity is more than or equal to 99.5%;

glucose was collected from Shanghai Aladdin Biotechnology Ltd, numbered: g116306, the purity is more than or equal to 99.5%;

glycerol was obtained from Shanghai Aladdin Biotechnology GmbH, numbered: g116206, the purity is more than or equal to 99.5%;

the zirconium dioxide full-porcelain tooth semi-finished product in the embodiment of the application is prepared by steps 1-4 in the embodiment of Chinese patent with the publication number of CN102302381B and publication date of 20131016.

Examples

Example 1

A dyed material, the components and their respective weights being as shown in Table 1, prepared by the steps of:

a1, preparing a liquid dyeing material according to colorimetric requirements; in the embodiment, the liquid dyeing material is formed by mixing a yellow dyeing material, an orange dyeing material, a clove color dyeing material and a glaze color dyeing material according to a weight ratio of 30:20:8: 0.4;

a2, mixing glaze powder and liquid dyeing material, adding anti-drying agent, and performing ultrasonic treatment at 25 deg.C and 20kHz for 5min to obtain mixed solution, wherein the anti-drying agent is ethylene glycol;

a3, grinding the mixed solution obtained in A2 to obtain dyeing material with fineness of 10-20 μm.

Examples 2 to 6

The dyeing material was prepared under the same conditions as in example 1 except that the used amounts of the raw materials were different, and the respective components and the respective amounts thereof used are shown in Table 1.

TABLE 1 Components and weights (kg) thereof in examples 1-6

Example 7

A dyed material obtained by grinding the dyed material to a fineness of 5 to 10 μm in step A3 under the same conditions as in example 3 except that the dyed material obtained in step A3 was ground to a fineness different from that of the dyed material obtained in step A3.

Example 8

A dyeing material, which is prepared by using glucose as an anti-drying agent in the present embodiment, is the same as in embodiment 7 except that the anti-drying agent is used in the same manner.

Example 9

A dyeing material, which is prepared under the same conditions as those in example 7 except that the use condition of the anti-drying agent is different, in this example, the anti-drying agent is glycerin.

Examples 10 to 13

A dyed material was produced under the same conditions as in example 9 except that the ultrasonic treatment conditions in the step A2 were different, and the ultrasonic treatment conditions in the step A2 were as shown in Table 2.

TABLE 2 examples 9-13 sonication conditions in step A2

Comparative example

Comparative examples 1 to 4

The dyeing material was prepared under the same conditions as in example 1 except that the used amounts of the raw materials were changed, and the respective amounts of the components and the amounts thereof used are shown in Table 3.

TABLE 3 Components and weights (kg) of comparative examples 1-4

Comparative example 5

A dyed material obtained by grinding the dyed material to a fineness of 20 to 30 μm in step A3 in the same manner as in example 1 except that the dyed material obtained in step A3 was ground to a fineness different from that obtained in step A3.

Application example

Application example 1

The application of the dyeing material on the zirconium dioxide all-ceramic tooth comprises the following steps: and coating the surface of the semi-finished zirconium dioxide full-porcelain tooth product with the coating thickness of 1mm, and sintering at 800 ℃ for 1h to obtain the finished zirconium dioxide full-porcelain tooth product.

Application example 2

The application of the dyeing material on the zirconium dioxide all-ceramic tooth is different from the application example 1 in the sintering process, and the other conditions are the same, wherein the sintering process in the application example is as follows: sintering the zirconium dioxide full porcelain tooth semi-finished product coated with the dyeing material at 850 ℃ for 1min, naturally cooling to 280 ℃, immediately heating to 850 ℃ and continuing sintering for 1min, naturally cooling to 280 ℃, heating to 850 ℃ again and sintering for 1min, and naturally cooling to 280 ℃ to obtain the zirconium dioxide full porcelain tooth semi-finished product.

Wherein the heating rate is 20 ℃.

Application examples 3 to 6

The application of a dyeing material on zirconium dioxide all-ceramic teeth is the same as that of application example 2 except that the parameters in the sintering process are different, and the conditions are specifically shown in table 4.

TABLE 4 parameters of sintering Process in application examples 2-6

Application examples 7 to 10

The application of a dyeing material to zirconium dioxide all-ceramic teeth is the same as that of application example 4 except that the temperature rise rate in the sintering process is different, and is specifically shown in table 5.

TABLE 5 application examples 4, 7-10 sintering Process ramp rates

Performance test

Test one:

the dyeing materials prepared in examples 1 to 13 and comparative examples 1 to 5 were applied to the surface of the semi-finished zirconia full-porcelain tooth by the application method in example 1 to prepare a finished zirconia full-porcelain tooth, and the finished zirconia full-porcelain tooth was used as a test sample. 180 volunteers who need to use dentures were selected as test persons and divided into 18 groups of 10 persons each. Selected volunteers are all male, the age interval is 25-35 years old, the eating habits are basically the same, and the teeth grinding habits are all existed during sleep. After 3 months of normal use, the test specimens were reviewed for appearance (including clarity and aesthetics), discoloration of the dyed material, and scored (1-10 points) to obtain an average of the final results, which are shown in Table 6 below.

Scoring criteria

Transparency: the transparency is closer to that of natural teeth within the range of 4-6 points;

the beauty degree is as follows: the higher the score, the more aesthetic;

fading condition: the higher the score, the more discoloration.

Table 6 test a performance test results

It can be seen from the data in table 6 that the dyed materials prepared in examples 1 to 13 of the present application, when coated on the surface of the zirconia all-ceramic tooth, can provide the zirconia all-ceramic tooth with transparency equivalent to that of a natural tooth and also have good aesthetic appearance. After 3 months of normal use, the color fading phenomenon is basically avoided.

Combining the data of example 1 and comparative example 1, it can be seen that decreasing the proportion of liquid staining material in the raw material, i.e. increasing the percentage of glaze powder, results in increased transparency of the staining material, which is more distinct from the transparency of natural teeth.

By combining the data of the example 1 and the data of the comparative examples 2 and 3, the anti-drying agent is not added in the comparative example 2, the proportion of the anti-drying agent in the raw materials is reduced in the comparative example 3, the attractiveness of the test sample is greatly reduced, and the fading condition is obviously increased.

Combining the data of example 1 and comparative example 4, it can be seen that the transparency of the dyed material is significantly reduced in comparative example 4 without adding glaze powder, and the test result is only 2.3 points.

It can be seen from the data of examples 3 and 7 and comparative example 5 that the dyed material has better transparency and aesthetic appearance when applied to the full-porcelain tooth, and is substantially free from discoloration, when the fineness of the dyed material is 5 to 20 μm. Further, when the fineness of the dyed material is 5 to 10 μm, the transparency and beauty of the zirconia full-ceramic tooth are further improved, and the discoloration phenomenon is less.

And (2) test II:

the dyeing material obtained in example 1 was applied to the surface of the semi-finished zirconia full porcelain tooth product by the application method in application examples 1 to 10 to obtain a finished zirconia full porcelain tooth product, and the finished zirconia full porcelain tooth product was used as a test sample. 100 volunteers who need to use dentures were selected as test persons and divided into 10 groups of 10 persons. Selected volunteers are all male, the age interval is 25-35 years old, the eating habits are basically the same, and the teeth grinding habits are all existed during sleep. After 3 months of normal use, the test specimens were reviewed for appearance (including clarity and aesthetics), discoloration of the dyed material, and scored (1-10 points) to obtain an average of the final results, which are shown in Table 7 below.

Scoring criteria

Transparency: the transparency is closer to that of natural teeth within the range of 4-6 points;

the beauty degree is as follows: the higher the score, the more aesthetic;

fading condition: the higher the score, the more discoloration.

Table 7 test two performance test results

Combining the data from application example 1 and application examples 2-6, it can be seen that the zirconium dioxide all-ceramic teeth obtained by applying the dyed material using the method of application examples 2-6 have less discoloration. The preferred range of the sintering temperature is 880-900 ℃, the preferred range of the sintering time is 1.4-1.6min, and the preferred range of the cooling temperature is 295-305 ℃. Among them, the application example 3 is a preferred embodiment and the data of the application examples 4 and 7-10 show that after the dyeing material is coated on the semi-finished product of the zirconium dioxide full-ceramic tooth, the preferred range of the temperature rise rate in the sintering process is 25-35 ℃, particularly when the temperature rise rate is 30 ℃, the prepared zirconium dioxide full-ceramic tooth has the best performance, and no fading phenomenon occurs after 3 months of use.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.