WO2017185477A1

WO2017185477A1 - Method for dyeing zirconium oxide dental porcelain

Info

Publication number: WO2017185477A1
Application number: PCT/CN2016/084140
Authority: WO
Inventors: 易元超
Original assignee: 成都贝施美医疗设备有限公司; 成都贝施美生物科技有限公司
Priority date: 2016-04-29
Filing date: 2016-05-31
Publication date: 2017-11-02
Also published as: CN105924228A

Abstract

A method for dyeing a zirconium oxide dental porcelain. The method comprises: preparing a dental porcelain (S1); dip dyeing (S2); first oven drying (S3); coloring (S4); second oven drying (S5); and sintering (S6). The method for dyeing the zirconium oxide provides the advantages of ease of implementation, standardization, excellent dyeing effects, lower sintering temperature, and lower costs. The dental zirconium oxide porcelain obtained by using the method has a uniform color, good aesthetics, and a translucent and glossy texture. The dental porcelain has high stability, aging resistance, and high strength.

Description

Description: A method for dyeing dental zirconia ceramics

[0001] The present invention relates to the field of ceramic preparation technology, and in particular to a method for dyeing dental zirconia ceramics.

Background technique

[0002] Dental ceramics refer to glass ceramic materials and articles for dental treatment and repair. Belongs to the category of medical devices. Dental ceramics are classified into type I and enamel type, type I dental ceramics are supplied in powder form, and enamel type dental ceramics are provided in various forms other than powder. Zirconium oxide ceramics have excellent mechanical properties, and their flexural strength exceeds 100 MPa. The thinner thickness can achieve high strength and is an ideal dental restoration material. In dental restoration, in addition to considering the mechanical properties of the material, attention should be paid to the color and aesthetic requirements of the material.

[0003] Chinese Patent No. CN102674888A discloses a coloring solution for dental zirconia ceramics and a method of use thereof. The patent mentions a dyeing method for dental zirconia ceramics, but the description is not specific, and the operation is not The specification increases the difficulty of dyeing, resulting in uneven dyeing and unsightly appearance.

[0004] Therefore, a simple operation and standardization method for improving the dyeing effect of the dental zirconia ceramic can be used to make the dental zirconia ceramic dyeing uniform and beautiful, the light-transparent jade texture, and the stability and anti-aging.

technical problem

[0005] The object of the present invention is to overcome the disadvantages of the prior art and provide a dyeing method for dental zirconia ceramics.

Technical solution

The object of the present invention is achieved by the following technical solutions: A method for dyeing dental zirconia ceramics, which consists of the following steps:

[0007] S1. Preparation of dental ceramics: preparing a pre-sintered dental zirconia ceramic block, performing a cutting process to obtain a dental zirconia ceramic;

[0008] S2. Dip Dyeing: The dental zirconia ceramic obtained in step S1 is placed in a dyeing solution, which is shaken and poured into a container to ensure that the dose completely covers the dental zirconia ceramic, and the plastic pliers are used in the dip dyeing process. The dental zirconia ceramic is continuously tumbling and taken out after 30~60s;

[0009] S3. The first drying: the dyed dental zirconia ceramic obtained in step S2 is dried, drying the crucible is 30~60min;

[0010] S4. Coloring: Step S3 to obtain a dental zirconia ceramic for coloring, the coating is applied to the dental zirconia ceramic by spraying, brushing or sponge application;

[0011] S5.

The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 30 to 60 min.

[0012] S6. Sintering: The dental zirconia ceramic obtained in step S5 is sintered, and the sintering temperature is 1400~1600.

°C, the sintering enthalpy is 3~5h, that is, the dental zirconia ceramic is obtained.

[0013] Further, the dyeing liquid is composed of the following raw materials by weight:

[0014] deionized water 800~1000; coloring agent 3~50; dispersing agent 0~10;

[0015] Complexing agent 0~7; thixotropic agent 0~10; color indicator 0~0.5; inorganic additive 0~0.5.

[0016] Further, the dip dyeing in the step S2 is to shake the dyeing liquid into the container to ensure that the dose completely covers the dental zirconia ceramic, and the dental zirconia ceramic is continuously tumbling using the plastic pliers during the dip dyeing process, 30 Take out after ~60s.

[0017] Further, the coloring agent includes a colored cation and a colored anion, wherein the colored cation is a combination of two or more of iron ions, cerium ions, cerium ions or manganese ions; The anion is a combination of one or more of chloride, nitrate, metavanadate or permanganate.

Further, the dispersing agent is a combination of one or more of triethylhexylphosphoric acid, sodium lauryl sulfate, methylpentanol or a cellulose derivative.

Further, the complexing agent is a combination of one or more of formic acid, acetic acid, phthalic acid or salicylic acid.

[0020] Further, the inorganic additive is a combination of one or more soluble salts of cerium, lanthanum, cerium or lanthanum. [0021] Further, the color indicator is methyl violet, malachite green, and Congo A combination of one or more of red or bromocresol green sodium.

[0022] Further, the thixotropic agent is a hydroxyethyl cellulose derivative, a polyvinyl alcohol, a polyacrylate or a hydrogenated product. A combination of one or more of castor oil.

Advantageous effects of the invention

Beneficial effect

[0023] The present invention has the following advantages: The dyeing method of the dental zirconia ceramic provided by the invention solves the problems existing in the existing dental zirconia ceramic dyeing method, and has the advantages of simple operation, standardization, good dyeing effect, and reduced sintering temperature. , the advantage of low cost. The dental zirconia ceramic obtained by the invention has uniform and beautiful dyeing, light-transparent jade texture, high stability, anti-aging and high strength.

Embodiments of the invention

[0024] The present invention will be further described below in conjunction with the embodiments, and the scope of the present invention is not limited to the following.

[0025] Example 1: A method of dyeing a dental zirconia ceramic, which consists of the following steps:

[1] preparing a dental ceramic: preparing a pre-sintered dental zirconia ceramic block, performing a cutting process to obtain a dental zirconia ceramic;

[0027] S2. Dip-dyeing: The dental zirconia ceramic obtained in step S1 is placed in a dyeing solution, which is shaken and poured into a container to ensure that the dose completely covers the dental zirconia ceramic, and plastic pliers are used in the dyeing process. The dental zirconia ceramic is continuously rolled and taken out after 30 seconds;

[0028] S3. The first drying: the dyed dental zirconia ceramic obtained in step S2 is dried, and the drying time is 30 min;

[0029] S4. Coloring: Step S3 to obtain a dental zirconia ceramic for painting, the brushing method is applied to the dental zirconia ceramic by a spraying method;

[0030] S5. The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 30 min.

S6. Sintering: The dental zirconia ceramic obtained in the step S5 was sintered at a sintering temperature of 1400 ° C and a calcined crucible for 3 h to obtain a dental zirconia ceramic.

[0032] The dyeing liquid is composed of the following raw materials by weight:

[0033] deionized water 800; coloring agent 3; dispersing agent 5;

[0034] Complexing agent 3.5; thixotropic agent 7; color indicator 0.3; inorganic additive 0.1. [0035] the colorant includes a colored cation and a colored anion, wherein the colored cation is a combination of iron ions and manganese ions; the coloring liquid anion is a combination of chloride ion and nitrate; the dispersing agent is cellulose a complexing agent is a combination of formic acid and acetic acid; the inorganic additive is a soluble salt of cerium; the color indicator is a combination of methyl violet and malachite green; the thixotropic agent is hydrogenated castor oil .

[0036] Example 2: A method of dyeing a dental zirconia ceramic, which consists of the following steps:

[0037] S1. Preparation of dental ceramics: preparing a pre-sintered dental zirconia ceramic block, performing a cutting process to obtain a dental zirconia ceramic;

[0038] S2. Dip-dyeing: The dental zirconia ceramic obtained in step S1 is placed in a dyeing solution, which is shaken and poured into a container to ensure that the dose completely covers the dental zirconia ceramic, and plastic pliers are used in the dyeing process. The dental zirconia ceramic is continuously rolled and taken out after 60s;

[0039] S3. The first drying: the dyed dental zirconia ceramic obtained in step S2 is dried, and the drying time is 60 min;

[0040] S4. Coloring: Step S3 to obtain a dental zirconia ceramic for coloring, the brushing method is applied to the dental zirconia ceramic by brushing;

[0041] S5. The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 60 min.

[0042] S6. Sintering: The dental zirconia ceramic obtained in the step S5 is sintered at a sintering temperature of 1600 ° C and a calcined crucible for 5 h to obtain a dental zirconia ceramic.

[0043] The dyeing liquid is composed of the following raw materials by weight:

[0044] deionized water 1000; colorant 50; dispersant 10;

[0045] Complexing agent 7; thixotropic agent 10; color indicator 0.5; inorganic additive 0.5.

[0046] The colorant includes a colored cation and a colored anion, wherein the colored cation is a combination of iron ion, cerium ion and cerium ion; the coloring liquid anion is chloride ion; and the dispersing agent is triethylhexyl Phosphoric acid; the complexing agent is a combination of formic acid, acetic acid and phthalic acid; the inorganic additive is a soluble salt of cerium; the color indicator is malachite green; the thixotropic agent is hydroxyethyl cellulose A combination of a derivative and a polyvinyl alcohol.

Example 3: A method of dyeing a dental zirconia ceramic, which consists of the following steps:

[0048] S1. Preparation of dental ceramics: preparation of pre-sintered dental zirconia ceramic blocks, cutting processing, obtaining teeth Zirconia ceramics;

[0049] S2. Dip-dyeing: The dental zirconia ceramic obtained in step S1 is placed in a dyeing solution, which is shaken and poured into a container to ensure that the dose completely covers the dental zirconia ceramic, and the plastic pliers are used in the dip dyeing process. The dental zirconia ceramic is continuously tumbling and taken out after 45 s;

[0050] S3. The first drying: the dyed dental zirconia ceramic obtained in step S2 is dried, and the drying time is 47 min;

[0051] S4. Coloring: Step S3 to obtain a dental zirconia ceramic for painting and coloring, the coating using a sponge to apply the dyeing liquid to the dental zirconia ceramic;

[0052] S5. The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 44 min.

S6. Sintering: The dental zirconia ceramic obtained in the step S5 was sintered at a sintering temperature of 1,450 ° C and a sintered crucible for 4 hours to obtain a dental zirconia ceramic.

[0054] The dyeing liquid is composed of the following raw materials by weight:

[0055] deionized water 900; colorant 27;

[0056] Complexing agent 2; thixotropic agent 4; inorganic additive 0.2.

[0057] the colorant includes a colored cation and a colored anion, wherein the colored cation is a combination of iron ions and cerium ions; the coloring liquid anion is a combination of metavanadate and permanganate; It is a combination of formic acid and acetic acid; the inorganic additive is a combination of soluble salts of cerium, lanthanum and cerium; the thixotropic agent is a combination of a hydroxyethyl cellulose derivative and polyvinyl alcohol.

Example 4: A method of dyeing a dental zirconia ceramic, which consists of the following steps:

[0059] S1. Preparation of dental ceramics: preparing a pre-sintered dental zirconia ceramic block, performing a cutting process to obtain a dental zirconia ceramic;

[0060] S2. Dip-dyeing: The dental zirconia ceramic obtained in step S1 is placed in a dyeing solution, which is shaken and poured into a container to ensure that the dose completely covers the dental zirconia ceramic, and plastic pliers are used in the dyeing process. The dental zirconia ceramic is continuously rolled and taken out after 35 seconds;

[0061] S3. The first drying: the dyed dental zirconia ceramic obtained in step S2 is dried, and the drying time is 45 min;

[0062] S4. Coloring: Step S3 to obtain a dental zirconia ceramic for painting, the coating is sprayed, Applying a dye solution to the dental zirconia ceramic by brushing or sponge application;

[0063] S5. The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 55 min.

S6. Sintering: The dental zirconia ceramic obtained in the step S5 was sintered at a sintering temperature of 1500 ° C and a calcined crucible of 3.5 h to obtain a dental zirconia ceramic.

[0065] The dyeing liquid is composed of the following raw materials by weight:

[0066] deionized water 850; colorant 45; dispersant 2;

Thixotropic agent 8; color indicator 0.4.

[0068] the colorant includes a colored cation and a colored anion, wherein the colored cation is a combination of iron ions, cerium ions, and manganese ions; the coloring liquid anion is a combination of chloride ions, nitrates, and metavanadate; The dispersing agent is a combination of triethylhexylphosphoric acid, sodium lauryl sulfate and methylpentanol; the color indicator is a combination of methyl violet, malachite green and Congo red; the thixotropic agent is A combination of a hydroxyethyl cellulose derivative, a polyvinyl alcohol, and a polyacrylate.

Example 5: A method of dyeing a dental zirconia ceramic, which consists of the following steps:

[0070] S1. Preparation of dental ceramics: preparing a pre-sintered dental zirconia ceramic block, performing a cutting process to obtain a dental zirconia ceramic;

[0071] S2. Dip-dyeing: The dental zirconia ceramic obtained in step S1 is placed in a dyeing liquid, which is shaken and poured into a container to ensure that the dose completely covers the dental zirconia ceramic, and the plastic pliers are used in the dyeing process. The dental zirconia ceramic is continuously rolled and taken out after 52s;

[0072] S3. The first drying: the dyed dental zirconia ceramic obtained in step S2 is dried, and the drying time is 39 min;

[0073] S4. Coloring: Step S3 to obtain a dental zirconia ceramic for coloring, the brushing method is applied to the dental zirconia ceramic by spraying;

[0074] S5. The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 58 min.

S6. Sintering: The dental zirconia ceramic obtained in the step S5 was sintered at a sintering temperature of 1580 ° C and a burnt crucible of 4.6 h to obtain a dental zirconia ceramic.

[0076] The dyeing liquid is composed of the following raw materials by weight: [0077] deionized water 870; colorant 22; dispersant 8.5;

[0078] Complexing agent 6; color indicator 0.45; inorganic additive 0.35.

[0079] The coloring agent includes a colored cation and a colored anion, wherein the colored cation is a combination of iron ion, cerium ion, cerium ion and manganese ion; the coloring liquid anion is chloride ion, nitrate, metavanadate And a combination of permanganate; the dispersing agent is a combination of triethylhexylphosphoric acid, sodium lauryl sulfate, methylpentanol and a cellulose derivative; the complexing agent is formic acid, acetic acid, phthalic acid The combination with salicylic acid; the inorganic additive is a combination of soluble salts of cerium, lanthanum, cerium and lanthanum; the color indicator is a combination of methyl violet, malachite green, Congo red and bromocresol green sodium.

Claims

Claim

[Claim 1] A method of dyeing a dental zirconia ceramic, characterized in that it consists of the following steps:

S1. Preparation of dental ceramics: Preparation of pre-sintered dental zirconia ceramic blocks for cutting

, obtaining dental zirconia ceramics;

52. Dip-dyeing: the dental zirconia ceramic obtained in step S1 is placed in the dyeing solution, and the dyeing time is 30~60s;

53. The first drying: the dental zirconia ceramic obtained by the step S2 is dried, and the drying time is 30 to 60 min;

54. Coloring: Step S3 to obtain a dental zirconia ceramic for painting, applying the dyeing liquid to the dental zirconia ceramic by spraying, brushing or sponge application;

55. The second drying: the dental zirconia ceramic obtained in the step S4 is dried, and the drying time is 30 to 60 min;

S6.

Sintering: The dental zirconia ceramic obtained in the step S5 is sintered at a sintering temperature of 1400 to 1600 ° C and a sintering enthalpy of 3 to 5 hours to obtain a dental zirconia ceramic.

[Claim 2] The method of dyeing a dental zirconia ceramic according to claim 1, wherein the dyeing liquid is composed of the following raw materials by weight:

Deionized water 800~1000; colorant 3~50; dispersant 0~10; complexing agent 0~7; thixotropic agent 0~10; color indicator 0~0.5; inorganic additive 0~0.5.

[Claim 3] The dyeing method of the dental zirconia ceramic according to claim 1 or 2, wherein the dip dyeing in the step S2 is to shake the dyeing liquid into a container to ensure that the dose completely covers the dental zirconia Ceramics, dental zirconia ceramics are continuously tumbling using plastic pliers during the dip dyeing process, and taken out after 30 to 60 seconds.

[Claim 4] The dyeing method of the dental zirconia ceramic according to claim 2, wherein the coloring agent comprises a colored cation and a colored anion, wherein the colored cation is iron ion, strontium ion, strontium ion Or a combination of two or more of manganese ions; the coloring liquid anion is one or more of chloride ion, nitrate, metavanadate or permanganate The combination.

[Claim 5] The method for dyeing dental zirconia ceramic according to claim 2, wherein the dispersing agent is triethylhexylphosphoric acid, sodium lauryl sulfate, methylpentanol or cellulose derived a combination of one or more of the compounds.

[Claim 6] The method for dyeing dental zirconia ceramic according to claim 2, wherein the complexing agent is a combination of one or more of formic acid, acetic acid, phthalic acid or salicylic acid .

[Claim 7] The method of dyeing a dental zirconia ceramic according to claim 2, wherein the inorganic additive is a combination of one or more of soluble salts of cerium, lanthanum, cerium or lanthanum.

[Claim 8] The method for dyeing dental zirconia ceramic according to claim 2, wherein the color indicator is one of methyl violet, malachite green, Congo red or bromocresol green sodium. Or a combination of multiples.

[Claim 9] The method for dyeing dental zirconia ceramic according to claim 2, wherein the thixotropic agent is a hydroxyethyl cellulose derivative, a polyvinyl alcohol, a polyacrylate or a hydrogenated castor oil. One or more combinations.