CN110467459B - High-precision dyeing method for zirconia ceramic block - Google Patents

High-precision dyeing method for zirconia ceramic block Download PDF

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CN110467459B
CN110467459B CN201910840288.6A CN201910840288A CN110467459B CN 110467459 B CN110467459 B CN 110467459B CN 201910840288 A CN201910840288 A CN 201910840288A CN 110467459 B CN110467459 B CN 110467459B
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zirconia
dyeing
zirconia ceramic
different
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CN110467459A (en
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唐洁
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Hunan Pengdeng Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5076Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with masses bonded by inorganic cements
    • C04B41/5089Silica sols, alkyl, ammonium or alkali metal silicate cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials

Abstract

The invention discloses a high-precision dyeing method of zirconia ceramic blocks, which comprises the following steps of firstly, selecting zirconia powder; secondly, adding promoter raw materials with different concentrations into each part of zirconia powder; thirdly, pressing and molding the zirconia powder with different marks in different layers; fourthly, blending a coloring agent, and mixing the raw materials; fifthly, putting the zirconia ceramic block obtained in the third step into the coloring agent prepared in the fourth step; and sixthly, taking out the zirconia ceramic blocks in the dyeing liquid obtained in the fifth step, and burning again to form the zirconia ceramic blocks with different required color gradients. In the dyeing process, the sintered block is dissolved in water to form a pasty colloid which is adsorbed on zirconia, so that the combination of the zirconia and a dyeing agent can be promoted, and when a zirconia ceramic block is processed, the promoter water glass forms gradient transformation with different concentrations, and the zirconia of different layers can absorb different dyeing agents with different absorption effects, so that uniform color change can be presented in sufficient time.

Description

High-precision dyeing method for zirconia ceramic block
Technical Field
The invention relates to the technical field of zirconia ceramic blocks, in particular to a high-precision dyeing method of zirconia ceramic blocks.
Background
Currently, in prosthodontics, color and light transmission are important indicators that affect the objectivity of restorations and teeth. The dental CAD/CAM technology is used for manufacturing the all-ceramic restoration, and a new way is opened up for the automatic processing of the restoration and the manufacturing of the high-strength all-ceramic crown bridge. The uncolored zirconia ceramic block is mostly white to ivory in color, and although the uncolored zirconia ceramic block can simulate the color of natural teeth to a certain extent, the uncolored zirconia ceramic block cannot meet the requirement of clinical restoration body color. Only when the zirconium oxide is colored, the color and the light transmittance of the zirconium oxide are adjusted to be close to those of the teeth to be restored, and the requirements of customers can be met. The existing coloring technology of zirconia ceramic blocks mainly comprises an internal dyeing method and an external dyeing method, wherein the internal dyeing method is to directly and uniformly add coloring oxides into powder, and the external dyeing method is to permeate dyeing liquid containing coloring matters into a dental pre-sintered blank body through soaking, brushing and the like, dry and sinter the blank body to form the dental pre-sintered blank body.
At present, colored full-ceramic zirconia materials are also used for tooth restoration to replace the traditional method of using color-shading ceramics, and the coloring method comprises two methods of endogenous coloring and exogenous coloring. The internal dyeing method is characterized in that colored rare earth metal oxide is mixed in powder, and the method can play a role in enabling the tooth coping to have color. The extrinsic dyeing is to soak the ceramic presintered body in a dyeing solution for 1-30min, dry and sinter to form. Although the two methods are fast and easy to operate, the two methods have more influencing factors and are easy to cause uneven dyeing, and after dyeing, denture processing procedures such as porcelain glazing and the like are still needed, so that the possibility of denture porcelain collapse still exists, and finally the application of the product fails.
For example, as disclosed in CN203749621U, a zirconia ceramic block with gradation change in color is obtained by a technique of making blanks from multiple layers of materials with different colors, but the color change is harsh and inconsistent; theoretically, as long as the number of layers is increased, the color change tends to be more natural and uniform, but from the aspect of a forming process, the number of layers cannot be increased too much, and the processing difficulty and the cost are increased. Other technical schemes propose a process of dip dyeing a dyeing solution and then sintering. However, the dip dyeing process can cause the change of some physical and chemical characteristics of the ceramic block blank, and the physical properties such as the strength of the finished ceramic block are affected. Therefore, the technical problem of manufacturing the zirconia ceramic block with uniform gradient color still cannot be reliably solved in the prior art.
Disclosure of Invention
The invention aims to provide a high-precision dyeing method for zirconia ceramic blocks, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a high-precision dyeing method of zirconia ceramic blocks comprises the following specific steps:
firstly, selecting zirconium oxide powder, and evenly dividing the zirconium oxide powder into different equal parts;
secondly, adding promoter raw materials with different concentrations into each part of zirconia powder, and marking for later use;
thirdly, pressing and molding the zirconia powder with different marks in different layers to form zirconia cakes, and sintering the cakes to form preliminary zirconia ceramic blocks;
fourthly, blending the coloring agent, mixing the raw materials, and fully and uniformly stirring to form the coloring agent;
fifthly, putting the zirconia ceramic block in the third step into the staining agent prepared in the fourth step, and fully placing the zirconia ceramic block to fully absorb the staining solution;
and sixthly, taking out the zirconia ceramic blocks in the dyeing liquid obtained in the fifth step, and burning again to form the zirconia ceramic blocks with different required color gradients.
Further, the coloring agent comprises the following components in percentage by weight:
5000 parts of deionized water;
10-50 parts of nitrate;
1-10 parts of hydrochloride;
preferably, the nitrate is composed of erbium nitrate and praseodymium nitrate, wherein the weight part of erbium nitrate is 5-30 parts, and the weight part of praseodymium nitrate is 1-20 parts.
Preferably, the hydrochloride is ferric chloride.
Furthermore, the accelerator mainly comprises water glass, and the effective component of the water glass is HSiO3 And H2SiO3The water glass is easily adsorbed on the surface of zirconia to form a hydrophilic film, and the hydrophilicity of the zirconia surface is increased and promoted.
Preferably, the water glass is formed by heating and melting quartz sand and sodium carbonate to form water glass sinter blocks, and the sinter blocks are dissolved in water to form a pasty colloid.
Compared with the prior art, the invention has the beneficial effects that: the invention discloses a high-precision dyeing method of a zirconia ceramic block, which is compared with the prior art and mainly characterized in that promoter water glass is added in the zirconia ceramic block, the water glass is a water glass sintered block formed by heating and melting quartz sand and sodium carbonate, the sintered block is dissolved in water to form a pasty colloid in the dyeing process, the pasty colloid is adsorbed on zirconia to promote the combination of the zirconia and a dyeing agent, and when the zirconia ceramic block is processed, the promoter water glass forms gradient transformation with different concentrations, so that the zirconia at different levels can absorb different dyeing agents and have different absorption effects, and uniform color change can be presented in sufficient time.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention provides a high-precision dyeing method of a zirconia ceramic block, which comprises the following specific steps:
firstly, selecting zirconium oxide powder, and evenly dividing the zirconium oxide powder into different equal parts;
secondly, adding promoter raw materials with different concentrations into each part of zirconia powder, and marking for later use;
thirdly, pressing and molding the zirconia powder with different marks in different layers to form zirconia cakes, and sintering the cakes to form preliminary zirconia ceramic blocks;
fourthly, blending the coloring agent, mixing the raw materials, and fully and uniformly stirring to form the coloring agent;
fifthly, putting the zirconia ceramic block in the third step into the staining agent prepared in the fourth step, and fully placing the zirconia ceramic block to fully absorb the staining solution;
and sixthly, taking out the zirconia ceramic blocks in the dyeing liquid obtained in the fifth step, and burning again to form the zirconia ceramic blocks with different required color gradients.
Further, the coloring agent comprises the following components in percentage by weight:
5000 parts of deionized water;
45 parts of nitrate;
8 parts of hydrochloride;
preferably, the nitrate is composed of erbium nitrate and praseodymium nitrate, wherein the weight part of erbium nitrate is 5-30 parts, and the weight part of praseodymium nitrate is 10 parts.
Preferably, the hydrochloride is ferric chloride.
Furthermore, the accelerator mainly comprises water glass, and the effective component of the water glass is HSiO3 And H2SiO3The water glass is easily adsorbed on the surface of zirconia to form a hydrophilic film, and the hydrophilicity of the zirconia surface is increased and promoted.
Preferably, the water glass is formed by heating and melting quartz sand and sodium carbonate to form water glass sinter blocks, and the sinter blocks are dissolved in water to form a pasty colloid.
Example 2
The invention provides a high-precision dyeing method of a zirconia ceramic block, which comprises the following specific steps:
firstly, selecting zirconium oxide powder, and evenly dividing the zirconium oxide powder into different equal parts;
secondly, adding promoter raw materials with different concentrations into each part of zirconia powder, and marking for later use;
thirdly, pressing and molding the zirconia powder with different marks in different layers to form zirconia cakes, and sintering the cakes to form preliminary zirconia ceramic blocks;
fourthly, blending the coloring agent, mixing the raw materials, and fully and uniformly stirring to form the coloring agent;
fifthly, putting the zirconia ceramic block in the third step into the staining agent prepared in the fourth step, and fully placing the zirconia ceramic block to fully absorb the staining solution;
and sixthly, taking out the zirconia ceramic blocks in the dyeing liquid obtained in the fifth step, and burning again to form the zirconia ceramic blocks with different required color gradients.
Further, the coloring agent comprises the following components in percentage by weight:
5000 parts of deionized water;
35 parts of nitrate;
9 parts of hydrochloride;
preferably, the nitrate is composed of erbium nitrate and praseodymium nitrate, wherein the weight part of erbium nitrate is 5-30 parts, and the weight part of praseodymium nitrate is 15 parts.
Preferably, the hydrochloride is ferric chloride.
Further, the accelerator is mainlyThe component is water glass, and the effective component of the water glass is HSiO3 And H2SiO3The water glass is easily adsorbed on the surface of zirconia to form a hydrophilic film, and the hydrophilicity of the zirconia surface is increased and promoted.
Preferably, the water glass is formed by heating and melting quartz sand and sodium carbonate to form water glass sinter blocks, and the sinter blocks are dissolved in water to form a pasty colloid.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. A high-precision dyeing method of zirconia ceramic blocks is characterized by comprising the following specific steps:
firstly, selecting zirconium oxide powder, and evenly dividing the zirconium oxide powder into different equal parts;
secondly, adding promoter raw materials with different concentrations into each part of zirconia powder, and marking for later use, wherein the promoter mainly comprises water glass, and the water glass is easily adsorbed on the surface of the zirconia to form a hydrophilic film so as to increase the hydrophilicity of the surface of the zirconia and promote the surface of the zirconia;
thirdly, pressing and molding the zirconia powder with different marks in different layers to form zirconia cakes, and sintering the cakes to form preliminary zirconia ceramic blocks;
fourthly, blending the coloring agent, mixing the raw materials, and fully and uniformly stirring to form the coloring agent;
fifthly, putting the zirconia ceramic block in the third step into the staining agent prepared in the fourth step, and fully placing the zirconia ceramic block to fully absorb the staining solution;
and sixthly, taking out the zirconia ceramic blocks in the dyeing liquid obtained in the fifth step, and burning again to form the zirconia ceramic blocks with different required color gradients.
2. The method for dyeing zirconia ceramic blocks with high precision as claimed in claim 1, wherein the dyeing agent is composed of the following components by weight percent:
5000 parts of deionized water;
10-50 parts of nitrate;
1-10 parts of hydrochloride.
3. A high-precision dyeing method for zirconia ceramic blocks as claimed in claim 2, characterized in that said nitrate is composed of 5-30 parts of erbium nitrate and 1-20 parts of praseodymium nitrate.
4. A method for dyeing zirconia porcelain piece with high precision according to claim 2 wherein said hydrochloride is ferric chloride.
5. A method for dyeing zirconia porcelain piece with high precision according to claim 4 wherein said water glass is a sintered water glass block formed by heating and melting quartz sand and sodium carbonate, and the sintered block is dissolved in water to form a paste colloid.
CN201910840288.6A 2019-09-06 2019-09-06 High-precision dyeing method for zirconia ceramic block Active CN110467459B (en)

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CN115707672A (en) * 2022-10-28 2023-02-21 湖南鹏登精密陶瓷有限公司 Method for preparing 3D gradient-color zirconia denture ceramic blank

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102285795A (en) * 2011-05-30 2011-12-21 北京大学口腔医学院 Dental compound-color cuttable zirconia ceramic and preparation method thereof
CN105367130A (en) * 2015-12-09 2016-03-02 秦皇岛泽克尼陶瓷科技有限公司 Gradient dyeing process of zirconia denture

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CN104909745B (en) * 2015-06-23 2017-03-22 成都贝施美生物科技有限公司 Preparation method for uniform gradient-colour zirconium oxide porcelain blocks
WO2018049331A1 (en) * 2016-09-09 2018-03-15 Jensen Industries Inc. Zirconia blank having a color gradient and methods of making same
CN107175747B (en) * 2017-05-12 2020-04-07 爱迪特(秦皇岛)科技股份有限公司 Dental zirconia repair material with uniform transition of strength and color and preparation method thereof

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102285795A (en) * 2011-05-30 2011-12-21 北京大学口腔医学院 Dental compound-color cuttable zirconia ceramic and preparation method thereof
CN105367130A (en) * 2015-12-09 2016-03-02 秦皇岛泽克尼陶瓷科技有限公司 Gradient dyeing process of zirconia denture

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