CN111732449B - Coloring agent and coloring method for three-dimensional coloring of zirconia ceramic dental crown - Google Patents
Coloring agent and coloring method for three-dimensional coloring of zirconia ceramic dental crown Download PDFInfo
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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- C04B41/5025—Coating 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 ceramic materials
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Abstract
The invention belongs to the technical field of ceramic teeth, and particularly relates to a coloring agent and a coloring method for three-dimensional coloring of a zirconia ceramic dental crown. The coloring agent comprises the following components in parts by weight: 1000 parts of water, 30-60 parts of polyethylene glycol, 100-200 parts of glycerin, 20-100 parts of zirconium oxide, 20-100 parts of erbium oxide, 5-100 parts of nitrate and 1-6 parts of indicator; the dyeing method comprises the steps of preparing a dyeing agent, primarily spraying the zirconia ceramic dental crown, carrying out contrast spraying on the zirconia ceramic dental crown and finishing dyeing on the zirconia ceramic dental crown. The coloring agent can directly dye the zirconia ceramic crown, and has good permeability and surface glossiness; the dyeing method can shorten the processing time of the zirconia ceramic dental crown, reduce the manufacturing cost, and has high simulation degree and good performance of the zirconia prosthesis.
Description
Technical Field
The invention belongs to the technical field of ceramic teeth, and particularly relates to a coloring agent and a coloring method for three-dimensional coloring of a zirconia ceramic dental crown.
Background
Orthodontic refers to the treatment process of irregular tooth arrangement, abnormal tooth morphology and abnormal tooth color and luster by means of oral technique. The existing orthodontic treatment is to satisfy the aesthetic demand and maintain the complete structure of the tooth tissue to the maximum extent at the same time in principle, and the porcelain veneer is a treatment means for orthodontics. The all-ceramic prosthesis has excellent aesthetic effect and mechanical property, and is favored by doctors and patients, wherein the zirconia ceramic has outstanding mechanical property and is more concerned; however, because the color of the base porcelain is chalk and the light transmission is poor, the base porcelain is required to be decorated or dyed, and because the thickness of the tooth is limited, when the base porcelain has a certain thickness, the facing porcelain attached to the surface can be influenced by the base porcelain, so that the color of the final all-porcelain restoration body is influenced.
In the prior art, a pre-formed colorant is usually adopted, a colorant such as rare earth oxide, transition metal oxide and the like is added into zirconia powder, and the zirconia powder is sintered in advance and then cut to present a final color. The ceramic dental crown processed by the pre-sintering method needs to be cut by a machine to be changed into a shape meeting the requirement; however, the method needs a plurality of cutting and polishing procedures, internal stress and tip cracks exist in the teeth easily due to improper operation, the strength of the prosthesis is affected, and high stress generated in the chewing process cannot be borne; cutting is a means of rough machining and has poor precision.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects, the invention provides the coloring agent and the coloring method for the three-dimensional coloring of the zirconia ceramic dental crown, the coloring agent can directly dye the zirconia ceramic dental crown, and the coloring agent has good permeability and good surface glossiness; the dyeing method can shorten the processing time of the zirconia ceramic dental crown, reduce the manufacturing cost, and has high simulation degree and good performance of the zirconia prosthesis.
The technical scheme adopted by the invention for solving the technical problems is as follows: the three-dimensional dyeing dye for the zirconia ceramic dental crown comprises the following components in parts by weight: comprises 1000 parts of water, 30-60 parts of polyethylene glycol, 100 parts of glycerin, 200 parts of zirconium oxide, 20-100 parts of erbium oxide, 5-100 parts of nitrate and 1-6 parts of indicator.
Further, the nitrate is one or more of erbium nitrate, ferric nitrate and zinc nitrate.
Further, the nitrate is erbium nitrate, ferric nitrate and zinc nitrate according to a mass ratio of 1: (0.5-2): (0.2-0.6).
A dyeing method for three-dimensional dyeing of zirconia ceramic dental crowns comprises the following steps:
s1, preparation of a coloring agent: taking water as a solvent, sequentially adding zirconium oxide, erbium oxide and nitrate into the water, stirring until no particles exist, continuously adding polyethylene glycol, glycerol and an indicator, and continuously stirring until the particles are completely dissolved to obtain a zirconium oxide ceramic dental crown three-dimensional dyeing agent;
s2, primary spraying of the zirconia ceramic crown: fixing the cut zirconia ceramic dental crown on a dyeing machine base, placing a coloring agent in a spray head of the dyeing machine, rotating the dyeing machine base at a rotation rate of 500 plus 5000r/min, wherein the spray head of the dyeing machine is a vertically arranged rectangular hole, the spray head moves up and down in the vertical direction, the distance from a moving lower base surface to the lower surface of the zirconia ceramic dental crown is 1/3-2/3 of the height of the zirconia ceramic dental crown, the distance from a moving upper base surface to the upper surface of the zirconia ceramic dental crown is 1/3-2/3 of the height of the zirconia ceramic dental crown, the movement period is 2-3s, and the spraying time is 4-10 s; baking the sprayed zirconia ceramic dental crown for 2-10min by using an infrared lamp to finish primary spraying of a coloring agent;
s3, comparison spray of the zirconia ceramic crown: after the primary spray baking is finished, stopping the base station of the dyeing machine from rotating, collecting and monitoring the surface color of the zirconia ceramic crown subjected to primary spray by adopting a color online monitoring device arranged on the side wall of the dyeing machine, and comparing the surface color with the painting color preset in a control system of the dyeing machine; if the color difference exists, the dyeing machine control system controls a color compensation gun head of the dyeing machine filled with the dyeing agent to perform supplementary spraying of the dyeing agent on a region needing color difference compensation, the supplementary spraying time is 1.5s-3s, and infrared ray baking is adopted for 1min-2 min; repeating the operation until the color is consistent with the color preset by the color online monitoring device;
s4, dyeing the zirconia ceramic crown: and placing the zirconia ceramic crown sprayed with the coloring agent in a microwave sintering furnace, wherein the sintering temperature is 1430-1500 ℃, and the sintering time is 0.5-2h, so as to finish the dyeing.
Further, the sintering vacuum degree in the microwave sintering furnace is 0.2-200 Pa.
Further, the microwave sintering furnace reaches the preset sintering temperature from room temperature, the temperature rise gradient is 400 ℃/min, and when the temperature reaches 1300 ℃ of 1200-.
The beneficial effects of the invention are:
1. the coloring agent is prepared from water, polyethylene glycol, glycerol, zirconia, erbium oxide, nitrate and an indicator, and the coloring agent can be better permeated into the zirconia ceramic crown by selecting the polyethylene glycol and the glycerol; the coloring agent contains a small amount of zirconia, when the coloring agent is used as a dental crown veneer, because the zirconia is the same as the zirconia dental crown crystal, the chemical connecting bond directly exists on the dental crown veneer attached on the dental crown, and the bonding strength between the coloring agent and the zirconia ceramic dental crown is high under the condition of not additionally using a bonding agent, the coloring layer is added on the surface of the dental crown, the strength of the tooth cannot be influenced when the tooth is shaped by water grinding and finish processing, the color adjustment is flexible, and the waste of the whole tooth cannot be caused because the color does not meet the requirement; when the dental crown directly permeates the zirconia for dyeing, the zirconia exists in the dyeing agent, so that the dental crown can permeate into pore canals of the original dental crown, the internal density of the tooth is increased, and the stress strength of the dyed tooth is improved; erbium oxide and nitrate are selected as coloring agents, so that the permeability and the optical effect of the zirconia ceramic crown are not influenced, and the coloring is uniform and lasting; the selected indicator does not influence the color development effect of the nitrate coloring agent and the glossiness of the surface of the zirconia ceramic dental crown, and the coloring process is controllable; the components of the coloring agent are synergistic, the coloring effect is good, the color is stable and durable, the bonding property of the coloring agent and a zirconia ceramic matrix is strong, and the coloring agent is not easy to fall off; the coloring agent is nontoxic, and can reduce the potential safety hazard of patients in oral cavity.
2. The spray dyeing method is adopted, so that the dyeing time is reduced, the dyeing uniformity is high, and the thickness is consistent; the dyed ceramics are detected by synchronously adopting a color online monitoring device, so that the simulation degree is high; the dyed zirconia ceramic dental crown is sintered by microwave, the heating speed is high, the growth of grain tissues can be inhibited, the density of the modified surface of the zirconia ceramic dental crown is improved, or the modified surface permeates into the dental crown with a pore passage to improve the density of the whole dental crown, and the formed zirconia ceramic dental crown has high strength and long service life; the dyed zirconia ceramic tooth does not need to be cut, and only needs to be polished by a water mill, so that cracks are prevented from appearing in the zirconia ceramic tooth crown, and the quality of the zirconia ceramic tooth is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
The three-dimensional dyeing dye for the zirconia ceramic dental crown comprises the following components in parts by weight: the indicator comprises 1000 parts of water, 30 parts of polyethylene glycol, 100 parts of glycerol, 25 parts of zirconia, 30 parts of erbium oxide, 20 parts of nitrate and 1 part of indicator; the nitrate is one or more of erbium nitrate, ferric nitrate and zinc nitrate; specifically, the nitrate is erbium nitrate, ferric nitrate and zinc nitrate according to a mass ratio of 1: 1: 0.2 mixing.
A dyeing method for three-dimensional dyeing of zirconia ceramic dental crowns comprises the following steps:
s1, preparation of a coloring agent: taking water as a solvent, sequentially adding zirconium oxide, erbium oxide and nitrate into the water, stirring until no particles exist, continuously adding polyethylene glycol, glycerol and an indicator, and continuously stirring until the particles are completely dissolved to obtain a staining agent for three-dimensional staining of the zirconia ceramic crown;
s2, primary spraying of the zirconia ceramic crown: fixing the cut zirconia ceramic crown on a dyeing machine base, placing a coloring agent into a spraying head of the dyeing machine, rotating the dyeing machine base, wherein the rotating speed is 800r/min, the spraying head of the dyeing machine is a vertically arranged rectangular hole, the spraying head vertically moves up and down, the distance from a moving lower base surface to the lower surface of the zirconia ceramic crown is 1/2 of the height of the zirconia ceramic crown, the distance from a moving upper base surface to the upper surface of the zirconia ceramic crown is 1/2 of the height of the zirconia ceramic crown, the moving period is 2s, and the spraying time is 8 s; baking the sprayed zirconia ceramic dental crown for 8min by using an infrared lamp to finish primary spraying of a coloring agent;
s3, comparison spray of the zirconia ceramic crown: after the primary spray baking is finished, stopping the base station of the dyeing machine from rotating, collecting and monitoring the surface color of the zirconia ceramic crown subjected to primary spray by adopting a color online monitoring device arranged on the side wall of the dyeing machine, and comparing the surface color with the painting color preset in a control system of the dyeing machine; if the color difference exists, the dyeing machine control system controls a color compensation gun head of the dyeing machine filled with the dyeing agent to perform supplementary spraying of the dyeing agent on a region needing color difference compensation, the supplementary spraying time is 2s, and infrared baking is adopted for 2 min; repeating the operation until the color is consistent with the color preset by the color online monitoring device;
s4, completing staining of the zirconia ceramic crown: placing the zirconia ceramic crown sprayed with the coloring agent in a microwave sintering furnace, wherein the sintering vacuum degree in the microwave sintering furnace is 0.2-200Pa, the sintering temperature is 1430-1500 ℃, the temperature of the microwave sintering furnace reaches the preset sintering temperature from room temperature, the temperature rise gradient is 300 ℃/min, and when the temperature reaches 1200-1300 ℃, the temperature rise gradient is 60 ℃/min; the sintering time was 1.8h, and dyeing was completed.
Example 2
The three-dimensional dyeing dye for the zirconia ceramic dental crown comprises the following components in parts by weight: the indicator comprises 1000 parts of water, 50 parts of polyethylene glycol, 150 parts of glycerol, 80 parts of zirconia, 60 parts of erbium oxide, 100 parts of nitrate and 6 parts of indicator; the nitrate is one or more of erbium nitrate, ferric nitrate and zinc nitrate; specifically, the nitrate is erbium nitrate, ferric nitrate and zinc nitrate according to a mass ratio of 1: 0.5: 0.6 mixing.
A dyeing method for three-dimensional dyeing of zirconia ceramic dental crowns comprises the following steps:
s1, preparation of a coloring agent: taking water as a solvent, sequentially adding zirconium oxide, erbium oxide and nitrate into the water, stirring until no particles exist, continuously adding polyethylene glycol, glycerol and an indicator, and continuously stirring until the particles are completely dissolved to obtain a staining agent for three-dimensional staining of the zirconia ceramic crown;
s2, primary spraying of the zirconia ceramic crown: fixing the cut zirconia ceramic crown on a dyeing machine base, placing a coloring agent into a spray head of the dyeing machine, rotating the dyeing machine base, wherein the rotation rate is 2000r/min, the spray head of the dyeing machine is a vertically arranged rectangular hole, the spray head moves up and down in the vertical direction, the distance from a moving lower base surface to the lower surface of the zirconia ceramic crown is 1/2 of the height of the zirconia ceramic crown, the distance from a moving upper base surface to the upper surface of the zirconia ceramic crown is 1/2 of the height of the zirconia ceramic crown, the movement period is 3s, and the spraying time is 6 s; baking the sprayed zirconia ceramic dental crown for 8min by using an infrared lamp to finish primary spraying of a coloring agent;
s3, comparison spray of the zirconia ceramic crown: after the primary spray baking is finished, stopping the base station of the dyeing machine from rotating, collecting and monitoring the surface color of the zirconia ceramic crown subjected to primary spray by adopting a color online monitoring device arranged on the side wall of the dyeing machine, and comparing the surface color with the painting color preset in a control system of the dyeing machine; if the color difference exists, the dyeing machine control system controls a color compensation gun head of the dyeing machine filled with the dyeing agent to perform supplementary spraying of the dyeing agent on a region needing color difference compensation, the supplementary spraying time is 2s, and infrared ray baking is adopted for 2 min; repeating the operation until the color is consistent with the color preset by the color online monitoring device;
s4, dyeing the zirconia ceramic crown: placing the zirconia ceramic crown sprayed with the coloring agent in a microwave sintering furnace, wherein the sintering vacuum degree in the microwave sintering furnace is 200Pa for 100-year and the sintering temperature is 1430-1500 ℃, the temperature of the microwave sintering furnace reaches the preset sintering temperature from room temperature, the temperature rise gradient is 400 ℃/min, and when the temperature reaches 1300 ℃ for 1200-year, the temperature rise gradient is 100 ℃/min; the sintering time is 0.8h, and dyeing is completed.
Example 3
The three-dimensional dyeing dye for the zirconia ceramic dental crown comprises the following components in parts by weight: the indicator comprises 1000 parts of water, 60 parts of polyethylene glycol, 200 parts of glycerol, 80 parts of zirconia, 100 parts of erbium oxide, 90 parts of nitrate and 5 parts of indicator; the nitrate is one or more of erbium nitrate, ferric nitrate and zinc nitrate; specifically, the nitrate is erbium nitrate, ferric nitrate and zinc nitrate according to a mass ratio of 1: 2: 0.2 mixing.
A dyeing method for three-dimensional dyeing of zirconia ceramic dental crowns comprises the following steps:
s1, preparation of a coloring agent: taking water as a solvent, sequentially adding zirconium oxide, erbium oxide and nitrate into the water, stirring until no particles exist, continuously adding polyethylene glycol, glycerol and an indicator, and continuously stirring until the particles are completely dissolved to obtain a zirconium oxide ceramic dental crown three-dimensional dyeing agent;
s2, primary spraying of the zirconia ceramic crown: fixing the cut zirconia ceramic crown on a dyeing machine base, placing a coloring agent in a spraying head of the dyeing machine, rotating the dyeing machine base at a rotation speed of 4000r/min, wherein the spraying head of the dyeing machine is a vertically arranged rectangular hole, the spraying head vertically moves up and down, the distance from a moving lower base surface to the lower surface of the zirconia ceramic crown is 2/3 of the height of the zirconia ceramic crown, the distance from a moving upper base surface to the upper surface of the zirconia ceramic crown is 2/3 of the height of the zirconia ceramic crown, the movement period is 2s, and the spraying time is 4 s; baking the sprayed zirconia ceramic dental crown for 5min by using an infrared lamp to finish primary spraying of a coloring agent;
s3, comparison spray of the zirconia ceramic crown: after the primary spray baking is finished, stopping the base station of the dyeing machine from rotating, collecting and monitoring the surface color of the zirconia ceramic crown subjected to primary spray by adopting a color online monitoring device arranged on the side wall of the dyeing machine, and comparing the surface color with the painting color preset in a control system of the dyeing machine; if the color difference exists, the dyeing machine control system controls a color compensation gun head of the dyeing machine filled with the dyeing agent to perform supplementary spraying of the dyeing agent on a region needing color difference compensation, the supplementary spraying time is 1.5s, and infrared ray baking is adopted for 1 min; repeating the operation until the color is consistent with the color preset by the color online monitoring device;
s4, placing the dyed zirconia ceramic crown in a microwave sintering furnace, wherein the sintering vacuum degree in the microwave sintering furnace is 0.2-50Pa, the sintering temperature is 1430-1500 ℃, the temperature of the microwave sintering furnace reaches the preset sintering temperature from room temperature, the temperature rise gradient is 350 ℃/min, and when the temperature reaches 1200-1300 ℃, the temperature rise gradient is 90 ℃/min; the sintering time is 0.5h, and dyeing is finished.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (2)
1. The three-dimensional dyeing dye for the zirconia ceramic dental crown is characterized by comprising the following components in parts by weight: comprises 1000 parts of water, 30-60 parts of polyethylene glycol, 100 parts of glycerol, 200 parts of-;
the nitrate is erbium nitrate, ferric nitrate and zinc nitrate according to a mass ratio of 1: (0.5-2): (0.2-0.6) mixing;
the indicator is one or more of methyl violet, methyl yellow, methyl red, litmus, indigo carmine or anthocyanin.
2. A dyeing method for three-dimensional dyeing of zirconia ceramic dental crowns is characterized by comprising the following steps,
s1, preparation of a coloring agent: taking water as a solvent, sequentially adding zirconium oxide, erbium oxide and nitrate into the water, stirring until no particles exist, continuously adding polyethylene glycol, glycerol and an indicator, and continuously stirring until the particles are completely dissolved to obtain a zirconium oxide ceramic dental crown three-dimensional dyeing agent;
s2, primary spraying of the zirconia ceramic crown: fixing the cut zirconia ceramic crown on a dyeing machine base, placing a dyeing agent in a spray head of the dyeing machine, rotating the dyeing machine base with the rotation rate of 500-5000r/min, vertically moving the spray head of the dyeing machine in the vertical direction, wherein the distance between a lower moving base surface and the lower surface of the zirconia ceramic crown is 1/3-2/3 of the height of the zirconia ceramic crown, the distance between an upper moving base surface and the upper surface of the zirconia ceramic crown is 1/3-2/3 of the height of the zirconia ceramic crown, the movement period is 2-3s, and the spraying time is 4-10 s; baking the sprayed zirconia ceramic dental crown for 2-10min by adopting an infrared lamp to finish the primary spraying of the coloring agent;
s3, comparison spray of the zirconia ceramic crown: after the primary spray baking is finished, stopping the base station of the dyeing machine from rotating, collecting and monitoring the surface color of the zirconia ceramic crown subjected to primary spray by adopting a color online monitoring device arranged on the side wall of the dyeing machine, and comparing the surface color with the painting color preset in a control system of the dyeing machine; if the color difference exists, the dyeing machine control system controls a color compensation gun head of the dyeing machine filled with the dyeing agent to perform supplementary spraying of the dyeing agent on a region needing color difference compensation, the supplementary spraying time is 1.5s-3s, and infrared ray baking is adopted for 1min-2 min; repeating the operation until the color is consistent with the color preset by the color online monitoring device;
s4, dyeing the zirconia ceramic crown: placing the zirconia ceramic crown sprayed with the coloring agent in a microwave sintering furnace, wherein the sintering temperature is 1430-1500 ℃, the sintering time is 0.5-2h, and the dyeing is finished, and the sintering vacuum degree in the microwave sintering furnace is 0.2-200 Pa; the microwave sintering furnace reaches the preset sintering temperature from room temperature, the temperature rise gradient is 400 ℃/min at 200-.
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| CN102499899A (en) * | 2011-10-25 | 2012-06-20 | 辽宁爱尔创生物材料有限公司 | Method for processing surface of zirconium oxide ceramic implant |
| CN103431918B (en) * | 2013-08-27 | 2016-05-11 | 东南大学 | The new method of its adhesive property is processed and improved to dental zirconium oxide base ceramic surface |
| 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 |
| CN105924228A (en) * | 2016-04-29 | 2016-09-07 | 成都贝施美生物科技有限公司 | Dyeing method for dental zirconia ceramic |
| CN107686379A (en) * | 2017-07-25 | 2018-02-13 | 歌尔股份有限公司 | The preparation method of zirconia ceramics with porous layer |
| CN109734444A (en) * | 2019-03-07 | 2019-05-10 | 珠海新茂义齿科技有限公司 | A kind of zirconium oxide immersion coloration and dyeing method |
| CN110655418A (en) * | 2019-10-25 | 2020-01-07 | 上海饶稷陶瓷材料有限公司 | High-strength zirconia ceramic dyeing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1807358A (en) * | 2006-01-24 | 2006-07-26 | 陈云 | Ceramic colorful sand and its preparation process |
| WO2013170705A1 (en) * | 2012-05-15 | 2013-11-21 | Shenzhen Upcera Co., Ltd | Coloring solution for dental zirconia ceramics and method for using the same |
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