CN109734444A - A kind of zirconium oxide immersion coloration and dyeing method - Google Patents
A kind of zirconium oxide immersion coloration and dyeing method Download PDFInfo
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- CN109734444A CN109734444A CN201910170929.1A CN201910170929A CN109734444A CN 109734444 A CN109734444 A CN 109734444A CN 201910170929 A CN201910170929 A CN 201910170929A CN 109734444 A CN109734444 A CN 109734444A
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Abstract
The invention discloses a kind of zirconium oxides to impregnate coloration and dyeing method, is related to Dental Erosion technical field.The following steps are included: nano zirconium dioxide, erbium oxide, cerium oxide, yttrium oxide and iron oxide are carried out raw material mixing, ground in the ball mill, time 10-20min is dried after mixing；Mixed-powder after grinding is dried, temperature is 60-90 DEG C, time 10-20h, and then addition polymeric adhesive makes mixed-powder blocking, is pre-sintered to the mixture after blocking, and temperature is 1200-1500 DEG C, time 2-3h；Zirconia blend after pre-sintering is crushed, is then added into ball mill and is ground.It is then sintered after being ground to zirconia material, is then crushed, ground again, then powder dyeing is carried out again, so that particulate matter colours, is then sintered and is coloured again again, and static pressure is carried out in idiosome form, final finished product uniform coloring, and stable structure.
Description
Technical field
The present invention relates to Dental Erosion technical field, specially a kind of zirconium oxide impregnates coloration and dyeing method.
Background technique
As the improvement of people's living standards, dental material using increasingly extensive.Currently, zirconium oxide is as a kind of novel
Biomaterial, have that intensity is big, hardness is high, good toughness and the excellent performances such as wear-resistant, while also agreeing have good biology
Compatibility, and it is widely used as dental prosthetic material.More extensive application prospect is just being shown in oral cavity material field.Oxidation
Zircon porcelain block is white, has different with the color and translucency of natural tooth, is not able to satisfy patient for beautiful requirement.For
Guarantee that the simulation quality of color of teeth, traditional method are while to increase the thickness of facing porcelain, but need to increase in this way using color porcelain is hidden
The preparation amount for adding artificial tooth, therefore, need to dye zirconium oxide, and zirconium oxide intrinsic colour and translucency are adjusted to repair with quasi-
The color and light transmittance of tooth are close, are just able to satisfy the demand of client.The dye technology of the artificial tooth of zirconium oxide pre-burning at present mainly has
Powder dyeing and two kinds of liquid dip method, interior dye method is that Direct Uniform adds coloring oxide directly in powder, and outer dye method is
Dentistry is pre-sintered green body and passes through the dyeing liquor of the infiltration such as immersion and brushing object containing coloring.In comparison, interior dye method is convenient and efficient, mesh
It is preceding to be clinically widely applied, but color range of choice is small.
The soaking and dyeing method of zirconium oxide is exactly first to carry out moulding to zirconium oxide at present, is then sintered, is impregnated after
Dyeing, traditional method have a very big defect, such as after the tooth installation of zirconium oxide, in use it is easy to appear
Cracked tooth or block fall the case where being even directly broken, and easy coloring is not allowed in zirconium oxide dyeing at present, so holding very much
Easily there is the different situation of color of teeth, in addition many zirconium oxide teeth will appear uneven color in use for some time
The problem of, so, it would be highly desirable to design a kind of new zirconium oxide color method.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of zirconium oxides to impregnate coloration and dyeing method, and it is fast to have coloring
And uniform intensity it is high the advantages that, solve the problems, such as that current zirconium oxide dyeing effect is poor.
(2) technical solution
To realize that above-mentioned coloring is fast and the uniform high purpose of intensity, the invention provides the following technical scheme: a kind of zirconium oxide
Impregnate coloration and dyeing method, comprising the following steps:
S1, nano zirconium dioxide, erbium oxide, cerium oxide, yttrium oxide and iron oxide are subjected to raw material mixing, in the ball mill
It is ground, time 10-20min is dried after mixing；
S2, the mixed-powder after grinding is dried, temperature is 60-90 DEG C, then high score is added in time 10-20h
Sub- bonding agent makes mixed-powder blocking, is pre-sintered to the mixture after blocking, and temperature is 1200-1500 DEG C, the time
For 2-3h；
S3, the zirconia blend after pre-sintering is crushed, is then added into ball mill and is ground, when
Between be 20-30min, obtain zirconia blend powder；
S4, the zirconia blend powder after grinding is immersed in dyeing liquor, time 20-30min, then will be impregnated
Zirconia blend powder afterwards carries out ultraviolet light drying, and temperature is 60-90 DEG C, time 10-20h；
Be added high polymer binder in S5, zirconia blend after the drying, carry out moulding, using mold dry-pressing at
Type obtains idiosome, and then idiosome is put into high-pressure chamber and carries out static pressure, obtains embryo block；
S6, embryo block is sintered, temperature is 1400-1500 DEG C, and pressure when sintering is 150-200MPa, sintering time
For 3-5h, preliminary zirconium dioxide porcelain block is formed；
S7, to zirconium dioxide porcelain block carry out surface processing, using computer with machine cut process combine by the way of pair
Zirconium dioxide porcelain block is cut and is ground, and then porcelain block is cleared up and dried；
S8, will treated that zirconium dioxide porcelain block is immersed in dyeing liquor carries out soaking and dyeing, time 20-30min；
S9, the zirconium dioxide porcelain block after dyeing is sintered again, obtains finished product.
Advanced optimize the technical program, in the S1, the weight ratio of erbium oxide and cerium oxide is zirconium dioxide
The weight ratio of 0.5-1%, yttrium oxide and iron oxide is the 0.1-2% of zirconium dioxide
Advanced optimize the technical program, in the S2 and S5, polymeric adhesive is the ethylene glycol solution of 2-6wt%.
Advanced optimize the technical program, in the S4 and S8, dyeing liquor is polyethylene glycol 1-5%, erbium oxide 0.1-
3%, the mixture of cobalt oxide 0.5-10% and ultrapure water.
Advanced optimize the technical program, in the S5, the pressure in high-pressure chamber is 100-200MPa.
Advanced optimize the technical program, in the S9, sintering processing is multi-steps sintering, and the temperature of first segment is 1000-
1300 DEG C, sintering time 20-30min, the temperature of second segment is 1300-1600 DEG C, sintering time 2-3h.
(3) beneficial effect
Compared with prior art, the present invention provides a kind of zirconium oxides to impregnate coloration and dyeing method, has following beneficial to effect
Fruit: it is then sintered after being ground to zirconia material, is then crushed, ground again, then carry out powder dye again
Then color is sintered again and colours again, and carry out static pressure in idiosome form so that particulate matter colours, final
Finished product uniform coloring, and stable structure.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment one:
1. a kind of zirconium oxide impregnates coloration and dyeing method, comprising the following steps:
S1, nano zirconium dioxide, erbium oxide, cerium oxide, yttrium oxide and iron oxide are subjected to raw material mixing, in the ball mill
It is ground, time 10min is dried after mixing, and the weight ratio of erbium oxide and cerium oxide is zirconium dioxide
0.5%, the weight ratio of yttrium oxide and iron oxide is the 0.1% of zirconium dioxide；
S2, the mixed-powder after grinding is dried, temperature is 60 DEG C, then polymeric adhesion is added in time 10h
Agent makes mixed-powder blocking, is pre-sintered to the mixture after blocking, and temperature is 1200 DEG C, time 2h, macromolecule
Bonding agent is the ethylene glycol solution of 2wt%；
S3, the zirconia blend after pre-sintering is crushed, is then added into ball mill and is ground, when
Between be 20min, obtain zirconia blend powder；
S4, the zirconia blend powder after grinding is immersed in dyeing liquor, dyeing liquor is polyethylene glycol 1%, oxidation
The mixture of erbium 0.1%, cobalt oxide 0.5% and ultrapure water, time 20min, then by the zirconia blend powder after immersion
End carries out ultraviolet light drying, and temperature is 60 DEG C, time 10h；
High polymer binder is added in S5, zirconia blend after the drying, polymeric adhesive is the second two of 2wt%
Alcoholic solution carries out moulding, dry-pressing formed using mold, obtains idiosome, then idiosome is put into high-pressure chamber and carries out static pressure, high
Pressing the pressure in storehouse is 100MPa, obtains embryo block；
S6, embryo block is sintered, temperature is 1400 DEG C, and pressure when sintering is 150MPa, sintering time 3h, is formed
Preliminary zirconium dioxide porcelain block；
S7, to zirconium dioxide porcelain block carry out surface processing, using computer with machine cut process combine by the way of pair
Zirconium dioxide porcelain block is cut and is ground, and then porcelain block is cleared up and dried；
S8, will treated that zirconium dioxide porcelain block is immersed in dyeing liquor carries out soaking and dyeing, dyeing liquor is polyethylene glycol
1%, the mixture of erbium oxide 0.1%, cobalt oxide 0.5% and ultrapure water, time 20min；
S9, the zirconium dioxide porcelain block after dyeing is sintered again, sintering processing is multi-steps sintering, the temperature of first segment
It is 1000 DEG C, sintering time 20min, the temperature of second segment is 1300 DEG C, and sintering time 2h obtains finished product.
Embodiment two:
1. a kind of zirconium oxide impregnates coloration and dyeing method, comprising the following steps:
S1, nano zirconium dioxide, erbium oxide, cerium oxide, yttrium oxide and iron oxide are subjected to raw material mixing, in the ball mill
It is ground, time 15min is dried after mixing, and the weight ratio of erbium oxide and cerium oxide is zirconium dioxide
0.8%, the weight ratio of yttrium oxide and iron oxide is the 1% of zirconium dioxide；
S2, the mixed-powder after grinding is dried, temperature is 75 DEG C, then polymeric adhesion is added in time 15h
Agent makes mixed-powder blocking, is pre-sintered to the mixture after blocking, and temperature is 1350 DEG C, time 2.5h, high score
Sub- bonding agent is the ethylene glycol solution of 4wt%；
S3, the zirconia blend after pre-sintering is crushed, is then added into ball mill and is ground, when
Between be 25min, obtain zirconia blend powder；
S4, the zirconia blend powder after grinding is immersed in dyeing liquor, dyeing liquor is polyethylene glycol 3%, oxidation
The mixture of erbium 2%, cobalt oxide 5% and ultrapure water, time 25min, then by the zirconia blend powder after immersion into
The drying of row ultraviolet light, temperature are 75 DEG C, time 15h；
High polymer binder is added in S5, zirconia blend after the drying, polymeric adhesive is the second two of 4wt%
Alcoholic solution carries out moulding, dry-pressing formed using mold, obtains idiosome, then idiosome is put into high-pressure chamber and carries out static pressure, high
Pressing the pressure in storehouse is 150MPa, obtains embryo block；
S6, embryo block is sintered, temperature is 1450 DEG C, and pressure when sintering is 170MPa, sintering time 4h, is formed
Preliminary zirconium dioxide porcelain block；
S7, to zirconium dioxide porcelain block carry out surface processing, using computer with machine cut process combine by the way of pair
Zirconium dioxide porcelain block is cut and is ground, and then porcelain block is cleared up and dried；
S8, will treated that zirconium dioxide porcelain block is immersed in dyeing liquor carries out soaking and dyeing, dyeing liquor is polyethylene glycol
3%, the mixture of erbium oxide 2%, cobalt oxide 5% and ultrapure water, time 25min；
S9, the zirconium dioxide porcelain block after dyeing is sintered again, sintering processing is multi-steps sintering, the temperature of first segment
It is 1200 DEG C, sintering time 25min, the temperature of second segment is 1500 DEG C, and sintering time 2.5h obtains finished product.
Embodiment three:
1. a kind of zirconium oxide impregnates coloration and dyeing method, comprising the following steps:
S1, nano zirconium dioxide, erbium oxide, cerium oxide, yttrium oxide and iron oxide are subjected to raw material mixing, in the ball mill
It is ground, time 20min is dried after mixing, and the weight ratio of erbium oxide and cerium oxide is zirconium dioxide
1%, the weight ratio of yttrium oxide and iron oxide is the 2% of zirconium dioxide；
S2, the mixed-powder after grinding is dried, temperature is 90 DEG C, then polymeric adhesion is added in time 20h
Agent makes mixed-powder blocking, is pre-sintered to the mixture after blocking, and temperature is 1500 DEG C, time 3h, macromolecule
Bonding agent is the ethylene glycol solution of 6wt%；
S3, the zirconia blend after pre-sintering is crushed, is then added into ball mill and is ground, when
Between be 30min, obtain zirconia blend powder；
S4, the zirconia blend powder after grinding is immersed in dyeing liquor, dyeing liquor is polyethylene glycol 5%, oxidation
The mixture of erbium 3%, cobalt oxide 10% and ultrapure water, time 30min, then by the zirconia blend powder after immersion into
The drying of row ultraviolet light, temperature are 90 DEG C, time 20h；
High polymer binder is added in S5, zirconia blend after the drying, polymeric adhesive is the second two of 6wt%
Alcoholic solution carries out moulding, dry-pressing formed using mold, obtains idiosome, then idiosome is put into high-pressure chamber and carries out static pressure, high
Pressing the pressure in storehouse is 200MPa, obtains embryo block；
S6, embryo block is sintered, temperature is 1500 DEG C, and pressure when sintering is 200MPa, sintering time 5h, is formed
Preliminary zirconium dioxide porcelain block；
S7, to zirconium dioxide porcelain block carry out surface processing, using computer with machine cut process combine by the way of pair
Zirconium dioxide porcelain block is cut and is ground, and then porcelain block is cleared up and dried；
S8, will treated that zirconium dioxide porcelain block is immersed in dyeing liquor carries out soaking and dyeing, dyeing liquor is polyethylene glycol
5%, the mixture of erbium oxide 3%, cobalt oxide 10% and ultrapure water, time 30min；
S9, the zirconium dioxide porcelain block after dyeing is sintered again, sintering processing is multi-steps sintering, the temperature of first segment
It is 1300 DEG C, sintering time 30min, the temperature of second segment is 1600 DEG C, and sintering time 3h obtains finished product.
The beneficial effects of the present invention are: after being ground to zirconia material then be sintered, then crushed, again into
Row grinding, then carries out powder dyeing again, so that particulate matter colours, is then sintered and colours again again, and in embryo
Static pressure, final finished product uniform coloring, and stable structure are carried out when volume morphing.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of zirconium oxide impregnates coloration and dyeing method, which comprises the following steps:
S1, nano zirconium dioxide, erbium oxide, cerium oxide, yttrium oxide and iron oxide are subjected to raw material mixing, carried out in the ball mill
Grinding, time 10-20min are dried after mixing；
S2, the mixed-powder after grinding is dried, temperature is 60-90 DEG C, time 10-20h, and it is viscous that macromolecule is then added
It connects agent and makes mixed-powder blocking, the mixture after blocking is pre-sintered, temperature is 1200-1500 DEG C, time 2-
3h；
S3, the zirconia blend after pre-sintering is crushed, is then added into ball mill and is ground, the time is
20-30min obtains zirconia blend powder；
S4, the zirconia blend powder after grinding is immersed in dyeing liquor, time 20-30min then will be after immersion
Zirconia blend powder carries out ultraviolet light drying, and temperature is 60-90 DEG C, time 10-20h；
High polymer binder is added in S5, zirconia blend after the drying, carries out moulding, it is dry-pressing formed using mold, it obtains
To idiosome, then idiosome is put into high-pressure chamber and carries out static pressure, obtains embryo block；
S6, embryo block is sintered, temperature is 1400-1500 DEG C, and pressure when sintering is 150-200MPa, sintering time 3-
5h forms preliminary zirconium dioxide porcelain block；
S7, surface processing is carried out to zirconium dioxide porcelain block, to dioxy in such a way that computer is combined with machine cut processing
Change zircon porcelain block to be cut and ground, then porcelain block is cleared up and dried；
S8, will treated that zirconium dioxide porcelain block is immersed in dyeing liquor carries out soaking and dyeing, time 20-30min；
S9, the zirconium dioxide porcelain block after dyeing is sintered again, obtains finished product.
2. a kind of zirconium oxide according to claim 1 impregnates coloration and dyeing method, which is characterized in that in the S1, oxidation
The weight ratio of erbium and cerium oxide is the 0.5-1% of zirconium dioxide, and the weight ratio of yttrium oxide and iron oxide is titanium dioxide
The 0.1-2% of zirconium.
3. a kind of zirconium oxide according to claim 1 impregnates coloration and dyeing method, which is characterized in that in the S2 and S5,
Polymeric adhesive is the ethylene glycol solution of 2-6wt%.
4. a kind of zirconium oxide according to claim 1 impregnates coloration and dyeing method, which is characterized in that in the S4 and S8,
Dyeing liquor is the mixture of polyethylene glycol 1-5%, erbium oxide 0.1-3%, cobalt oxide 0.5-10% and ultrapure water.
5. a kind of zirconium oxide according to claim 1 impregnates coloration and dyeing method, which is characterized in that in the S5, high pressure
Pressure in storehouse is 100-200MPa.
6. a kind of zirconium oxide according to claim 1 impregnates coloration and dyeing method, which is characterized in that in the S9, sintering
Mode is multi-steps sintering, and the temperature of first segment is 1000-1300 DEG C, and the temperature of sintering time 20-30min, second segment are
1300-1600 DEG C, sintering time 2-3h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111732449A (en) * | 2020-06-22 | 2020-10-02 | 嘉兴饶稷科技有限公司 | Coloring agent and coloring method for three-dimensional coloring of zirconia ceramic dental crown |
| CN111807865A (en) * | 2020-07-14 | 2020-10-23 | 嘉兴饶稷科技有限公司 | High-strength and high-hardness ceramic teethridge base station |
| CN115124338A (en) * | 2022-06-27 | 2022-09-30 | 潮州三环（集团）股份有限公司 | Color coating slurry, color zirconia ceramic and preparation method thereof |
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| CN104909745A (en) * | 2015-06-23 | 2015-09-16 | 成都贝施美生物科技有限公司 | Preparation method for uniform gradient-colour zirconium oxide porcelain blocks |
| CN105924162A (en) * | 2016-04-29 | 2016-09-07 | 成都贝施美生物科技有限公司 | Dyeing process for dental zirconia restoration |
| CN106187319A (en) * | 2016-07-27 | 2016-12-07 | 珠海新茂义齿科技有限公司 | A kind of zirconium oxide soaks coloration and dyeing technique |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104909745A (en) * | 2015-06-23 | 2015-09-16 | 成都贝施美生物科技有限公司 | Preparation method for uniform gradient-colour zirconium oxide porcelain blocks |
| CN105924162A (en) * | 2016-04-29 | 2016-09-07 | 成都贝施美生物科技有限公司 | Dyeing process for dental zirconia restoration |
| CN106187319A (en) * | 2016-07-27 | 2016-12-07 | 珠海新茂义齿科技有限公司 | A kind of zirconium oxide soaks coloration and dyeing technique |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111732449A (en) * | 2020-06-22 | 2020-10-02 | 嘉兴饶稷科技有限公司 | Coloring agent and coloring method for three-dimensional coloring of zirconia ceramic dental crown |
| CN111807865A (en) * | 2020-07-14 | 2020-10-23 | 嘉兴饶稷科技有限公司 | High-strength and high-hardness ceramic teethridge base station |
| CN111807865B (en) * | 2020-07-14 | 2022-07-05 | 嘉兴饶稷科技有限公司 | High-strength and high-hardness ceramic teethridge base station |
| CN115124338A (en) * | 2022-06-27 | 2022-09-30 | 潮州三环（集团）股份有限公司 | Color coating slurry, color zirconia ceramic and preparation method thereof |
| CN115124338B (en) * | 2022-06-27 | 2023-02-28 | 潮州三环（集团）股份有限公司 | Color coating slurry, color zirconia ceramic and preparation method thereof |
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