CN114133241A - Yellow zirconia ceramic material and preparation method thereof - Google Patents

Yellow zirconia ceramic material and preparation method thereof Download PDF

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CN114133241A
CN114133241A CN202111510326.5A CN202111510326A CN114133241A CN 114133241 A CN114133241 A CN 114133241A CN 202111510326 A CN202111510326 A CN 202111510326A CN 114133241 A CN114133241 A CN 114133241A
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zirconia
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杨瑶刚
王德昌
高勇
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Changyu Holding Group Co ltd
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    • C04B2235/9661—Colour

Abstract

The invention belongs to the technical field of colored zirconia ceramics, and particularly relates to a yellow zirconia ceramic material and a preparation method thereof. The preparation method of the yellow zirconia ceramic material comprises the following steps: weighing 30-40 parts of sodium fluoride, 5-10 parts of magnesium oxide, 40-55 parts of ammonium metavanadate, 1-2 parts of iron oxide and 5-10 parts of zinc oxide according to parts by weight, uniformly mixing, adding into deionized water, adding a grinding aid, and uniformly ball-milling to obtain a colorant slurry; adding zirconia powder into deionized water, adding a dispersing agent, and uniformly ball-milling to obtain zirconia slurry; and adding the colorant slurry into the zirconia slurry, mixing, granulating, molding and sintering to obtain the yellow zirconia ceramic material. The yellow zirconia ceramic material prepared by the invention has the advantages of good glossiness, stable chemical property, transparent and bright color, high hardness and high toughness, and is suitable for industrial production.

Description

Yellow zirconia ceramic material and preparation method thereof
Technical Field
The invention belongs to the technical field of colored zirconia ceramics, and particularly relates to a yellow zirconia ceramic material and a preparation method thereof.
Background
The yttrium-stabilized zirconia ceramic has excellent performances of high strength, high toughness, wear resistance, corrosion resistance and the like, is widely applied to the fields of aerospace, biomedicine, electronic components and the like, and has penetrated into every corner of our lives. In recent years, with the development of science and technology, the single-color ceramic cannot meet the requirements of people on the appearance of structural ceramics, and the colorful zirconia ceramics are gradually deepened into the work, study and life of the public, so that the development of the colorful zirconia ceramics has wide research significance and development prospect.
At present, the synthesis of colored zirconia is increasingly diversified, and the most critical step is to uniformly distribute a coloring phase in a ceramic matrix. In order to prepare the colored zirconia ceramics with excellent performance, researchers have made many improvements from raw materials to preparation methods, however, the problems of uneven color formation, poor color stability, complex preparation process and the like still exist.
Patent CN201810437739.7 discloses a preparation method of yellow zirconia ceramic, which is to mix yttrium-stabilized zirconia powder with vanadium oxide or ammonium vanadate in a ball mill, add a dispersant to perform ball milling, mix uniformly and dry, and then grind to obtain yellow zirconia ceramic powder; pre-calcining the prepared yellow zirconia powder in a muffle furnace at 1180 ℃ for 2-5h, and then cooling to room temperature along with the furnace to obtain a vanadium-zirconium solid solution; grinding and crushing the prepared vanadium-zirconium solid solution, granulating, and then performing dry pressing or cold isostatic pressing to obtain a yellow zirconia biscuit; and sintering the prepared zirconia ceramic biscuit at high temperature to obtain yellow zirconia ceramic. According to the invention, vanadium-zirconium solid solution is formed by pre-sintering the colorant vanadium oxide or ammonium vanadate and yttrium-stabilized zirconia, so that the high-temperature stability of vanadium oxide is improved, and the successful preparation of yellow zirconia ceramic is realized, but the preparation process is relatively complex and is not suitable for industrial production.
Patent CN201911213134.0 discloses a yellow zirconia ceramic powder, which is prepared from the following materials in parts by mass: 0.28 to 0.32 part of MgO and 0.19 to 0.25 part of Al2O30.33 to 0.37 part of SiO22.9 to 3.2 parts of Y2O30.48 to 0.52 parts of Pr6O11, 95-96 parts of ZrO2Stirring to form a mixture; then mixing and ball-milling 0.8-1.2 parts of the mixture, 10-14 parts of grinding medium, 1.2-1.5 parts of deionized water and 0.01-0.02 part of dispersant until D50 is less than or equal to 0.4 mu m; drying at 80-150 ℃, and grinding until D50 is less than or equal to 0.2mm to obtain product powder. The powder is purple gray and forms yellow zirconia ceramics after sintering. The hair isAdding Pr when necessary6O and Al2O3The sintering temperature is reduced, the sintered ceramic is ensured to be yellow, the raw material cost is high, the ceramic is not suitable for mass production, the benefit is low, and the hardness of the zirconia ceramic obtained by low-temperature sintering is not high.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the yellow zirconia ceramic material has the advantages of good glossiness, stable chemical property, bright and bright color, high hardness and high toughness; the invention also provides a simple and feasible preparation method, which has low cost and simple operation and is suitable for industrial production.
The preparation method of the yellow zirconia ceramic material comprises the following steps:
(1) weighing 30-40 parts of sodium fluoride, 5-10 parts of magnesium oxide, 40-55 parts of ammonium metavanadate, 1-2 parts of ferric oxide and 5-10 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water, adding a grinding aid, and uniformly ball-milling to obtain colorant slurry;
(3) adding zirconia powder into deionized water, adding a dispersing agent, and uniformly ball-milling to obtain zirconia slurry;
(4) adding a colorant slurry into a zirconia slurry according to the percentage of 2-5 wt% of colorant powder and 98-95 wt% of zirconia powder, and uniformly mixing to obtain a mixed slurry;
(5) spraying, granulating and sieving the mixed slurry to obtain zirconia ceramic powder, and preparing the ceramic powder into a ceramic green body by a dry pressing process and cold isostatic pressing;
(6) and sintering the ceramic green body to obtain the yellow zirconia ceramic material.
The zirconia powder is yttrium-stabilized zirconia powder, the content of yttrium is 5.6-5.8%, and the particle size D50 is 0.43-0.45 μm.
In the components of the colorant, sodium fluoride, ammonium metavanadate and ferric oxide are chromogenic substances, and are mixed according to a proper proportion to mainly provide yellow color after the zirconia ceramic is sintered, and the magnesium oxide and the zinc oxide mainly play a role in enhancing the stability of the chromogenic substances and enabling the chromogenic substances to have luster. Under the mutual coordination of all the components, a more stable yellow ceramic material is obtained.
In the colorant slurry in the step (2), the solid content of the colorant powder is 65-80 wt%.
In the step (2), the grinding aid is at least one of linoleic acid, fatty acid, monoglyceride and lanolin; the addition amount of the grinding aid is 0.4-1% of the total mass of the colorant powder.
In the zirconia slurry obtained in the step (3), the solid content of the zirconia powder is 70-75 wt%.
In the step (3), the dispersant is at least one of stearic acid, polyethylene glycol and stearamide; the addition amount of the dispersing agent is 0.05-0.1% of the total mass of the zirconia powder.
And (4) slowly pouring the colorant slurry into the zirconium oxide slurry, and continuously stirring to uniformly mix the colorant slurry and the zirconium oxide slurry.
In the step (5), the inlet air temperature of spray granulation is 185-195 ℃, the outlet air temperature is 80-90 ℃, and the rotating speed is 10000 rpm.
And after spray granulation, sieving the mixture by a sieve of 80-100 meshes. To obtain zirconia ceramic powder with uniform grain diameter.
Setting the pressure of dry pressing to be 20-25 MPa; and (3) keeping the pressure of cold isostatic pressing at 140-160 MPa for 2-3 min, and slowly decompressing to take out the ceramic green body.
In the step (6), the sintering temperature is 1430-1480 ℃, and the sintering time is 14-16 h.
The invention also provides a yellow zirconia ceramic material prepared by the preparation method, and the color values are L (65-70), a (10-15) and b (35-45).
The strength of the yellow zirconia ceramic material is more than 900MPa (GB/T232-2010); vickers hardness of more than 1300(GB/T4340.1-2009), fracture toughness of more than 8.0 MPa-m1/2(GB/T 4161-1984)。
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, through reasonably designing the formula of the colorant powder and the synergistic effect of the colorant powder and the zirconia powder, the yellow zirconia ceramic material prepared by high-temperature sintering has stable chemical properties, good glossiness, transparent and bright color, high strength, high hardness and good toughness;
(2) the invention respectively carries out dispersion grinding on the colorant powder and the zirconia powder, and then carries out mixing granulation to ensure that the coloring phase is uniformly distributed in the ceramic matrix, the preparation method is simple and is suitable for industrial production, the strength of the prepared zirconia ceramic material is higher than 900MPa, the Vickers hardness is higher than 1300, and the fracture toughness is higher than 8.0 MPa.m1/2And the color values are in the range of L (65-70), a (15-20) and b (35-45), and the color value is yellow.
Detailed Description
The present invention will be described in further detail with reference to examples, but the following descriptions are only preferred examples of the present invention and should not be construed as limiting the scope of the examples of the present invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
The raw materials used in the examples are commercially available conventional products, wherein the zirconia powder is commercially available yttrium-stabilized zirconia powder, the yttrium content is 5.6-5.8%, and the particle size D50 is 0.43-0.45 μm. In the industrial production, the yttrium content and the granularity index of each batch of zirconia powder can slightly change, and the influence on the performance of the prepared zirconia ceramic material can be ignored within the index range.
Example 1
A preparation method of a yellow zirconia ceramic material comprises the following steps:
(1) weighing 38 parts of sodium fluoride, 5 parts of magnesium oxide, 50 parts of ammonium metavanadate, 2 parts of ferric oxide and 5 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water to prepare slurry with the solid content of 70%, adding linoleic acid accounting for 0.4% of the mass of the colorant powder, and uniformly ball-milling to obtain the colorant slurry;
(3) adding zirconia powder into deionized water to prepare slurry with the solid content of 72%, adding stearic acid accounting for 0.05% of the mass of the zirconia powder, and uniformly ball-milling to obtain zirconia slurry;
(4) adding the colorant slurry into the zirconia slurry according to the percentage of 2 wt% of colorant powder and 98 wt% of zirconia powder, and uniformly mixing to obtain mixed slurry;
(5) spray granulating the mixed slurry, wherein the air inlet temperature is 190 ℃, the air outlet temperature is 90 ℃, the rotation speed is 10000rpm, sieving by a 80-mesh sieve after granulation to obtain zirconia ceramic powder, dry-pressing and molding under 25MPa, cold isostatic pressing and molding under 150MPa, keeping the pressure for 2min, and slowly reducing the pressure to prepare a ceramic green body;
(6) and sintering the ceramic green body at the temperature of 1430 ℃ for 14h to obtain the yellow zirconia ceramic material.
Example 2
A preparation method of a yellow zirconia ceramic material comprises the following steps:
(1) weighing 38 parts of sodium fluoride, 4 parts of magnesium oxide, 48 parts of ammonium metavanadate, 1 part of ferric oxide and 8 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water to prepare slurry with the solid content of 65%, adding fatty acid accounting for 0.5% of the mass of the colorant powder, and uniformly ball-milling to obtain colorant slurry;
(3) adding zirconia powder into deionized water to prepare slurry with the solid content of 75%, adding stearic acid accounting for 0.06% of the mass of the zirconia powder, and uniformly ball-milling to obtain zirconia slurry;
(4) adding the colorant slurry into the zirconia slurry according to the percentage of 3 wt% of colorant powder and 97 wt% of zirconia powder, and uniformly mixing to obtain mixed slurry;
(5) spray granulating the mixed slurry, wherein the air inlet temperature is 185 ℃, the air outlet temperature is 80 ℃, the rotation speed is 10000rpm, sieving by a 80-mesh sieve after granulation to obtain zirconia ceramic powder, dry-pressing and molding under the pressure of 20MPa, cold isostatic pressing and molding under the pressure of 140MPa, keeping the pressure for 3min, and slowly reducing the pressure to prepare a ceramic green body;
(6) and sintering the ceramic green body at 1450 ℃ for 14.5h to obtain the yellow zirconia ceramic material.
Example 3
A preparation method of a yellow zirconia ceramic material comprises the following steps:
(1) weighing 36 parts of sodium fluoride, 7 parts of magnesium oxide, 49 parts of ammonium metavanadate, 2 parts of ferric oxide and 6 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water to prepare slurry with solid content of 78%, adding lanolin accounting for 0.8% of the mass of the colorant powder, and uniformly ball-milling to obtain colorant slurry;
(3) adding zirconia powder into deionized water to prepare slurry with the solid content of 73%, adding polyethylene glycol accounting for 0.06% of the mass of the zirconia powder, and uniformly ball-milling to obtain zirconia slurry;
(4) adding the colorant slurry into the zirconia slurry according to the percentage of 4 wt% of colorant powder and 96 wt% of zirconia powder, and uniformly mixing to obtain mixed slurry;
(5) spray granulating the mixed slurry, wherein the air inlet temperature is 195 ℃, the air outlet temperature is 90 ℃, the rotation speed is 10000rpm, sieving with a 100-mesh sieve after granulation to obtain zirconia ceramic powder, dry-pressing and molding under the pressure of 20MPa, cold isostatic pressing and molding under the pressure of 160MPa, keeping the pressure for 2min, and slowly reducing the pressure to prepare a ceramic green body;
(6) sintering the ceramic green body at 1460 ℃ for 15h to obtain the yellow zirconia ceramic material.
Example 4
A preparation method of a yellow zirconia ceramic material comprises the following steps:
(1) weighing 40 parts of sodium fluoride, 6 parts of magnesium oxide, 44 parts of ammonium metavanadate, 1 part of ferric oxide and 9 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water to prepare slurry with solid content of 80%, adding lanolin accounting for 0.8% of the mass of the colorant powder, and uniformly ball-milling to obtain colorant slurry;
(3) adding zirconia powder into deionized water to prepare slurry with the solid content of 75%, adding polyethylene glycol accounting for 0.1% of the mass of the zirconia powder, and uniformly ball-milling to obtain zirconia slurry;
(4) adding the colorant slurry into the zirconia slurry according to the percentage of 5 wt% of colorant powder and 95 wt% of zirconia powder, and uniformly mixing to obtain mixed slurry;
(5) spray granulating the mixed slurry, wherein the air inlet temperature is 185 ℃, the air outlet temperature is 85 ℃, the rotation speed is 10000rpm, sieving with a 100-mesh sieve after granulation to obtain zirconia ceramic powder, dry-pressing and molding under 25MPa, cold isostatic pressing and molding under 150MPa, keeping the pressure for 2.5min, and slowly reducing the pressure to prepare a ceramic green body;
(6) and sintering the ceramic green body at the temperature of 1480 ℃ for 15 hours to obtain the yellow zirconia ceramic material.
Comparative example 1
This comparative example replaces the zinc oxide in the colorant with alumina to prepare a yellow zirconia ceramic material by the following method:
(1) weighing 38 parts of sodium fluoride, 5 parts of magnesium oxide, 50 parts of ammonium metavanadate, 2 parts of ferric oxide and 5 parts of aluminum oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water to prepare slurry with the solid content of 70%, adding linoleic acid accounting for 0.4% of the mass of the colorant powder, and uniformly ball-milling to obtain the colorant slurry;
(3) adding zirconia powder into deionized water to prepare slurry with the solid content of 72%, adding stearic acid accounting for 0.05% of the mass of the zirconia powder, and uniformly ball-milling to obtain zirconia slurry;
(4) adding the colorant slurry into the zirconia slurry according to the percentage of 2 wt% of colorant powder and 98 wt% of zirconia powder, and uniformly mixing to obtain mixed slurry;
(5) spray granulating the mixed slurry, wherein the air inlet temperature is 190 ℃, the air outlet temperature is 90 ℃, the rotation speed is 10000rpm, sieving by a 80-mesh sieve after granulation to obtain zirconia ceramic powder, dry-pressing and molding under 25MPa, cold isostatic pressing and molding under 150MPa, keeping the pressure for 2min, and slowly reducing the pressure to prepare a ceramic green body;
(6) and sintering the ceramic green body at the temperature of 1430 ℃ for 14h to obtain the yellow zirconia ceramic material.
Comparative example 2
In the comparative example, sodium fluoride in the colorant was replaced by calcium fluoride to prepare a yellow zirconia ceramic material by the following method:
(1) weighing 38 parts of calcium fluoride, 5 parts of magnesium oxide, 50 parts of ammonium metavanadate, 2 parts of ferric oxide and 5 parts of aluminum oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water to prepare slurry with the solid content of 70%, adding linoleic acid accounting for 0.4% of the mass of the colorant powder, and uniformly ball-milling to obtain the colorant slurry;
(3) adding zirconia powder into deionized water to prepare slurry with the solid content of 72%, adding stearic acid accounting for 0.05% of the mass of the zirconia powder, and uniformly ball-milling to obtain zirconia slurry;
(4) adding the colorant slurry into the zirconia slurry according to the percentage of 2 wt% of colorant powder and 98 wt% of zirconia powder, and uniformly mixing to obtain mixed slurry;
(5) spray granulating the mixed slurry, wherein the air inlet temperature is 190 ℃, the air outlet temperature is 90 ℃, the rotation speed is 10000rpm, sieving by a 80-mesh sieve after granulation to obtain zirconia ceramic powder, dry-pressing and molding under 25MPa, cold isostatic pressing and molding under 150MPa, keeping the pressure for 2min, and slowly reducing the pressure to prepare a ceramic green body;
(6) and sintering the ceramic green body at the temperature of 1430 ℃ for 14h to obtain the yellow zirconia ceramic material.
Comparative example 3
In the comparative example, the colorant powder and the zirconia powder are mixed and then ground to prepare the yellow zirconia ceramic material, and the method comprises the following steps:
(1) weighing 38 parts of sodium fluoride, 5 parts of magnesium oxide, 50 parts of ammonium metavanadate, 2 parts of ferric oxide and 5 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding 2 wt% of colorant powder and 98 wt% of zirconia powder into deionized water to prepare slurry with the solid content of 70%, then adding linoleic acid accounting for 0.4% of the mass of the colorant powder and stearic acid accounting for 0.05% of the mass of the zirconia powder, and uniformly ball-milling to obtain mixed slurry;
(3) spraying and granulating the mixed slurry, sieving the granulated mixed slurry with a 80-mesh sieve to obtain zirconia ceramic powder, and preparing the ceramic powder into a ceramic green body by a dry pressing process and cold isostatic pressing;
(4) and sintering the ceramic green body at the temperature of 1430 ℃ for 14h to obtain the yellow zirconia ceramic material.
The yellow zirconia ceramic materials prepared in the above examples and comparative examples are subjected to performance detection, wherein the color difference value detection method is GB/T7921-1997 determination standard of uniform color space and color difference formula; the strength detection method is a GB/T232-2010 bending test method; the Vickers hardness detection method is GB/T4340.1-2009 Vickers hardness test; the fracture toughness detection method is GB/T4161-1984 fracture toughness test. The test results are shown in table 1.
TABLE 1 Performance test results for yellow zirconia ceramic materials
Figure BDA0003405476050000061
Figure BDA0003405476050000071
As can be seen from Table 1, the yellow zirconia ceramic obtained by the preparation method disclosed by the invention is stable in coloring effect after being sintered at high temperature, stable in color values in the ranges of L (65-70), a (15-20) and b (35-45), obvious in yellow, higher than 900MPa in strength, higher than 1300 in Vickers hardness and higher than 8.0 MPa-m in fracture toughness1/2And the mechanical property is excellent.

Claims (10)

1. A preparation method of a yellow zirconia ceramic material is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing 30-40 parts of sodium fluoride, 5-10 parts of magnesium oxide, 40-55 parts of ammonium metavanadate, 1-2 parts of ferric oxide and 5-10 parts of zinc oxide according to parts by weight, and uniformly mixing to obtain colorant powder;
(2) adding colorant powder into deionized water, adding a grinding aid, and uniformly ball-milling to obtain colorant slurry;
(3) adding zirconia powder into deionized water, adding a dispersing agent, and uniformly ball-milling to obtain zirconia slurry;
(4) adding a colorant slurry into a zirconia slurry according to the percentage of 2-5 wt% of colorant powder and 98-95 wt% of zirconia powder, and uniformly mixing to obtain a mixed slurry;
(5) spraying, granulating and sieving the mixed slurry to obtain zirconia ceramic powder, and preparing the ceramic powder into a ceramic green body by a dry pressing process and cold isostatic pressing;
(6) and sintering the ceramic green body to obtain the yellow zirconia ceramic material.
2. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: the zirconia powder is yttrium-stabilized zirconia powder, the content of yttrium is 5.6-5.8%, and the particle size D50 is 0.43-0.45 μm.
3. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the colorant slurry in the step (2), the solid content of the colorant powder is 65-80 wt%.
4. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the step (2), the grinding aid is at least one of linoleic acid, fatty acid, monoglyceride and lanolin; the addition amount of the grinding aid is 0.4-1% of the total mass of the colorant powder.
5. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the zirconia slurry obtained in the step (3), the solid content of the zirconia powder is 70-75 wt%.
6. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the step (3), the dispersant is at least one of stearic acid, polyethylene glycol and stearamide; the addition amount of the dispersing agent is 0.05-0.1% of the total mass of the zirconia powder.
7. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the step (5), after spray granulation, sieving with a sieve of 80-100 meshes.
8. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the step (5), the air inlet temperature of spray granulation is 185-195 ℃, and the air outlet temperature is 80-90 ℃.
9. The method for preparing a yellow zirconia ceramic material according to claim 1, wherein: in the step (6), the sintering temperature is 1430-1480 ℃, and the sintering time is 14-16 h.
10. A yellow zirconia ceramic material is characterized in that: the color values are L (65-70), a (15-20), b (35-45) prepared by the preparation method of any one of claims 1-9.
CN202111510326.5A 2021-12-11 2021-12-11 Yellow zirconia ceramic material and preparation method thereof Pending CN114133241A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115677346A (en) * 2022-11-07 2023-02-03 北京赛乐米克材料科技有限公司 Preparation method of color zirconium gem ceramic nose pad

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115677346A (en) * 2022-11-07 2023-02-03 北京赛乐米克材料科技有限公司 Preparation method of color zirconium gem ceramic nose pad
CN115677346B (en) * 2022-11-07 2023-09-12 北京赛乐米克材料科技有限公司 Preparation method of colored zirconium precious stone ceramic nose pad

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