CN109400150B - High-strength pink zirconia ceramic powder and preparation method and application thereof - Google Patents
High-strength pink zirconia ceramic powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-strength pink zirconia ceramic powder, which comprises zirconia and an additional oxide; the content of the added oxide is 0.5-4.0 mol% of erbium oxide, 0.5-4.0 mol% of yttrium oxide, 0.1-0.3 mol% of magnesium oxide and 0.1-0.3 mol% of aluminum oxide relative to zirconium oxide. In addition, a preparation method and application of the high-strength pink zirconia ceramic powder are also disclosed. The invention optimizes the formula to obtain the powder raw material with stable components and excellent performance, and is beneficial to obtaining pink aesthetic ceramic products with high strength, good toughness, good color development, high glossiness and few surface defects, thereby being capable of well meeting the severe processing requirements in practical application, being beneficial to widening the application field of the pink aesthetic ceramic products and having obvious economic benefit and wide application prospect.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to pink zirconia ceramic powder for consumer electronics products and a preparation method and application thereof.
Background
The zirconia ceramics has the advantages of high strength, high hardness, corrosion resistance and the like, and in addition, the zirconia ceramics also has the advantages of low thermal conductivity coefficient, low thermal expansion coefficient, low friction coefficient, high chemical stability and the like. Therefore, the zirconia ceramics have wide application and are widely used in the fields of refractory materials, high-temperature structural materials, electronic materials, materials for daily-use kitchenware, molds, solid fuel cells, oxygen sensors and the like.
In recent years, due to the characteristics of excellent performance and good biocompatibility of zirconia, no stimulation to human bodies and the like, the zirconia has been used in consumer products such as bracelets, watch chains, buttons, smart watches, smart phones, computers and the like. Due to the strict requirements of manufacturing and inspection of consumer electronics (such as smart watches, smart phones, computers and the like), higher requirements are put forward on both performance and processing of zirconia ceramics. In addition, as the living standard of people is continuously improved, the aesthetic requirements of consumers on product devices are also synchronously improved; moreover, with the application and popularization of new technologies such as 5G network and wireless charging, the market demand of zirconia aesthetic ceramics is further expanded. However, most of the existing consumer electronics products are made of black and white zirconia ceramics, and the existing consumer electronics products lack more beautiful color products and cannot well meet the use requirements of consumers. Therefore, in recent years, colored zirconia ceramics have been studied and developed, but they have defects such as dull color, poor appearance, and particularly low mechanical properties, and it is difficult to satisfy practical requirements of manufacturing, processing, market, and application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-strength pink zirconia ceramic powder which is formed by optimizing a formula so as to be suitable for synthesizing a powder raw material with stable components and excellent performance, thereby being beneficial to obtaining aesthetic ceramic products with high strength, good toughness, good color development, high gloss and few surface defects. The invention also aims to provide a preparation method and application of the high-strength pink zirconia ceramic powder.
The purpose of the invention is realized by the following technical scheme:
the invention provides a high-strength pink zirconia ceramic powder, which comprises zirconia and an additional oxide; the content of the added oxide is 0.5-4.0 mol% of erbium oxide, 0.5-4.0 mol% of yttrium oxide, 0.1-0.3 mol% of magnesium oxide and 0.1-0.3 mol% of aluminum oxide relative to zirconium oxide. Preferably, the content of the added oxide is 0.5 to 3.5 mol% of erbium oxide, 0.5 to 3.5 mol% of yttrium oxide, 0.1 to 0.25 mol% of magnesium oxide, and 0.1 to 0.25 mol% of aluminum oxide with respect to zirconium oxide.
In the scheme, the raw material of the zirconium oxide is zirconium oxychloride with the same amount; the raw material substances of the added oxide are erbium nitrate, yttrium nitrate, magnesium carbonate and aluminum ammonium sulfate which are equivalent correspondingly.
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the high-strength pink zirconia ceramic powder provided by the invention comprises the following steps:
(1) firstly, dissolving zirconium oxychloride in water to form a zirconium oxychloride aqueous solution, then dissolving erbium nitrate and yttrium nitrate in the zirconium oxychloride aqueous solution according to the proportion, adding alkali with the concentration of 3-5 mol/L as a precipitating agent, controlling the pH value of the system to be 7.0-10.0, completely converting zirconium, erbium and yttrium elements into precipitates, filtering, washing and drying to obtain a precursor I;
(2) dissolving magnesium carbonate in acid with the concentration of 3-5 mol/L according to the proportion until the magnesium carbonate is completely dissolved, then adding alkali with the concentration of 3-5 mol/L as a precipitator, controlling the pH value of the system to be 8.0-10.0 to completely precipitate metal ions in the acid, and filtering, washing and drying the solution to obtain a precursor II;
(3) dissolving aluminum ammonium sulfate in 3-5 mol/L acid according to the proportion until the aluminum ammonium sulfate is completely dissolved, then adding alkali with the concentration of 3-5 mol/L as a precipitating agent, controlling the pH value of the system to be 3.0-5.0, completely precipitating metal ions in the solution, and filtering, washing and drying the solution to obtain a precursor III;
(4) and uniformly mixing the precursor I, the precursor II and the precursor III, and calcining and crushing to obtain the high-strength pink zirconia ceramic powder.
Further, the alkali in the preparation method is one or the combination of ammonia water, ammonium bicarbonate and ammonium carbonate; the acid is one or the combination of hydrochloric acid, nitric acid and sulfuric acid. In the step (4), the calcining temperature is 800-1200 ℃, and the heat preservation time is 3-8 h; the particle size of the crushed powder is less than 1 mu m.
The application of the high-strength pink zirconia ceramic powder provided by the invention is a pink zirconia aesthetic ceramic product prepared by taking the ceramic powder as a raw material. The preparation method of the aesthetic ceramic product comprises the steps of manufacturing a ceramic blank by using the ceramic powder as a raw material, and sintering at 1450-1550 ℃ to obtain the high-strength pink zirconia aesthetic ceramic product.
The invention has the following beneficial effects:
(1) according to the invention, by optimizing the formula composition of the raw materials and carrying out precipitation reaction step by using a liquid phase method according to different contained metal ions, the reaction is more sufficient and uniform, so that different required precursors are obtained by batch synthesis.
(2) After the zirconia ceramic powder is prepared into a ceramic blank, pink is presented through high-temperature sintering, and the obtained pink zirconia aesthetic ceramic product not only has excellent appearance performances of good color development, high glossiness, few surface defects and the like, but also has excellent mechanical properties of high strength, good toughness and the like, can meet the harsh processing requirements in practical application, and is beneficial to widening the application field.
(3) The pink zirconia aesthetic ceramic product prepared by the invention has the flexural strength of 1150-1300 MPa and the density of not less than 6.10g/cm3The Vickers hardness is 1200-1300 Hv, and the color value is 5-1300 a*≤15、-3≤b*≤3、75≤L*Less than or equal to 85 percent, and the performance of the product is far superior to that of the prior similar products.
The present invention will be described in further detail with reference to examples.
Detailed Description
The embodiment of the invention provides high-strength pink zirconia ceramic powder, which comprises zirconia and an additional oxide in chemical composition; wherein the content of the added oxide is 0.5-4.0 mol% of erbium oxide, 0.5-4.0 mol% of yttrium oxide, 0.1-0.3 mol% of magnesium oxide, and 0.1-0.3 mol% of aluminum oxide, relative to zirconium oxide. The chemical composition of each example is shown in table 1.
TABLE 1 chemical composition of high Strength Pink zirconia ceramic powder for the examples of the invention
The raw material of the zirconium oxide in the embodiment of the invention is zirconium oxychloride with the same amount; the raw material substances of the added oxide are erbium nitrate, yttrium nitrate, magnesium carbonate and aluminum ammonium sulfate which are equivalent correspondingly.
The preparation method of the high-strength pink zirconia ceramic powder comprises the following steps:
(1) firstly, dissolving zirconium oxychloride in water to form a 100g/L zirconium oxychloride aqueous solution, then dissolving erbium nitrate and yttrium nitrate in the zirconium oxychloride aqueous solution according to the proportion shown in Table 1, adding 3-5 mol/L alkali as a precipitating agent, controlling the pH value of the system to be 7.0-10.0, completely converting zirconium, erbium and yttrium elements into precipitates, filtering, washing and drying to obtain a precursor I;
(2) dissolving magnesium carbonate in acid with the concentration of 3-5 mol/L according to the proportion shown in the table 1 until the magnesium carbonate is completely dissolved, then adding alkali with the concentration of 3-5 mol/L as a precipitator, controlling the pH value of the system to be 8.0-10.0, completely precipitating metal ions in the acid, and filtering, washing and drying the solution to obtain a precursor II;
(3) dissolving aluminum ammonium sulfate in 3-5 mol/L acid according to the proportion shown in Table 1 until the aluminum ammonium sulfate is completely dissolved, then adding alkali with the concentration of 3-5 mol/L as a precipitating agent, controlling the pH value of the system to be 3.0-5.0, completely precipitating metal ions in the solution, and filtering, washing and drying the solution to obtain a precursor III;
(4) uniformly mixing the precursor I, the precursor II and the precursor III, calcining at the temperature of 800-1200 ℃, and keeping the temperature for 3-8 hours; then crushing the mixture until the particle size is less than 1 mu m to obtain the high-strength pink zirconia ceramic powder.
The preparation method of each example has the process parameters shown in table 2.
TABLE 2 Process parameters of the preparation method of high strength pink zirconia ceramic powder according to the embodiments of the present invention
Note: the precipitator A is ammonium carbonate, the precipitator B is ammonia water, and the precipitator C is ammonium bicarbonate;
acid D is hydrochloric acid, acid E is nitric acid, and acid F is sulfuric acid.
According to the invention, the ceramic powder of each embodiment is used as a raw material to manufacture a ceramic blank by adopting a process in the prior art, and then the ceramic blank is sintered for 2 hours at the temperature of 1450-1550 ℃, so that the high-strength pink zirconia aesthetic ceramic product is obtained. The sintering temperatures and performance indexes of the ceramic products of the examples are shown in Table 3 and Table 4, respectively.
TABLE 3 sintering temperatures of ceramic products of examples of the invention
TABLE 4 Performance index of ceramic products of the examples of the present invention
Claims (2)
1. A preparation method of high-strength pink zirconia ceramic powder is characterized by comprising the following steps: the chemical composition of the pink zirconia ceramic powder is zirconia and an additional oxide; the content of the added oxide relative to the zirconia is 0.5-4.0 mol% of erbium oxide, 0.5-4.0 mol% of yttrium oxide, 0.1-0.3 mol% of magnesium oxide and 0.1-0.3 mol% of aluminum oxide; the raw material of the zirconium oxide is zirconium oxychloride with the same quantity; the raw material substances of the added oxide are correspondingly erbium nitrate, yttrium nitrate, magnesium carbonate and aluminum ammonium sulfate with the same amount; the preparation method comprises the following steps:
(1) firstly, dissolving zirconium oxychloride in water to form a zirconium oxychloride aqueous solution, then dissolving erbium nitrate and yttrium nitrate in the zirconium oxychloride aqueous solution, adding alkali with the concentration of 3-5 mol/L as a precipitating agent, controlling the pH value of a system to be 7.0-10.0, completely converting zirconium, erbium and yttrium elements into precipitates, filtering, washing and drying to obtain a precursor I;
(2) dissolving the magnesium carbonate in one or a combination of hydrochloric acid, nitric acid and sulfuric acid with the concentration of 3-5 mol/L until the magnesium carbonate is completely dissolved, then adding alkali with the concentration of 3-5 mol/L as a precipitating agent, controlling the pH value of the system to be 8.0-10.0, completely precipitating metal ions in the alkali, and filtering, washing and drying to obtain a precursor II;
(3) dissolving the aluminum ammonium sulfate in one or a combination of 3-5 mol/L hydrochloric acid, nitric acid and sulfuric acid until the aluminum ammonium sulfate is completely dissolved, then adding alkali with the concentration of 3-5 mol/L as a precipitating agent, controlling the pH value of the system to be 3.0-5.0, completely precipitating metal ions in the aluminum ammonium sulfate, and filtering, washing and drying the aluminum ammonium sulfate to obtain a precursor III;
(4) uniformly mixing the precursor I, the precursor II and the precursor III, calcining at 800-1200 ℃, preserving heat for 3-8 hours, and then crushing until the particle size is less than 1 mu m to obtain high-strength pink zirconia ceramic powder; the ceramic powder is used as a raw material to manufacture a ceramic blank body, and the ceramic blank body is sintered at the temperature of 1450-1550 ℃ to obtain the high-strength pink zirconia aesthetic ceramic product, wherein the breaking strength of the high-strength pink zirconia aesthetic ceramic product is 1150-1300 MPa, and the density of the high-strength pink zirconia aesthetic ceramic product is not less than 6.10g/cm3The Vickers hardness is 1200-1300 Hv, and the color value is 5-1300 a* ≤15、-3≤b* ≤3、75≤L*≤85。
2. The method for preparing high-strength pink zirconia ceramic powder according to claim 1, wherein: the alkali is one or the combination of ammonia water, ammonium bicarbonate and ammonium carbonate.
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