A method for producing a zirconia ceramic rod

Abstract

The application discloses a preparation method of a zirconia ceramic rod and belongs to the technical field of ceramic rods. The preparation method comprises the following steps: step 1, hydroxyapatite is added into distilled water, the temperature is increased to 50-60 DEG C, phosphate ester is added and stirred, suction filtration is carried out, and drying is carried out to obtain modified hydroxyapatite; step 2, zirconia, yttrium oxide, titanium oxide, the modified hydroxyapatite and a binder are mixed to obtain a mud; step 3, the mud is extruded to obtain a blank, drying and sintering are carried out, and a zirconia ceramic rod is obtained. The raw materials are reasonably matched and selected, the zirconia ceramic rod with high compressive strength and excellent wear resistance is prepared, the cost is economic, and industrial production is met.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of ceramic rods, and particularly relates to a preparation method of a zirconia ceramic rod. BACKGROUND

[0002] With the continuous development of science and technology, breakthroughs have also been made in industrial ceramics, especially the research and development of multiphase composite ceramics and nanoceramics. The zirconia ceramic rod is a ceramic rod made of zirconia material, which has the characteristics of high strength, high density, wear resistance, corrosion resistance and high temperature resistance, and is widely used in electronic paste, semiconductors, new energy, nanometer new materials, medical devices and refractory materials.

[0003] At present, the ceramic material composed of single zirconia has relatively single performance and cannot meet the use in multiple fields, and the zirconia used is usually nanoscale or microscale, and has a large specific surface area, and the particles are prone to mutual aggregation. In order to effectively improve the performance, it is necessary to optimize the ceramic composition and improve the comprehensive performance of the zirconia ceramic material, which is also a hot spot in the field of ceramics. CN102765943A discloses a preparation method of a zirconia ceramic rod for flame spraying, the main raw material composition and weight percentage of the ceramic rod are Al2O32%-3%, SiO3% 4%, Fe0 0.02%-0.03%, TiO2 0.75%-0.85%, CaO 3.90%-3.95%, and the balance is ZrO2, but the fusion between the raw materials is poor, the density of the formed material is low, and the wear resistance of the finally prepared zirconia ceramic rod is poor. SUMMARY

[0004] The purpose of the present application is to provide a preparation method of a zirconia ceramic rod to solve the problem of poor compressive strength of the zirconia ceramic rod.

[0005] The purpose of the present application can be achieved by the following technical solutions:

[0006] A preparation method of a zirconia ceramic rod, comprising the following steps:

[0007] Step 1, hydroxyapatite is added to distilled water, heated to 50-60℃, phosphate ester is added and stirred, filtered, and dried to obtain modified hydroxyapatite;

[0008] Step 2, zirconia, yttrium oxide, titanium oxide, modified hydroxyapatite and a binder are mixed to obtain a mud;

[0009] Step 3, the mud is extruded to obtain a green body, dried, sintered, and a zirconia ceramic rod is obtained.

[0010] As a further scheme of the present application, the amount ratio of hydroxyapatite, distilled water and phosphate ester in step 1 is 1-1.1g: 15mL: 2-2.2g.

[0011] As a further scheme of the present application, the phosphate ester is one of hexadecyl phosphate ester and octadecyl phosphate ester.

[0012] As a further scheme of the present application, the weight ratio of zirconium oxide, yttrium oxide, titanium oxide, modified hydroxyapatite and adhesive is 80-95 parts: 15-20 parts: 5-8 parts: 5-10 parts: 15-18 parts.

[0013] As a further scheme of the present application, the particle size of zirconium oxide is 600-800nm.

[0014] As a further scheme of the present application, the particle size of yttrium oxide is 200-400nm.

[0015] As a further scheme of the present application, the particle size of titanium oxide is 200-300nm.

[0016] As a further scheme of the present application, the adhesive is carboxymethyl cellulose. The carboxymethyl cellulose can make the metal oxide in the slurry fully dispersed, and can also prevent the problem of sedimentation of large-size metal oxide particles, so that a uniform distribution of coating material is prepared; and the high-temperature compressive strength of the ceramic rod is improved.

[0017] As a further scheme of the present application, the drying temperature in step 3 is 130-150℃, and the drying time in step 3 is 3-5h.

[0018] As a further scheme of the present application, the sintering temperature in step 3 is 1200-1500℃, and the sintering time in step 3 is 10-12h.

[0019] The present application has the following beneficial effects:

[0020] The present application provides a new preparation method of zirconia ceramic rod, which can prepare zirconia ceramic rod with high compressive strength and excellent wear resistance by reasonable collocation and selection of raw materials, and the cost is economic, which meets the industrial production.

[0021] The modified hydroxyapatite in the application is obtained by reacting hydroxyapatite with phosphate and then coating on the surface of the hydroxyapatite, which can improve the hydrophobic property of the hydroxyapatite, make it better dispersed in the raw materials, and effectively improve the acid resistance of the composite material. The modified hydroxyapatite is doped with zirconia, yttria, titania and other raw materials, which can make the metal oxide maintain good sintering stability and grain size, and the phosphate group at the other end of the phosphate group on the surface of the hydroxyapatite can form a bond with zirconia, yttria and titania, improve the bonding strength between the raw materials, and then improve the density of the ceramic rod and enhance the compressive strength and wear resistance of the ceramic rod.

[0022] In the application, yttria is added to change the phase transition temperature of zirconia, so that the unstable zirconia phase at room temperature is converted into a stable or metastable state, which has more excellent heat resistance, corrosion resistance and ceramic toughening characteristics. DETAILED DESCRIPTION

[0023] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, not all. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the application.

[0024] Embodiment 1

[0025] The embodiment provides a preparation method of a zirconia ceramic rod, and the steps are as follows:

[0026] Step 1: 1g of hydroxyapatite is added to 15mL of distilled water, heated to 50℃, 2g of phosphate is added for stirring, filtered, and dried to obtain modified hydroxyapatite;

[0027] Step 2: 80 parts of zirconia, 15 parts of yttria, 5 parts of titania, 5 parts of modified hydroxyapatite and 15 parts of carboxymethyl cellulose are mixed to obtain a paste;

[0028] Step 3: the paste is extruded to obtain a green body, dried at 130℃ for 4.5h, sintered, the sintering temperature is 1200℃, and the sintering time is 11h to obtain a zirconia ceramic rod.

[0029] Embodiment 2

[0030] The difference between the embodiment 2 and the embodiment 1 is only that:

[0031] Step 1: 1.05g of hydroxyapatite is added to 15mL of distilled water, heated to 50℃, 2.2g of phosphate is added for stirring, filtered, and dried to obtain modified hydroxyapatite; the rest of the raw materials and steps are the same as those in the embodiment 1.

[0032] Example 3

[0033] The difference from Example 1 is only that:

[0034] Step 1, 1.1 g of hydroxyapatite is added to 15 mL of distilled water, heated to 50°C, 2.1 g of phosphate is added for stirring, suction filtration, drying, to obtain modified hydroxyapatite; the rest of the raw materials and steps are the same as Example 1.

[0035] Example 4

[0036] The difference from Example 1 is only that:

[0037] 5 parts of modified hydroxyapatite are replaced by 6 parts of modified hydroxyapatite. The rest of the raw materials and steps are the same as Example 1.

[0038] Example 5

[0039] The difference from Example 1 is only that:

[0040] 5 parts of modified hydroxyapatite are replaced by 8 parts of modified hydroxyapatite. The rest of the raw materials and steps are the same as Example 1.

[0041] Example 6

[0042] The difference from Example 2 is only that:

[0043] Step 2, 88 parts of zirconia, 16 parts of yttria, 6 parts of titanium oxide, 8 parts of modified hydroxyapatite and 16 parts of carboxymethyl cellulose are mixed to obtain a paste; the rest of the raw materials and steps are the same as Example 2.

[0044] Example 7

[0045] The difference from Example 2 is only that:

[0046] Step 2, 95 parts of zirconia, 18 parts of yttria, 8 parts of titanium oxide, 9 parts of modified hydroxyapatite and 17 parts of carboxymethyl cellulose are mixed to obtain a paste; the rest of the raw materials and steps are the same as Example 2.

[0047] Example 8

[0048] The difference from Example 2 is only that:

[0049] Step 3, the paste is extruded to obtain a blank, dried at 145°C for 4h, sintered, the sintering temperature is 1200°C, the sintering time is 10h, to obtain a zirconia ceramic rod. The rest of the raw materials and steps are the same as Example 2.

[0050] Example 9

[0051] The difference from Example 8 is only that:

[0052] Step 3, the mud is extruded to obtain a blank, dried at 145°C for 4h, sintered at 1450°C for 11.5h to obtain a zirconia ceramic rod. The remaining raw materials and steps are the same as in Example 8.

[0053] Comparative Example 1

[0054] Compared with Example 1, no modified hydroxyapatite is added:

[0055] Step 1, 80 parts of zirconia, 15 parts of yttria, 5 parts of titania and 15 parts of carboxymethyl cellulose are mixed to obtain a mud;

[0056] Step 2, the mud is extruded to obtain a blank, dried at 130°C for 4.5h, sintered at 1200°C for 11h to obtain a zirconia ceramic rod.

[0057] Comparative Example 2

[0058] Compared with Example 1, the amount of modified hydroxyapatite is different:

[0059] 5 parts of modified hydroxyapatite is replaced by 3.5 parts of modified hydroxyapatite; the remaining raw materials and steps are the same as in Example 1.

[0060] Comparative Example 3

[0061] Compared with Example 1, the amount of modified hydroxyapatite is different:

[0062] 5 parts of modified hydroxyapatite is replaced by 11.5 parts of modified hydroxyapatite; the remaining raw materials and steps are the same as in Example 1.

[0063] Comparative Example 4

[0064] Compared with Example 2, the only difference is:

[0065] Step 2, 75 parts of zirconia, 15 parts of yttria, 5 parts of titania, 5 parts of modified hydroxyapatite and 15 parts of carboxymethyl cellulose are mixed to obtain a mud; the remaining raw materials and steps are the same as in Example 2.

[0066] Comparative Example 5

[0067] Compared with Example 2, the only difference is:

[0068] Step 3, the mud is extruded to obtain a blank, dried at 120°C for 4.5h, sintered at 1200°C for 11h to obtain a zirconia ceramic rod. The remaining raw materials and steps are the same as in Example 2.

[0069] Comparative Example 6

[0070] The difference compared with Example 2 is only that:

[0071] Step 3, the mud is extruded to obtain a blank, dried at 130℃ for 4.5h, sintered at 1600℃ for 11h to obtain a zirconia ceramic rod. The rest of the raw materials and steps are the same as Example 2.

[0072] Performance tests are carried out on Examples 1-9 and Comparative Examples 1-6: the zirconia ceramic rods obtained are subjected to compressive strength tests according to the JIS R1601-2008 Fine Ceramics Bending Strength Test Method. The test results are shown in Table 1:

[0073] Table 1

[0074]

[0075] As can be seen from Table 1, the zirconia ceramic rods prepared in Examples 1-9 have high compressive strength and wear resistance. As can be seen from Example 1 and Comparative Examples 1-3, no modified hydroxyapatite is added in Comparative Example 1, 3.5 parts of modified hydroxyapatite is added in Comparative Example 2, and 11.5 parts of modified hydroxyapatite is added in Comparative Example 3, and the compressive strength and wear resistance of the zirconia ceramic rods obtained in Comparative Examples 1-3 are lower than that of Example 1; thus, by adding the modified hydroxyapatite to the raw materials such as zirconia, yttrium oxide and titanium oxide for doping in the present application, the metal oxides can maintain good sintering stability and grain size, and the phosphate groups of the phosphate ester can form a bond with the zirconia, yttrium oxide and titanium oxide, thereby improving the bonding strength between the raw materials, and further improving the density of the ceramic rod and the compressive strength and wear resistance of the ceramic rod. As can be seen from Example 2 and Comparative Examples 4-6, the selection, amount and step parameters of the raw materials in the preparation method of the zirconia ceramic rod will affect the compressive strength and wear resistance of the zirconia ceramic rod prepared.

[0076] It should be noted that, in this document, relational terms such as first and second and the like can be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises", "comprising", or any other variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus.

[0077] While embodiments of the application have been shown and described, it is to be understood that the embodiments described are merely exemplary of the principles and application of the present application. Numerous modifications and adaptions can be effected without departing from the spirit and scope of the present application, which is not limited to the exact construction and arrangement described. It is intended, therefore, to cover all modifications and adaptions that fall within the scope of the claims and their equivalents.

Claims

1. A method for producing a zirconia ceramic rod, characterized by, The method comprises the following steps: Step 1, adding hydroxyapatite into distilled water, heating to 50-60 DEG C, adding phosphate ester, stirring, filtering, drying, to obtain modified hydroxyapatite, wherein the weight ratio of hydroxyapatite, distilled water and phosphate ester is 1-1.1g: 15ml: 2-2.2g; Step 2, mixing zirconium oxide, yttrium oxide, titanium oxide, modified hydroxyapatite and adhesive to obtain a paste, wherein the weight ratio of zirconium oxide, yttrium oxide, titanium oxide, modified hydroxyapatite and adhesive is 80-95: 15-20: 5-8: 5-10: 15-18; Step 3, extruding the paste to obtain a blank, drying, sintering, to obtain a zirconia ceramic rod; wherein the drying temperature is 130-150 DEG C, the drying time is 3-5h; the sintering temperature is 1200-1500 DEG C, and the sintering time is 10-12h.

2. The method of claim 1, wherein the zirconia ceramic rod is prepared by the steps of: The phosphate ester is one of hexadecyl phosphate ester and octadecyl phosphate ester. ​ 3. The method for preparing a zirconia ceramic rod according to claim 1, characterized in that, The particle size of the zirconium oxide is 600-800nm.

4. The method of claim 1, wherein the zirconia ceramic rod is prepared by the steps of: The particle size of the yttrium oxide is 200-400nm.

5. The method for preparing a zirconia ceramic rod according to claim 1, characterized in that, The particle size of the titanium oxide is 200-300nm.

6. The method of claim 1, wherein the zirconia ceramic rod is prepared by the steps of: The adhesive is carboxymethyl cellulose.

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