CN111675537A - Preparation method of modified toughened zirconia-based ceramic material and product thereof - Google Patents
Preparation method of modified toughened zirconia-based ceramic material and product thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a modified toughened zirconia-based ceramic material and a product thereof. The prepared material is a modified toughened zirconia-based ceramic material, and the chemical composition of the material is ZraYbbGecNddYeOxWherein a is 87.2-93.9, b is 3-6, c is 0.5-1.5, d is 1-2, e is 1.5-3, and x satisfies the total number of oxygen atoms required by the valence of other elements. The material provided by the invention has the characteristics of higher phase stability, high toughness and compactness, and the highest fracture toughness of the material can reach 12.33 MPa.m1/2Maximum hardness of 1130HV10(ii) a The bending strength is 910.3 MPa; the compactness was 98.3%.
Description
Technical Field
The invention belongs to the technical field of zirconia-based ceramics, and particularly relates to a preparation method of a modified toughened zirconia-based ceramic material and a product thereof.
Background
The protective tube is a circuit failure protector, when the current in the circuit reaches a certain preset value, the current is cut off to protect the circuit from passing too much current, and the circuit is prevented from being damaged. The ceramic fuse tube is mostly applied to intelligent instruments and other electronic devices, such as mobile phone chargers and the like, the structure and the shell of the fuse tube have the capabilities of isolating the external environment and resisting impact, the purpose of protecting the melt in the fuse tube and protecting the circuit within the specified parameters and requirements is achieved, and therefore for the ceramic fuse tube, the ceramic is required to have excellent mechanical properties, such as toughness, hardness, strength, pressure-bearing capacity and the like.
Zirconia ceramics find wide application in modern industrial fields, for example as extrusion and wire drawing dies, Solid Oxide Fuel Cells (SOFC)s) The catalyst or the catalyst carrier, the phase change toughening ceramic, the automobile engine part, the oxygen sensor, the thermal barrier coating for the aeroengine and the like.
Zirconia is widely used as a ceramic material, but the performance of zirconia as a ceramic material cannot meet the requirements of the existing practical production, so that the modification of zirconia is the main means for improving the performance of zirconia at present. Wherein the 3Y-TZP has the best combination of strength and toughness and is widely applied as structural ceramics. However, due to the sensitivity of stress-induced phase change toughening to temperature, the phase change toughening fails with the rise of temperature, and the medium-high temperature performance of zirconia is not ideal enough. Furthermore, hydrothermal aging makes its use in corresponding environments limited (e.g. repeated steam sterilization of medical tools, bioimplants, steam turbine components, etc.). The advantages of different rare earth stabilizers can be effectively combined by utilizing a co-doping stabilization method, wherein the Ce-Y co-stabilized zirconia has the advantages of 3Y-TZP and Ce-TZP, the mechanical property and the ageing resistance are relatively good, but compared with Y-TZP, the grain size is still larger, and the mechanical property still needs to be further improved. Because the toughness of the TZP is mainly ensured by stress-induced transformation toughening, which means that there is a certain limit to improving the toughness of the TZP in this way, and toughening the zirconia by using a proper second phase becomes an effective means. Therefore, how to further optimize the friction resistance and the high-temperature phase stability of the zirconium oxide while simultaneously realizing the strengthening and toughening of the zirconium oxide through the component design and the process optimization is a series of technical problems to be solved urgently. In addition, the distribution and content of the rare earth elements have great influence on the mechanical properties of the zirconia, the influence rule and mechanism of the interaction, distribution and content of the rare earth elements doped in the multi-element rare earth co-stabilized zirconia on the microstructure and the mechanical properties are not clear, the strengthening and toughening mechanism and the synergistic relationship among the mechanisms are not clear, and therefore, the improvement on the toughness, hardness, bending strength and compactness of the zirconia-based ceramic material still needs to be solved at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a modified toughened zirconia-based ceramic material and a product thereof, aiming at the defects in the prior art, wherein the modified toughened zirconia-based ceramic material has higher fracture toughness, hardness, bending strength and compactness, and the application of the modified toughened zirconia-based ceramic material in the manufacture of a fuse for charging a mobile phone.
The invention adopts the following technical scheme:
1. a preparation method of a modified toughened zirconia-based ceramic material comprises the following steps:
1) firstly, nanometer superfine ZrO is firstly prepared2Sieving the powder with a 200-mesh sieve;
2) the desired ZrO2，Yb2O3，GeO2，Nd2O3，Y2O3According to ZraYbbGecNddYeOxThe method comprises the following steps of weighing, placing the weighed materials in a ball milling tank for ball milling, wherein a is 87.2-93.9, b is 3-6, c is 0.5-1.5, d is 1-2, e is 1.5-3, and x meets the stoichiometric ratio of the total number of oxygen atoms required by the valence of other elements, and then placing the weighed materials in the ball milling tank for ball milling, wherein a ball milling medium is absolute ethyl alcohol;
3) after the ball milling is finished, the obtained suspension is dried in vacuum, grinding is carried out after drying, and the ground powder is sieved by a 200-mesh sieve;
4) calcining the sieved powder in a muffle furnace at 700-850 ℃ for 1-2.5 h, granulating the obtained powder after calcining, preforming the granulated powder by a tablet press, pressing the preformed powder under 200-300 MPa to obtain a blank, sintering the obtained blank in the muffle furnace at 1350-1600 ℃ for 1-3 h, and cooling the blank to room temperature along with the furnace to obtain the ceramic.
Preferably, the ball milling tank in the step 2) is a polyethylene ball milling tank, and 3Y-TZP balls are used for ball milling.
Preferably, the step 2) further comprises 2 wt% of alumina.
Preferably, the ball milling speed in the step 2) is 330-400 r/min, and the ball milling time is 8-14 h.
Preferably, the vacuum drying in the step 3) is drying for 16-24 hours in a vacuum oven at 65-80 ℃ to remove ethanol.
Preferably, in the step 4), the temperature rise rate of calcining at 700-850 ℃ for 1-2.5 h is 4-6 ℃/min; the temperature rise rate of sintering at 1350-1600 ℃ for 1-3 h is 10 ℃/min. The other technical scheme of the invention is that the modified toughened zirconia-based ceramic material is prepared based on the preparation method.
Preferably, the fracture toughness of the modified toughened zirconia-based ceramic material is 11.45-12.33 MPa-m1/2The highest hardness is 1100-1130 HV10(ii) a The bending strength is 894.5-910.3 MPa; the compactness is 98.1-98.3%.
The invention also provides a technical scheme of application of the multi-element toughened zirconia-based ceramic material in manufacturing of the protective tube for charging the mobile phone based on the application of the multi-element toughened zirconia-based ceramic material.
Compared with the prior art, the invention has at least the following beneficial effects:
1) the modified toughened zirconia-based ceramic material provided by the invention is prepared by mixing, wet grinding, drying, grinding, sieving, pre-sintering, compression molding and sintering raw materials, the preparation process is simple, and the formed modified toughened zirconia-based ceramic material has high density and excellent main mechanical indexes, and is suitable for industrial popularization.
2) The alumina additive is added in the ball milling process, so that the compactness of the zirconia ceramic material is improved.
3) The fracture toughness, hardness, bending strength and compactness of the zirconia-based ceramic material are improved through the synergistic effect of multiple elements, and the fracture toughness of the zirconia-based ceramic material obtained through co-doping of multiple rare earths is 11.45-12.33 MPa-m1/2The highest hardness is 1100-1130 HV10(ii) a The bending strength is 894.5-910.3 MPa; the compactness is 98.1-98.3%.
In conclusion, the modified toughened zirconia-based ceramic material prepared by the invention is an ideal material for practical application, and is particularly applied to manufacturing of a fuse tube for charging a mobile phone.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The invention discloses a preparation method of a modified toughened zirconia-based ceramic material, which comprises the following steps:
1) firstly, nanometer superfine ZrO is firstly prepared2Sieving the powder with a 200-mesh sieve;
2) the desired ZrO2，Yb2O3，GeO2，Nd2O3，Y2O3According to ZraYbbGecNddYeOxThe method comprises the following steps of weighing, adding 2 wt% of alumina, putting the alumina into a polyethylene ball milling tank, and carrying out ball milling by using 3Y-TZP balls, wherein a is 87.2-93.9, b is 3-6, c is 0.5-1.5, d is 1-2, e is 1.5-3, and x meets the stoichiometric ratio of the total number of oxygen atoms required by the valence of other elements, wherein the ball milling medium is absolute ethyl alcohol; the ball milling speed is 330-400 r/min, and the ball milling time is 8-14 h;
3) after the ball milling is finished, drying the obtained powder in a vacuum oven at 65-80 ℃ for 16-24 h to remove ethanol, grinding the dried powder, and sieving the ground powder with a 200-mesh sieve;
4) calcining the sieved powder in a muffle furnace at 700-850 ℃ for 1-2.5 h, wherein the heating rate is 4-6 ℃/min, granulating the obtained powder after calcining, preforming the granulated powder through a tablet press, pressing the preformed powder under 200-300 MPa to form a blank, sintering the obtained blank in the muffle furnace at 1350-1600 ℃ for 1-3 h, wherein the heating rate is 10 ℃/min, and cooling to room temperature along with the furnace to obtain the ceramic.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. The components of the embodiments of the present invention generally shown may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a modified toughened zirconia-based ceramic material comprises the following steps:
1) firstly, nanometer superfine ZrO is firstly prepared2Sieving the powder with a 200-mesh sieve;
2) the desired ZrO2，Yb2O3，GeO2，Nd2O3，Y2O3According to ZraYbbGecNddYeOxWherein a is 90.5, b is 4.5, c is 1, d is 1.5, e is 2.5, x satisfies the stoichiometric ratio of the total number of oxygen atoms required by the valence of other elements, 2 wt% of alumina is added, and then the mixture is placed in a polyethylene ball milling tank to be ball milled by 3Y-TZP balls, wherein the ball milling medium is absolute ethyl alcohol; the ball milling speed is 380r/min, and the ball milling time is 12 h;
3) after the ball milling is finished, drying the obtained powder in a vacuum oven at 80 ℃ for 24 hours to remove ethanol, grinding the dried powder, and sieving the ground powder with a 200-mesh sieve;
4) calcining the sieved powder in a muffle furnace at 800 ℃ for 2h, wherein the heating rate is 5 ℃/min, granulating the obtained powder after calcining, preforming the granulated powder by a tablet press, pressing the preformed powder under 300MPa to form a blank, sintering the obtained blank in the muffle furnace at 1600 ℃ for 2h, wherein the heating rate is 10 ℃/min, and cooling to room temperature along with the furnace to obtain the ceramic.
Example 2
A preparation method of a modified toughened zirconia-based ceramic material comprises the following steps:
1) firstly, nanometer superfine ZrO is firstly prepared2Sieving the powder with a 200-mesh sieve;
2) the desired ZrO2，Yb2O3，GeO2，Nd2O3，Y2O3According to ZraYbbGecNddYeOxWeighing the components in a stoichiometric ratio of a to 91.5, b to 4, c to 0.5, d to 2, e to 2 and x to satisfy the total oxygen atom number required by the valence of other elements, adding 2 wt% of alumina, and ball-milling the components in a polyethylene ball-milling tank by using 3Y-TZP balls, wherein the ball-milling medium is absolute ethyl alcohol; the ball milling speed is 380r/min, and the ball milling time is 12 h;
3) after the ball milling is finished, drying the obtained powder in a vacuum oven at 75 ℃ for 24h to remove ethanol, grinding the dried powder, and sieving the ground powder with a 200-mesh sieve;
4) calcining the sieved powder in a muffle furnace at 850 ℃ for 1.5h, wherein the heating rate is 6 ℃/min, granulating the obtained powder after calcining, preforming the granulated powder by a tablet press, pressing under 250MPa to obtain a blank, sintering the obtained blank in the muffle furnace at 1500 ℃ for 3h, wherein the heating rate is 10 ℃/min, and cooling to room temperature along with the furnace to obtain the ceramic.
Comparative example has the formula ZraYbbGecNddYeOxThe preparation parameters and conditions were the same as in example 1 except that a, b, c, d and e were different, and the specific parameters are shown in Table 1:
TABLE 1 Main Properties of zirconia-based materials
In conclusion, the modified toughened zirconia-based ceramic material prepared by the invention is an ideal ceramic material due to high fracture toughness, high hardness, high bending strength and high compactness, and the comparison between the example 1 and the comparative examples 1-13 shows that the components have a synergistic effect, and the addition of Yb, Ge, Nd and Y can improve the fracture toughness, hardness, bending strength and compactness of the zirconia-based ceramic material.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A preparation method of a modified toughened zirconia-based ceramic material is characterized by comprising the following steps: the preparation method comprises the following steps:
1) firstly, nanometer superfine ZrO is firstly prepared2Sieving the powder with a 200-mesh sieve;
2) the desired ZrO2，Yb2O3，GeO2，Nd2O3，Y2O3According to ZraYbbGecNddYeOxThe method comprises the following steps of weighing, placing the weighed materials in a ball milling tank for ball milling, wherein a is 87.2-93.9, b is 3-6, c is 0.5-1.5, d is 1-2, e is 1.5-3, and x meets the stoichiometric ratio of the total number of oxygen atoms required by the valence of other elements, and then placing the weighed materials in the ball milling tank for ball milling, wherein a ball milling medium is absolute ethyl alcohol;
3) after the ball milling is finished, the obtained suspension is dried in vacuum, grinding is carried out after drying, and the ground powder is sieved by a 200-mesh sieve;
4) calcining the sieved powder in a muffle furnace at 700-850 ℃ for 1-2.5 h, granulating the obtained powder after calcining, preforming the granulated powder by a tablet press, pressing the preformed powder under 200-300 MPa to obtain a blank, sintering the obtained blank in the muffle furnace at 1350-1600 ℃ for 1-3 h, and cooling the blank to room temperature along with the furnace to obtain the ceramic.
2. The method of claim 1, wherein: the ball milling tank in the step 2) is a polyethylene ball milling tank, and 3Y-TZP balls are used for ball milling.
3. The method of claim 1, wherein: the step 2) also comprises 2 wt% of alumina.
4. The method of claim 1, wherein: in the step 2), the ball milling speed is 330-400 r/min, and the ball milling time is 8-14 h.
5. The method of claim 1, wherein: the vacuum drying in the step 3) is drying for 16-24 hours in a vacuum oven at 65-80 ℃ to remove ethanol.
6. The method of claim 1, wherein: in the step 4), the temperature rise rate of calcining at 700-850 ℃ for 1-2.5 h is 4-6 ℃/min; the temperature rise rate of sintering at 1350-1600 ℃ for 1-3 h is 10 ℃/min.
7. A modified toughened zirconia-based ceramic material prepared by the method of any one of claims 1 to 6.
8. The modified toughened zirconia-based ceramic material of claim 7, wherein: the modified toughened zirconia-based ceramic material has the fracture toughness of 11.45-12.33 MPa-m1/2The highest hardness is 1100-1130 HV10(ii) a The bending strength is 894.5-910.3 MPa; the compactness is 98.1-98.3%.
9. The use of the multi-element toughened zirconia-based ceramic material of claim 7 or 8 in the manufacture of a fuse for charging a mobile phone.
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| CN114195489A (en) * | 2021-11-18 | 2022-03-18 | 新化县众鑫陶瓷有限公司 | Method for manufacturing high-breaking ceramic fuse tube ceramic body |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195489A (en) * | 2021-11-18 | 2022-03-18 | 新化县众鑫陶瓷有限公司 | Method for manufacturing high-breaking ceramic fuse tube ceramic body |
| CN114195489B (en) * | 2021-11-18 | 2023-02-17 | 新化县众鑫陶瓷有限公司 | Method for manufacturing high-breaking ceramic fuse tube ceramic body |
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Application publication date: 20200918 |