CN108546138B - Nano zirconia ceramic material and preparation method thereof - Google Patents
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Abstract
The invention provides a nano zirconia ceramic material and a preparation method thereof, which is prepared by taking yttrium-stabilized nano zirconia as a matrix, adding micron alumina as a reinforcing phase, taking nano iron sesquioxide, nano calcium carbonate and boron nitride as sintering aids and carrying out hot-pressing sintering. The ceramic tool and die has better comprehensive mechanical property, high hardness and wear resistance, and good toughness.
Description
Technical Field
The invention belongs to the technical field of ceramic tool and die materials, and particularly relates to a nano zirconia ceramic material and a preparation method thereof.
Background
The ceramic cutter has high hardness and wear resistance, shows excellent cutting performance in high-speed cutting and dry cutting, and is a cutter material with great development prospect. However, most of the currently applied ceramic cutting tool materials are limited to micron composite ceramics, and the mechanical properties, especially the strength and toughness of the materials are still to be further improved. According to the Hall-pitch relationship: the smaller the grain size, the higher the strength of the ceramic material. Therefore, the research and development of nano-modified nano-micron composite ceramic cutting tool materials are one of the main directions for the development of cutting tool materials in the future. The nano composite ceramic cutting tool material which has been studied so far mainly comprises Si3N4/TiNn、Si3N4/TiCn、Si3N4-Al2O3n-TiC-Y2O3、Al2O3/TiC/SiCn、Al2O3/TiCn、Al2O3/Al2O3n/SiCn、Al2O3/Ti(C0.7N0.3)n/SiCn、Al2O3/SiC/SiCn、Al2O3the/TiC/TiNn and the like have better mechanical property and cutting property than micron composite ceramic cutter materials.
Zirconia ceramics have excellent mechanical properties, have been a hot topic in experimental and theoretical research, and have been widely used as structural ceramics, wear-resistant and corrosion-resistant ceramics, high-temperature electrolyte materials and the like in the industrial fields of ceramics, machinery, chemical engineering, electronics, energy and the like. Wherein, the yttria-stabilized tetragonal polycrystalline zirconia material is one of zirconia toughened ceramics. The sintering temperature is low, the interior of the material contains high-content tetragonal zirconia phase at room temperature, the phase change toughening effect is achieved, and the excellent mechanical property is shown. If the magnetic particle dispersion phase is added into the zirconia matrix, the excellent mechanical property of the zirconia matrix is considered, the property of the zirconia matrix in the aspect of function is increased, the application field of the zirconia matrix is widened, and the structure-function integration is realized.
As can be seen from the existing research, the ceramic material still has the problems of high cost, insufficient toughness, large brittleness, uneven hardness, poor heat dissipation, poor self-lubrication and the like, and needs to be solved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a nano zirconia ceramic material, and the ceramic tool and die has better comprehensive mechanical properties, high hardness and wear resistance, and good toughness.
The technical scheme of the invention is realized as follows:
a nanometer zirconia ceramic material is prepared by taking yttrium-stabilized nanometer zirconia as a matrix, adding micrometer alumina as a reinforcing phase, taking nanometer ferric oxide, nanometer calcium carbonate and boron nitride as sintering aids, and performing hot-pressing sintering, wherein the nanometer zirconia ceramic material comprises the following raw material components in percentage by weight: 7-15% of micron aluminum oxide, 1-3% of nano calcium carbonate, 0.6-1.2% of boron nitride, 2-5% of nano ferric oxide and the balance yttrium-stabilized nano zirconium oxide; wherein, the sintering aid needs to be pretreated.
In some preferred embodiments of the present invention, the method for pretreating the sintering aid comprises: firstly, putting nano ferric oxide and nano calcium carbonate into a water solution of hydroxyl cellulose for stirring and dispersing, then adding boron nitride for stirring and dispersing, filtering, washing a filter cake, then carrying out vacuum drying, and then grinding.
In some preferred embodiments of the present invention, the mass concentration of the hydroxycellulose in the aqueous solution of hydroxycellulose is 2 to 6%.
In some preferred embodiments of the present invention, the yttrium-stabilized nanozirconia comprises 4 to 6 mol% yttrium.
Another object of the present invention is to provide a method for preparing a nano zirconia ceramic material, comprising the following steps:
(1) weighing yttrium-stabilized nano zirconia according to a proportion, taking polyvinyl alcohol as a dispersing agent, taking the mass of the yttrium-stabilized nano zirconia as a base number, adding 0.2-1.0 wt% of the dispersing agent, taking a proper amount of absolute ethyl alcohol as a dispersion medium, preparing yttrium-stabilized zirconia suspension, stirring and ultrasonically dispersing, and adjusting the pH value of the suspension to 3-4;
(2) weighing alumina according to a certain proportion, carrying out ball milling, continuously drying at the temperature of 110-120 ℃ in an electric heating vacuum drying oven, completely drying, sieving in inert gas flow, adding absolute ethyl alcohol to prepare alumina suspension, and fully stirring and ultrasonically dispersing;
(3) uniformly mixing the yttrium-stabilized nano zirconia suspension obtained in the step 1), the alumina suspension obtained in the step 2) and a sintering aid, adding an organic binder solvent, fully mixing and grinding, sintering by a hot pressing method, and pressing and sintering the ground mixture in a hot pressing furnace for molding.
In some preferred embodiments of the present invention, the sintering process parameters in the hot pressing method in step (3) are: the heat preservation temperature is 1150-1250 ℃, the hot pressing pressure is 18-28 MPa, the heat preservation time is 40-80 min, and the temperature rise rate is 15-25 ℃/min.
In some preferred embodiments of the present invention, the organic binder solvent is a mixture of PVB and isopropyl alcohol in a weight ratio of 1: 2.
The invention has the beneficial effects that:
according to the invention, the pretreated sintering aid of the nano iron sesquioxide, the nano calcium carbonate and the boron nitride is used for replacing the traditional magnesium oxide and silicon oxide as the sintering aid, and the nano iron sesquioxide is found to promote sintering and improve the hardness and the wear resistance of the ceramic. After the nano ferric oxide, the nano calcium carbonate and the boron nitride are subjected to the hydroxycellulose soaking treatment, a unique strengthening and toughening mechanism is formed by the nano ferric oxide, the nano calcium carbonate and the boron nitride and other components, and the synergistic effect of a plurality of toughening and reinforcing mechanisms such as zirconium oxide phase change toughening, crack deflection, crack branching, crack bridging and the like is realized, so that the mechanical property of the material is improved, the toughness of the ceramic material can be obviously improved, the porosity of the material is rapidly reduced, the density of the material is improved, and the sintering temperature of a tetragonal polycrystalline zirconium oxide (TZP) material is reduced to a greater extent.
Detailed Description
Example 1
A nanometer zirconia ceramic material is prepared by taking yttrium-stabilized nanometer zirconia as a matrix, adding micrometer alumina as a reinforcing phase, taking nanometer ferric oxide, nanometer calcium carbonate and boron nitride as sintering aids, and performing hot-pressing sintering, wherein the nanometer zirconia ceramic material comprises the following raw material components in percentage by weight: 10% of micron aluminum oxide, 2% of nano calcium carbonate, 0.8% of boron nitride, 3% of nano iron oxide and the balance of yttrium-stabilized nano zirconia, wherein the nano zirconia contains 5 mol% of yttrium; the pretreatment method of the sintering aid comprises the following steps: firstly, putting nano ferric oxide and nano calcium carbonate into a hydroxyl cellulose aqueous solution with the mass concentration of 4% for stirring and dispersing, then adding boron nitride for stirring and dispersing, filtering, washing a filter cake, then performing vacuum drying, and then grinding.
The preparation method of the nano zirconia ceramic material comprises the following steps:
(1) weighing yttrium-stabilized nano zirconia according to a proportion, taking polyvinyl alcohol as a dispersing agent, taking the mass of the yttrium-stabilized nano zirconia as a base number, adding 0.7 wt% of the dispersing agent, taking a proper amount of absolute ethyl alcohol as a dispersion medium, preparing yttrium-stabilized zirconia suspension, stirring and ultrasonically dispersing, and adjusting the pH value of the suspension to 3;
(2) weighing alumina according to a certain proportion, ball-milling, continuously drying at 110 ℃ in an electric heating vacuum drying oven, completely drying, sieving in inert gas flow, adding absolute ethyl alcohol to prepare alumina suspension, and fully stirring and ultrasonically dispersing;
(3) uniformly mixing the yttrium-stabilized nano zirconia suspension obtained in the step 1), the alumina suspension obtained in the step 2) and a sintering aid, adding an organic binder solvent (the organic binder solvent is formed by mixing PVB and isopropanol according to a weight ratio of 1: 2), fully mixing and grinding, sintering by a hot pressing method, and pressing and sintering the ground mixture in a hot pressing furnace for molding. The sintering technological parameters of the hot pressing method are as follows: the heat preservation temperature is 1140 ℃, the hot pressing pressure is 25MPa, the heat preservation time is 60min, the heating rate is 18 ℃/min, and the heat preservation is carried out for 120min at the temperature of 1000 ℃.
Cutting the prepared ceramic material sample, and measuring the mechanical property parameters as follows: flexural strength 1180MPa and fracture toughness 13.15 MPa-m1/2And a Vickers hardness of 18.32 GPa.
Example 2
A nanometer zirconia ceramic material is prepared by taking yttrium-stabilized nanometer zirconia as a matrix, adding micrometer alumina as a reinforcing phase, taking nanometer ferric oxide, nanometer calcium carbonate and boron nitride as sintering aids, and performing hot-pressing sintering, wherein the nanometer zirconia ceramic material comprises the following raw material components in percentage by weight: 7% of micron aluminum oxide, 3% of nano calcium carbonate, 0.6% of boron nitride, 5% of nano iron oxide and the balance of yttrium-stabilized nano zirconium oxide, wherein the nano zirconium oxide contains 4 mol% of yttrium; the pretreatment method of the sintering aid comprises the following steps: firstly, putting nano ferric oxide and nano calcium carbonate into a 2% hydroxyl cellulose water solution by mass concentration, stirring and dispersing, then adding boron nitride, stirring and dispersing, filtering, washing a filter cake, then performing vacuum drying, and then grinding.
The preparation method of the nano zirconia ceramic material comprises the following steps:
(1) weighing yttrium-stabilized nano zirconia according to a proportion, taking polyvinyl alcohol as a dispersing agent, taking the mass of the yttrium-stabilized nano zirconia as a base number, adding 0.2 wt% of the dispersing agent, taking a proper amount of absolute ethyl alcohol as a dispersion medium, preparing yttrium-stabilized zirconia suspension, stirring and ultrasonically dispersing, and adjusting the pH value of the suspension to be 4;
(2) weighing alumina according to a certain proportion, ball-milling, continuously drying in an electrothermal vacuum drying oven at 120 ℃, sieving in inert gas flow after completely drying, adding absolute ethyl alcohol to prepare alumina suspension, fully stirring and ultrasonically dispersing;
(3) uniformly mixing the yttrium-stabilized nano zirconia suspension obtained in the step 1), the alumina suspension obtained in the step 2) and a sintering aid, adding an organic binder solvent (the organic binder solvent is formed by mixing PVB and isopropanol according to a weight ratio of 1: 2), fully mixing and grinding, sintering by a hot pressing method, and pressing and sintering the ground mixture in a hot pressing furnace for molding. The sintering technological parameters of the hot pressing method are as follows: the heat preservation temperature is 1150 ℃, the hot pressing pressure is 18MPa, the heat preservation time is 80min, the heating rate is 15 ℃/min, and 100 heat preservation is applied at 1000 ℃.
Cutting the prepared ceramic material sample, and measuring the mechanical property parameters as follows: bending strength 1086MPa, fracture toughness 12.35 MPa.m1/2And a Vickers hardness of 17.16 GPa.
Example 3
A nanometer zirconia ceramic material is prepared by taking yttrium-stabilized nanometer zirconia as a matrix, adding micrometer alumina as a reinforcing phase, taking nanometer ferric oxide, nanometer calcium carbonate and boron nitride as sintering aids, and performing hot-pressing sintering, wherein the nanometer zirconia ceramic material comprises the following raw material components in percentage by weight: 15% of micron aluminum oxide, 1% of nano calcium carbonate, 1.2% of boron nitride, 2% of nano iron oxide and the balance of yttrium-stabilized nano zirconia, wherein the nano zirconia contains 6 mol% of yttrium; the pretreatment method of the sintering aid comprises the following steps: firstly, putting nano ferric oxide and nano calcium carbonate into a hydroxy cellulose aqueous solution with the mass concentration of 6 percent, stirring and dispersing, then adding boron nitride, stirring and dispersing, filtering, washing a filter cake, then carrying out vacuum drying, and then grinding.
The preparation method of the nano zirconia ceramic material comprises the following steps:
(1) weighing yttrium-stabilized nano zirconia according to a proportion, taking polyvinyl alcohol as a dispersing agent, taking the mass of the yttrium-stabilized nano zirconia as a base number, adding 1.0 wt% of the dispersing agent, taking a proper amount of absolute ethyl alcohol as a dispersion medium, preparing yttrium-stabilized zirconia suspension, stirring and ultrasonically dispersing, and adjusting the pH value of the suspension to be 4;
(2) weighing alumina according to a certain proportion, ball-milling, continuously drying in an electrothermal vacuum drying oven at 120 ℃, sieving in inert gas flow after completely drying, adding absolute ethyl alcohol to prepare alumina suspension, fully stirring and ultrasonically dispersing;
(3) uniformly mixing the yttrium-stabilized nano zirconia suspension obtained in the step 1), the alumina suspension obtained in the step 2) and a sintering aid, adding an organic binder solvent (the organic binder solvent is formed by mixing PVB and isopropanol according to a weight ratio of 1: 2), fully mixing and grinding, sintering by a hot pressing method, and pressing and sintering the ground mixture in a hot pressing furnace for molding. The sintering technological parameters of the hot pressing method are as follows: the heat preservation temperature is 1250 ℃, the hot pressing pressure is 28MPa, the heat preservation time is 40min, the heating rate is 25 ℃/min, and the heat preservation is carried out for 150min at 1000 ℃.
Cutting the prepared ceramic material sample, and measuring the mechanical property parameters as follows: bending strength of 1148MPa and fracture toughness of 12.11MPa m1/2And a Vickers hardness of 17.45 GPa.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The nanometer zirconia ceramic material is characterized by being prepared by taking yttrium-stabilized nanometer zirconia as a matrix, adding micrometer alumina as a reinforcing phase, taking nanometer ferric oxide, nanometer calcium carbonate and boron nitride as sintering aids and sintering by hot pressing, wherein the nanometer zirconia ceramic material comprises the following raw materials in percentage by weight: 7-15% of micron aluminum oxide, 1-3% of nano calcium carbonate, 0.6-1.2% of boron nitride, 2-5% of nano ferric oxide and the balance yttrium-stabilized nano zirconium oxide; wherein the sintering aid needs to be pretreated;
the pretreatment method of the sintering aid comprises the following steps: firstly, putting nano ferric oxide and nano calcium carbonate into a water solution of hydroxyl cellulose for stirring and dispersing, then adding boron nitride for stirring and dispersing, filtering, washing a filter cake, then carrying out vacuum drying, and then grinding.
2. The nano zirconia ceramic material of claim 1, wherein the pretreatment method of the sintering aid comprises: firstly, putting nano ferric oxide and nano calcium carbonate into a water solution of hydroxyl cellulose for stirring and dispersing, then adding boron nitride for stirring and dispersing, filtering, washing a filter cake, then carrying out vacuum drying, and then grinding.
3. The nano zirconia ceramic material of claim 2, wherein the mass concentration of the hydroxycellulose in the aqueous solution of hydroxycellulose is 2-6%.
4. The nano zirconia ceramic material of claim 1 wherein the yttrium stabilized nano zirconia comprises 4 to 6 mol% yttrium.
5. The method for preparing nano zirconia ceramic material according to any one of claims 1 to 4, comprising the steps of:
(1) weighing yttrium-stabilized nano zirconia according to a proportion, taking polyvinyl alcohol as a dispersing agent, taking the mass of the yttrium-stabilized nano zirconia as a base number, adding 0.2-1.0 wt% of the dispersing agent, taking a proper amount of absolute ethyl alcohol as a dispersion medium, preparing yttrium-stabilized zirconia suspension, stirring and ultrasonically dispersing, and adjusting the pH value of the suspension to 3-4;
(2) weighing alumina according to a certain proportion, carrying out ball milling, continuously drying at the temperature of 110-120 ℃ in an electric heating vacuum drying oven, completely drying, sieving in inert gas flow, adding absolute ethyl alcohol to prepare alumina suspension, and fully stirring and ultrasonically dispersing;
(3) uniformly mixing the yttrium-stabilized nano zirconia suspension obtained in the step 1), the alumina suspension obtained in the step 2) and a sintering aid, adding an organic binder solvent, fully mixing and grinding, sintering by a hot pressing method, and pressing and sintering the ground mixture in a hot pressing furnace for molding.
6. The preparation method of the nano zirconia ceramic material according to claim 5, wherein the sintering process parameters of the hot pressing method in the step (3) are as follows: the heat preservation temperature is 1150-1250 ℃, the hot pressing pressure is 18-28 MPa, the heat preservation time is 40-80 min, and the temperature rise rate is 15-25 ℃/min.
7. The method for preparing nano zirconia ceramic material according to claim 5, wherein the organic binder solvent is a mixture of PVB and isopropanol in a weight ratio of 1: 2.
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| CN104649655A (en) * | 2015-02-14 | 2015-05-27 | 济南大学 | Preparation method of special low-density grinding ball for cement grinding mill |
| CN106747433A (en) * | 2017-02-28 | 2017-05-31 | 安徽拓吉泰新型陶瓷科技有限公司 | Zirconium oxide-based nano ceramic tool die material and preparation method thereof |
| CN106977198A (en) * | 2017-03-13 | 2017-07-25 | 南京云启金锐新材料有限公司 | Hot pressed sintering zirconia composite ceramics insulating part and preparation method thereof |
| CN108033796A (en) * | 2017-12-08 | 2018-05-15 | 安徽雷萨重工机械有限公司 | A kind of refractory material of high-strength mechanical properties |
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| CN104649655A (en) * | 2015-02-14 | 2015-05-27 | 济南大学 | Preparation method of special low-density grinding ball for cement grinding mill |
| CN106747433A (en) * | 2017-02-28 | 2017-05-31 | 安徽拓吉泰新型陶瓷科技有限公司 | Zirconium oxide-based nano ceramic tool die material and preparation method thereof |
| CN106977198A (en) * | 2017-03-13 | 2017-07-25 | 南京云启金锐新材料有限公司 | Hot pressed sintering zirconia composite ceramics insulating part and preparation method thereof |
| CN108033796A (en) * | 2017-12-08 | 2018-05-15 | 安徽雷萨重工机械有限公司 | A kind of refractory material of high-strength mechanical properties |
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