CN117658632A - High-hardness high-wear-resistance ceramic material for ceramic tiles and preparation method thereof - Google Patents
High-hardness high-wear-resistance ceramic material for ceramic tiles and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 125
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 80
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 238000003825 pressing Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 28
- 239000003792 electrolyte Substances 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 239000011812 mixed powder Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000012466 permeate Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 17
- 238000005299 abrasion Methods 0.000 description 16
- 239000013078 crystal Substances 0.000 description 8
- 238000002490 spark plasma sintering Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 4
- -1 aluminum ions Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009770 conventional sintering Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 210000003464 cuspid Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The invention belongs to the technical field of material preparation, and particularly discloses a high-hardness high-wear-resistance ceramic material for ceramic tiles and a preparation method thereof, wherein the ceramic material comprises the following components in detail from bottom to top: 8-10mm of ceramic matrix and 60-70 mu m of wear-resistant layer; the ceramic matrix is a blank body obtained by pressing and sintering raw materials; the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :80-90 parts of Cr 2 O 3 :75-80 parts of Nb 2 O 5 :135-140 parts, ta 2 O 5 :220-230 parts of MoO 3 :145-160 parts of C:48-60 parts; the invention adopts discharge sintering to prepare the ceramic matrix and micro-arc oxidation to prepare the wear-resistant layer, thus realizing the enhancement of the wear resistance and hardness of the ceramic.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a high-hardness high-wear-resistance ceramic material for ceramic tiles and a preparation method thereof.
Background
With the continuous development of ceramic materials, the ceramic materials are widely applied to life by virtue of excellent mechanical properties, and in recent years, a series of high-hardness and wear-resistant ceramic materials such as diamond glaze, wear-resistant bricks and the like appear on the market; at present, the ceramic material is mainly used for improving the hardness and the wear resistance by adjusting the components of the glaze to increase the compactness of a glass network structure, such as increasing the silicon content in the glaze, but the sintering temperature of the traditional ceramic is about 1200 ℃, the large increase of the silicon and aluminum content can lead to the temperature rise of the glaze, the overlarge viscosity is caused, the surface flatness is reduced, the air bubbles in the ceramic are not easy to discharge, and the comprehensive mechanical property of the ceramic is further reduced; the daily ceramic needs to be scraped by hard metal such as knife and fork for a long time in the use process, and has higher requirements on the hardness and the wear resistance of ceramic materials, so that the market needs a ceramic material with high hardness and high wear resistance;
the micro-arc oxidation technology is an emerging surface modification technology, has the characteristics of strong operability, high efficiency, low cost, small pollution and the like, and the film prepared by the micro-arc oxidation technology has high hardness, good wear resistance and corrosion resistance and wide application prospect.
Disclosure of Invention
Aiming at the situation, the invention provides the ceramic material with high hardness and high wear resistance for the ceramic tile and the preparation method thereof, and aims to solve the problems of low hardness and poor wear resistance of the ceramic material.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the invention provides a high-hardness high-wear-resistance ceramic material for ceramic tiles, which comprises the following components in detail from bottom to top: 8-10mm of ceramic matrix and 60-70 mu m of wear-resistant layer.
The ceramic matrix is a blank body obtained by pressing and sintering raw materials;
the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :80-90 parts of Cr 2 O 3 :75-80 parts of Nb 2 O 5 :135-140 parts, ta 2 O 5 :220-230 parts of MoO 3 :145-160 parts of C:48-60 parts.
The invention also provides a preparation method of the high-hardness high-wear-resistance ceramic material for the ceramic tile, which specifically comprises the following steps:
(1) Preparing a ceramic matrix: weighing TiO 2 、Cr 2 O 3 、Nb 2 O 5 、Ta 2 O 5 、MoO 3 Placing the powder C in a roller ball milling tank, adding absolute ethyl alcohol for ball milling, wherein the ball milling medium is silicon nitride, filtering, drying, grinding and sieving with a 100-mesh sieve to obtain mixed powder;
(2) Preparing a ceramic matrix: placing the mixed powder obtained in the step (1) into a die, prepressing the mixed powder by adopting a tablet press, placing the die loaded with the mixed powder into a discharge plasma sintering furnace, pressing the die in the sintering process, setting the pressure to 3000MPa, sintering by adopting direct current pulse, wherein the current lasts for 15ms, taking the intermittent 3ms as a pulse, and heating and preserving the heat at intervals of 5ms after 10 current pulses, cooling to 600 ℃ at the cooling rate of 100 ℃/min, and cooling along with the furnace to obtain a ceramic matrix;
(3) And (3) preparing a wear-resistant layer: polishing the ceramic matrix obtained in the step (2) by 2000-mesh sand paper for 2min, placing the polished ceramic matrix in an electrolytic cell to ensure that electrolyte can completely permeate the ceramic matrix, wherein the electrolyte is prepared from Na (PO) 3 ) 6 、Na 2 SiO 3 、Na 2 WO 4 、NaAlO 2 And water, adopting a carbon rod as a cathode, adopting the ceramic matrix obtained in the step (2) as an anode, adjusting the pH of electrolyte to 10-11, and setting the forward current density to 5A/dm 2 A negative current density of 1A/dm 2 The frequency is 500Hz, the duty ratio is 30%, the voltage is rapidly increased from 0V to 500V within 5min, the temperature is kept for 60-80min, and the ceramic material is obtained after cooling and drying.
Preferably, in the step (1), the ball-to-liquid ratio is 4:1:2, the ball milling rotating speed is 80-100r/min, and the ball milling time is 22-24h; the drying temperature is 60-65 ℃ and the drying time is 24 hours;
preferably, in the step (2), the pre-pressing treatment pressure is set to 10MPa, and the pre-pressing treatment time is 1.5-2h; the heating rate is 100 ℃/min, the heating temperature is 1600-1700 ℃, and the heat preservation time is 10-12min;
preferably, in step (3), na (PO 3 ) 6 With Na and Na 2 SiO 3 The mass ratio of Na is 1:1 2 WO 4 With NaAlO 2 The mass ratio of Na is 1:1 2 SiO 3 With NaAlO 2 The mass ratio of (2) to (1), the concentration of the electrolyte is 1.2-1.25g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The drying temperature is 60-65deg.C, and the drying time is 8-10h.
The beneficial effects obtained by the invention are as follows:
the ceramic substrate is prepared by adopting discharge sintering on raw materials, and the wear resistance and hardness of the ceramic are enhanced by adopting a mode of preparing a wear-resistant layer by micro-arc oxidation; the raw materials are sintered into a ceramic matrix by spark plasma, pulse current is generated in the spark plasma sintering process, plasma is contained in the pulse current, pressure is applied in the sintering process, and the combined action of the plasma and the pressure is beneficial to reducing the sintering temperature of the powder, so that the powder can be sintered and densified rapidly; the spark plasma sintering has the characteristics of uniform heating, high heating speed, low sintering temperature, short sintering time and high production efficiency, the heating speed is high, the sintering temperature is low, the sintering time is short, the growth of crystal grains can be avoided, the ceramic crystal grains are fine, the fine crystal strengthening effect is generated, the tissue density is increased, and the hardness and the wear resistance of the ceramic are increased; the uniform heating ensures the uniform size of ceramic grains, effectively reduces the stress concentration generated in the ceramic material, and improves the comprehensive mechanical properties of the ceramic; aluminum ions and tungsten ions in the electrolyte form a wear-resistant layer on the surface of the ceramic matrix, micro-arc oxidation is carried out under the action of current and pressure to form a tungsten oxide and aluminum oxide composite metal layer, and aluminum oxide is of a hexagonal structure, so that the hardness and wear resistance of the ceramic material can be remarkably improved; the wear-resistant layer consists of a crystalline phase and an amorphous phase, so that the hardness and deformation characteristics of the wear-resistant layer are combined, and the wear-resistant performance of the wear-resistant layer is improved; the wear-resistant layer grows from the ceramic matrix in situ, is metallurgically combined with the ceramic matrix, is more tightly combined with the ceramic matrix, and the hardness and wear resistance of the ceramic material are enhanced.
Drawings
FIG. 1 is a graph showing the microhardness results of a ceramic material with high hardness and high wear resistance for ceramic tiles;
FIG. 2 is a graph of the abrasion resistance test result of the ceramic material with high hardness and high abrasion resistance for ceramic tiles;
FIG. 3 is a surface SEM result diagram of a ceramic material with high hardness and high wear resistance for ceramic tiles, which is obtained by the invention;
FIG. 4 is a SEM result chart of a fused cross section of a ceramic material with high hardness and high wear resistance for ceramic tiles, which is obtained by the invention;
FIG. 5 is a graph showing the macroscopic morphology results of a ceramic material with high hardness and high wear resistance for ceramic tiles.
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present invention. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the scope of the present application.
The experimental methods in the following examples are all conventional methods unless otherwise specified; the test materials used in the examples described below, unless otherwise specified, were purchased from commercial sources.
TiO 2 (CasNo. 1317-70-0), available from Beijing Inock technologies Co., ltd., product number A60660;
Cr 2 O 3 (CasNo: 1308-38-9), available from Beijing Inocover technologies Co., ltd., cat. No. A95953;
Nb 2 O 5 (CasNo: 1313-96-8), available from Beijing Inockai technologies Co., ltd., cat. No. A81394;
Ta 2 O 5 (CasNo: 1314-61-0), available from Beijing Inocover technologies Co., ltd., cat. No. A54445;
MoO 3 (CasNo: 1313-27-5), available from Beijing Inocover technologies Co., ltd., product number A30070;
c (CasNo: 7440-44-0), available from Beijing enokie technologies Co., ltd., product number I11113;
absolute ethyl alcohol (CasNo. 64-17-5), available from Beijing enokie technologies Co., ltd., product number G00004;
Na(PO 3 ) 6 (CasNo: 10124-56-8), available from Beijing Inocover technologies Co., ltd., product number A80460;
Na 2 SiO 3 (CasNo: 10213-79-3), available from Beijing Inocover technologies Co., ltd., cat. No. A44948;
Na 2 WO 4 (CasNo: 10213-10-2), available from Beijing Inockai technologies Co., ltd., product number A24099;
NaAlO 2 (CasNo: 11138-49-1), available from Beijing Inocover technologies Inc., cat# A61847.
Example 1
The ceramic material for the ceramic tile comprises the following components in detail from bottom to top: the ceramic matrix is 8mm, and the wear-resistant layer is 60 mu m.
The ceramic matrix is a blank body obtained by pressing and sintering raw materials;
the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :80 parts of Cr 2 O 3 :75 parts of Nb 2 O 5 :135 parts, ta 2 O 5 :220 parts of MoO 3 :145 parts, C:48 parts.
The invention also provides a preparation method of the high-hardness high-wear-resistance ceramic material for the ceramic tile, which specifically comprises the following steps:
(1) Preparing a ceramic matrix: weighing TiO 2 、Cr 2 O 3 、Nb 2 O 5 、Ta 2 O 5 、MoO 3 Placing the materials in a roller ball milling tank, adding absolute ethyl alcohol for ball milling, wherein the ball milling medium is silicon nitride, the ball-to-liquid ratio is 4:1:2, ball milling is carried out for 22 hours under the condition that the ball milling rotating speed is 80r/min, filtering, drying for 24 hours at 60 ℃, grinding and sieving with a 100-mesh sieve to obtain mixed powder;
(2) Preparing a ceramic matrix: placing the mixed powder obtained in the step (1) into a die, prepressing by adopting a tablet press, wherein the prepressing pressure is set to be 10MPa, the prepressing time is set to be 1.5h, placing the die loaded with the mixed powder into a discharge plasma sintering furnace, pressing the die in the sintering process, setting the pressure to be 3000MPa, sintering by adopting direct current pulse, keeping the current for 15ms, taking intermittent 3ms as a pulse, heating to 1600 ℃ at the heating rate of 100 ℃/min at intervals of 5ms after 10 current pulses, preserving heat for 10min, cooling to 600 ℃ at the cooling rate of 100 ℃/min, and cooling along with the furnace to obtain a ceramic matrix;
(3) And (3) preparing a wear-resistant layer: polishing the ceramic matrix obtained in the step (2) by 2000-mesh sand paper for 2min, placing the polished ceramic matrix in an electrolytic cell to ensure that electrolyte can completely permeate the ceramic matrix, wherein the electrolyte is prepared from Na (PO) 3 ) 6 、Na 2 SiO 3 、Na 2 WO 4 、NaAlO 2 Is combined with water, na (PO) 3 ) 6 With Na and Na 2 SiO 3 The mass ratio of Na is 1:1 2 WO 4 With NaAlO 2 The mass ratio of Na is 1:1 2 SiO 3 With NaAlO 2 The mass ratio of (2) to (1) is 2, and the concentration of the electrolyte is 1.2g/cm 3 Adopting a carbon rod as a cathode, adopting the ceramic matrix obtained in the step (2) as an anode, adjusting the pH of electrolyte to 10, and setting the forward current density to 5A/dm 2 A negative current density of 1A/dm 2 The frequency is 500Hz, the duty ratio is 30%, the voltage is rapidly increased from 0V to 500V within 5min, the temperature is kept for 60min, the cooling is carried out, and the drying is carried out for 8h at 60 ℃ to prepareObtaining the ceramic material.
Example 2
The ceramic material for the ceramic tile comprises the following components in detail from bottom to top: the ceramic matrix is 8mm, and the wear-resistant layer is 60 mu m.
The ceramic matrix is a blank body obtained by pressing and sintering raw materials;
the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :80 parts of Cr 2 O 3 :75 parts of Nb 2 O 5 :135 parts, ta 2 O 5 :220 parts of MoO 3 :145 parts, C:48 parts.
The invention also provides a preparation method of the high-hardness high-wear-resistance ceramic material for the ceramic tile, which specifically comprises the following steps:
(1) Preparing a ceramic matrix: weighing TiO 2 、Cr 2 O 3 、Nb 2 O 5 、Ta 2 O 5 、MoO 3 Placing the materials in a roller ball milling tank, adding absolute ethyl alcohol for ball milling, wherein the ball milling medium is silicon nitride, the ball-to-liquid ratio is 4:1:2, ball milling is carried out for 24 hours under the condition that the ball milling rotating speed is 100r/min, filtering, drying for 24 hours at 65 ℃, grinding and sieving with a 100-mesh sieve to obtain mixed powder;
(2) Preparing a ceramic matrix: placing the mixed powder obtained in the step (1) into a die, prepressing by adopting a tablet press, wherein the prepressing pressure is set to be 10MPa, the prepressing time is set to be 2 hours, placing the die loaded with the mixed powder into a discharge plasma sintering furnace, pressing the die in the sintering process, wherein the pressure is set to be 3000MPa, sintering is carried out by adopting direct current pulse, the current lasts for 15ms, the intermittent current is 3ms as one pulse, the interval is 5ms after 10 current pulses, the heating rate is 100 ℃/min, the temperature is kept for 12min, the cooling rate is 100 ℃/min, the temperature is reduced to 600 ℃, and the ceramic matrix is obtained after furnace cooling;
(3) And (3) preparing a wear-resistant layer: polishing the ceramic matrix obtained in the step (2) by 2000-mesh sand paper for 2min, placing the polished ceramic matrix in an electrolytic cell to ensure that electrolyte can completely permeate the ceramic matrix, wherein the electrolyte is prepared from Na (PO) 3 ) 6 、Na 2 SiO 3 、Na 2 WO 4 、NaAlO 2 Is combined with water, na (PO) 3 ) 6 With Na and Na 2 SiO 3 The mass ratio of Na is 1:1 2 WO 4 With NaAlO 2 The mass ratio of Na is 1:1 2 SiO 3 With NaAlO 2 The mass ratio of (2) to (1), the concentration of the electrolyte is 1.25g/cm 3 Adopting a carbon rod as a cathode, adopting the ceramic matrix obtained in the step (2) as an anode, adjusting the pH of electrolyte to 11, and setting the forward current density to 5A/dm 2 A negative current density of 1A/dm 2 The frequency is 500Hz, the duty ratio is 30%, the voltage is rapidly increased from 0V to 500V within 5min, the temperature is kept for 80min, the ceramic material is obtained after cooling and drying for 10h at 65 ℃.
Example 3
The ceramic material for the ceramic tile comprises the following components in detail from bottom to top: the ceramic matrix is 10mm, and the wear-resistant layer is 70 mu m.
The ceramic matrix is a blank body obtained by pressing and sintering raw materials;
the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :90 parts of Cr 2 O 3 :80 parts of Nb 2 O 5 :140 parts of Ta 2 O 5 :230 parts of MoO 3 :160 parts of C:60 parts.
The invention also provides a preparation method of the high-hardness high-wear-resistance ceramic material for the ceramic tile, which specifically comprises the following steps:
(1) Preparing a ceramic matrix: weighing TiO 2 、Cr 2 O 3 、Nb 2 O 5 、Ta 2 O 5 、MoO 3 Placing the materials in a roller ball milling tank, adding absolute ethyl alcohol for ball milling, wherein the ball milling medium is silicon nitride, the ball-to-liquid ratio is 4:1:2, ball milling is carried out for 22 hours under the condition that the ball milling rotating speed is 80r/min, filtering, drying for 24 hours at 60 ℃, grinding and sieving with a 100-mesh sieve to obtain mixed powder;
(2) Preparing a ceramic matrix: placing the mixed powder obtained in the step (1) into a die, prepressing by adopting a tablet press, wherein the prepressing pressure is set to be 10MPa, the prepressing time is set to be 1.5h, placing the die loaded with the mixed powder into a discharge plasma sintering furnace, pressing the die in the sintering process, setting the pressure to be 3000MPa, sintering by adopting direct current pulse, keeping the current for 15ms, taking intermittent 3ms as a pulse, heating to 1600 ℃ at a heating rate of 100 ℃/min at intervals of 5ms after 10 current pulses, preserving heat for 10min, cooling to 600 ℃ at a cooling rate of 100 ℃/min, and cooling along with the furnace to obtain a ceramic matrix;
(3) And (3) preparing a wear-resistant layer: polishing the ceramic matrix obtained in the step (2) by 2000-mesh sand paper for 2min, placing the polished ceramic matrix in an electrolytic cell to ensure that electrolyte can completely permeate the ceramic matrix, wherein the electrolyte is prepared from Na (PO) 3 ) 6 、Na 2 SiO 3 、Na 2 WO 4 、NaAlO 2 Is combined with water, na (PO) 3 ) 6 With Na and Na 2 SiO 3 The mass ratio of Na is 1:1 2 WO 4 With NaAlO 2 The mass ratio of Na is 1:1 2 SiO 3 With NaAlO 2 The mass ratio of (2) to (1) is 2, and the concentration of the electrolyte is 1.2g/cm 3 Adopting a carbon rod as a cathode, adopting the ceramic matrix obtained in the step (2) as an anode, adjusting the pH of electrolyte to 10, and setting the forward current density to 5A/dm 2 A negative current density of 1A/dm 2 The frequency is 500Hz, the duty ratio is 30%, the voltage is rapidly increased from 0V to 500V within 5min, the temperature is kept for 60min, the cooling is carried out, and the ceramic material is prepared after drying for 8h at 60 ℃.
Example 4
The ceramic material for the ceramic tile comprises the following components in detail from bottom to top: the ceramic matrix is 10mm, and the wear-resistant layer is 70 mu m.
The ceramic matrix is a blank body obtained by pressing and sintering raw materials;
the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :90 parts of Cr 2 O 3 :80 parts of Nb 2 O 5 :140 parts of Ta 2 O 5 :230 parts of MoO 3 :160 parts of C:60 parts.
The invention also provides a preparation method of the high-hardness high-wear-resistance ceramic material for the ceramic tile, which specifically comprises the following steps:
(1) Preparing a ceramic matrix: weighing TiO 2 、Cr 2 O 3 、Nb 2 O 5 、Ta 2 O 5 、MoO 3 Placing the materials in a roller ball milling tank, adding absolute ethyl alcohol for ball milling, wherein the ball milling medium is silicon nitride, the ball-to-liquid ratio is 4:1:2, ball milling is carried out for 24 hours under the condition that the ball milling rotating speed is 100r/min, filtering, drying for 24 hours at 65 ℃, grinding and sieving with a 100-mesh sieve to obtain mixed powder;
(2) Preparing a ceramic matrix: placing the mixed powder obtained in the step (1) into a die, prepressing by adopting a tablet press, wherein the prepressing pressure is set to be 10MPa, the prepressing time is set to be 2 hours, placing the die loaded with the mixed powder into a discharge plasma sintering furnace, pressing the die in the sintering process, wherein the pressure is set to be 3000MPa, sintering is carried out by adopting direct current pulse, the current lasts for 15ms, the intermittent current is 3ms as one pulse, the interval is 5ms after 10 current pulses, the heating rate is 100 ℃/min, the temperature is kept for 12min, the cooling rate is 100 ℃/min, the temperature is reduced to 600 ℃, and the ceramic matrix is obtained after furnace cooling;
(3) And (3) preparing a wear-resistant layer: polishing the ceramic matrix obtained in the step (2) by 2000-mesh sand paper for 2min, placing the polished ceramic matrix in an electrolytic cell to ensure that electrolyte can completely permeate the ceramic matrix, wherein the electrolyte is prepared from Na (PO) 3 ) 6 、Na 2 SiO 3 、Na 2 WO 4 、NaAlO 2 Is combined with water, na (PO) 3 ) 6 With Na and Na 2 SiO 3 The mass ratio of Na is 1:1 2 WO 4 With NaAlO 2 The mass ratio of Na is 1:1 2 SiO 3 With NaAlO 2 The mass ratio of (2) to (1), the concentration of the electrolyte is 1.25g/cm 3 Adopting a carbon rod as a cathode, adopting the ceramic matrix obtained in the step (2) as an anode, adjusting the pH of electrolyte to 11, and setting the forward current density to 5A/dm 2 A negative current density of 1A/dm 2 The frequency is 500Hz, the duty ratio is 30%, the voltage is rapidly increased from 0V to 500V within 5min, the temperature is kept for 80min, the ceramic material is obtained after cooling and drying for 10h at 65 ℃.
Comparative example 1
This comparative example provides a ceramic material with high hardness and high wear resistance for ceramic tiles and a method for preparing the same, which is different from example 1 only in that a conventional sintering process is adopted for a ceramic matrix instead of a plasma discharge sintering process, and the rest components and the content of the components are the same as those in example 1.
Comparative example 2
This comparative example provides a ceramic material for ceramic tile having high hardness and high abrasion resistance and a method for preparing the same, which is different from example 1 only in that no abrasion resistant layer is contained in all components, and the remaining components and the content of the components are the same as in example 1.
Experimental example
1. Microhardness measurement
The hardness of examples 1 to 4 and comparative examples 1 to 2 of the present invention was measured by using a Vickers hardness tester, and the test force of 0.02kg was applied for 15 seconds.
2. Wear resistance test
The ceramic materials obtained in examples 1-4 and comparative examples 1-2 were processed to 15mm by 20mm by 4mm, dry friction performance of the ceramic layer was tested using a UMT-TriboLab frictional wear tester, GCr15 steel ball was selected as a grinding member, frictional displacement was set to 5mm, frictional frequency was selected to 20Hz, frictional time was 10min, and the abraded powder was collected, weighed with a CP225D high-precision analytical balance with a precision of up to 0.01mg, and the amount of abrasion was recorded.
3. SEM analysis
The invention adopts a jsm-6480 scanning electron microscope to observe the microstructure of the ceramic material obtained in the example 1.
4. Macroscopic morphology observation
The invention adopts an Olympus OLS4000 laser confocal microscope to observe the macroscopic morphology of the ceramic material obtained in the example 1.
Analysis of results
FIG. 1 is a graph showing the microhardness results of a ceramic material with high hardness and high wear resistance for ceramic tiles, wherein the microhardness of examples 1-4 is greater than 1350HV0.02, the microhardness of comparative example 1 is less than 1150HV0.02, and the microhardness of comparative example 2 is less than 1100HV0.02;
FIG. 2 is a graph showing the results of abrasion resistance experiments of a ceramic material with high hardness and high abrasion resistance for ceramic tiles, wherein the abrasion loss of each of examples 1-4 and comparative example 1 is less than 0.2mg, and the abrasion loss of comparative example 2 is more than 0.6mg;
according to the analysis of the results of fig. 1 and 2, compared with comparative example 1, the spark plasma sintering has the characteristics of uniform heating, high heating rate, low sintering temperature, short sintering time and high production efficiency, raw materials are manufactured into a ceramic matrix through spark plasma sintering, plasma in pulse current and pressure are jointly acted on the ceramic matrix in the spark plasma sintering process, the sintering temperature of powder is favorably reduced, the spark plasma sintering finishes sintering in a short time at a great heating rate, the growth of crystal grains is effectively avoided, the crystal grains in the ceramic matrix are tiny, fine grain strengthening effect is generated, the tissue density and the number of crystal boundaries are increased, the slip resistance of dislocation in the ceramic matrix is increased, the dislocation slip distance is prolonged, more energy is required to be consumed in dislocation movement, and the hardness and the wear resistance of the ceramic matrix are increased; the spark plasma sintering ensures that the ceramic matrix is heated uniformly, ensures the uniform size of ceramic grains, effectively reduces excessive growth of few grains in the ceramic matrix, effectively avoids stress concentration in the ceramic material, and enhances the hardness and wear resistance of the ceramic matrix; since comparative example 1 includes the abrasion resistant layer, the abrasion loss in comparative example 1 is not much different from examples 1 to 4, since the ceramic matrix in comparative example 1 is prepared by a conventional sintering method in which the temperature rising rate is only 5 to 15 ℃/min, the crystal grain is liable to grow up at a high temperature, even the phenomenon of secondary recrystallization of the crystal grain occurs, the number of grain boundaries in the ceramic matrix is reduced, and the hardness of the ceramic is remarkably reduced; compared with the comparative example 2, aluminum ions and tungsten ions in the electrolyte form a wear-resistant layer on the surface of the ceramic matrix, micro-arc oxidation is carried out under the action of current and pressure to form a tungsten oxide and aluminum oxide composite metal layer, and aluminum oxide has a hexagonal structure and extremely high hardness, so that the hardness and wear resistance of the ceramic material can be remarkably improved; the wear-resistant layer consists of a crystalline phase and an amorphous phase, so that the hardness and deformation characteristics of the wear-resistant layer are combined, and the wear-resistant performance of the wear-resistant layer is improved; the wear-resistant layer grows from the ceramic matrix in situ and is metallurgically combined with the ceramic matrix, the combination between the wear-resistant layer and the ceramic matrix is tighter, and the hardness and the wear resistance of the ceramic material are enhanced; since the abrasion resistant layer is not included in comparative example 2, the alumina and tungsten oxide components in the abrasion resistant layer have higher hardness, and can provide good abrasion resistance, microhardness and abrasion resistance of comparative example 2 are remarkably reduced compared with examples 1 to 4.
FIG. 3 is a graph showing SEM results of the surface of a ceramic material of high hardness and high abrasion resistance for ceramic tile, as shown in example 1, where the ceramic material has significant discharge holes and small number of cracks, because micro-arc oxidation is a "breakdown-melting-cooling-re-breakdown" process, and anodic electrolysis and the generation of the plating layer on the surface of the anode occur simultaneously.
Fig. 4 is a drawing showing the SEM result of the fusion cross section of the ceramic material with high hardness and high wear resistance for ceramic tiles, wherein the wear-resistant layer grows in situ from the ceramic matrix, and the wear-resistant layer and the ceramic matrix are obviously fused at high temperature, and the fusion lines at the cross section are in a canine-tooth staggered structure.
FIG. 5 is a graph showing the macroscopic morphology results of the ceramic material with high hardness and high wear resistance, which is obtained by the invention, wherein in the micro-arc oxidation process, aluminum and tungsten form oxide particles on the surface of a ceramic matrix, and the growth of the particles on the surface of the ceramic material is uniform and the surface of the ceramic material is smooth under macroscopic observation.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (5)
1. The ceramic material with high hardness and high wear resistance for the ceramic tile is characterized in that: the ceramic material comprises the following components from bottom to top: 8-10mm of ceramic matrix and 60-70 mu m of wear-resistant layer; the ceramic matrix is a blank body obtained by pressing and sintering raw materials; the raw materials specifically comprise the following components in parts by weight: tiO (titanium dioxide) 2 :80-90 parts of Cr 2 O 3 :75-80 parts of Nb 2 O 5 :135-140 parts, ta 2 O 5 :220-230 parts of MoO 3 :145-160 parts of C:48-60 parts.
2. The method for preparing the ceramic material with high hardness and high wear resistance for ceramic tiles according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
(1) Preparing a ceramic matrix: weighing TiO 2 、Cr 2 O 3 、Nb 2 O 5 、Ta 2 O 5 、MoO 3 Placing the powder C in a roller ball milling tank, adding absolute ethyl alcohol for ball milling, wherein the ball milling medium is silicon nitride, filtering, drying, grinding and sieving with a 100-mesh sieve to obtain mixed powder;
(2) Preparing a ceramic matrix: placing the mixed powder obtained in the step (1) into a die, prepressing the mixed powder by adopting a tablet press, placing the die loaded with the mixed powder into a discharge plasma sintering furnace, pressing the die in the sintering process, setting the pressure to 3000MPa, sintering by adopting direct current pulse, wherein the current lasts for 15ms, taking the intermittent 3ms as a pulse, and heating and preserving the heat at intervals of 5ms after 10 current pulses, cooling to 600 ℃ at the cooling rate of 100 ℃/min, and cooling along with the furnace to obtain a ceramic matrix;
(3) And (3) preparing a wear-resistant layer: polishing the ceramic matrix obtained in the step (2) by 2000-mesh sand paper for 2min, placing the polished ceramic matrix in an electrolytic cell to ensure that electrolyte can completely permeate the ceramic matrix, wherein the electrolyte is prepared from Na (PO) 3 ) 6 、Na 2 SiO 3 、Na 2 WO 4 、NaAlO 2 And water, adopting a carbon rod as a cathode, adopting the ceramic matrix obtained in the step (2) as an anode, and regulatingThe pH value of the electrolyte is 10-11, and the forward current density is set to 5A/dm 2 A negative current density of 1A/dm 2 The frequency is 500Hz, the duty ratio is 30%, the voltage is rapidly increased from 0V to 500V within 5min, the temperature is kept for 60-80min, and the ceramic material is obtained after cooling and drying.
3. The method for preparing the ceramic material with high hardness and high wear resistance for ceramic tiles according to claim 2, wherein the method comprises the following steps: in the step (1), the ball-to-liquid ratio is 4:1:2, the ball milling rotating speed is 80-100r/min, and the ball milling time is 22-24h; the drying temperature is 60-65 ℃ and the drying time is 24 hours.
4. The method for preparing the ceramic material with high hardness and high wear resistance for ceramic tiles according to claim 3, wherein the method comprises the following steps: in the step (2), the pre-pressing treatment pressure is set to be 10MPa, and the pre-pressing treatment time is 1.5-2h; the heating rate is 100 ℃/min, the heating temperature is 1600-1700 ℃, and the heat preservation time is 10-12min.
5. The method for preparing the ceramic material with high hardness and high wear resistance for ceramic tiles according to claim 4, wherein the method comprises the following steps: in step (3), na (PO) 3 ) 6 With Na and Na 2 SiO 3 The mass ratio of Na is 1:1 2 WO 4 With NaAlO 2
The mass ratio of Na is 1:1 2 SiO 3 With NaAlO 2 The mass ratio of (2) to (1), the concentration of the electrolyte is 1.2-1.25g/cm 3 ；
The drying temperature is 60-65deg.C, and the drying time is 8-10h.
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