A method for preparing flexural and wear-resistant ceramics

By mixing materials such as potassium feldspar with nanomaterials such as nanocerium oxide and nanomolybdenum disulfide, a uniformly dispersed slurry is formed to produce flexural and wear-resistant ceramics, which solves the problem of insufficient wear resistance and flexural strength of existing ceramic tiles, and achieves ceramic materials with high flexural strength and good wear resistance.

CN119683980BActive Publication Date: 2025-05-13GUANGDONG XINRUNCHENG CERAMICS
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Patent Information

Application Number
CN202510214329.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-26
Publication Date
2025-05-13
Estimated Expiration
2045-02-26

AI Technical Summary

Technical Problem

The wear resistance and flexural strength of existing ceramic tiles are insufficient, resulting in insufficient mechanical strength, limiting their use.

Method used

By mixing potassium feldspar, sodium feldspar, kaolin, serpentine, dolomite, nanozirconia, nanoceria, nanomolybdenum disulfide, silicon carbide fibers, polyethylene glycol, fullerene trifluoromethyl derivatives and solvents, a uniformly dispersed slurry is formed, and a flexural and wear-resistant ceramic is produced by spray granulation, press molding and sintering.

Benefits of technology

The prepared flexural and wear-resistant ceramics have high flexural strength (can exceed 70MPa) and good wear resistance (grinding pit length does not exceed 8.5mm), which significantly improves the mechanical strength of the ceramics.

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Abstract

The invention belongs to the technical field of ceramics, and discloses a method for preparing a flexural and wear-resistant ceramic. The preparation method comprises the following steps: by weight, 40 parts of potassium feldspar, 10-25 parts of sodium feldspar, 1-10 parts of kaolin, 1-10 parts of serpentine, 5-25 parts of dolomite, 2-9 parts of nano zirconium oxide, 0.1-1 parts of nano cerium oxide, 0.1-1 parts of nano molybdenum disulfide, 0.1-0.8 parts of silicon carbide fiber, 0.5-2.5 parts of polyethylene glycol, 0.1-0.6 parts of fullerene trifluoromethyl derivatives, 0.1-3 parts of sodium dodecyl sulfate, 0.1-2 parts of sodium tripolyphosphate, and 10-60 parts of solvent are mixed to obtain slurry, spray granulation, obtain blanks, press molding, obtain green blanks, sinter, and obtain flexural and wear-resistant ceramics. The flexural strength of the flexural and wear-resistant ceramics can exceed 70MPa, and the grinding pit length does not exceed 8.5mm.
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Description

Technical Field

[0001] The invention belongs to the technical field of ceramics, and in particular relates to a method for preparing flexural and wear-resistant ceramics. Background Art

[0002] Ceramics are classified into building ceramics, daily-use ceramics and functional ceramics, among which building ceramics and daily-use ceramics are widely used in daily production and life. Ceramic bricks in the prior art are generally made of potassium feldspar, sodium feldspar, talc, calcite and kaolin as raw materials, and are made by grinding, mixing, pressing and calcining. However, this type of ceramic brick has the problems of poor wear resistance and insufficient flexural strength, which makes the mechanical strength of the ceramic brick insufficient, thereby limiting the use of ceramic bricks. In order to improve the mechanical strength of ceramic bricks, the prior art has improved the wear resistance and flexural strength of ceramic bricks by adding kyanite, titanium dioxide and fiber as raw materials. The flexural strength of the obtained ceramic material or ceramic brick is also difficult to exceed 68MPa, and the grinding pit length is too large.

[0003] Therefore, there is an urgent need to provide a ceramic with improved wear resistance and flexural strength. Summary of the invention

[0004] The present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art. To this end, the present invention provides a method for preparing a flexural and wear-resistant ceramic. The flexural and wear-resistant ceramic prepared by the method for preparing a flexural and wear-resistant ceramic of the present invention has both high flexural strength and good wear resistance, the flexural strength can exceed 70MPa, and the grinding pit length does not exceed 8.5mm.

[0005] The anti-bending and wear-resistant ceramics of the present invention are prepared by mixing potassium feldspar, sodium feldspar, kaolin, serpentine, dolomite, nano zirconium oxide, nano cerium oxide, nano molybdenum disulfide, silicon carbide fiber, polyethylene glycol, fullerene trifluoromethyl derivatives, and solvents to obtain a uniformly dispersed slurry, and then spray granulation, compression molding, and sintering to obtain the anti-bending and wear-resistant ceramics. Among them, by using polyethylene glycol, sodium dodecyl sulfate, sodium tripolyphosphate, and solvents, each component (potassium feldspar, sodium feldspar, kaolin, serpentine, dolomite, nano zirconium oxide, nano cerium oxide, nano molybdenum disulfide, silicon carbide fiber, fullerene trifluoromethyl derivative) is uniformly dispersed, and anti-bending and wear-resistant ceramics with uniform performance can be obtained. The use of nano cerium oxide, nano molybdenum disulfide, silicon carbide fiber, and fullerene trifluoromethyl derivatives in combination with other components significantly improves the wear resistance of the anti-bending and wear-resistant ceramics obtained by sintering. Nano-molybdenum disulfide has a two-dimensional structural characteristic and also has good wear resistance. Silicon carbide fiber has a one-dimensional structure and its uniform dispersion helps to improve the flexural strength of ceramics. Fullerene trifluoromethyl derivatives have zero-dimensional structural characteristics. Nano-cerium oxide is further introduced. Through the interaction of these five specific substances, a stable spatial network structure can be formed. Nano-cerium oxide is dispersed in the spatial network structure, which helps to relieve the stress generated during external contact such as folding and friction, and can make the flexural and wear-resistant ceramics have high flexural strength and wear resistance.

[0006] Further introduction of nano-terbium fluoride, which is combined with nano-cerium oxide and dispersed in the spatial network structure, helps to further relieve the stress generated during external contact such as folding and friction, and can make the fold-resistant and wear-resistant ceramics have high folding strength and wear resistance.

[0007] The present invention provides a method for preparing a flexural and wear-resistant ceramic, comprising the following steps:

[0008] By weight, 40 parts of potassium feldspar, 10-25 parts of sodium feldspar, 1-10 parts of kaolin, 1-10 parts of serpentine, 5-25 parts of dolomite, 2-9 parts of nano zirconium oxide, 0.1-1 parts of nano cerium oxide, 0.1-1 parts of nano molybdenum disulfide, 0.1-0.8 parts of silicon carbide fiber, 0.5-2.5 parts of polyethylene glycol, 0.1-0.6 parts of fullerene trifluoromethyl derivative, 0.1-3 parts of sodium dodecyl sulfate, 0.1-2 parts of sodium tripolyphosphate and 10-60 parts of solvent are mixed to obtain slurry, and then spray granulation is carried out to obtain a blank, and then compression molding is carried out to obtain a green blank, and sintering is carried out to prepare the anti-bending and wear-resistant ceramic.

[0009] Preferably, the solvent comprises water, hexafluoroisopropanol and methyl formate.

[0010] Preferably, the volume ratio of water to hexafluoroisopropanol and methyl formate in the solvent is 10:(0.5-2.5):(0.5-2.5), and more preferably 10:1:1.

[0011] Preferably, the fullerene trifluoromethyl derivative is selected from C 60 (CF3) 12 , C 60 (CF3) 16 At least one of .

[0012] Preferably, the silicon carbide fiber has a diameter of 5-8 μm and a length of 20-50 μm, and more preferably has a diameter of 6-7 μm and a length of 20-30 μm.

[0013] Preferably, nano-terbium fluoride is added before adding the silicon carbide fiber. Adding the nano-terbium fluoride first and then adding the silicon carbide fiber helps to evenly disperse the nano-terbium fluoride.

[0014] Preferably, the particle size of the nano-terbium fluoride is 10-50 nm, more preferably 20-30 nm.

[0015] Preferably, the amount of nano-terbium fluoride added is 0.1-0.6 parts. Adding a small amount of nano-terbium fluoride can also cooperate with fullerene trifluoromethyl derivatives to make the compatibility of each component better, thereby improving the ceramic spatial network structure's resistance to external friction and stability during folding, and promoting the flexural strength and wear resistance of flexural and wear-resistant ceramics.

[0016] Preferably, the sintering temperature is 1220-1300° C., and the sintering time is 40-70 minutes; further preferably, the sintering temperature is 1250-1290° C., and the sintering time is 50-70 minutes.

[0017] Preferably, the sintering is performed by heating the temperature to 1220-1300° C. at a rate of 8-15° C. / min.

[0018] Preferably, the sintering further includes a cooling process.

[0019] Preferably, during the cooling process, the temperature is first cooled to 450-500°C at a rate of 10-12°C / min, then cooled to 100-150°C at a rate of 1-8°C / min, and finally cooled to room temperature at a rate of 3-5°C / min. The staged cooling rate is helpful to further release the internal stress of the flexural and wear-resistant ceramics, and to improve the flexural strength of the flexural and wear-resistant ceramics.

[0020] Preferably, by weight, 0.3-1 parts of polydimethylsiloxane is added before adding the solvent.

[0021] Preferably, a method for preparing a flexural and wear-resistant ceramic comprises the following steps:

[0022] By weight, 40 parts of potassium feldspar, 15-20 parts of sodium feldspar, 5-10 parts of kaolin, 4-8 parts of serpentine, 8-20 parts of dolomite, 3-8 parts of nano zirconium oxide, 0.2-0.8 parts of nano cerium oxide, 0.1-0.6 parts of nano terbium fluoride, 0.2-0.8 parts of nano molybdenum disulfide, 0.2-0.6 parts of silicon carbide fiber, 0.5-2.0 parts of polyethylene glycol, 0.2-0.6 parts of fullerene trifluoromethyl derivative, 0.5-3 parts of sodium dodecyl sulfate, 0.1-2 parts of sodium tripolyphosphate, 0.3-1 parts of polydimethylsiloxane and 20-60 parts of solvent are mixed to obtain slurry, and then spray granulation is carried out to obtain a blank, and then compression molding is carried out to obtain a green blank, and sintering is carried out to prepare the flexural and wear-resistant ceramic.

[0023] The above-mentioned anti-bending and wear-resistant ceramics can be designed into the shape of bricks during molding, and finally sintered to obtain wear-resistant ceramic bricks.

[0024] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0025] (1) The flexural and wear-resistant ceramics of the present invention are prepared by mixing potassium feldspar, sodium feldspar, kaolin, serpentine, dolomite, nano zirconium oxide, nano cerium oxide, nano molybdenum disulfide, silicon carbide fiber, polyethylene glycol, fullerene trifluoromethyl derivative, and solvent to obtain a uniformly dispersed slurry, and then spray granulation, compression molding, and sintering to obtain the flexural and wear-resistant ceramics. Among them, by using polyethylene glycol, sodium dodecyl sulfate, sodium tripolyphosphate, and solvent, each component (potassium feldspar, sodium feldspar, kaolin, serpentine, dolomite, nano zirconium oxide, nano cerium oxide, nano molybdenum disulfide, silicon carbide fiber, and fullerene trifluoromethyl derivative) is uniformly dispersed, and a flexural and wear-resistant ceramic with uniform performance can be obtained. The use of nano cerium oxide, nano molybdenum disulfide, silicon carbide fiber, and fullerene trifluoromethyl derivative in combination with other components significantly improves the wear resistance of the sintered flexural and wear-resistant ceramics. Nano-molybdenum disulfide has a two-dimensional structural characteristic and also has good wear resistance. Silicon carbide fiber has a one-dimensional structure and its uniform dispersion helps to improve the flexural strength of ceramics. Fullerene trifluoromethyl derivatives have zero-dimensional structural characteristics. Nano-cerium oxide is further introduced. Through the interaction of these five specific substances, a stable spatial network structure can be formed. Nano-cerium oxide is dispersed in the spatial network structure, which helps to relieve the stress generated during external contact such as folding and friction, and can make the flexural and wear-resistant ceramics have high flexural strength and wear resistance.

[0026] (2) The present invention further introduces nano-terbium fluoride, which is dispersed in a spatial network structure in combination with nano-cerium oxide, which helps to further alleviate the stress generated during external contact such as folding and friction, and enables the fold-resistant and wear-resistant ceramic to have high folding strength and wear resistance.

[0027] (3) Under the specific staged cooling rate of the present invention, it is helpful to further release the internal stress of the flexural and wear-resistant ceramics, and help to improve the flexural strength of the flexural and wear-resistant ceramics. DETAILED DESCRIPTION

[0028] In order to make the technical scheme of the present invention more clearly understood by those skilled in the art, the following embodiments are listed for illustration. It should be pointed out that the following embodiments do not limit the protection scope of the present invention.

[0029] Unless otherwise specified, the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.

[0030] The potassium feldspar, sodium feldspar, kaolin, serpentine, dolomite, nano zirconium oxide, nano cerium oxide, and nano molybdenum disulfide particles used below can pass through a 200-300 mesh sieve.

[0031] The diameter of silicon carbide fibers is 6-7 μm and the length is 20-30 μm.

[0032] The particle size of nano-terbium fluoride is 30-40nm.

[0033] Example 1: Preparation of flexural and wear-resistant ceramics

[0034] A method for preparing a flexural and wear-resistant ceramic comprises the following steps:

[0035] By weight, 40 parts of potassium feldspar, 15 parts of sodium feldspar, 5 parts of kaolin, 4 parts of serpentine, 8 parts of dolomite, 4 parts of nano zirconium oxide, 0.2 parts of nano cerium oxide, 0.5 parts of nano molybdenum disulfide, 0.3 parts of silicon carbide fiber, 0.7 parts of polyethylene glycol, and a fullerene trifluoromethyl derivative (C 60 (CF3) 12 ) 0.4 parts, 0.5 parts of sodium dodecyl sulfate, 0.3 parts of sodium tripolyphosphate, and 50 parts of solvent (the volume ratio of water to hexafluoroisopropanol and methyl formate is 10:1:1) are mixed, the stirring speed is 700 rpm, the stirring time is 60 minutes, and a slurry is obtained, which is then spray granulated to obtain a blank, which is then pressed to obtain a green body, and the temperature is raised to 1250°C at a rate of 10°C / min and sintered for 60 minutes, and then naturally cooled to room temperature to obtain a flexural and wear-resistant ceramic.

[0036] Example 2: Preparation of flexural and wear-resistant ceramics

[0037] A method for preparing a flexural and wear-resistant ceramic comprises the following steps:

[0038] By weight, 40 parts of potassium feldspar, 18 parts of sodium feldspar, 8 parts of kaolin, 6 parts of serpentine, 10 parts of dolomite, 6 parts of nano zirconium oxide, 0.5 parts of nano cerium oxide, 0.6 parts of nano molybdenum disulfide, 0.2 parts of silicon carbide fiber, 0.5 parts of polyethylene glycol, and a fullerene trifluoromethyl derivative (C 60 (CF3) 12 ) 0.3 parts, 0.4 parts of sodium dodecyl sulfate, 0.4 parts of sodium tripolyphosphate, 0.4 parts of polydimethylsiloxane, and 50 parts of solvent (the volume ratio of water to hexafluoroisopropanol and methyl formate is 10:1.2:1.2) are mixed, the stirring speed is 700 rpm, and the stirring time is 60 minutes to obtain a slurry, which is then spray granulated to obtain a blank, which is then pressed to obtain a green body, and the temperature is raised to 1250°C at a rate of 10°C / min and sintered for 60 minutes, and then naturally cooled to room temperature to obtain a flexural and wear-resistant ceramic.

[0039] Example 3: Preparation of flexural and wear-resistant ceramics

[0040] A method for preparing a flexural and wear-resistant ceramic comprises the following steps:

[0041] By weight, 40 parts of potassium feldspar, 18 parts of sodium feldspar, 8 parts of kaolin, 6 parts of serpentine, 10 parts of dolomite, 6 parts of nano zirconium oxide, 0.5 parts of nano cerium oxide, 0.6 parts of nano molybdenum disulfide, 0.2 parts of silicon carbide fiber, 0.5 parts of polyethylene glycol, and a fullerene trifluoromethyl derivative (C 60 (CF3) 12 ) 0.3 parts, sodium dodecyl sulfate 0.4 parts, sodium tripolyphosphate 0.4 parts, polydimethylsiloxane 0.4 parts, solvent (the volume ratio of water to hexafluoroisopropanol and methyl formate is 10:1.2:1.2) 50 parts are mixed, the stirring speed is 700 rpm, the stirring time is 60 minutes, and a slurry is obtained, and then spray granulation is carried out to obtain a blank, and then compression molding is carried out to obtain a green body, the temperature is increased to 1250°C at a rate of 10°C / min, sintered for 60 minutes, and then cooled. During the cooling process, it is first cooled to 480°C at a rate of 10°C / min, then cooled to 100°C at a rate of 6°C / min, and finally cooled to room temperature at a rate of 3°C / min to obtain a flexural and wear-resistant ceramic.

[0042] Example 4: Preparation of flexural and wear-resistant ceramics

[0043] A method for preparing a flexural and wear-resistant ceramic comprises the following steps:

[0044] By weight, 40 parts of potassium feldspar, 18 parts of sodium feldspar, 8 parts of kaolin, 6 parts of serpentine, 10 parts of dolomite, 6 parts of nano zirconium oxide, 0.5 parts of nano cerium oxide, 0.5 parts of nano terbium fluoride, 0.6 parts of nano molybdenum disulfide, 0.2 parts of silicon carbide fiber, 0.5 parts of polyethylene glycol, and a fullerene trifluoromethyl derivative (C 60 (CF3) 12 ) 0.3 parts, sodium dodecyl sulfate 0.4 parts, sodium tripolyphosphate 0.4 parts, polydimethylsiloxane 0.4 parts, solvent (the volume ratio of water to hexafluoroisopropanol and methyl formate is 10:1.2:1.2) 50 parts are mixed, the stirring speed is 700 rpm, the stirring time is 60 minutes, and a slurry is obtained, and then spray granulation is carried out to obtain a blank, and then compression molding is carried out to obtain a green body, the temperature is increased to 1250°C at a rate of 10°C / min, sintered for 60 minutes, and then cooled. During the cooling process, it is first cooled to 480°C at a rate of 10°C / min, then cooled to 100°C at a rate of 6°C / min, and finally cooled to room temperature at a rate of 3°C / min to obtain a flexural and wear-resistant ceramic.

[0045] Comparative Example 1

[0046] Compared with Example 2, the difference of Comparative Example 1 is that the silicon carbide fiber in Example 2 is replaced by an equal amount of basalt fiber, and other raw materials and processes are the same as those in Example 2.

[0047] Comparative Example 2

[0048] Compared with Example 2, the difference of Comparative Example 2 is that an equal amount of hexagonal boron nitride is used to replace the nano molybdenum disulfide in Example 2, and other raw materials and processes are the same as those in Example 2.

[0049] Comparative Example 3

[0050] Compared with Example 2, the difference of Comparative Example 3 is that the nano-cerium oxide in Example 2 is replaced by an equal amount of nano-zirconium oxide, and the other raw materials and processes are the same as those in Example 2.

[0051] Comparative Example 4

[0052] Compared with Example 2, the difference of Comparative Example 4 is that an equal amount of sodium dodecyl sulfate is used to replace the sodium tripolyphosphate in Example 2, and other raw materials and processes are the same as those in Example 2.

[0053] Product effect testing

[0054] The flexural and wear-resistant ceramics prepared in Examples 1-4 and the flexural and wear-resistant ceramics prepared in Comparative Examples 1-4 were taken as test samples. The size of the samples was set to 300mm*300mm*6mm. The wear resistance of the samples was tested in accordance with GB / T12988-2009, and the flexural strength of the samples was tested in accordance with GB / T2542-2012 "Test Methods for Wall Bricks". The results are shown in Table 1.

[0055] Table 1

[0056]

[0057] It can be seen from Table 1 that the wear resistance and flexural strength of the flexural and wear-resistant ceramics prepared in the examples of the present invention are significantly better than those in comparative examples 1-3.

[0058] It can be seen from Example 2 and Comparative Example 1 that silicon carbide fibers cannot be simply replaced by basalt fibers. This is mainly because the unique structure and chemical composition of silicon carbide fibers enable silicon carbide fibers to be more evenly distributed in the flexural and wear-resistant ceramic system of the present invention, thereby improving the wear resistance and flexural strength of the flexural and wear-resistant ceramics.

[0059] It can be seen from Example 2 and Comparative Examples 2-3 that hexagonal boron nitride cannot replace nano-molybdenum disulfide, and nano-zirconium oxide cannot replace nano-cerium oxide. The reason may be that nano-molybdenum disulfide has better dispersibility with fullerene fluoride and other components, and nano-cerium oxide has specific electronic interactions with fullerene fluoride, which is beneficial to maintain the stable spatial structure of the ceramic, thereby helping to resist stress mutations caused by external friction. Sodium dodecyl sulfate and sodium tripolyphosphate together as specific surfactants significantly improve the dispersion uniformity of each component.

Claims

1. A method for preparing flexural and wear-resistant ceramics, characterized in that: The following steps are involved: By weight, 40 parts of potassium feldspar, 10-25 parts of sodium feldspar, 1-10 parts of kaolin, 1-10 parts of serpentine, 5-25 parts of dolomite, 2-9 parts of nano zirconium oxide, 0.1-1 parts of nano cerium oxide, 0.1-1 parts of nano molybdenum disulfide, 0.1-0.8 parts of silicon carbide fiber, 0.5-2.5 parts of polyethylene glycol, 0.1-0.6 parts of fullerene trifluoromethyl derivative, 0.1-3 parts of sodium dodecyl sulfate, 0.1-2 parts of sodium tripolyphosphate, and 10-60 parts of solvent are mixed to obtain a slurry, and then spray granulation is performed to obtain a blank, and then compression molding is performed to obtain a green blank, and sintering is performed to obtain the anti-bending and wear-resistant ceramic; The fullerene trifluoromethyl derivative is selected from C 60 (CF3) 12 , C 60 (CF3) 16 At least one of; Before adding the silicon carbide fiber, nano terbium fluoride is also added; The sintering process also includes a cooling process, in which the temperature is first cooled to 450-500°C at a rate of 10-12°C / min, then cooled to 100-150°C at a rate of 1-8°C / min, and finally cooled to room temperature at a rate of 3-5°C / min.

2. The preparation method according to claim 1, characterized in that: The solvents include water, hexafluoroisopropanol and methyl formate.

3. The preparation method according to claim 2, characterized in that: The volume ratio of water to hexafluoroisopropanol and methyl formate in the solvent is 10:(0.5-2.5):(0.5-2.5).

4. The preparation method according to claim 1, characterized in that: The silicon carbide fiber has a diameter of 5-8 μm and a length of 20-50 μm.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The sintering temperature is 1220-1300° C., and the sintering time is 40-70 minutes.

6. The preparation method according to any one of claims 1 to 4, characterized in that: The sintering is performed by heating the temperature to 1220-1300° C. at a rate of 8-15° C. / min.

7. The preparation method according to claim 1, characterized in that: Before adding the solvent, 0.3-1 parts of polydimethylsiloxane is also added by weight.

8. The preparation method according to claim 7, characterized in that: The following steps are involved: By weight, 40 parts of potassium feldspar, 15-20 parts of sodium feldspar, 5-10 parts of kaolin, 4-8 parts of serpentine, 8-20 parts of dolomite, 3-8 parts of nano zirconium oxide, 0.2-0.8 parts of nano cerium oxide, 0.1-0.6 parts of nano terbium fluoride, 0.2-0.8 parts of nano molybdenum disulfide, 0.2-0.6 parts of silicon carbide fiber, 0.5-2.0 parts of polyethylene glycol, 0.2-0.6 parts of fullerene trifluoromethyl derivative, 0.5-3 parts of sodium dodecyl sulfate, 0.1-2 parts of sodium tripolyphosphate, 0.3-1 parts of polydimethylsiloxane and 20-60 parts of solvent are mixed to obtain slurry, and then spray granulation is carried out to obtain a blank, and then compression molding is carried out to obtain a green blank, and sintering is carried out to prepare the flexural and wear-resistant ceramic.

Citation Information

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