CN118108482A - Method for preparing high-strength building ceramic blank by adding calcium-magnesium sintering aid containing forsterite - Google Patents
Method for preparing high-strength building ceramic blank by adding calcium-magnesium sintering aid containing forsterite Download PDFInfo
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- CN118108482A CN118108482A CN202410279192.8A CN202410279192A CN118108482A CN 118108482 A CN118108482 A CN 118108482A CN 202410279192 A CN202410279192 A CN 202410279192A CN 118108482 A CN118108482 A CN 118108482A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 136
- 238000005245 sintering Methods 0.000 title claims abstract description 37
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052839 forsterite Inorganic materials 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 23
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 38
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 239000010453 quartz Substances 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 19
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 19
- 239000010433 feldspar Substances 0.000 claims abstract description 19
- NWXHSRDXUJENGJ-UHFFFAOYSA-N calcium;magnesium;dioxido(oxo)silane Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O NWXHSRDXUJENGJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052637 diopside Inorganic materials 0.000 claims abstract description 18
- 239000011787 zinc oxide Substances 0.000 claims abstract description 17
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 16
- 239000000454 talc Substances 0.000 claims abstract description 16
- 235000012222 talc Nutrition 0.000 claims abstract description 16
- 229910052623 talc Inorganic materials 0.000 claims abstract description 16
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 10
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000000748 compression moulding Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- 230000008569 process Effects 0.000 description 15
- 238000013001 point bending Methods 0.000 description 8
- 238000010998 test method Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 6
- 238000009472 formulation Methods 0.000 description 6
- 229910052863 mullite Inorganic materials 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 229910052661 anorthite Inorganic materials 0.000 description 4
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000005034 decoration Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003238 silicate melt Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 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
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007952 growth promoter Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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Abstract
A method for preparing a high-strength building ceramic blank by adding a calcium-magnesium sintering aid containing forsterite belongs to the technical field of building ceramic preparation, and is characterized by comprising the following steps: proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum, 3 parts of forsterite and 0 or 2 parts of diopside are added with water, ball milling is carried out in a rapid ball mill, the slurry is dried, then the material particles are manually manufactured, compression molding is carried out, and the material particles are sintered in a roller kiln at 1170 ℃ for 70 minutes, thus obtaining the high-strength building ceramic blank. The raw materials adopted by the technical scheme are low in price, the adding mode is simple, and the industrial production is easy. The calcium-magnesium sintering aid containing forsterite is used as an auxiliary raw material, so that the crystal phase composition and microstructure of the building ceramic can be optimized, and the flexural strength of the building ceramic can be improved to meet the requirements of high-load application places.
Description
Technical Field
A method for preparing a high-strength building ceramic blank by adding a calcium-magnesium sintering aid containing forsterite belongs to the technical field of building ceramic preparation.
Background
Compared with other decorative materials, the building ceramic has the advantages of good decorative performance, strong weather resistance and the like, has obvious advantages in the aspects of inner and outer wall decoration, ground decoration and the like, and is highly loved by consumers in market application. The traditional building ceramic is prepared from quartz, feldspar, kaolinite and other raw materials through mixing, ball milling, granulating, compression molding and roller kiln sintering, and has short sintering period and high sintering speed. The crystal phase only contains a small amount of mullite phase and unmelted quartz phase, the partially melted quartz is easy to precipitate again in the cooling process to form cristobalite, and the expansion coefficient difference between the quartz phase and the glass phase causes defects such as cracks, so that the strength of the building ceramic is low, and the use effect of building decoration and finishing materials is affected. The existing method for preparing the high-strength building ceramic is to add fibers or second-phase particles for reinforcement, and also has the modes of prestress and the like through a glaze layer.
The technical scheme of the Chinese patent 202211498023.0 is as follows: the powder grain size and chemical composition ratio are utilized, namely, firstly, the feldspar raw material and the siliceous raw material are ground into the medium grain size of 3 to 6 microns, then the clay raw material, the high alumina raw material, the calcareous raw material and the glass reinforced component which is easy to dissolve in water are mixed, then all the raw materials obtained by mixing are ground into the medium grain size of 8 to 12 microns, the granules are prepared under the action of the grinding aid, the physical-reaction type composite reinforcing agent and the diluent, and then the high-strength ceramic sheet is obtained by pressing and sintering.
The Chinese patent 202210503892.1 is prepared by using ingredients with high silicon dioxide content (74% -79%), and the building ceramic with high strength and high silicon content is sintered.
The crystallization inducer and the crystal growth promoter with specific granularity requirements are added in the Chinese patent No. 202211148742.X, the corresponding chemical composition and granularity requirements are strictly controlled, and three-dimensional network mullite whiskers are grown in situ under the roller kiln firing condition, so that the high-toughness and high-strength building ceramic rock plate blank is produced.
From the above, in the process of batching, a calcium-magnesium sintering aid containing forsterite is added to regulate and control the crystallization behavior of the building ceramic in the firing process, various crystal phases are introduced to improve the microstructure of the building ceramic, and a crack generation and expansion mechanism of the building ceramic under load is optimized, so that a method for improving the strength of the building ceramic has not been reported yet.
Disclosure of Invention
The invention aims to provide a method for preparing a high-strength building ceramic blank by adding a calcium-magnesium sintering aid containing forsterite, which is characterized by comprising the following steps of:
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum, 3 parts of forsterite and 0 or 2 parts of diopside, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the high-strength building ceramic green body.
Wherein the mass percentages of the materials in the step (1) are respectively 44.64 percent of kaolin, 17.86 percent of feldspar, 26.79 percent of quartz, 2.23 percent of barium carbonate, 0.45 percent of zinc oxide, 3.57 percent of pyrophyllite, 1.79 percent of talcum, 2.68 percent of forsterite and 0 percent of diopside; or kaolin 43.86%, feldspar 17.54%, quartz 26.32%, barium carbonate 2.19%, zinc oxide 0.44%, pyrophyllite 3.51%, talcum 1.75%, forsterite 2.63% and diopside 1.75%. Kaolin, feldspar and quartz are used as blank base materials, and the mass ratio of the kaolin to the feldspar to the quartz is 50:20:30 respectively. Barium carbonate, zinc oxide, pyrophyllite, talcum, forsterite and diopside are used as sintering aids, and the mass ratio of the barium carbonate to the zinc oxide to the kaolin is 2.5 respectively: 0.5:4:2:3:0 or 2:50. the optimal mass ratio of diopside to kaolin is 2:50. in the process mentioned in the step (3), the crystal phase is transformed when the temperature is reduced after the high-strength building ceramic blank is sintered, so that the volume of the blank is changed severely and microcracks are generated, the barium carbonate is decomposed into barium oxide, and the barium carbonate and the zinc oxide act cooperatively, so that the severe change of the sintered volume can be limited, and the generation probability of the cracks is reduced. In the high temperature sintering process mentioned in the step (3), pyrophyllite, talcum, forsterite and diopside can assist in melting silicate melt, so that not only can the shrinkage rate of the blank be improved, but also basic elements for forming crystalline phases can be provided. In the production process of the roller kiln for quick firing, quartz is melted in silicate melt and reacts with aluminum, calcium and magnesium elements to form a composite crystalline phase containing quartz, mullite, anorthite, magnesium silicate and the like, so that the microstructure inside a green body is changed, the crack generation and expansion modes in the cracking process of the green body caused by loading are changed, and the strength of the building ceramic green body is greatly improved.
The invention has the beneficial effects that:
1. the adopted raw materials are low in price, the adding mode is simple, and the industrial production is easy;
2. the calcium-magnesium sintering aid containing forsterite is used as an auxiliary raw material, so that the crystal phase composition and microstructure of the building ceramic can be optimized, the flexural strength of the building ceramic can be improved, and the requirements of high-load application places can be met;
3. the process flow of the technical scheme has high similarity with the process flow of the traditional building ceramic, and is beneficial to industrial production.
Drawings
FIG. 1 is an X-ray diffraction XRD spectrum of a high-strength architectural ceramic blank obtained in example 1.
FIG. 2 is a SEM photograph of a high strength architectural ceramic blank made in example 1.
FIG. 3 is an X-ray diffraction XRD spectrum of the high strength architectural ceramic blank obtained in example 2.
FIG. 4 is a SEM photograph of a high strength architectural ceramic blank made in example 2.
FIG. 5 is an X-ray diffraction XRD spectrum of the architectural ceramic blank obtained in comparative example 1.
FIG. 6 is a SEM photograph of the architectural ceramic blank obtained in comparative example 1.
Detailed Description
Example 1
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum and 3 parts of forsterite, and water is added to make the mass ratio of the materials to the water be 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The formulation mentioned in step (1) of this example 1 was free of diopside sintering aid. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 13.46%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks were tested, with crushing times of 14, 42 and 14 respectively. The flexural strength was measured by the three-point bending test method to be 42.71 MPa, 62.82, MPa and 42.69 MPa.
FIG. 1 is an X-ray diffraction XRD spectrum of a high-strength architectural ceramic blank obtained in example 1. The green body is found to contain: quartz phase (JCPDS card numbers 01-0649, corresponding to diffraction peaks at 20.8050, 26.5597, 31.1257, 38.4305, 54.7953, 57.1436, and 67.9309 degrees) mullite phase (JCPDS card numbers 74-2419, corresponding to diffraction peaks at 61.5601 degrees of 2θ) and anorthite phase (JCPDS card numbers 70-0287, corresponding to diffraction peaks at 7.0127, 11.0918, and 49.9832 degrees of 2θ).
FIG. 2 is a SEM photograph of a high strength architectural ceramic blank made in example 1. The porosity is lower, holes have certain connectivity, a small amount of microcracks exist, and a small amount of crystal phases exist in the section glass phase, so that the surface evenness of the fracture is lower, the crack is deflected to a certain extent under the action of the crystal phases in the expansion process, and the increase of the breaking times and the breaking strength is realized.
Example 2
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum, 3 parts of forsterite and 2 parts of diopside, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a high-strength building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the high-strength building ceramic green body.
The high-strength building ceramic body prepared in the step (3) has an average linear shrinkage rate of 14.18 percent after being sintered. Placing the high-strength building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the high-strength building ceramic body to freely fall to the ground paved by the ceramic tile, marking the ground as one time, repeating the test until the high-strength building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the ground as the breaking times. Three high-strength building ceramic blanks are tested, the crushing times are 28, 50 and 43 respectively, and cracks generated by the blanks with high crushing times in the crushing process are bent and uneven. The flexural strength was measured by the three-point bending test method to be 50.31 MPa, 52.56 MPa and 55.60 MPa.
FIG. 3 is an X-ray diffraction XRD spectrum of the high strength architectural ceramic blank obtained in example 2. The green body is found to contain: quartz phase (JCPDS card numbers 01-0649, corresponding to diffraction peaks at degrees 26.4489, 26.6792, 55.2052, and 59.7582 degrees) mullite phase (JCPDS card numbers 74-2419, corresponding to diffraction peaks at degrees 54.0763 and 65.8199 degrees) cristobalite phase (JCPDS card numbers 82-1404, corresponding to diffraction peaks at degrees 38.4545, 54.6397, 56.4226, and 65.1633 degrees) anorthite phase (JCPDS card numbers 70-0287, corresponding to diffraction peaks at degrees 13.8937, 18.6436, 22.3237, 35.8451, 42.2803, and 44.7336 degrees) anorthite phase (JCPDS card numbers 87-2033, corresponding to diffraction peaks at degrees 51.1468 degrees) may be used.
FIG. 4 is a SEM photograph of a high strength architectural ceramic blank made in example 2. The porosity is low, kong Duowei closed pores, more crystal phases exist in the section, so that the surface flatness of the fracture is low, and the crack is proved to deflect to a certain extent under the action of the crystal phases in the expansion process, so that the remarkable increase of the breaking times and the breaking strength is realized.
The selection and the amount of the sintering aid in examples 1 and 2 are determined through the experimental process of adding the aid for a long time and a plurality of times, and the sintering aid and the corresponding specific amount in examples 1 and 2 can obtain the high-strength building ceramic blank with high flexural strength and small flexural strength dispersity. The following comparative examples are mainly different in the sintering aids selected, and the impact of different sintering aids on the mechanical properties of the building ceramic body is described by taking the crushing times and the flexural strength of the building ceramic prepared in the step (3) as main reference basis, so that the effect of improving the mechanical properties of the building ceramic body is greatly different under the conditions of different sintering aids and different amounts.
Comparative example 1
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar and 30 parts of quartz, and water is added to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The ingredients in step (1) of this comparative example 1 were the base materials of the conventional architectural ceramic body, and no sintering aid was added. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 13.83%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks are tested, the crushing times are respectively 3, 13 and 13, and cracks generated by the blanks in the crushing process are relatively straight. The flexural strength was measured by the three-point bending test method to be 32.01 MPa, 46.34 MPa and 48.96 MPa.
FIG. 5 is an X-ray diffraction XRD spectrum of the architectural ceramic blank obtained in comparative example 1. The green body is found to contain: quartz phase (JCPDS card numbers 01-0649, corresponding to diffraction peaks at 20.9179, 26.7905, 50.2372, and 59.9189 degrees of 2θ), mullite phase (JCPDS card numbers 74-2419, corresponding to diffraction peaks at 16.6873, 40.9034, 62.7503, 67.3446, and 68.0029 degrees of 2θ), and cristobalite phase (JCPDS card numbers 82-1404, corresponding to diffraction peaks at 43.4540 degrees of 2θ).
FIG. 6 is a SEM photograph of the architectural ceramic blank obtained in comparative example 1. The porosity is higher, the holes are communicated, the microcracks communicated inside are more, the surface flatness of the fracture is high, and the crack hardly deflects in the expansion process, so that the crushing times are low and the breaking strength is not high.
Comparative example 2
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum and 1.5 parts of forsterite, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The formulation mentioned in step (1) of this comparative example 2 was free of diopside sintering aid. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 13.11%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks are tested, the crushing times are respectively 5, 22 and 10, and the crushing times are more dispersed. The flexural strength was measured by the three-point bending test method to be 33.67 MPa, 49.22 MPa and 38.53 MPa.
Comparative example 3
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum and 4.5 parts of forsterite, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The formulation mentioned in step (1) of this comparative example 3 was free of diopside sintering aid. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 14.09%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks are tested, the crushing times are respectively 3, 1 and 42, and the crushing times are too dispersed. The flexural strength was tested by the three-point bending test method to be 32.71 MPa, 62.82 MPa and 30.69 MPa.
Comparative example 4
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum and 6 parts of forsterite, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The formulation mentioned in step (1) of this comparative example 4 was free of diopside sintering aid. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 12.87%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks are tested, the crushing times are respectively 2, 6 and 46, and the crushing times are more dispersed. The flexural strength was 31.52 MPa, 63.96 MPa and 33.24 MPa as tested by the three-point bending test method.
Comparative example 5
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum, 3 parts of forsterite and 1 part of diopside, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The small amount of diopside added when the sintering aid is added at the time of the formulation mentioned in step (1) of this comparative example 5. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 13.20%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks are tested, the crushing times are respectively 2,2 and 4, the crushing times are low, and cracks generated by the blanks in the crushing process are flat. The flexural strength was tested by the three-point bending test method to be 27.71 MPa, 28.82 MPa and 31.69 MPa.
Comparative example 6
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum, 3 parts of forsterite and 4 parts of diopside, and adding water to ensure that the mass ratio of the material to the water is 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the building ceramic green body.
The small amount of diopside added when the sintering aid is added at the time of the formulation mentioned in step (1) of this comparative example 6. The average linear shrinkage rate of the sintered building ceramic blank body prepared in the step (3) is 14.11%. Placing the building ceramic body prepared in the step (3) at a position with the height of 1.4 meters, enabling the building ceramic body to freely fall to the ground paved by the ceramic tile, marking the building ceramic body as one time, repeating the test until the building ceramic body is changed into two halves from one side to the other side due to crack propagation, and marking the building ceramic body as the breaking times. Three building ceramic blanks are tested, the crushing times are respectively 4, 5 and 37, and the crushing times are more dispersed. The flexural strength was measured by the three-point bending test method to be 30.76 MPa, 33.95 MPa and 52.78 MPa.
Claims (1)
1. A method for preparing a high-strength building ceramic blank by adding a calcium-magnesium sintering aid containing forsterite is characterized by comprising the following steps of:
(1) Proportioning according to the mass ratio: 50 parts of kaolin, 20 parts of feldspar, 30 parts of quartz, 2.5 parts of barium carbonate, 0.5 part of zinc oxide, 4 parts of pyrophyllite, 2 parts of talcum, 3 parts of forsterite and 0 or 2 parts of diopside, namely the materials are respectively in percentage by mass: 44.64% of kaolin, 17.86% of feldspar, 26.79% of quartz, 2.23% of barium carbonate, 0.45% of zinc oxide, 3.57% of pyrophyllite, 1.79% of talcum and 2.68% of forsterite; or kaolin 43.86%, feldspar 17.54%, quartz 26.32%, barium carbonate 2.19%, zinc oxide 0.44%, pyrophyllite 3.51%, talcum 1.75%, forsterite 2.63% and diopside 1.75%, and adding water to make the mass ratio of the material to water be 100:80, after ball milling for 10 minutes in a rapid ball mill, drying the slurry at 120 ℃ and manually manufacturing material particles;
(2) Placing the material particles prepared in the step (1) into a mould, and forming by 200 MPa to produce a building ceramic green body;
(3) And (3) placing the building ceramic green body prepared in the step (2) in a roller kiln, and sintering at 1170 ℃ for 70 minutes to obtain the high-strength building ceramic green body.
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