CN115838274A - High-toughness and high-strength building ceramic rock slab blank and preparation method thereof - Google Patents
High-toughness and high-strength building ceramic rock slab blank and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of ceramic materials, and discloses a high-toughness high-strength building ceramic rock plate blank and a preparation method thereof. The ceramic rock plate blank comprises, by weight, 100 parts of a blank base material 85-90 parts, a crystallization inducer 2-5 parts and a crystal growth promoter 6-10 parts; the high toughness and the high strength of the rock plate blank can be ensured by controlling the proportion of the components, and in addition, the invention also discloses a preparation method of the high toughness and high strength building ceramic rock plate blank. According to the invention, through the addition of the crystallization inducer and the crystal growth promoter and the optimization of the formula system, the continuous three-dimensional network-shaped mullite whiskers can be grown in situ from the blank under the condition of low-temperature quick firing, the fracture toughness and the strength of the rock plate blank are effectively improved, the problem that the ceramic rock plate is easy to crack when being cut is solved, the processability of the ceramic rock plate is improved, and the application scene of the ceramic rock plate is favorably widened.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to a high-toughness high-strength building ceramic rock plate blank and a preparation method thereof.
Background
The ceramic rock plate is gradually known by the market as a main pushing product in recent years in the building ceramic industry, and becomes a domestic popular household building material. The ceramic rock plate is made by pressing natural raw materials through a large-tonnage press and firing at a high temperature of more than 1200 ℃. The rock plate is a trend product of ceramic tiles gradually developing towards materialization. As a new species in the field of home furnishing, the ceramic rock plate has very strong applicability, can be deeply processed, and can be used as a decorative material and a structural main material. However, in the process of processing and using, the rock plate often has the situations of cutting, punching and cracking, and the widening of the application field of the rock plate is severely limited.
In the prior art, in order to improve the strength and toughness of a rock plate blank, a part of whiskers or crystals such as aluminum oxide, zirconium oxide and the like are added on the basis of the formula of the existing blank. However, the added whiskers and crystals are difficult to be uniformly dispersed in the blank, the blank is difficult to ensure the sufficient thermodynamic and kinetic conditions for the mullite growth in the body fluid phase of the blank under the low-temperature fast-firing condition, and network-shaped bridges are difficult to form only by the added whiskers and a small amount of crystals, so that the aims of improving the strength and the fracture toughness are fulfilled. Therefore, how to grow the continuous three-dimensional network-shaped mullite whiskers in situ on the rock plate blank under the low-temperature fast-firing condition and how to enable the mullite whiskers to be uniformly distributed can effectively improve the fracture toughness and strength of the rock plate blank so as to solve the problem that the ceramic rock plate is easy to crack when being cut, and the method has important practical value.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-toughness high-strength building ceramic rock plate blank and a preparation method thereof. By adding the crystallization inducer and the crystal growth promoter and optimizing a formula system, the invention can lead the body to grow the mullite whisker with a three-dimensional network in situ under the condition of low-temperature quick firing, effectively improves the fracture toughness and the strength of the rock plate body, solves the problem that the ceramic rock plate is easy to crack when being cut, improves the processability of the ceramic rock plate and is beneficial to widening the application scene of the ceramic rock plate.
The specific technical scheme of the invention is as follows:
in a first aspect, the invention provides a high-toughness and high-strength building ceramic rock plate blank, which comprises, by weight, 100 parts of a blank base material 85-90 parts, a crystallization inducer 2-5 parts and a crystal growth promoter 6-10 parts. Wherein:
the base material of the green body comprises, by weight, 100 parts of water-washed kaolin 12-20 parts, ball clay 5-8 parts, illite 4-8 parts, pyrophyllite 15-25 parts, potassium anorthite 20-45 parts, porcelain stone 5-15 parts, wollastonite 1-3 parts and calcined talc 2-5 parts.
The crystallization inducer comprises one or a combination of a plurality of alpha-alumina powder, zirconia powder and mullite powder. The fineness of the crystallization inducer is 2-10 mu m, and the D90 is less than 10 mu m.
The crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of lithium carbonate, 5-15 parts of vanadium pentoxide, 20-35 parts of quartz, 2-15 parts of calcium phosphate, 10-15 parts of boric acid and 15-25 parts of potassium carbonate. The fineness of the crystal growth promoter is D90 less than 2 mu m.
The mullite grows in situ in the ceramic in the prior art, and usually requires very high sintering temperature or longer sintering time, and the mullite crystal can grow rapidly in situ under the condition of low-temperature fast firing (1180-1240 ℃ and 65-85 min) of a building ceramic blank by adding a crystallization inducer and a crystal growth promoter with a specific formula in the process of preparing the ceramic rock plate blank. Wherein:
the addition of the crystallization inducer can ensure that the mullite crystals in the rock plate blank structure have enough and uniformly dispersed crystal nucleus sites, so that the mullite crystals can easily grow around the crystal nucleus sites at high temperature. We have found that the fineness of the crystallization inducer affects the number and distribution of the crystal nuclei and thus the distribution of the mullite crystals. Finally, the fineness of the powder is controlled to be 2-10 mu m, and the effect is best in the range that D90 is less than 10 mu m. During the crystallization process, crystal nuclei are formed firstly and then grow around the crystal nuclei. The crystallization inducer added in the invention is used as a crystal nucleus for mullite growth, and the formation process of the crystal nucleus is reduced. When the particle size is too small, the melting is reduced or eliminated at a high temperature stage, and the crystal grows abnormally and becomes coarse due to an excessive particle size. On the other hand, the crystallization inducer is used as a crystal nucleus for mullite growth, the addition amount is more critical, excessive addition can increase the sintering temperature of a blank, and too little addition can reduce the number of the crystal nuclei.
The addition of the crystal growth promoter can reduce the reaction temperature of the system, so that more silicon dioxide and aluminum trioxide are melted in the liquid phase, and more aluminum sources and silicon sources are provided for the growth of the in-situ mullite in the liquid phase; in addition, lithium and vanadium in the crystal growth promoter can improve the growth speed of mullite crystals in the liquid phase of the rock plate blank under the condition of low-temperature and quick firing. We have found that the control of the fineness of the crystal growth promoter affects the reaction temperature of the system and the growth promoting effect of mullite. Finally, the fineness of the powder is controlled within the range of D90 less than 2 mu m, and the effect is optimal. The crystal growth promoter has the function of promoting the mullite crystals to rapidly grow around crystal nuclei, and the fused reaction of the mullite crystals entering a liquid phase is influenced by too large granularity, so that the aim of promoting the growth of the mullite in the liquid phase is fulfilled. On the other hand, the addition amount of the crystal growth promoter is more critical, the components of the crystal growth promoter can reduce the sintering temperature of the green body when the addition amount is too large, the green body is easy to deform in the sintering process, and the effect of promoting the growth of mullite is difficult to achieve when the addition amount is too small.
In addition, the invention optimizes a blank formula system, and the composition of the blank formula system must meet the requirement of mullite (3 Al) 2 O 3 ·2SiO 2 ) The fully grown components mainly meet the requirements of silicon and aluminum, but the sintering temperature of the blank is increased due to the overhigh proportion of the silicon and the aluminum, so the optimization is needed, and the effect is better within the optimization range of the invention.
In conclusion, the invention can lead the body to grow the mullite whisker with three-dimensional network shape in situ under the condition of low temperature and fast burning by controlling the adding amount and the fineness of the crystallization inducer and the crystal growth accelerant and optimizing the body formula system, thereby effectively improving the fracture toughness and the strength of the rock plate body. Solves the problems that in the prior art, the crystal whisker and the crystal are directly added in the blank body, so that the crystal whisker and the crystal are difficult to disperse uniformly, and the crystal is difficult to form network-shaped bridging in the low-temperature quick-firing process of the blank body, thereby achieving the aim of improving the strength and the fracture toughness.
In a second aspect, the invention provides a method for preparing a high-toughness high-strength building ceramic rock plate blank, which comprises the following steps:
(1) Weighing the raw materials of the crystal growth promoter according to the proportion, mixing, melting, water quenching, crushing and drying to obtain the crystal growth promoter.
(2) Weighing raw materials of each component of the blank base material according to the proportion, mixing, adding water, carrying out ball milling, then adding a crystallization inducer and a crystal growth promoter, and continuing ball milling to obtain slurry.
(3) And sieving, deironing and spray drying the slurry to obtain blank powder.
(4) And after the blank powder is aged, carrying out dry pressing forming, drying, ink-jet printing, glazing and sintering to obtain the high-toughness and high-strength building ceramic rock slab blank.
Preferably, in the step (1), the melting temperature is 1300 to 1350 ℃.
Preferably, in the step (2), the time of the first ball milling is 10-20h, and the time of the second ball milling is 1-2h.
Preferably, in step (2), 45-65wt% of water is added.
Preferably, in the step (4), the time for the aging treatment is 40 to 50 hours.
Preferably, in the step (4), the firing temperature is 1180-1240 ℃ and the total firing time is 60-140min.
Preferably, in step (4), the fracture toughness of the finally obtained architectural ceramic rock plate blank is more than 1.65 MPa-m 1/2 The modulus of rupture is more than or equal to 75MPa.
Compared with the prior art, the invention has the following technical effects:
(1) The invention can lead the body to grow the mullite whisker with three-dimensional network shape in situ under the condition of low temperature and fast burning by controlling the adding amount and the fineness of the crystallization inducer and the crystal growth accelerant and optimizing the body base material formula system, thereby effectively improving the fracture toughness and the strength of the rock plate body. Solves the problems that in the prior art, the crystal whisker and the crystal are directly added in the blank body, so that the crystal whisker and the crystal are difficult to disperse uniformly, and the crystal is difficult to form network-shaped bridging in the low-temperature quick-firing process of the blank body, thereby achieving the aim of improving the strength and the fracture toughness.
(2) The ceramic rock plate blank prepared by the invention has the fracture toughness of more than 1.65 MPa.m 1/2 The fracture modulus is more than or equal to 75Mpa, the problem that the ceramic rock plate is easy to crack when being cut is solved, the processability of the ceramic rock plate is improved, and the application scene of the ceramic rock plate is favorably widened.
Drawings
FIG. 1 is an electron microscope scan of a ceramic rock blank prepared in accordance with example 1 of the present invention;
FIG. 2 is an electron micrograph of a ceramic rock plate blank prepared according to example 2 of the present invention;
FIG. 3 is an electron microscope scan of a ceramic rock blank prepared in accordance with example 3 of the present invention;
FIG. 4 is an electron micrograph of a ceramic rock blank prepared according to example 4 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
A high-toughness high-strength building ceramic rock slab blank comprises, by weight, 100 parts of 85-90 parts of a blank base material, 2-5 parts of a crystallization inducer and 6-10 parts of a crystal growth promoter. Wherein:
the base material of the green body comprises, by weight, 100 parts of water-washed kaolin 12-20 parts, ball clay 5-8 parts, illite 4-8 parts, pyrophyllite 15-25 parts, potassium anorthite 20-45 parts, porcelain stone 5-15 parts, wollastonite 1-3 parts and calcined talc 2-5 parts.
The crystallization inducer comprises one or a combination of a plurality of alpha-alumina powder, zirconia powder and mullite powder. The fineness of the crystallization inducer is 2-10 mu m, and the D90 is less than 10 mu m.
The crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of lithium carbonate, 5-15 parts of vanadium pentoxide, 20-35 parts of quartz, 2-15 parts of calcium phosphate, 10-15 parts of boric acid and 15-25 parts of potassium carbonate. The fineness of the crystal growth promoter is D90 less than 2 mu m.
A preparation method of a high-toughness high-strength building ceramic rock plate blank comprises the following steps:
(1) Weighing the raw materials of the crystal growth promoter according to the proportion, mixing, melting at 1300-1350 ℃, and obtaining the crystal growth promoter after water quenching, crushing and drying.
(2) Weighing raw materials of each component of the blank base material according to the proportion, mixing, adding 45-65wt% of water, carrying out ball milling for 10-20h, then adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1-2h to obtain the slurry.
(3) And sieving, deironing and spray drying the slurry to obtain blank powder.
(4) Aging the blank powder for 40-50h, dry-pressing for molding, drying, ink-jet printing, glazing, and firing (1180-1240 ℃,60-140 mmin) to obtain the product with fracture toughness of more than 1.65 MPa-m 1/2 And the modulus of rupture is more than or equal to 75MPa.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and all the conventional reagent products can be obtained by commercial purchase.
Example 1
A high-toughness high-strength building ceramic rock slab blank comprises 89 parts of a blank base material, 5 parts of a crystallization inducer and 6 parts of a crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 7 parts of ball clay, 5 parts of illite, 22 parts of pyrophyllite, 36 parts of Indian potash feldspar, 10 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the high-toughness and high-strength building ceramic rock slab blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And ageing the rock plate blank powder for 48 hours, then performing dry pressing forming, drying, ink-jet printing and glazing, and then firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the high-toughness and high-strength building ceramic rock slab blank.
Example 2
A high-toughness high-strength building ceramic rock slab blank comprises 89 parts of a blank base material, 2 parts of a crystallization inducer and 9 parts of a crystal growth promoter;
the green body base material comprises, by weight, 100 parts of washed kaolin 15 parts, ball clay 7 parts, illite 5 parts, pyrophyllite 22 parts, indian potash feldspar 36 parts, porcelain stone 10 parts, wollastonite 2 parts and calcined talc 3 parts;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 18 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the high-toughness and high-strength building ceramic rock slab blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the high-toughness and high-strength building ceramic rock slab blank.
Example 3
A high-toughness high-strength building ceramic rock slab blank comprises 89 parts of a blank base material, 5 parts of a crystallization inducer and 6 parts of a crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 7 parts of ball clay, 5 parts of illite, 22 parts of pyrophyllite, 36 parts of Indian potash feldspar, 10 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is mullite powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 18 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the high-toughness and high-strength building ceramic rock slab blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the building ceramic rock plate blank with high toughness and high strength.
Example 4
A high-toughness high-strength building ceramic rock slab blank comprises 89 parts of a blank base material, 5 parts of a crystallization inducer and 6 parts of a crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 7 parts of ball clay, 5 parts of illite, 22 parts of pyrophyllite, 36 parts of Indian potash feldspar, 10 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 25 parts of lithium carbonate, 12 parts of vanadium pentoxide, 25 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 17 parts of potassium carbonate.
The preparation method of the high-toughness and high-strength building ceramic rock slab blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the building ceramic rock plate blank with high toughness and high strength.
Example 5
A high-toughness high-strength building ceramic rock slab blank comprises 89 parts of a blank base material, 5 parts of a crystallization inducer and 6 parts of a crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 8 parts of ball clay, 5 parts of illite, 24 parts of pyrophyllite, 30 parts of Indian potash feldspar, 12 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 25 parts of lithium carbonate, 12 parts of vanadium pentoxide, 25 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 17 parts of potassium carbonate.
The preparation method of the high-toughness and high-strength building ceramic rock slab blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the high-toughness and high-strength building ceramic rock slab blank.
Example 6
A high-toughness high-strength building ceramic rock slab blank comprises 89 parts of a blank base material, 5 parts of a crystallization inducer and 6 parts of a crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 7 parts of ball clay, 5 parts of illite, 22 parts of pyrophyllite, 36 parts of Indian potash feldspar, 10 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is zirconium oxide powder: mullite =1:1, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m; the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the high-toughness and high-strength building ceramic rock slab blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the high-toughness and high-strength building ceramic rock slab blank.
Comparative example 1 (comparison with example 1, only with the difference that the green body base formulation has not been optimized)
A building ceramic rock slab blank comprises 89 parts of blank base material, 5 parts of crystallization inducer and 6 parts of crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 4 parts of ball clay, 4 parts of illite, 10 parts of pyrophyllite, 49 parts of indian potash feldspar, 20 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 18 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the building ceramic rock plate blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the building ceramic rock plate blank.
Comparative example 2 (comparison with example 1, only with the difference that the green body base formulation has not been optimized)
A building ceramic rock slab blank comprises 89 parts of blank base material, 5 parts of crystallization inducer and 6 parts of crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 12 parts of ball clay, 8 parts of illite, 30 parts of pyrophyllite, 18 parts of Indian potash feldspar, 6 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 18 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the building ceramic rock plate blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining a building ceramic rock plate blank.
Comparative example 3 (compared with example 1, only difference is that the grain size of the crystallization inducer is too large)
A building ceramic rock plate blank comprises 89 parts of blank base material, 5 parts of crystallization inducer and 6 parts of crystal growth promoter;
the green body base material comprises, by weight, 100 parts of water-washed kaolin, 7 parts of ball clay, 5 parts of illite, 22 parts of pyrophyllite, 36 parts of Indian potash feldspar, 10 parts of porcelain stone, 2 parts of wollastonite and 3 parts of calcined talc;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 10-30 mu m, and D90 is more than 20 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 18 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the building ceramic rock plate blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is D90 less than 2 mu m;
(2) Preparing materials according to the base materials of the blank, mixing, adding 65wt% of water, performing ball milling for 20h, adding a crystallization inducer and a crystal growth promoter, and continuing ball milling for 1h to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the building ceramic rock plate blank.
Comparative example 4 (compared with example 1, the difference is only that the grain size of the crystal growth promoter is too large)
A building ceramic rock slab blank comprises 89 parts of blank base material, 5 parts of crystallization inducer and 6 parts of crystal growth promoter;
the green body base material comprises, by weight, 100 parts of washed kaolin 15 parts, ball clay 7 parts, illite 5 parts, pyrophyllite 22 parts, indian potash feldspar 36 parts, porcelain stone 10 parts, wollastonite 2 parts and calcined talc 3 parts;
wherein the crystallization inducer is alpha-alumina powder, the fineness of the crystallization inducer is 2-10 mu m, and D90 is less than 10 mu m;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of a glass frit, 18 parts of lithium carbonate, 9 parts of vanadium pentoxide, 32 parts of quartz, 9 parts of calcium phosphate, 12 parts of boric acid and 20 parts of potassium carbonate.
The preparation method of the building ceramic rock plate blank comprises the following steps:
(1) The crystal growth promoter is prepared by weighing and mixing the raw materials of the crystal growth promoter, melting at 1320 ℃, and performing water quenching, crushing and drying on the mixture. The fineness of the crystal growth promoter is 3-20 mu m, and D90 is more than 10 mu m;
(2) Preparing materials according to the components of the base material of the blank, mixing, adding 65wt% of water, performing ball milling for 20 hours, adding a crystallization inducer and a crystal growth promoter, and continuously performing ball milling for 1 hour to obtain slurry;
(3) Sieving, deironing and spray drying the slurry to obtain rock plate blank powder;
(4) And (3) ageing the powder of the rock plate blank for 48h, then performing dry pressing, drying, ink-jet printing, glazing and firing. The sintering temperature is 1210 ℃, and the total sintering time is 85min. Obtaining the building ceramic rock plate blank.
Performance testing
The architectural ceramic rock plate blanks obtained in examples 1-6 and the respective proportions were subjected to performance testing, wherein: the water absorption rate is detected by referring to GB/T4100-2015; the modulus of rupture is detected by referring to GB/T4100-2015; detecting the fracture toughness by referring to GB/T23806-2009; detecting the thermal shock resistance by referring to GB/T4100-2015; the frost resistance was examined with reference to GB/T4100-2015. The results obtained are shown in table 1:
TABLE 1 examination of the Properties of the high-toughness, high-strength architectural ceramic rock slab blanks obtained in examples 1-6
From the comparison of the data in the above table:
comparative example 1: compared with the example 1, the difference is only that the formula of the green body base material is not optimized, the proportion of flux raw materials such as potash feldspar and porcelain stone in the green body base material is high, and the clay raw materials are few, so that the temperature of the glass phase in the green body is low, the alumina component capable of providing mullite formation and growth in the liquid phase component is reduced, the proportion of alkali metal in the green body is high, the expansion coefficient of the glass phase is large, and the fracture toughness and the thermal shock resistance are reduced.
Comparative example 2: compared with the embodiment 1, the difference is that the formula of the green body base material is not optimized, mainly the proportion of the flux raw materials and the proportion of the clay raw materials in the green body base material are low, so that the sintering temperature of the green body is increased, the quantity of liquid phases is reduced, the temperature of the liquid phases is increased, and under the condition of low-temperature quick firing, the high-temperature liquid phase of the green body is not enough to have enough time to melt more aluminum-silicon components beneficial to the growth of mullite, so that the water absorption rate is increased, and the fracture modulus and the fracture toughness are reduced.
Comparative example 3: compared with the example 1, the difference is that the grain diameter of the crystallization inducer is too large, the fineness of the crystallization inducer is 10-30 μm, and the D90 is more than 20 μm. The crystallization inducer added in the invention is used as a crystal nucleus for mullite growth, and the formation process of the crystal nucleus is reduced. The excessive particle size causes the number of crystal nuclei to decrease, and the crystals grow abnormally and become coarse. It is difficult to achieve the effect of increasing fracture toughness by forming network-like mullite crystals.
Comparative example 4: compared with the example 1, the difference is that the grain diameter of the crystal growth promoter is too large, the fineness of the crystal growth promoter is 3-20 μm, and D90 is more than 10 μm. The crystal growth promoter added in the invention has the function of promoting the mullite crystals to rapidly grow around crystal nuclei, and the fused reaction of the mullite crystals entering a liquid phase is influenced by too large granularity, so that the aim of promoting the growth of the mullite in the liquid phase is fulfilled. And thus the modulus of rupture and fracture toughness are lowered.
In addition, FIGS. 1-4 are, in sequence, electron microscope scans of ceramic rock plate blanks prepared in examples 1-4 of the present invention. From the figure, it can be observed that the mullite whiskers grown in situ are uniformly dispersed and present a three-dimensional network.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. A high-toughness high-strength building ceramic rock slab blank is characterized in that: comprises 85-90 parts of blank base material, 2-5 parts of crystallization inducer and 6-10 parts of crystal growth promoter by weight part of 100 parts; wherein:
the green body base material comprises, by weight, 100 parts of water-washed kaolin 12-20 parts, ball clay 5-8 parts, illite 4-8 parts, pyrophyllite 15-25 parts, potassium anorthite 20-45 parts, porcelain stone 5-15 parts, wollastonite 1-3 parts and calcined talc 2-5 parts;
the crystallization inducer comprises one or a combination of more of alpha-alumina powder, zirconia powder and mullite powder;
the crystal growth promoter is a glass frit, and the raw materials comprise, by weight, 100 parts of lithium carbonate, 5-15 parts of vanadium pentoxide, 20-35 parts of quartz, 2-15 parts of calcium phosphate, 10-15 parts of boric acid and 15-25 parts of potassium carbonate.
2. A high toughness, high strength architectural ceramic rock panel blank according to claim 1, wherein: the fineness of the crystallization inducer is 2-10 mu m, and the D90 is less than 10 mu m.
3. A high toughness, high strength architectural ceramic rock panel blank according to claim 2, wherein: the fineness of the crystal growth promoter is D90 less than 2 mu m.
4. A method for preparing the high toughness high strength architectural ceramic rock plate blank according to any one of claims 1 to 3, characterized by the steps of:
(1) Weighing the raw materials of the crystal growth promoter according to the proportion, mixing, melting, and performing water quenching, crushing and drying to obtain the crystal growth promoter;
(2) Weighing raw materials of each component of the blank base material according to the proportion, mixing, adding water, carrying out ball milling, then adding a crystallization inducer and a crystal growth promoter, and continuing ball milling to obtain slurry;
(3) Screening, deironing and spray drying the slurry to obtain blank powder;
(4) And after the blank powder is aged, carrying out dry pressing forming, drying, ink-jet printing, glazing and sintering to obtain the high-toughness and high-strength building ceramic rock slab blank.
5. The method of claim 4, wherein: in the step (1), the melting temperature of the crystal growth promoter is 1300-1350 ℃.
6. The method of claim 4, wherein: in the step (2), the time of the first ball milling is 10-20h, and the time of the second ball milling is 1-2h.
7. The method of claim 4 or 6, wherein: in the step (2), 45-65% of water is added to wt%.
8. The method of claim 4, wherein: in the step (4), the time for ageing treatment of the blank powder is 40-50h.
9. The method of claim 4 or 8, wherein: in the step (4), the firing temperature is 1180-1240 ℃ and the total firing time is 60-140min.
10. The method of claim 4, wherein: in the step (4), the fracture toughness of the finally obtained building ceramic rock plate blank body>1.65 MPa·m 1/2 The modulus of rupture is more than or equal to 75MPa.
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