CN113601693B - Process technology for preparing strengthened and toughened rock plate by layering distribution - Google Patents

Process technology for preparing strengthened and toughened rock plate by layering distribution Download PDF

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CN113601693B
CN113601693B CN202111178761.2A CN202111178761A CN113601693B CN 113601693 B CN113601693 B CN 113601693B CN 202111178761 A CN202111178761 A CN 202111178761A CN 113601693 B CN113601693 B CN 113601693B
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powder
rock plate
distribution
toughened
distributing
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CN113601693A (en
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赵威
钟保民
金国庭
徐登翔
李智鸿
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Foshan Dongpeng Ceramic Co Ltd
Foshan Dongpeng Ceramic Development Co Ltd
Guangdong Dongpeng Holdings Co Ltd
Qingyuan Nafuna Ceramics Co Ltd
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Foshan Dongpeng Ceramic Co Ltd
Foshan Dongpeng Ceramic Development Co Ltd
Guangdong Dongpeng Holdings Co Ltd
Qingyuan Nafuna Ceramics Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B13/00—Feeding the unshaped material to moulds or apparatus for producing shaped articles; Discharging shaped articles from such moulds or apparatus
    • B28B13/02—Feeding the unshaped material to moulds or apparatus for producing shaped articles
    • B28B13/0215—Feeding the moulding material in measured quantities from a container or silo
    • B28B13/022—Feeding several successive layers, optionally of different materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/004—Devices for shaping artificial aggregates from ceramic mixtures or from mixtures containing hydraulic binder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/04—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers
    • B28B11/044—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers with glaze or engobe or enamel or varnish
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B13/00—Feeding the unshaped material to moulds or apparatus for producing shaped articles; Discharging shaped articles from such moulds or apparatus
    • B28B13/02—Feeding the unshaped material to moulds or apparatus for producing shaped articles
    • B28B13/0215—Feeding the moulding material in measured quantities from a container or silo
    • B28B13/0225—Feeding specific quantities of material at specific locations in the mould
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

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Abstract

The invention relates to the technical field of rock plates and ceramic large plates, in particular to a process technology for preparing a strengthened and toughened rock plate by layering and distributing materials. According to the technical scheme, the toughened rock plate is prepared by the partitioned layered distribution, so that the optimal effect of toughening of the rock plate can be achieved under the condition of the minimum using amount of the tetragonal phase zirconia, and the cost of raw materials is reduced.

Description

Process technology for preparing strengthened and toughened rock plate by layering distribution
Technical Field
The invention relates to the technical field of rock plates and ceramic large plates, in particular to a process technology for preparing a strengthened and toughened rock plate by layering and distributing materials.
Background
The ceramic rock plate has the advantages of health, environmental protection, fire resistance, high temperature resistance, bacteria resistance, easy cleaning, wear resistance, scratch resistance and the like, and is widely applied to the fields of household table boards, furniture panels, electric appliance panels, external walls, floors and the like. In recent years, as the rock plate forming technology is continuously mature and the application field is further expanded, all large ceramic enterprises compete to enter the field of ceramic rock plates.
However, the rock plate is used as a household table top and a household panel, and any cutting, polishing, drilling, chamfering and other machining processes need to be carried out, and due to the fact that the toughness of the rock plate is poor, 30% -50% or even higher cutting cracks can occur when the rock plate product is machined, the product yield is low, later-stage use of the product is seriously affected, production cost is increased, and the easiness in machining cracks become a bottleneck limiting development of the rock plate.
The application number 202010864905.9 discloses a non-breakable rock plate and a preparation method thereof, the application improves the breaking modulus and the breaking strength of the rock plate by adding silicon carbide and a reinforcing agent, and the silicon carbide reacts from 900 ℃ to generate carbon dioxide and carbon monoxide gas to be discharged due to the addition of the silicon carbide, so that the defect of pores is easily generated in the interior of the rock plate and glaze surface, and the high-quality rate is reduced. Chinese patent application No. 202010954969.8 discloses a high-strength ceramic rock plate and a method for preparing the same. The method realizes the high strength of the ceramic rock plate by setting the composition of the rock plate blank, the ground glaze and the overglaze, can achieve the required effect only by highly matching the rock plate blank, the ground glaze and the overglaze, and cannot easily achieve the purpose of improving the strength of the rock plate under the condition that the blank, the ground glaze and the overglaze slightly fluctuate and any two are not perfectly combined in production. Therefore, how to reduce the cracking condition of the rock plate during mechanical processing is still a problem that needs to be solved by rock plate enterprises.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a process technology for preparing a strengthened and toughened rock plate by layered distribution, wherein a rock plate blank is prepared by layered distribution, tetragonal-phase zirconia powder is added into the raw material of the rock plate blank, and the tetragonal-phase zirconia expands in volume during phase change to close the tips of cracks, prevent the cracks from expanding and increase the crack induction energy of the strengthened and toughened rock plate, so that the cracking phenomenon of the rock plate in later-stage mechanical processing can be greatly reduced, and the problem that the traditional rock plate is easy to crack during mechanical processing is solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; the raw material of the powder B comprises 3-6% of tetragonal phase zirconia powder and 94-97% of base material by mass percent; the raw material of the powder C comprises 7-10% of tetragonal-phase zirconia powder and 90-93% of base material, the raw material of the powder D comprises 11-15% of tetragonal-phase zirconia powder and 85-89% of base material, and the tetragonal-phase zirconia powder consists of tetragonal-phase zirconia and stabilizing agent;
(2) area division: dividing the material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be mechanically cut and processed, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be mechanically cut and processed;
(3) carrying out layered distribution in a post-processing area of a distribution mould, carrying out layered distribution in a non-processing area or distributing powder A or powder B in the non-processing area, wherein the layered distribution specifically comprises the following steps: distributing powder C or powder D at the bottom of a distributing mold to obtain a bottom layer, distributing powder A or powder B on the surface of the bottom layer to obtain a first middle layer, and distributing powder C or powder D on the surface of the first middle layer to obtain a surface layer; after the material distribution is finished, pressing and forming to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Further, five layers of cloth are distributed in the post-processing area, and the operation method comprises the following steps:
distributing powder C or powder D at the bottom of the post-processing area to obtain a bottom layer:
distributing powder B or powder C on the surface of the bottom layer to obtain a second middle layer;
distributing A or powder B on the surface of the second intermediate layer to obtain a first intermediate layer;
distributing powder B or powder C on the surface of the first intermediate layer to obtain a third intermediate layer;
and spreading powder C or powder D on the surface of the third middle layer to obtain a surface layer.
Further, five layers of cloth are distributed in the post-processing area, and the operation method comprises the following steps:
distributing powder D at the bottom of the post-processing area to obtain a bottom layer:
distributing powder B or powder C on the surface of the bottom layer to obtain a second middle layer;
distributing powder A on the surface of the second intermediate layer to obtain a first intermediate layer;
distributing powder B or powder C on the surface of the first intermediate layer to obtain a third intermediate layer;
and spreading powder D on the surface of the third middle layer to obtain a surface layer.
Further, in the step (1), the stabilizing agent is yttrium oxide or strontium oxide.
Furthermore, the tetragonal zirconia powder contains 1.5 to 3.5 percent of yttrium oxide or 8 to 16 percent of strontium oxide by mole fraction, and the balance is tetragonal zirconia.
Further, the cloth thickness of the bottom layer and the cloth thickness of the surface layer respectively account for 10% -20% of the total cloth thickness;
the cloth thickness of the first middle layer accounts for 60% -80% of the total cloth thickness.
Further, the cloth thickness of the bottom layer, the cloth thickness of the second middle layer, the cloth thickness of the third middle layer and the cloth thickness of the surface layer respectively account for 10% -20% of the total cloth thickness;
the cloth thickness of the first middle layer accounts for 20% -60% of the cloth thickness.
Further, in the step (4), the firing temperature profile of the strengthened and toughened rock plate comprises:
a preheating section: raising the temperature from normal temperature to 300 ℃;
an oxidative decomposition section: from 300 ℃ to 1000 ℃;
a sintering section: from 1000 ℃ to 1200 ℃;
a cooling section: cooling from 1200 deg.C to normal temperature.
Further, in the cooling section, the cooling rate from 1200 ℃ to 600 ℃ is 35-45 ℃/min, the cooling rate from 600 ℃ to 550 ℃ is 12-15 ℃/min, the cooling rate from 550 ℃ to 300 ℃ is 45-50 ℃/min, and the cooling rate from 300 ℃ to 250 ℃ is 12-15 ℃/min.
Further, in the step (1), the raw materials of the base material comprise, by mass, 15-22% of black mud, 15-25% of diopside, 15-25% of kaolin, 10-16% of potash feldspar, 8-10% of albite, 12-20% of bentonite and 5-10% of reclaimed materials.
The technical scheme has the following beneficial effects that:
1. according to the technical scheme, the rock plate blank is prepared by adopting partitioned layered distribution, and the toughened rock plate is prepared by utilizing the phase change toughening of the tetragonal phase zirconia, so that the volume of the tetragonal phase zirconia expands during phase change, the tip of a crack is closed, the crack is prevented from expanding, and the crack induction energy of the toughened rock plate is increased, so that the later-stage mechanical processing cracking phenomenon of the rock plate can be greatly reduced.
2. This technical scheme sets the region that need carry out the mechanical cutting processing with obtough rock plate to the postprocessing region, and the region that need not carry out cutting processing sets to not process the region, thereby corresponding divide into the postprocessing region and not process the region with the cloth mould, five layers of cloth are carried out in the postprocessing region, compare with three-layer cloth, all can make the crack induction energy, intensity and fracture toughness of the postprocessing region of obtough rock plate that the preparation obtained show and improve, and when reaching the same intensity, fracture toughness and crack induction energy, adopt five layers of cloth and more can save the material cost.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; the raw material of the powder B comprises 3-6% of tetragonal zirconia powder and 94-97% of base material by mass percent; the raw material of the powder C comprises 7-10% of tetragonal-phase zirconia powder and 90-93% of base material, the raw material of the powder D comprises 11-15% of tetragonal-phase zirconia powder and 85-89% of base material, and the tetragonal-phase zirconia powder consists of tetragonal-phase zirconia and stabilizing agent;
(2) area division: dividing the material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be mechanically cut and processed, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be mechanically cut and processed;
(3) the method comprises the following steps of carrying out layered distribution in a post-processing area of a distribution mould, carrying out layered distribution in a non-processing area or distributing and applying powder A or powder B in the non-processing area, wherein the layered distribution specifically comprises the following steps: distributing powder C or powder D at the bottom of the distributing mold to obtain a bottom layer, distributing powder A or powder B on the surface of the bottom layer to obtain a first middle layer, and distributing powder C or powder D on the surface of the first middle layer to obtain a surface layer; after the material distribution is finished, pressing and forming to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
The rock plate is often used as a household table top and a household panel, and is required to be subjected to mechanical processing such as random cutting, grinding, drilling, chamfering and the like, because the toughness of the existing rock plate under high strength is low, 30 to 50 percent or even higher cutting cracking can occur during mechanical processing, so that the product percent of pass is low, and the later use of the product is seriously influenced, in order to solve the problems, the technical scheme adopts a partition layering material distribution method to prepare a rock plate blank, and utilizes tetragonal phase zirconia phase transformation toughening to prepare the toughening rock plate, so that the tetragonal phase zirconia expands in volume during phase transformation, the tip of a crack is closed, the crack is prevented from expanding and the crack induction energy of the toughening rock plate is increased, the strength and the fracture toughness of the toughening rock plate are obviously improved, the cracking phenomenon of the rock plate in later mechanical processing can be greatly reduced, and the technical scheme adopts partition layering material distribution to prepare the toughening rock plate, the optimum effect of strengthening and toughening the rock plate can be achieved under the condition of the minimum usage of tetragonal phase zirconia, thereby reducing the cost of raw materials.
It is to be noted that the crack-inducing energy means energy required for causing cracks in the internal defects of the material. The higher the crack initiation energy is, the greater the force for generating through cracks by the crack propagation under stress in the post-processing is, and the cracks can be generated only if the through cracks are generated. When the post-processing is stressed, the air holes are crack sources, cracks are expanded from stress concentration positions of the air holes, the front ends of the crack expansion are crack tips, the tetragonal phase zirconia is subjected to phase change to expand the volume, the crack tips are closed under extrusion force, the cracks can be continuously expanded by larger force, and the purpose of improving the crack induction energy is achieved. Therefore, the technical scheme can effectively prevent the surface of the toughened rock plate from penetrating through cracks by improving the crack induction energy.
Specifically, the tetragonal zirconia has a transformation toughening mechanismTetragonal zirconia (t-ZrO) when subjected to external impact2) Will convert to monoclinic phase zirconia (m-ZrO)2) The volume of the zirconium oxide is increased due to the phase change, partial external impact force is counteracted, and the purpose of toughening is achieved, the technical scheme is that tetragonal phase zirconium oxide powder is added into a rock plate raw material, the crack induction energy can be improved when the rock plate is stressed (or impacted) by utilizing the principle of the increase of the phase change volume of the tetragonal phase zirconium oxide, the formation of through cracks on the surface of the rock plate is prevented, and the purpose of reducing the cutting crack proportion of the rock plate is further achieved, the strength and the toughness of the rock plate are firstly increased and then reduced along with the increase of the tetragonal phase zirconium oxide powder in the rock plate raw material, and a peak value appears at 15 percent, so the technical scheme divides the rock plate powder into powder A, powder B, powder C and powder D, the mass percentages of the tetragonal phase zirconium oxide powder in the four kinds of powder are different, and the bottom layer and the surface layer are not restrained and are easy to crack, therefore, the bottom layer and the surface layer adopt powder C with the mass percent of tetragonal zirconia powder being 7-10% or powder D with the mass percent being 11-15%, and the middle layer is bound by the surface layer and the bottom layer, so that the first middle layer is coated with powder B with less tetragonal zirconia powder mass percent or coated with powder A without tetragonal zirconia powder, and the effect of enhancing the strength and toughness of the toughened rock plate can be achieved by carrying out layered distribution, and meanwhile, the cost of raw materials can be reduced.
It is worth explaining that, when a small amount of tetragonal zirconia is sintered at a low temperature of 100-400 ℃, phase change can occur without external impact force, so that the tetragonal zirconia is converted into monoclinic zirconia, the content of the tetragonal zirconia in the rock plate is reduced, and the volume increasing effect and the toughening effect of the tetragonal zirconia are reduced when the toughened rock plate is subjected to external force, therefore, the stabilizing agent is added into the tetragonal zirconia powder, the phase change of the tetragonal zirconia during sintering at the low temperature of 100-400 ℃ can be effectively avoided, the toughness of the toughened rock plate during mechanical processing is further increased, and the cracking problem of the toughened rock plate during mechanical processing is further reduced.
By way of further illustration, zirconia is generally classified as tetragonalPhase zirconium oxide (t-ZrO)2) Monoclinic phase zirconium oxide (m-ZrO)2) And cubic phase zirconium oxide (c-ZrO)2) Wherein, monoclinic phase zirconia (m-ZrO)2) No phase change and volume expansion under stress, and the effect of closing the crack tip, even though the cubic phase of zirconium oxide (c-ZrO)2) When stressed, the zirconium oxide partially converted into monoclinic phase (m-ZrO)2) But cubic phase zirconia (c-ZrO)2) The phase change and the volume change are small, the crack tips appearing in mechanical cutting are difficult to be closed, and the technical scheme selects tetragonal phase zirconium oxide (t-ZrO)2) Is due to tetragonal zirconia (t-ZrO)2) The phase change is carried out under stress to convert into monoclinic zirconia (m-ZrO)2) During the process, the volume expansion of 7% -10% is accompanied, the volume change is large, the tip of a crack generated during mechanical cutting can be closed, the crack induction energy is improved, and therefore cracking of the toughened rock plate is effectively avoided.
Further, according to the technical scheme, the area, needing to be subjected to mechanical cutting machining, of the toughened rock plate is set as the post-machining area, the area, needing not to be subjected to cutting machining, is set as the non-machining area, so that the material distribution die is correspondingly divided into the post-machining area and the non-machining area, and layered material distribution is performed in the post-machining area, so that the strength, the fracture toughness and the crack induction energy of the post-machining area can be effectively improved, and the cracking phenomenon during cutting is avoided.
According to the technical scheme, layered material distribution can be carried out in a non-processing area, the overall strength, the fracture toughness and the crack induction energy of the strengthening and toughening rock plate can be improved, however, the cost can be increased if the whole strengthening and toughening rock plate is made of the layered material distribution, and the cracking is less in the non-processing area due to no need of mechanical cutting, so that the preferable condition is that powder A without tetragonal phase zirconia powder or powder B with a small amount of tetragonal phase zirconia powder is distributed in the non-processing area, the proportion of cracking of the strengthening and toughening rock plate in the mechanical cutting process can be effectively reduced by carrying out the partitioned layered material distribution on the strengthening and toughening rock plate, and the tetragonal phase zirconia (t-ZrO) is adopted2) The powder has higher price, and the distribution by areas and layers can reachOn the premise of reducing the post-processing cracking proportion, the raw material cost is reduced.
The strength of the existing rock plate is generally 55-65MPa, and the fracture toughness is generally 1.2-1.4 MPa/m2In the technical scheme, three layers of cloth are distributed in the post-processing area, compared with the non-processing area, the strength of the post-processing area of the prepared strengthening and toughening rock plate is improved by 40-55%, and the fracture toughness is improved by 15-20%, so that the three layers of cloth are distributed in the post-processing area, the crack induction energy of the post-processing area of the strengthening and toughening rock plate can be effectively improved, and the strength and the fracture toughness of the strengthening and toughening rock plate are effectively improved, therefore, the phenomenon that the post-processing area cracks during cutting can be effectively avoided, the strength, the fracture toughness and the crack induction energy of the post-processing area of the strengthening and toughening rock plate prepared only in the post-processing area by three layers of cloth are not greatly different from the performance of the strengthening and toughening rock plate prepared by three layers of cloth in the whole cloth mold, but the strengthening and toughening rock plate is prepared by a partitioning and layering cloth mode, the cost can be greatly saved.
Further, five layers of cloth are carried out in the post-processing area, and the operation method is as follows:
applying powder C or powder D at the bottom of the post-processing area to obtain a bottom layer:
distributing powder B or powder C on the surface of the bottom layer to obtain a second middle layer;
distributing A or powder B on the surface of the second intermediate layer to obtain a first intermediate layer;
distributing powder B or powder C on the surface of the first middle layer to obtain a third middle layer;
and spreading powder C or powder D on the surface of the third middle layer to obtain a surface layer.
In one embodiment of the invention, five layers of cloth are carried out in the post-processing area, compared with three layers of cloth, the strength, the fracture toughness and the crack induction energy of the post-processing area of the prepared toughened rock plate can be obviously improved, and when the same strength, the fracture toughness and the crack induction energy are achieved, the raw material cost can be further saved by adopting the five layers of cloth.
Further, five layers of cloth are carried out in the post-processing area, and the operation method is as follows:
applying powder D at the bottom of the post-processing area to obtain a bottom layer:
distributing powder B or powder C on the surface of the bottom layer to obtain a second middle layer;
distributing powder A on the surface of the second intermediate layer to obtain a first intermediate layer;
distributing powder B or powder C on the surface of the first middle layer to obtain a third middle layer;
and spreading powder D on the surface of the third middle layer to obtain a surface layer.
In another embodiment of the invention, the powder D is used as the raw material of the bottom layer and the surface layer, the powder A is used as the raw material of the first middle layer, and the powder B or the powder C is used as the raw material of the second middle layer and the third middle layer.
Stated further, in step (1), the stabilizing agent is yttria or strontium oxide.
It should be noted that although other oxides such as magnesium oxide and calcium oxide have a certain stabilizing effect, the effect is not good, and yttrium oxide or strontium oxide is used as a stabilizer to effectively prevent tetragonal zirconia from phase transformation.
Further, the tetragonal zirconia powder contains 1.5 to 3.5 percent of yttria or 8 to 16 percent of strontium oxide by mole fraction, and the rest is tetragonal zirconia.
By adding 1.5-3.5% of yttrium oxide or 8-16% of strontium oxide into the tetragonal-phase zirconia powder, the tetragonal-phase zirconia can be prevented from being transformed into monoclinic-phase zirconia due to phase change in a sintering area at a low temperature of 100-400 ℃, so that enough tetragonal-phase zirconia can be kept in the strengthened and toughened rock plate, and when mechanical cutting is carried out, the tetragonal-phase oxidation is changed in phase and expanded in volume, the crack tip can be closed and the crack induction energy can be improved, so that the problem that the strengthened and toughened rock plate cracks when mechanical cutting is carried out is effectively avoided.
Since monoclinic phase zirconia does not undergo phase transition and causes volume expansion when subjected to an external impact force, monoclinic phase zirconia does not have the effect of closing the tips of cracks and improving the crack-inducing energy, and therefore, when the proportion of tetragonal phase zirconia in the toughened rock plate is reduced and monoclinic phase zirconia appears, the toughened rock plate has lower toughness and is easy to crack during mechanical processing.
If the amount of yttrium oxide or strontium oxide added is too small, the toughened rock plate is likely to crack due to the presence of a portion of monoclinic phase zirconium oxide in the rock plate, and if the amount of yttrium oxide or strontium oxide added is too large, the stabilization effect is increased, but the reinforcing effect is not significant, and the cost is increased, so the amount of yttrium oxide added is set to 1.5% to 3.5% and the amount of strontium oxide added is set to 8% to 16%.
Further, the cloth thickness of the bottom layer and the cloth thickness of the surface layer respectively account for 10% -20% of the total cloth thickness;
the cloth thickness of the first middle layer accounts for 60% -80% of the total cloth thickness.
Further, the cloth thickness of the bottom layer, the cloth thickness of the second middle layer, the cloth thickness of the third middle layer and the cloth thickness of the surface layer respectively account for 10% -20% of the total cloth thickness;
the thickness of the cloth of the first middle layer accounts for 20% -60% of the thickness of the cloth.
When dividing five layers from bottom to top with the post-processing region and carrying out the cloth, can reach the intensity of the strengthening and toughening rock plate of preferred improvement, toughness and the effect that the crackle induced energy through the thickness of injecing every layer, and can effectively reduce material cost, if the surface course, the bottom, when the thickness of second intermediate level and third intermediate level is great, though the intensity in strengthening and toughening rock plate post-processing region, toughness and crackle induced energy are higher, but can make material cost greatly increased, if the surface course, the bottom, the thickness of second intermediate level and third intermediate level is less, then the intensity in strengthening and toughening rock plate post-processing region, toughness and crackle induced energy are lower, easy fracture when the cutting.
Stated further, in step (4), the firing temperature profile of the strengthened rock plate includes:
a preheating section: raising the temperature from normal temperature to 300 ℃;
an oxidative decomposition section: from 300 ℃ to 1000 ℃;
a sintering section: from 1000 ℃ to 1200 ℃;
a cooling section: cooling from 1200 deg.C to normal temperature.
It is worth to be noted that the mechanical water and the absorbed water in the rock plate blank body at the preheating section are discharged, the oxidation of organic matters and carbon, the carbonate decomposition, the removal of crystal water and the crystal form transformation occur in the rock plate blank body at the oxidative decomposition section, and the rock plate blank body is vitrified into porcelain at high temperature at the firing section; in the cooling section, the liquid phase in the raw material is crystallized, and the glass phase substances are solidified to form the rock plate.
Further, in the cooling section, the cooling rate from 1200 ℃ to 600 ℃ is 35-45 ℃/min, the cooling rate from 600 ℃ to 550 ℃ is 12-15 ℃/min, the cooling rate from 550 ℃ to 300 ℃ is 45-50 ℃/min, and the cooling rate from 300 ℃ to 250 ℃ is 12-15 ℃/min.
Because the free quartz can generate crystal form transformation at 573 ℃ and 273 ℃, alpha-quartz is transformed into beta-quartz at 573 ℃, the volume shrinkage is 0.82%, the alpha-quartz is transformed into the beta-quartz at 270 ℃, the volume shrinkage is 2.8%, when the volume is changed, large internal stress can be generated, the internal structure of the rock plate can be damaged, and the 'cutting crack' is easily caused, the cooling rate of reducing the temperature from 600 ℃ to 550 ℃ is set to be 12-15 ℃/min, and the cooling rate of reducing the temperature from 300 ℃ to 250 ℃ is also set to be 12-15 ℃/min, and the internal stress can be prevented by reducing the cooling rate, so that the rock plate is prevented from cracking.
Further, in the step (1), the raw materials of the base material comprise, by mass, 15-22% of black mud, 15-25% of diopside, 15-25% of kaolin, 10-16% of potash feldspar, 8-10% of albite, 12-20% of bentonite and 5-10% of reclaimed materials.
The usage amount of diopside is increased in the raw material formula of the base material, the content of CaO is increased, the crystal phase in the rock plate is increased, the glass phase is reduced, and the internal stress is reduced.
In particular, the recycled material refers to the recycling of waste products, filter mud and the like in ceramic factoriesThe recycled powder comprises 16.90 percent of AL by mass percent2O370.96% SiO20.33% of CaO, 0.99% of MgO and 0.79% of Fe2O30.23% of TiO23.10% of K2O and 2.79% of Na2O, 3.85% loss on ignition.
The technical solution is further illustrated below by reference to examples and comparative examples.
Example 1
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein the raw material of powder B comprises 6% of tetragonal zirconia powder and 94% of base material, the raw material of powder C comprises 10% of tetragonal zirconia powder and 90% of base material, the raw material of powder D comprises 15% of tetragonal zirconia powder and 85% of base material, and the tetragonal zirconia powder comprises 2.5mol% of yttrium oxide and 97.5mol% of tetragonal zirconia IV; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) carrying out layered material distribution in a post-processing area and a non-processing area of the material distribution mould, wherein the layered material distribution specifically comprises the following steps: distributing powder C at the bottom of a distribution mould with the thickness of 2mm to obtain a bottom layer, distributing powder A on the surface of the bottom layer with the thickness of 6mm to obtain a middle layer, distributing powder D on the surface of the middle layer with the thickness of 2mm to obtain a surface layer, after the distribution is finished, performing compression molding to obtain a rock plate blank,
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Example 2
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein, the raw material of the powder B consists of 6 percent of tetragonal phase zirconia powder and 94 percent of base material; the raw material of the powder C consists of 10% of tetragonal zirconia powder and 90% of base material, the raw material of the powder D consists of 15% of tetragonal zirconia powder and 85% of base material, and the tetragonal zirconia powder consists of 2.5mol% of yttrium oxide and 97.5mol% of tetragonal zirconia; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) carrying out layered material distribution in a post-processing area and a non-processing area of the material distribution mould, wherein the layered material distribution specifically comprises the following steps: distributing powder C at the bottom of a distribution mould, wherein the distribution thickness is 2mm to obtain a bottom layer, distributing powder B on the surface of the bottom layer, the distribution thickness is 6mm to obtain a middle layer, distributing powder D on the surface of the middle layer, the distribution thickness is 2mm to obtain a surface layer, and after the distribution is finished, performing compression molding to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Example 3
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein, the raw material of the powder B consists of 5 percent of tetragonal phase zirconia powder and 95 percent of base material; the raw material of the powder C comprises 10% of tetragonal zirconia powder and 90% of base material, the raw material of the powder D consists of 15% of tetragonal zirconia powder and 85% of base material, and the tetragonal zirconia powder consists of 10mol% of yttrium oxide and 90mol% of tetragonal zirconia; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) carrying out layered material distribution in a post-processing area and a non-processing area of the material distribution mould, wherein the layered material distribution specifically comprises the following steps: distributing powder D at the bottom of the distribution mould, wherein the thickness of the distribution is 1mm to obtain a bottom layer: distributing powder B on the surface of the bottom layer, wherein the thickness of the distributed powder B is 2mm, and obtaining a second middle layer; distributing powder A on the surface of the second middle layer, wherein the thickness of the distributed powder A is 4mm, and thus obtaining a first middle layer; distributing powder B on the surface of the first middle layer, wherein the distribution thickness is 2mm, and obtaining a third middle layer; distributing the powder D on the surface of the third middle layer, wherein the distribution thickness is 1mm to obtain a surface layer, and after the distribution is finished, performing compression molding to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Example 4
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein, the raw material of the powder B consists of 5 percent of tetragonal phase zirconia powder and 95 percent of base material; the raw material of the powder C consists of 10% of tetragonal zirconia powder and 90% of base material, the raw material of the powder D consists of 15% of tetragonal zirconia powder and 85% of base material, and the tetragonal zirconia powder consists of 10mol% of yttrium oxide and 90mol% of tetragonal zirconia; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) the method comprises the following steps of (1) carrying out layered material distribution in a post-processing area and a non-processing area of a material distribution die, wherein the layered material distribution specifically comprises the following steps: distributing powder D at the bottom of the distribution mould, wherein the thickness of the distribution is 1mm, and obtaining a bottom layer: distributing powder B on the surface of the bottom layer, wherein the thickness of the distributed powder B is 2mm, and obtaining a second middle layer; distributing powder A on the surface of the second middle layer, wherein the thickness of the distributed powder A is 4mm, and thus obtaining a first middle layer; distributing powder C on the surface of the first middle layer, wherein the thickness of the distributed powder C is 2mm, and obtaining a third middle layer; distributing the powder D on the surface of the third middle layer, wherein the distribution thickness is 1mm to obtain a surface layer, and after the distribution is finished, performing compression molding to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Example 5
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein, the raw material of the powder B consists of 5 percent of tetragonal phase zirconia powder and 95 percent of base material; the raw material of the powder C consists of 10% of tetragonal zirconia powder and 90% of base material, the raw material of the powder D consists of 15% of tetragonal zirconia powder and 85% of base material, and the tetragonal zirconia powder consists of 2.5mol% of yttrium oxide and 97.5mol% of tetragonal zirconia; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) carrying out layered material distribution in a post-processing area and a non-processing area of the material distribution mould, wherein the layered material distribution specifically comprises the following steps: distributing powder C at the bottom of the post-processing area, wherein the distribution thickness is 2mm to obtain a bottom layer, distributing powder B on the surface of the bottom layer, the distribution thickness is 6mm to obtain a middle layer, distributing powder D on the surface of the middle layer, wherein the distribution thickness is 2mm to obtain a surface layer, and distributing powder A in the central area, wherein the distribution thickness is 10 mm; after the material distribution is finished, the material is pressed and formed to obtain a rock plate blank,
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Example 6
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein, the raw material of the powder B consists of 5 percent of tetragonal phase zirconia powder and 95 percent of base material; the raw material of the powder C consists of 10% of tetragonal zirconia powder and 90% of base material, the raw material of the powder D consists of 15% of tetragonal zirconia powder and 85% of base material, and the tetragonal zirconia powder consists of 10mol% of yttrium oxide and 90mol% of tetragonal zirconia; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) carrying out layered material distribution in a post-processing area and a non-processing area of the material distribution mould, wherein the layered material distribution specifically comprises the following steps: distributing powder D at the bottom of the post-processing area, wherein the thickness of the distributed powder D is 1mm, and obtaining a bottom layer: distributing powder B on the surface of the bottom layer, wherein the thickness of the distributed powder B is 2mm, and obtaining a second middle layer; distributing powder A on the surface of the second middle layer, wherein the thickness of the distributed powder A is 4mm, and thus obtaining a first middle layer; distributing powder C on the surface of the first middle layer, wherein the thickness of the distributed powder C is 2mm, and obtaining a third middle layer; distributing powder D on the surface of the third middle layer, wherein the distribution thickness is 1mm, so as to obtain a surface layer, and distributing powder A in the central area, wherein the distribution thickness is 10 mm; after the material distribution is finished, pressing and forming to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Example 7
A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials comprises the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; wherein, the raw material of the powder B comprises 5 percent of tetragonal zirconia powder and 95 percent of base material, the raw material of the powder C comprises 10 percent of tetragonal zirconia powder and 90 percent of base material, the raw material of the powder D comprises 15 percent of tetragonal zirconia powder and 85 percent of base material, and the tetragonal zirconia powder comprises 10mol percent of yttrium oxide and 90mol percent of tetragonal zirconia; the raw materials of the base material comprise 20 percent of black mud, 19 percent of diopside, 21 percent of kaolin, 13 percent of potash feldspar, 9 percent of albite, 13 percent of bentonite and 5 percent of reclaimed materials;
(2) the method comprises the following steps of (1) dividing a material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be subjected to mechanical cutting processing, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be subjected to cutting processing;
(3) carrying out layered material distribution in a post-processing area and a non-processing area of the material distribution mould, wherein the layered material distribution specifically comprises the following steps: distributing powder D at the bottom of the post-processing area, wherein the thickness of the distributed powder D is 1mm, and obtaining a bottom layer: distributing powder C on the surface of the bottom layer, wherein the thickness of the distributed powder C is 2mm, and obtaining a second middle layer; distributing powder A on the surface of the second middle layer, wherein the thickness of the distributed powder A is 4mm, and thus obtaining a first middle layer; distributing powder C on the surface of the first middle layer, wherein the thickness of the distributed powder C is 2mm, and obtaining a third middle layer; distributing powder D on the surface of the third middle layer, wherein the distribution thickness is 1mm, so as to obtain a surface layer, and distributing powder A in the central area, wherein the distribution thickness is 10 mm; after the material distribution is finished, pressing and forming to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
Comparative example 1
A process technology of a rock plate comprises the following steps:
(1) preparing powder by adopting a spray granulation method, wherein the raw materials of the powder are base materials, and the raw materials of the base materials comprise 20% of black mud, 19% of diopside, 21% of kaolin, 13% of potash feldspar, 9% of albite, 13% of bentonite and 5% of reclaimed materials;
(2) distributing powder in a distributing mould, wherein the thickness of the distributed powder is 10mm, and obtaining a rock plate blank;
(3) and sequentially carrying out glaze spraying, ink-jet printing and sintering on the surface of the rock plate blank, wherein in the process of a sintering cooling section, the cooling rate of cooling from 650 ℃ to 500 ℃ is 13 ℃/min, the cooling rate of cooling from 350 ℃ to 200 ℃ is 12 ℃/min, and sintering to obtain the rock plate.
Specifically, the strength and the fracture toughness of the rock plate obtained in the comparative example are detected according to rock plate group mark, and the strength and the fracture toughness of the rock plate obtained in the comparative example are detected to be 59MPa and 1.3MPa/m2。
Comparative example 2
The preparation method of the comparative example and the composition of the raw materials between the layers were substantially the same as in example 6, except that the raw material of the tetragonal zirconia powder in the comparative example consisted only of tetragonal zirconia, and contained no stabilizer, and a strengthened and toughened rock plate was prepared.
Specifically, the strength and fracture toughness of the strengthened rock plates obtained in examples 1 to 6 and comparative example 2 were measured according to the rock plate group mark, respectively, wherein examples 5 and 6 were measured for strength and fracture toughness at the post-processing region, and the strength improvement ratio and the fracture toughness improvement ratio of the strengthened rock plates obtained in examples 1 to 6 and comparative example 2 were calculated with respect to the rock plate of comparative example 1.
Wherein the strength improvement ratio =
Figure 57178DEST_PATH_IMAGE001
；
Fracture toughness improvement ratio =
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；
In the formula, A1 is a toughened rock panel made in any one of examples 1-6 and comparative example 2, and A0 is a rock panel made in comparative example 1.
The results of the tests of examples 1-6 and comparative example 2 are shown in table 1 below:
Figure 255259DEST_PATH_IMAGE003
as shown in table 1, the strength and fracture toughness of the toughened rock plates prepared in examples 1 to 6 are both significantly improved as compared with those of comparative document 1, and it is known from the results of the tests in examples 1 and 2 that when the materials of the bottom layer and the face layer are the same and powder B containing 5% tetragonal zirconia powder is distributed in the first middle layer, the strength and fracture toughness of the prepared toughened rock plates are improved, and it is also known that when the total content of tetragonal zirconia powder in each layer of the rock plate material is increased, the strength of the prepared toughened rock plates is increased, the fracture toughness is increased, and the crack induction energy of the toughened rock plates is increased.
From the results of the tests of examples 2 and 5 and the results of the tests of examples 4 and 6, it can be seen that when the number of layers of the laminate is equal to the raw material of each layer, the strength and fracture toughness of the post-processed region of the toughened rock plate prepared by using the partitioned laminate distribution material are substantially equal to those of the toughened rock plate prepared by using only the laminate distribution material without performing the partitioned distribution material, and thus it can be seen that, although the powder a containing no tetragonal zirconia powder is distributed in the non-processed region, the strength, fracture toughness and crack induction energy of the post-processed region are not affected, and therefore, preferably, the toughened rock plate prepared by using the partitioned laminate distribution material in the present technical solution can not only reduce the rate of cracking occurring in the subsequent machining, but also effectively reduce the raw material cost.
From the test results of comparative example 2, it is known that when the tetragonal zirconia powder consisted of only tetragonal zirconia without a stabilizer, the strength, fracture toughness and crack induction energy of the resulting strengthened and toughened rock plate were greatly reduced.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.

Claims (10)

1. A process technology for preparing a strengthened and toughened rock plate by layering and distributing materials is characterized by comprising the following steps:
(1) preparing materials: preparing four parts of base materials, wherein the raw material of the powder A consists of one part of base material, adding tetragonal-phase zirconia powder with different mass into the other three parts of base materials respectively, and preparing powder B, powder C and powder D after spray granulation respectively; the raw material of the powder B comprises 3-6% of tetragonal phase zirconia powder and 94-97% of base material by mass percent; the raw material of the powder C comprises 7-10% of tetragonal-phase zirconia powder and 90-93% of base material, the raw material of the powder D comprises 11-15% of tetragonal-phase zirconia powder and 85-89% of base material, and the tetragonal-phase zirconia powder consists of tetragonal-phase zirconia and stabilizing agent;
(2) area division: dividing the material distribution mould into a post-processing area and a non-processing area, wherein the post-processing area is an area where the strengthened and toughened rock plate needs to be mechanically cut and processed, and the non-processing area is an area where the strengthened and toughened rock plate does not need to be mechanically cut and processed;
(3) carrying out layered distribution in a post-processing area of a distribution mould, carrying out layered distribution in a non-processing area or distributing powder A or powder B in the non-processing area, wherein the layered distribution specifically comprises the following steps: distributing powder C or powder D at the bottom of a distributing mold to obtain a bottom layer, distributing powder A or powder B on the surface of the bottom layer to obtain a first middle layer, and distributing powder C or powder D on the surface of the first middle layer to obtain a surface layer; after the material distribution is finished, pressing and forming to obtain a rock plate blank;
(4) and sequentially carrying out glaze spraying and ink-jet printing on the surface of the rock plate blank, and sintering to obtain the toughened rock plate.
2. The process technology for preparing the strengthened and toughened rock plate by the layered distribution material as claimed in claim 1, is characterized in that five layers of material distribution are carried out in the post-processing area, and the operation method is as follows:
distributing powder C or powder D at the bottom of the post-processing area to obtain a bottom layer:
distributing powder B or powder C on the surface of the bottom layer to obtain a second middle layer;
distributing A or powder B on the surface of the second intermediate layer to obtain a first intermediate layer;
distributing powder B or powder C on the surface of the first intermediate layer to obtain a third intermediate layer;
and spreading powder C or powder D on the surface of the third middle layer to obtain a surface layer.
3. The process technology for preparing the strengthened and toughened rock plate by the layered distribution material as claimed in claim 2, is characterized in that five layers of material distribution are carried out in the post-processing area, and the operation method is as follows:
distributing powder D at the bottom of the post-processing area to obtain a bottom layer:
distributing powder B or powder C on the surface of the bottom layer to obtain a second middle layer;
distributing powder A on the surface of the second intermediate layer to obtain a first intermediate layer;
distributing powder B or powder C on the surface of the first intermediate layer to obtain a third intermediate layer;
and spreading powder D on the surface of the third middle layer to obtain a surface layer.
4. The process technology for preparing the strengthened and toughened rock plate by the layered distribution material as claimed in claim 1, wherein in the step (1), the stabilizing agent is yttrium oxide or strontium oxide.
5. The process technology for preparing the strengthened and toughened rock plate by the layered distribution material according to claim 4, wherein the tetragonal zirconia powder contains 1.5-3.5% of yttria or 8-16% of strontium oxide by mole fraction, and the balance is tetragonal zirconia.
6. The process technology for preparing the toughened rock plate by the layered distribution material as claimed in claim 1, wherein the distribution thickness of the bottom layer and the distribution thickness of the surface layer respectively account for 10% -20% of the total distribution thickness;
the cloth thickness of the first middle layer accounts for 60% -80% of the total cloth thickness.
7. The process technology for preparing the toughened rock plate by the layered distribution material as claimed in claim 2, wherein the distribution thickness of the bottom layer, the distribution thickness of the second intermediate layer, the distribution thickness of the third intermediate layer and the distribution thickness of the surface layer respectively account for 10% -20% of the total distribution thickness;
the cloth thickness of the first middle layer accounts for 20% -60% of the cloth thickness.
8. The process technology for preparing the strengthened rock plate by the layered distribution material as claimed in claim 1, wherein in the step (4), the firing temperature curve of the strengthened rock plate comprises:
a preheating section: raising the temperature from normal temperature to 300 ℃;
an oxidative decomposition section: from 300 ℃ to 1000 ℃;
a sintering section: from 1000 ℃ to 1200 ℃;
a cooling section: cooling from 1200 deg.C to normal temperature.
9. The process technology for preparing the strengthened and toughened rock plate by the layered distribution material as claimed in claim 8, wherein in the cooling section, the cooling rate from 1200 ℃ to 600 ℃ is 35-45 ℃/min, the cooling rate from 600 ℃ to 550 ℃ is 12-15 ℃/min, the cooling rate from 550 ℃ to 300 ℃ is 45-50 ℃/min, and the cooling rate from 300 ℃ to 250 ℃ is 12-15 ℃/min.
10. The process technology for preparing the strengthened and toughened rock plate by the layered distribution material as claimed in claim 1, wherein in the step (1), the raw materials of the base material comprise, by mass percent, 15-22% of black mud, 15-25% of diopside, 15-25% of kaolin, 10-16% of potash feldspar, 8-10% of albite, 12-20% of bentonite and 5-10% of reclaimed materials.
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