CN110978228A - Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process - Google Patents
Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process Download PDFInfo
- Publication number
- CN110978228A CN110978228A CN201911100056.3A CN201911100056A CN110978228A CN 110978228 A CN110978228 A CN 110978228A CN 201911100056 A CN201911100056 A CN 201911100056A CN 110978228 A CN110978228 A CN 110978228A
- Authority
- CN
- China
- Prior art keywords
- powder
- ceramic
- gradient
- mold
- irrigation film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- B28B7/00—Moulds; Cores; Mandrels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G25/00—Watering gardens, fields, sports grounds or the like
- A01G25/06—Watering arrangements making use of perforated pipe-lines located in the soil
-
- 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
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/28—Cores; Mandrels
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/636—Polysaccharides or derivatives 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- 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
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
-
- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
Abstract
The invention discloses a ceramic irrigation film preparation die and a gradient ceramic irrigation film preparation process, wherein the die comprises an outer die, a pressure rod and an inner core; the outer die is of a hollow columnar structure comprising a bottom surface, the pressurizing rod is arranged in the outer die, and a hole is reserved in the center of the pressurizing rod and the center of the bottom surface of the outer die for the inner core to be vertically inserted. The preparation process of the gradient ceramic irrigation film comprises the following steps: firstly, preparing slurry and precursor powder; preparation of gradient ceramics by green body solid state forming processAnd (5) irrigating the film. The porous SiO prepared by adopting the preparation mold and the preparation process of the invention2/Si3N4Complex phase gradient ceramic irrigation film: the former mode of adhesion between the support body and the membrane layer is changed, the thermal stress between the support body and the membrane layer is fundamentally alleviated, and the bonding strength between the support body and the membrane layer is improved; meanwhile, the pore difference between the bonding layer and the film layer in an interlayer bonding mode is improved, so that the pore gradient presents gradient change along the water flow direction, and the filtration flux is increased.
Description
Technical Field
The invention belongs to the technical field of water-saving agricultural irrigation in dry areas, and particularly relates to a mold and a gradient ceramic irrigation film prepared by a green body solid-state forming process.
Background
The microporous ceramic drip irrigation emitter is a novel infiltrating irrigation equipment, and compared with the traditional equipment, the microporous ceramic drip irrigation emitter has the advantages of easiness in cleaning, blockage resistance and the like. The core of the ceramic drip irrigation emitter is microporous ceramic which is uniformly distributed on the pore size. Uniformly distributed pores are easy to achieve industrially, but ceramic pores are generally made smaller if better filtration is to be achieved. However, the smaller pores increase filtration efficiency, but reduce outflow and reduce irrigation efficiency.
One current idea to address the above problem is to replace the microporous ceramic in drip emitters with a gradient ceramic. When the ceramic layer is used, the ceramic layer with low porosity is placed towards the water inlet, and the ceramic layer with high porosity is placed towards the water outlet. Therefore, only relatively small flow is lost on the basis of greatly improving the filtering efficiency. One of the preparation processes of the gradient ceramic is interlayer painting, which has good effect but has the following problems: the adhesive is coated between layers, and thermal stress is easily generated between the support body and the film layer due to the mismatching of expansion coefficients, so that the bonding strength between the film layer and the support body is influenced, and the service life of the film layer and the support body in a high-temperature environment is influenced. At present, in order to improve the strength of a ceramic film layer, the thickness of the film layer is only increased, so that the filtration resistance is increased, and the filtration flux of the ceramic film is reduced. Therefore, how to improve the bonding strength between the ceramic membrane support and the membrane layer without reducing the filtration flux of the membrane becomes a research hotspot, and is also a key technology of the process for enabling the ceramic membrane to be widely applied.
Disclosure of Invention
Aiming at the problems, the invention firstly provides a ceramic irrigation film preparation mold, and on the basis, provides a gradient ceramic irrigation film preparation process based on the ceramic irrigation film preparation mold, so as to solve the problem that the bonding strength between a ceramic film support and a film layer and the filtration flux of the film cannot be simultaneously ensured by the conventional interlayer coating process.
Therefore, the invention adopts the following technical scheme:
a ceramic irrigation film preparation mold comprises an outer mold, a pressure rod and an inner core; the outer die is of a hollow columnar structure comprising a bottom surface, the pressurizing rod is arranged in the outer die, and a hole is reserved in the center of the pressurizing rod and the center of the bottom surface of the outer die for the inner core to be vertically inserted; the outer die comprises a first die body and a second die body which have the same structure, the first die body or the second die body is of a structure formed by vertically dividing the outer die, and an inner sliding rail and an outer sliding rail are respectively arranged on the first die body or the second die body along the vertical dividing surface; the outer slide rail comprises a convex outer arc edge, and the outer arc edge is formed by connecting a plurality of equal-diameter arcs with different diameters; the inner slide rail is used for being embedded into the outer slide rail so that the first die body and the second die body can be connected in a nested mode.
Further, the difference between the outer diameter and the inner diameter of the outer die is 10mm-20mm, the difference between the overall height of the ceramic irrigation film preparation die and the height of the outer die is 30mm-35mm, and the height of the pressure rod is not less than the difference between the overall height of the ceramic irrigation film preparation die and the height of the outer die.
Further, the hole left in the center of the pressurizing rod and the center of the bottom surface of the outer die comprises: the horizontal cross section of the inner core is of a cross-shaped structure, and the holes are of a cross-shaped structure which is hollow inside and matched with the inner core structure.
Meanwhile, the invention also provides a preparation process of the gradient ceramic irrigation film, which comprises the following steps:
firstly, preparing slurry and precursor powder:
the slurry adopts a slurry containing sodium carboxymethylcellulose, silica sol, talcum powder and Si3N4Preparing a raw material of powder;
the preparation of the precursor powder comprises the following steps: preparation of SiO-containing materials2Powder, Si3N4Powder, talc and Al2O3Respectively adding dextrin with gradient mass content into the mixed powder to obtain multiple groups of precursor powder;
step two, preparing the gradient ceramic irrigation film by adopting a green body solid state forming process:
adding silica sol with the same mass content into different precursor powder, and isostatic pressing by adopting the ceramic irrigation film preparation mould to prepare a plurality of ceramic wafer green compacts;
and carrying out gradient arrangement on the ceramic wafer green bodies according to the mass content of dextrin, injecting slurry into the inner core for solid-state forming, and sintering to obtain the gradient ceramic irrigation film.
Further, in the first step, sodium carboxymethylcellulose, silica sol, talcum powder, deionized water and Si3N4Mixing the powder to prepare slurry, adding a dispersing agent into the slurry, and preparing the slurry by a ball milling method.
Further, in the step one, SiO2Powder, Si3N4Powder, talc powder and Al2O3Mixing the powder, and ball-milling for 24 hours by using a vacuum ball mill to prepare mixed powder; the rotation speed of the vacuum ball mill is 240r/min, and the revolution speed is 360 r/min.
Further, in step one, SiO2Powder, Si3N4Powder, talc powder and Al2O3The mass mixing ratio of the powder is 70-30: 30-10: 90-10:30-10.
Further, in the first step, dextrin is respectively added into the mixed powder to prepare mixed powder with the mass contents of 10 wt%, 15 wt%, 20 wt%, 25 wt% and 30 wt% of dextrin, and the mixed powder is placed into a vacuum ball mill to be ball-milled for 24 hours to prepare precursor powder.
Further, in the second step, after part of the precursor powder is taken out and added with silica sol, the ceramic irrigation film is adopted to prepare a mold, the ceramic irrigation film is subjected to cold isostatic pressing under the pressure of 12MPa to form ceramic wafer green bodies with the height of 3-4mm and the diameter of 40-45mm, and the ceramic wafer green bodies are dried in the shade.
Further, in the second step, polishing and grinding the ceramic wafer green bodies to the thickness of 2.5-3mm, assembling the ceramic wafer green bodies according to the sequence of mass content of dextrin from small to large, and injecting slurry into the inner core to wait for the slurry to be coagulated; in the second step, the sintering conditions include: sintering at 1200 ℃ and 1300 ℃ for 2h, wherein the heating rate is less than 30 ℃/h.
Compared with the prior art, the invention has the following technical effects:
the preparation mold is adopted, and the green body solid forming process is combined to prepare the porous SiO2/Si3N4Complex phase gradient ceramic irrigation film:
(1) the traditional mode of interlayer adhesion of the support body and the membrane layer is changed, the thermal stress between the support body and the membrane layer is fundamentally alleviated, the bonding strength between the support body and the membrane layer is improved and can reach more than 3.7N/mm, and the interlayer expansion rate is reduced by about 50 percent compared with the traditional method;
(2) the pore difference between the bonding layer and the film layer in the interlayer bonding mode is improved, so that the pore gradient presents gradient change along the water flow direction, the filtration resistance is reduced, and the filtration flux is increased;
(3) the technical problem that the film layer prepared by the traditional dip coating method is thick and the film layer prepared by the spray coating method is uneven in thickness is solved to a certain extent, and the phenomenon of uneven thickness of the bonding layer in the traditional method is improved.
Drawings
FIG. 1 is a schematic view of a mold used in the present invention;
FIG. 2 is a schematic view of an outer mold of the present invention, wherein a is a drawing of disassembled parts, and b is a schematic view of the whole outer mold;
FIG. 3 is a schematic view of a compression bar of the present invention;
FIG. 4 is a schematic view of the core of the present invention;
FIG. 5 is a schematic diagram of the preparation of a pore gradient distribution sample according to the present invention.
In the figures, the meaning of the reference numerals is:
the die comprises an outer slide rail 1, an inner slide rail 2, a first die body 3, a second die body 4, a hole 5, a pressurizing rod 6, an inner core 7 and an outer die 8.
Detailed Description
The process principle of the invention is as follows: the porous SiO prepared by adopting the preparation mould and combining the preparation process of the invention2/Si3N4The complex phase gradient ceramic irrigation film has low permeability coefficient due to the low dextrin content at one side of the water inlet. When the water that contains silt flows to the side of intaking of complex phase pottery, inside only the tiny silt granule of particle size can enter into ceramic pore along with the rivers, most silt can be blockked at the ceramic layer outside. When water flows continuously in the complex phase ceramic, the dextrin content in the complex phase ceramic is continuously increased, so that the resistance of the water flow is reducedSmall, the seepage flux of the ceramic irrigation membrane is improved. Therefore, the porous SiO prepared by the equipment and the process of the invention2/Si3N4The multiphase gradient ceramic irrigation film has excellent irrigation performance and filtering performance, and has low cost and simple preparation cost.
Example 1:
following the above technical solution, as shown in fig. 1 to 5, this embodiment provides a ceramic irrigation film-making mold, which is composed of an outer mold 8, an inner core 7 and a pressure bar 6. The outer die 8 is structural steel and is a round cylindrical structure with one side being provided with a bottom, the overall height h1, the base height h2 and the inner diameter d1 of the outer die are determined according to the thickness and the diameter of the prepared ceramic body, and the difference between the outer diameter d2 and the inner diameter d1 is about 10mm-20 mm. The outer mold consists of two parts, namely a first mold body 3 and a second mold body 4, wherein the shapes and the sizes of the first mold body 3 and the second mold body 4 are completely the same, and generally, the overall height h1 can be set to be 50mm, and the base height h2 can be set to be 20 mm. An outer slide rail and an inner slide rail are designed at the half circumference of the first mold body 3 and the second mold body 4, the shapes of the inner slide rail and the outer slide rail are shown in fig. 2, and the outer arc edge of the slide rail is formed by three equal-diameter circular arcs with different diameters. In use, the first body 3 and the second body 4 are nested together to form the outer mould 8. In order to facilitate grouting the interior of the composite gradient ceramic and limiting the inner core, the center of the base is provided with a symmetrical cross-shaped hole, and the axial length of the hole is 5 mm. The inner core is a structural steel bar with a cross-shaped hole in the cross section. The pressure rod 6 is made of structural steel, the height h3 and the diameter d3 of the pressure rod need to meet the requirement that h3 is not less than (h1-h2), and d3 is approximately equal to d1-0.05 mm.
Example 2:
this example provides a porous SiO for irrigation2/Si3N4The preparation method of the gradient ceramic comprises the following steps:
firstly, preparing slurry and precursor powder:
(1) firstly, cheap sodium carboxymethylcellulose, silica sol, talcum powder (800 meshes), deionized water and Si3N4Mixing the powders (600 mesh) at a certain ratio to obtain slurry, and adding appropriate dispersantPreparing slurry by a ball milling method, sealing the obtained slurry in a conical flask, oscillating and mixing for 6 hours at the frequency of 40kHz by using an ultrasonic oscillator, and placing the slurry in the conical flask for later use;
(2) mixing SiO2Powder (325 mesh), Si3N4Powder (600 mesh), talcum powder (800 mesh) and Al2O3Mixing the powder (400 meshes) according to a certain proportion, ball-milling for 24 hours by using a vacuum ball mill (the rotation speed: 240r/min, the revolution speed: 360r/min) to prepare mixed powder 0, and taking out for later use;
(3) respectively adding a proper amount of dextrin into the mixed powder to prepare mixed powder 1, 2, 3, 4 and 5 with the mass contents of the dextrin of 10 wt%, 15 wt%, 20 wt%, 25 wt% and 30 wt%. Putting the mixed powder 1, 2, 3, 4 and 5 into a vacuum ball mill (rotation speed: 240r/min, revolution speed: 360r/min) for ball milling for 24 hours to prepare precursor powder 1, 2, 3, 4 and 5, and taking out for later use;
step two, preparing the gradient ceramic irrigation film by adopting a green body solid state forming process:
(1) respectively taking out about 15g of precursor powder 1, 2, 3, 4 and 5, adding a proper amount of silica sol, carrying out cold isostatic pressing on the precursor powder under the pressure of 12MPa to obtain ceramic plates 1, 2, 3, 4 and 5 with the height of about 3-4mm and the diameter of about 40mm by using the detachable die provided by the invention, demoulding, and drying in the shade for 6 hours;
(2) polishing and grinding the ceramic plates 1, 2, 3, 4 and 5 to about 2.5mm by using 600-mesh sand paper, assembling the ceramic plates according to the sequence of mass content of dextrin from small to large, slowly injecting slurry into an inner core of the gradient ceramic by using an injector, and taking out the slurry after the slurry is coagulated;
(3) and (3) placing the bonded ceramic in a drying box (drying temperature: 60 ℃) for 1h, then taking out, placing in a high-temperature box type furnace, and sintering at the temperature of 1200 ℃ and 1300 ℃ for 2h (the temperature rise rate in the process is less than 30 ℃/h), thus obtaining the finished product.
In the above preparation method, the dispersant may be any one of sodium citrate, polyacrylic acid and polypropylene.
In the above preparation method, the SiO2Powder (325 mesh))、Si3N4Powder (600 mesh), talcum powder (800 mesh) and Al2O3The mass mixing ratio of the powder (400 meshes) is 70-30: 30-0: 90-10:30-10.
In the preparation method, the mass content of the dextrin can be adjusted by changing the addition amount of the dextrin according to actual requirements. Meanwhile, in the preparation method, the thickness of the prepared and polished ceramic wafer can be changed according to actual requirements.
Example 3:
this example provides a porous SiO for irrigation2/Si3N4The preparation method of the gradient ceramic comprises the following steps:
firstly, preparing slurry and precursor powder:
(1) firstly, 10g of sodium carboxymethylcellulose, 30g of talcum powder (800 meshes) and 10g of Si3N4The powder (600 meshes) is mixed according to the proportion to prepare the powder, the obtained mixture powder is placed in an alumina pot of a ball mill, 15-25 agate beads with the diameter of 8-12mm are added, then the rotation speed of the ball mill is adjusted to 240r/min, the revolution speed is adjusted to 360r/min, and the ball milling is carried out for 2h to prepare the ceramic powder. Adding 20mL of deionized water, 20mL of silica sol and 5g of sodium citrate into the obtained ceramic powder, mixing, sealing the slurry in a conical flask, mixing by using an ultrasonic oscillator under the oscillation of 40kHz frequency for 6 hours, and placing in the conical flask for later use;
(2) 70g of SiO2Powder (325 mesh), 30g Si3N4Powder (600 mesh), 30g talc (800 mesh), 10gAl2O3Mixing the powder (400 meshes) according to a ratio, putting the obtained mixed powder into an alumina pot of a ball mill, adding 10-15 agate beads with the diameter of 20-25mm, ball-milling for 24 hours by using a vacuum ball mill (the rotation speed: 120r/min and the revolution speed: 120r/min) to obtain mixed powder 0, and taking out for later use;
(3) respectively adding a proper amount of dextrin into the mixed powder 0 to prepare mixed powder 1, 2, 3, 4 and 5 with the mass contents of the dextrin of 10 wt%, 15 wt%, 20 wt%, 25 wt% and 30 wt%. Putting the mixed powder 1, 2, 3, 4 and 5 into a vacuum ball mill (rotation speed: 240r/min, revolution speed: 360r/min) for ball milling for 24 hours to prepare precursor powder 1, 2, 3, 4 and 5, and taking out for later use;
step two, preparing the gradient ceramic irrigation film by adopting a green body solid state forming process:
(1) approximately 100g of the precursor powders 1, 2, 3, 4, and 5 were taken out, respectively, and 20mL of silica sol was added thereto, and then the precursor powders 1, 2, 3, 4, and 5 were placed in a stirrer and stirred at a high speed for 30 minutes, respectively, to obtain ceramic powders 1, 2, 3, 4, and 5. Combining an outer mold and an inner core of the mold A, placing the combined outer mold and inner core on a horizontal plane, taking out about 15g of ceramic powder to uniformly fill the outer mold, carrying out cold isostatic pressing on the ceramic powder under the pressure of 12MPa to form ceramic plates 1, 2, 3, 4 and 5 with the height of about 3-4mm and the diameter of about 40mm, demoulding, and placing the ceramic plates in a shade place for drying for 6 hours;
(2) polishing and grinding the ceramic plates 1, 2, 3, 4 and 5 to about 2.5mm by using 600-mesh sand paper, assembling the ceramic plates to a mold B in the sequence from small mass content to large mass content of dextrin, slowly injecting slurry into an inner core of the gradient ceramic by using an injector, opening the mold B after the slurry is condensed, and taking out the mold B; and (3) placing the bonded ceramic in a drying box (drying temperature: 60 ℃) for 1h, then taking out, placing in a high-temperature box type furnace, and sintering at 1200-1300 ℃ for 2h (the temperature rise rate in the process is less than 30 ℃/h), thus obtaining the finished product.
Example 4:
this example provides a porous SiO for irrigation2/Si3N4The preparation method of the gradient ceramic comprises the following steps:
firstly, preparing slurry and precursor powder:
(1) firstly, 5g of sodium carboxymethylcellulose, 35g of talcum powder (800 meshes) and 10g of Si3N4The powder (600 meshes) is mixed according to the proportion to prepare the powder, the obtained mixture powder is placed in an alumina pot of a ball mill, 15-25 agate beads with the diameter of 8-12mm are added, then the rotation speed of the ball mill is adjusted to 240r/min, the revolution speed is adjusted to 360r/min, and the ball milling is carried out for 2h to prepare the ceramic powder. Adding 20mL of deionized water, 20mL of silica sol and 5g of sodium citrate into the obtained ceramic powder, mixing, sealing the slurry in a conical flask, and vibrating with an ultrasonic oscillator at the frequency of 40kHzAfter mixing for 6h, placing in a conical flask for later use;
(2) 80g of SiO2Powder (325 mesh), 20g Si3N4Powder (600 mesh), 30g talc (800 mesh), 10gAl2O3Mixing the powder (400 meshes) according to a ratio, putting the obtained mixed powder into an alumina pot of a ball mill, adding 10-15 agate beads with the diameter of 20-25mm, ball-milling for 24 hours by using a vacuum ball mill (the rotation speed: 120r/min and the revolution speed: 120r/min) to obtain mixed powder 0, and taking out for later use;
(3) respectively adding a proper amount of dextrin into the mixed powder 0 to prepare mixed powder 1, 2, 3, 4 and 5 with the mass contents of the dextrin of 10 wt%, 15 wt%, 20 wt%, 25 wt% and 30 wt%. Putting the mixed powder 1, 2, 3, 4 and 5 into a vacuum ball mill (rotation speed: 240r/min, revolution speed: 360r/min) for ball milling for 24 hours to prepare precursor powder 1, 2, 3, 4 and 5, and taking out for later use;
step two, preparing the gradient ceramic irrigation film by adopting a green body solid state forming process:
(1) approximately 100g of the precursor powders 1, 2, 3, 4, and 5 were taken out, respectively, and 20mL of silica sol was added thereto, and then the precursor powders 1, 2, 3, 4, and 5 were placed in a stirrer and stirred at a high speed for 30 minutes, respectively, to obtain ceramic powders 1, 2, 3, 4, and 5. Combining an outer mold and an inner core of the mold A, placing the combined outer mold and inner core on a horizontal plane, taking out about 15g of ceramic powder to uniformly fill the outer mold, carrying out cold isostatic pressing on the ceramic powder under the pressure of 12MPa to form ceramic plates 1, 2, 3, 4 and 5 with the height of about 3-4mm and the diameter of about 40mm, demoulding, and placing the ceramic plates in a shade place for drying for 6 hours;
(2) polishing and grinding the ceramic plates 1, 2, 3, 4 and 5 to about 2.5mm by using 600-mesh sand paper, assembling the ceramic plates to a mold B in the sequence from small mass content to large mass content of dextrin, slowly injecting slurry into an inner core of the gradient ceramic by using an injector, opening the mold B after the slurry is condensed, and taking out the mold B;
(3) and (3) placing the bonded ceramic in a drying box (drying temperature: 60 ℃) for 1h, then taking out, placing in a high-temperature box type furnace, and sintering at 1200-1300 ℃ for 2h (the temperature rise rate in the process is less than 30 ℃/h), thus obtaining the finished product.
The performance of the gradient ceramics prepared by the preparation methods of the embodiments 3 and 4 is compared with the performance of the gradient ceramics respectively prepared by the methods of compression molding (comparative example 1), slip casting (comparative example 2) and common interlayer smearing (comparative example 3) on the market, and the bending strength, the shearing strength, the bonding strength, the impact strength, the peeling strength and the interlayer thermal expansion rate of the structure are tested, and the test results are as follows:
the above table shows that: the gradient ceramic prepared by the method has high-strength impact-resistant strength, the lifting amplitude can reach more than 30% compared with the existing bonding method, the gradient ceramic prepared by the method has greatly improved bonding, bending resistance and shearing strength compared with the ceramic structure prepared by the existing method, the peeling-resistant strength is high and can reach more than 3.7N/mm, the interlayer expansion rate is reduced by about 50% compared with the existing method, and the integral performance is good.
Claims (10)
1. A ceramic irrigation film preparation mold is characterized by comprising an outer mold, a pressurizing rod and an inner core; the outer mold is of a hollow columnar structure comprising a bottom surface, the pressurizing rod is of a columnar structure and is arranged in the outer mold, and a hole is reserved in the center of the pressurizing rod and the center of the bottom surface of the outer mold for the inner core to be vertically inserted;
the outer die comprises a first die body and a second die body which have the same structure, the first die body or the second die body is of a structure formed by vertically dividing the outer die, and an inner sliding rail and an outer sliding rail are respectively arranged on the first die body or the second die body along the vertical dividing surface;
the outer slide rail comprises a convex outer arc edge, and the outer arc edge is formed by connecting a plurality of equal-diameter arcs with different diameters; the inner slide rail is used for being embedded into the outer slide rail so that the first die body and the second die body can be connected in a nested mode.
2. The ceramic irrigation film preparation mold according to claim 1, wherein the difference between the outer diameter and the inner diameter of the outer mold is 10mm to 20mm, the difference between the overall height of the ceramic irrigation film preparation mold and the height of the outer mold is 30mm to 35mm, and the height of the pressure bar is not less than the difference between the overall height of the ceramic irrigation film preparation mold and the height of the outer mold.
3. The mold for making a ceramic irrigation film as claimed in claim 1, wherein the holes formed in the center of the pressurizing bar and the center of the bottom surface of the outer mold comprise: the horizontal cross section of the inner core is of a cross-shaped structure, and the holes are of a cross-shaped structure which is hollow inside and matched with the inner core structure.
4. A preparation process of a gradient ceramic irrigation film is characterized by comprising the following steps:
firstly, preparing slurry and precursor powder:
the slurry adopts a slurry containing sodium carboxymethylcellulose, silica sol, talcum powder and Si3N4Preparing a raw material of powder;
the preparation of the precursor powder comprises the following steps: preparation of SiO-containing materials2Powder, Si3N4Powder, talc and Al2O3Respectively adding dextrin with gradient mass content into the mixed powder to obtain multiple groups of precursor powder;
step two, preparing the gradient ceramic irrigation film by adopting a green body solid state forming process:
respectively adding silica sol with the same mass content into different precursor powders, and respectively carrying out isostatic pressing by using the ceramic irrigation film preparation mould of any one of claims 1-3 to prepare a plurality of ceramic chip green bodies;
and carrying out gradient arrangement on the ceramic wafer green bodies according to the mass content of dextrin, injecting slurry into the inner core for solid-state forming, and sintering to obtain the gradient ceramic irrigation film.
5. The process for preparing a gradient ceramic irrigation film according to claim 4, wherein in the first step, sodium carboxymethylcellulose, silica sol, talcum powder, deionized water and Si are added3N4Powder ofMixing to prepare slurry, adding a dispersing agent into the slurry, and preparing the slurry by a ball milling method.
6. The process for preparing a gradient ceramic irrigation film according to claim 4, wherein in the first step, SiO is added2Powder, Si3N4Powder, talc powder and Al2O3Mixing the powder, and ball-milling for 24 hours by using a vacuum ball mill to prepare mixed powder; the rotation speed of the vacuum ball mill is 240r/min, and the revolution speed is 360 r/min.
7. The process for preparing a gradient ceramic irrigation film according to claim 6, wherein in the first step, SiO is added2Powder, Si3N4Powder, talc powder and Al2O3The mass mixing ratio of the powder is 70-30: 30-10: 90-10:30-10.
8. The process for preparing a gradient ceramic irrigation film according to claim 4, wherein in the first step, dextrin is respectively added into the mixed powder to prepare mixed powder with the dextrin contents of 10 wt%, 15 wt%, 20 wt%, 25 wt% and 30 wt%, and the mixed powder is put into a vacuum ball mill to be ball-milled for 24 hours to prepare precursor powder.
9. The process for preparing a gradient ceramic irrigation film according to claim 4, wherein in the second step, after part of the precursor powder is taken out and added into silica sol, the ceramic irrigation film preparation mold is used for cold isostatic pressing under the pressure of 12MPa to form ceramic wafer green bodies with the height of 3-4mm and the diameter of 40-45mm, and the ceramic wafer green bodies are dried in the shade.
10. The preparation process of the gradient ceramic irrigation film as claimed in claim 4, wherein in the second step, the ceramic wafer green bodies are polished and ground to a thickness of 2.5-3mm, and are assembled in the order from small to large according to the mass content of dextrin, and then slurry is injected into the inner core to be coagulated; in the second step, the sintering conditions include: sintering at 1200 ℃ and 1300 ℃ for 2h, wherein the heating rate is less than 30 ℃/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911100056.3A CN110978228B (en) | 2019-11-12 | 2019-11-12 | Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911100056.3A CN110978228B (en) | 2019-11-12 | 2019-11-12 | Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110978228A true CN110978228A (en) | 2020-04-10 |
| CN110978228B CN110978228B (en) | 2021-10-15 |
Family
ID=70084017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911100056.3A Active CN110978228B (en) | 2019-11-12 | 2019-11-12 | Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110978228B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114683376A (en) * | 2022-03-29 | 2022-07-01 | 安徽紫朔环境工程技术有限公司 | A pottery microporous filter body preparation facilities for purifying harmful substance of industrial flue gas |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01122920A (en) * | 1987-11-04 | 1989-05-16 | Seiko Epson Corp | Superconductor |
| US4902314A (en) * | 1987-11-25 | 1990-02-20 | Hidetoshi Nakajima | Gas filter |
| JP2000052328A (en) * | 1998-08-06 | 2000-02-22 | Ngk Spark Plug Co Ltd | Manufacture of powder molded body and manufacture of powder sintered body |
| EP1070533B1 (en) * | 1999-02-01 | 2007-04-04 | Ngk Insulators, Ltd. | Method for manufacturing filter having ceramic porous film as separating film |
| CN101670244A (en) * | 2009-09-27 | 2010-03-17 | 南京工业大学 | Method for preparing nanofiltration membrane supporting body with gradient holes |
| CN103894075A (en) * | 2014-03-07 | 2014-07-02 | 中南大学 | Heterogeneous composite ceramic with gradient holes and preparation method for ceramic |
| CN104174298A (en) * | 2014-08-20 | 2014-12-03 | 武汉工程大学 | Preparation method of gradient silicon carbide ceramic membrane for water purification |
| CN104529442A (en) * | 2015-01-16 | 2015-04-22 | 河南理工大学 | Non-pressure infiltration preparation process of functionally graded piezoelectric material (FGPM) |
| CN105819866A (en) * | 2016-03-22 | 2016-08-03 | 烟台大学 | Method for preparing silicon nitride-silicon dioxide gradient wave-transmitting composite ceramic |
| CN205607732U (en) * | 2016-05-12 | 2016-09-28 | 山东科技大学 | Mould of preparation hole concrete sample |
| CN106145912A (en) * | 2016-07-01 | 2016-11-23 | 西北农林科技大学 | A kind of micropore ceramics douche and preparation method thereof |
| CN108083811A (en) * | 2017-12-14 | 2018-05-29 | 西安交通大学 | A kind of double gradient porous ceramics materials and preparation method thereof |
-
2019
- 2019-11-12 CN CN201911100056.3A patent/CN110978228B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01122920A (en) * | 1987-11-04 | 1989-05-16 | Seiko Epson Corp | Superconductor |
| US4902314A (en) * | 1987-11-25 | 1990-02-20 | Hidetoshi Nakajima | Gas filter |
| JP2000052328A (en) * | 1998-08-06 | 2000-02-22 | Ngk Spark Plug Co Ltd | Manufacture of powder molded body and manufacture of powder sintered body |
| EP1070533B1 (en) * | 1999-02-01 | 2007-04-04 | Ngk Insulators, Ltd. | Method for manufacturing filter having ceramic porous film as separating film |
| CN101670244A (en) * | 2009-09-27 | 2010-03-17 | 南京工业大学 | Method for preparing nanofiltration membrane supporting body with gradient holes |
| CN103894075A (en) * | 2014-03-07 | 2014-07-02 | 中南大学 | Heterogeneous composite ceramic with gradient holes and preparation method for ceramic |
| CN104174298A (en) * | 2014-08-20 | 2014-12-03 | 武汉工程大学 | Preparation method of gradient silicon carbide ceramic membrane for water purification |
| CN104529442A (en) * | 2015-01-16 | 2015-04-22 | 河南理工大学 | Non-pressure infiltration preparation process of functionally graded piezoelectric material (FGPM) |
| CN105819866A (en) * | 2016-03-22 | 2016-08-03 | 烟台大学 | Method for preparing silicon nitride-silicon dioxide gradient wave-transmitting composite ceramic |
| CN205607732U (en) * | 2016-05-12 | 2016-09-28 | 山东科技大学 | Mould of preparation hole concrete sample |
| CN106145912A (en) * | 2016-07-01 | 2016-11-23 | 西北农林科技大学 | A kind of micropore ceramics douche and preparation method thereof |
| CN108083811A (en) * | 2017-12-14 | 2018-05-29 | 西安交通大学 | A kind of double gradient porous ceramics materials and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 翟萍等: "ZrO2颗粒对Si3N4/SiO2陶瓷复合材料性能的影响", 《陶瓷》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114683376A (en) * | 2022-03-29 | 2022-07-01 | 安徽紫朔环境工程技术有限公司 | A pottery microporous filter body preparation facilities for purifying harmful substance of industrial flue gas |
| CN114683376B (en) * | 2022-03-29 | 2023-10-31 | 安徽紫朔环境工程技术有限公司 | Ceramic microporous filter preparation device for purifying industrial flue gas harmful substances |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110978228B (en) | 2021-10-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102417366B (en) | Pore gradient silicon carbide porous ceramic and preparation method thereof | |
| CN110368818B (en) | Preparation method of high-flux flat ceramic membrane | |
| CN103691330B (en) | A kind of preparation technology of porous stainless steel membrane | |
| CN108706978B (en) | Method for preparing silicon carbide ceramic matrix composite by combining spray granulation with 3DP and CVI | |
| CN105236936B (en) | A kind of multichannel aluminium oxide flat ceramic film support, its preparation method and application | |
| CN107188596B (en) | Porous gradient silicon nitride-silicon carbide composite ceramic and preparation method and application thereof | |
| CN110386827A (en) | A kind of reverse foamed material and its preparation method and application | |
| CN110981197A (en) | Preparation method of wet-process dry-grain polished crystal brick and polished crystal brick | |
| CN101181798A (en) | Multi-gradient porous ceramic mold for ceramic injection forming and making method | |
| CN110978228B (en) | Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process | |
| US4976903A (en) | Shaping molds and shaping of ceramic bodies by using such shaping molds | |
| US6165398A (en) | Method of slip casting powdery material, using a water resistant mold with self-water absorbent ability | |
| CN105622079A (en) | Preparing method for molecular sieving membrane support | |
| CN106588073A (en) | Process for preparing novel laminated porous ceramic | |
| AU2020103424A4 (en) | Ceramic irrigation film preparation mold and gradient ceramic irrigation film preparation process | |
| CN109079963B (en) | Single-side pressure grouting forming mold and manufacturing method of ITO (indium tin oxide) plane target | |
| CN109289299B (en) | A kind of double water route Multi-layer composite ceramic filter plates and preparation method thereof | |
| CN110723964B (en) | Barrier layer, sintering mold and preparation method thereof | |
| CN111253148A (en) | Ceramic filter membrane preparation method and ceramic filter membrane | |
| CN115521158B (en) | Preparation method of high-air-permeability ceramic fiber filter tube | |
| CN114478054B (en) | Porous ceramic and preparation method thereof | |
| CN115196976A (en) | Gradient porous ceramic and preparation method thereof | |
| CN113385052B (en) | Alumina-based ceramic flat membrane | |
| CN114953102A (en) | Device and method for preparing seamless ceramic hollow floating ball through hollow pressurized grouting | |
| CN109534818B (en) | Porous ceramic membrane preparation mold and method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |