CN107759230B - Toughened ceramic gel injection molding method - Google Patents

Toughened ceramic gel injection molding method Download PDF

Info

Publication number
CN107759230B
CN107759230B CN201710952306.0A CN201710952306A CN107759230B CN 107759230 B CN107759230 B CN 107759230B CN 201710952306 A CN201710952306 A CN 201710952306A CN 107759230 B CN107759230 B CN 107759230B
Authority
CN
China
Prior art keywords
ceramic
drying
water
temperature
blank
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.)
Active
Application number
CN201710952306.0A
Other languages
Chinese (zh)
Other versions
CN107759230A (en
Inventor
刘名剑
王征
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuxi Tecceram Fine Ceramic Co ltd
Original Assignee
Wuxi Tecceram Fine Ceramic Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Wuxi Tecceram Fine Ceramic Co ltd filed Critical Wuxi Tecceram Fine Ceramic Co ltd
Priority to CN201710952306.0A priority Critical patent/CN107759230B/en
Publication of CN107759230A publication Critical patent/CN107759230A/en
Application granted granted Critical
Publication of CN107759230B publication Critical patent/CN107759230B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802Powder coating materials
    • C04B35/62805Oxide ceramics
    • C04B35/62807Silica or silicates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
    • B28B11/243Setting, e.g. drying, dehydrating or firing ceramic articles
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
    • C04B35/6303Inorganic additives
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
    • C04B35/632Organic additives
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • C04B35/63448Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63488Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6023Gel casting
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606Drying

Abstract

The invention belongs to the technical field of ceramic preparation. The invention provides a method for injection molding toughened ceramic gel, which aims at solving the problems of easy cracking and difficult processing in the drying process of the conventional structural ceramic and aims at solving the problems in the prior art. The invention improves the microstructure of the polymer, improves the plasticity of the ceramic body, and greatly improves the drying performance of a wet body and the processability of a dry ceramic body by the approaches of pretreating the ceramic raw material, improving the drying method of the ceramic body and the like.

Description

Toughened ceramic gel injection molding method
Technical Field
The invention relates to a preparation method of a ceramic material, in particular to a method for molding a toughened ceramic gel injection mold, and belongs to the technical field of ceramic preparation.
Background
At present, the requirements on materials in industrial production are more and more strict, and structural ceramics are more and more widely applied to various industrial industries due to excellent mechanical and thermal properties of the structural ceramics.
Structural ceramics are mostly prepared by wet forming. The wet forming is a method for injecting ceramic slurry into a mold to be cured to form a ceramic blank, ceramic products with various complicated shapes can be easily prepared by the wet forming, but the traditional wet forming process such as slip casting can not ensure the uniform density of the formed blank, and the product can not ensure the accuracy of the shape and the size of the product due to the defects of cracking and the like caused by the large shrinkage of the product in the drying and sintering process due to the existence of a liquid phase.
The gel casting process combines ceramic slip casting technology and high molecular chemical polymerization theory perfectly, and the principle is that firstly, ceramic slurry with low viscosity and high solid content is prepared, then under the action of initiator and catalyst, organic monomer and cross-linking agent are cross-linked and polymerized to form three-dimensional network structure, the ceramic particles are locked in the blank by the three-dimensional network structure and are cured and formed in situ, finally, the ceramic blank with high strength and uniform density and capable of being processed by precision machine is obtained. The gel casting technology has very important significance for preparing high-performance ceramic materials with complex shapes and uniform component requirements.
However, the polymer obtained by the gel casting technology has high rigidity and large residual stress of a ceramic blank, and the blank is easy to crack, deform and the like in the drying process. In addition, the resulting green body, while high in strength, is less tough and tends to wear the tool during machining.
The inventor previously developed a structural ceramic water-based gel injection molding method, which improves the plasticity of a molded blank body, reduces the residual stress of the blank body, lightens the cracking phenomenon in the drying process to a certain extent and improves the processing performance of the blank body by adding glycerol or Tween 80 as a plasticizer into a raw material solution, but the problems of cracking of the blank body during drying and processability of the dried blank body are still to be improved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a toughening ceramic gel injection molding method, which improves the microstructure of a polymer to improve the plasticity of a ceramic blank body by pretreating a ceramic raw material, avoids cracking of a wet blank during drying and increases the processability of a dry ceramic blank.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a method for molding toughened ceramic gel comprises the following steps:
(1) adding a ceramic raw material into a ball milling tank, grinding the ceramic raw material into ceramic powder of 0.1-1 mu m, adding the ceramic powder into a mixed solution of ethanol and water, dropwise adding polyvinylpyrrolidone (PVP) and ammonia water while stirring, then ultrasonically dispersing at room temperature, then adding ethyl orthosilicate into the solution under the condition of continuous stirring, reacting at room temperature for 4-24 h, and centrifugally drying to obtain silicon dioxide coated ceramic powder; the volume ratio of the ethanol to the water to the ethyl orthosilicate is (20-50): 1 (1-2), the volume ratio of the water to the ammonia water is (2-10): 1, the ceramic powder accounts for 1-10 wt% of the whole system, and the PVP accounts for 1-5 wt% of the ceramic powder;
(2) weighing an organic monomer and a crosslinking agent, putting the organic monomer and the crosslinking agent into a beaker, adding deionized water to fully dissolve the organic monomer and the crosslinking agent, then adding a dispersing agent and an aqueous cosolvent, fully stirring, adjusting the pH of the system to be 8-11 by using ammonia water, adding a plasticizer and an initiator into the solution, uniformly stirring, adding the silicon dioxide coated ceramic powder in the step (1), performing ultrasonic dispersion for 10-30 min at room temperature, adding a catalyst, rapidly stirring, and removing bubbles dissolved in ceramic slurry in vacuum; the ceramic slurry comprises 1-3 wt% of organic monomers, 1 (5-30) of a cross-linking agent and the organic monomers, 8-20 wt% of deionized water, 0.5-2 wt% of a dispersing agent, 0-10 wt% of a water-based cosolvent, 20-50 wt% of an organic monomer, 0.01-1 wt% of an initiator and 0.01-1 wt% of a catalyst, wherein the mass ratio of the cross-linking agent to the organic monomers is 1;
(3) carefully injecting the ceramic slurry in the step (2) into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water-cooling the mold, demolding to obtain a ceramic wet blank, immersing the ceramic wet blank into an ethanol water solution for 12 hours, then placing the ceramic wet blank in a constant-temperature and constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 92% for drying for 48 hours, and then placing the ceramic wet blank in a constant-temperature and constant-humidity drying box with the temperature of 80 ℃ and the relative humidity of 20% for drying for 12 hours; and after drying, machining the ceramic thread of M8 on a green body of the lathe by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at a speed of 0.6 ℃/min, preserving heat for 1h, heating to 1600 ℃ at a speed of 3 ℃/min, preserving heat for 2h to obtain a ceramic product, and finally performing quality detection.
In one embodiment, the organic monomer is any one of acrylamide, methacrylamide, N-methylolacrylamide, N-N' methylenebisacrylamide, methacrylamide, acrylic acid, methacrylic acid, and hydroxyethyl acrylate; the cross-linking agent is Methylene Bisacrylamide (MBAM) or poly (vinyl glycol) dimethacrylate (PEGDAM).
In one embodiment, the dispersant is any one of citric acid, ammonium Citrate (CT), hydroxymethyl cellulose, polyacrylic acid and its copolymer (PAA), Polyethyleneimine (PEI); the water-soluble cosolvent is any one of ethanol, ethylene glycol, n-propanol, 1, 2-propylene glycol, n-butanol, 1, 4-butanediol, 1, 6-hexanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and glycerol.
In one embodiment, the plasticizer is polyethylene glycol, polymethacrylamide, glycerol or triethylene glycol acetate; the initiator is any one of Ammonium Persulfate (APS), hydrogen peroxide and azo [ 2-imidazoline-2-propane ] hydrochloride (AZIP).
In one embodiment, the catalyst is Tetramethylethylenediamine (TEMED).
In one embodiment, the ceramic powder is alumina, zirconia, silicon nitride or aluminum titanate.
As can be seen from the above description, the present invention has the following advantages:
1. the ceramic raw material is pretreated to obtain ceramic powder with the surface coated with silicon dioxide, on one hand, the rich hydroxyl groups on the surface of the silicon dioxide improve the hydrophilicity of the surface of ceramic powder particles, the ceramic powder is easier to stably disperse to obtain ceramic slurry with good dispersibility, and a ceramic blank with a uniform structure and few internal defects is obtained after in-situ curing; on the other hand, the silicon dioxide coated on the surface of the ceramic powder can compensate microcracks appearing on the surface of the ceramic blank in the drying process, improve the bending strength of the ceramic blank, inhibit the growth of crystal grains in the sintering process, form a compact and uniform ceramic blank and play a role in toughening;
2. during drying, a method of immersing the green body in an alcohol aqueous solution and then drying the green body step by step at different humidity and temperature is adopted, so that the green body can be quickly dried, and the green body can be effectively prevented from being cracked in the drying process.
3. The water-soluble cosolvent is added into the ceramic slurry, so that the viscosity of the ceramic slurry and the viscosity of a reaction system in a polymerization process can be reduced, and the in-situ solidification of the ceramic slurry is facilitated;
4. the ball milling of the ball mill is changed into the ultrasonic treatment of the dispersion mode of the ceramic powder, so that the introduction of impurities in the ball milling process can be avoided;
5. adding an initiator before ultrasonic dispersion, wherein the initiator can be uniformly distributed in the ceramic slurry, so as to ensure that all parts of the system react simultaneously, and obtain a ceramic wet blank with a uniform structure, so as to reduce the residual stress in the blank and reduce the dry cracking of the blank in the drying process;
Detailed Description
The features of the present invention will be further illustrated by the following examples, but the present invention is not limited to the examples.
Example 1:
weighing 3g of methacrylamide and 0.6g of MBAM, putting the methacrylamide and the MBAM into a beaker, adding 20g of deionized water to fully dissolve the methacrylamide and the MBAM, then adding 2g of ammonium citrate to fully stir, adjusting the pH of a system to be 8-11 by using ammonia water, then adding 0.9g of glycerol and 0.3ml of 10% APS into the solution to stir uniformly, adding 100g of ceramic powder, performing ultrasonic dispersion at room temperature for 30min, then adding 0.03g of TEMED, rapidly stirring, and removing bubbles dissolved in ceramic slurry in vacuum; then carefully injecting the ceramic slurry into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water cooling the mould, demoulding to obtain wet ceramic rod blanks with diameters of 15mm, 35mm, 40mm, 43mm and 45mm respectively; drying the wet ceramic rod blank for 72h at room temperature, and then drying the wet ceramic rod blank for 12h in an electric heating drying oven at the temperature of 80 ℃; and after drying, machining the ceramic thread of M8 by using a lathe green body by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at the speed of 0.6 ℃/min, keeping the temperature for 1h, heating to 1600 ℃ at the speed of 3 ℃/min, and keeping the temperature for 2 h.
The results show that the ceramic rod with the diameter of 15mm has no cracking phenomenon during drying and heat treatment, the sintered relative density reaches 99 percent, but the ceramic rods with other diameters have obvious cracking phenomenon after drying. A sample is selected as a cylinder with the diameter of 15mm to be used for green body processing test, the green body processing condition is that the machine rotating speed is 100rpm, and the corresponding surface speed is 9.4 sm/min. The feed rate was 0.35 mm/revolution and the feed rate was 0.5 mm. The green body processing result shows that the green body has high enough strength, but the green body has poor plasticity, so that the screw thread of M8 has severe breaking angle and is seriously worn on a hard alloy cutter.
Example 2:
adding 10g of ceramic powder into a mixed solution of 100ml of ethanol and 5ml of water, dropwise adding 0.5g of polyvinylpyrrolidone (PVP) and 0.5g of ammonia water while stirring, then ultrasonically dispersing at room temperature, then adding 10ml of ethyl orthosilicate into the solution under the condition of continuous stirring, reacting at room temperature for 4-24 h, and centrifugally drying to obtain the silicon dioxide coated ceramic powder.
Weighing 3g of methacrylamide and 0.6g of MBAM, putting the methacrylamide and the MBAM into a beaker, adding 20g of deionized water to fully dissolve the methacrylamide and the MBAM, then adding 2g of ammonium citrate to fully stir, adjusting the pH of a system to be 8-11 by using ammonia water, then adding 0.9g of glycerol and 0.3ml of 10% APS into the solution to stir uniformly, adding 100g of silicon dioxide coated ceramic powder, adding 0.03g of TEMED after ultrasonic dispersion is carried out for 30min at room temperature, rapidly stirring, and then removing bubbles dissolved in ceramic slurry in vacuum; then carefully injecting the ceramic slurry into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water cooling the mould, demoulding to obtain wet ceramic rod blanks with diameters of 15mm, 35mm, 40mm, 43mm and 45mm respectively; drying the wet ceramic rod blank for 72h at room temperature, and then drying the wet ceramic rod blank for 12h in an electric heating drying oven at the temperature of 80 ℃; and after drying, machining the ceramic thread of M8 by using a lathe green body by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at the speed of 0.6 ℃/min, keeping the temperature for 1h, heating to 1600 ℃ at the speed of 3 ℃/min, and keeping the temperature for 2 h.
The results show that the ceramic rods with the diameters of 15mm and 35mm have no cracking phenomenon in the drying and heat treatment processes, the sintering relative densities are 99% and 98%, respectively, and the ceramic rods with other diameters have obvious cracking after being dried. The ceramic rods with the diameters of 15mm and 35mm are selected to be subjected to green body processing tests according to the processing conditions in the embodiment 1, and the results show that no corner collapse phenomenon occurs during thread processing, the damage to the cutter is less, and the processing performance is improved.
Example 3:
weighing 3g of methacrylamide and 0.6g of MBAM, putting the methacrylamide and the MBAM into a beaker, adding 20g of deionized water to fully dissolve the methacrylamide and the MBAM, then adding 2g of ammonium citrate to fully stir, adjusting the pH of a system to be 8-11 by using ammonia water, then adding 0.9g of glycerol and 0.3ml of 10% APS into the solution to stir uniformly, adding 100g of the silica-coated ceramic powder prepared in the embodiment 2, ultrasonically dispersing for 30min at room temperature, then adding 0.03g of TEMED, rapidly stirring, and then removing bubbles dissolved in ceramic slurry in vacuum; then carefully injecting the ceramic slurry into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water cooling the mould, demoulding to obtain wet ceramic rod blanks with diameters of 15mm, 35mm, 40mm, 43mm and 45mm respectively; soaking the ceramic rod wet blank into an ethanol water solution for 12 hours, then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 92% for drying for 48 hours, and then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 80 ℃ and the relative humidity of 20% for drying for 12 hours; and after drying, machining the ceramic thread of M8 by using a lathe green body by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at the speed of 0.6 ℃/min, keeping the temperature for 1h, and heating to 1600 ℃ at the speed of 3 ℃/min, and keeping the temperature for 2 h.
The results showed that the ceramic rods with diameters of 15mm, 35mm and 40mm did not crack during drying and heat treatment, the sintered relative densities were 99%, 98% and 97%, respectively, and the ceramic rods with other diameters cracked significantly after drying. The ceramic rods with the diameters of 15mm and 35mm are selected to be subjected to green body processing tests according to the processing conditions in the embodiment 1, and the results show that no corner collapse phenomenon occurs during thread processing, the damage to the cutter is less, and the processing performance is improved.
Example 4:
weighing 3g of methacrylamide and 0.6g of MBAM, putting the methacrylamide and the MBAM into a beaker, adding 18g of deionized water to fully dissolve the methacrylamide and the MBAM, then adding 2g of ammonium citrate and 2g of ethanol to fully stir, adjusting the pH of a system to be 8-11 by using ammonia water, then adding 0.9g of glycerol and 0.3ml of 10% APS into the solution to stir uniformly, adding 100g of the silicon dioxide coated ceramic powder prepared in the embodiment 2, adding 0.03g of TED after performing ultrasonic dispersion for 30min at room temperature, rapidly stirring, and removing bubbles dissolved in ceramic slurry in vacuum; then carefully injecting the ceramic slurry into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water cooling the mould, demoulding to obtain wet ceramic rod blanks with diameters of 15mm, 35mm, 40mm, 43mm and 45mm respectively; soaking the ceramic rod wet blank into an ethanol water solution for 12 hours, then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 92% for drying for 48 hours, and then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 80 ℃ and the relative humidity of 20% for drying for 12 hours; and after drying, machining the ceramic thread of M8 by using a lathe green body by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at the speed of 0.6 ℃/min, keeping the temperature for 1h, and heating to 1600 ℃ at the speed of 3 ℃/min, and keeping the temperature for 2 h.
The results showed that the ceramic rods with diameters of 15mm, 35mm and 40mm did not crack during drying and heat treatment, the sintered relative densities were 99%, 99% and 97%, the ceramic rods with diameters of 43mm cracked slightly after drying, and the ceramic rods with diameters of 45mm cracked significantly after drying. The ceramic rods with the sample diameters of 15mm and 35mm are selected to be subjected to green body processing tests according to the processing conditions in the embodiment 1, and the results show that no corner collapse phenomenon occurs during thread processing, the damage to the cutter is less, and the processing performance is improved.
Example 5:
weighing 3g of methacrylamide and 0.6g of MBAM, putting the methacrylamide and the MBAM into a beaker, adding 20g of deionized water to fully dissolve the methacrylamide and the MBAM, then adding 2g of ammonium citrate and 2g of ethanol to fully stir, adjusting the pH of a system to be 8-11 by using ammonia water, adding 0.9g of glycerol into the solution to stir uniformly, adding 100g of the silica-coated ceramic powder prepared in the embodiment 2, adding 0.3ml of 10% APS and 0.03g of TED after performing ultrasonic dispersion for 30min at room temperature, rapidly stirring, and removing bubbles dissolved in ceramic slurry in vacuum; then carefully injecting the ceramic slurry into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water cooling the mould, demoulding to obtain wet ceramic rod blanks with diameters of 15mm, 35mm, 40mm, 43mm and 45mm respectively; soaking the ceramic rod wet blank into an ethanol water solution for 12 hours, then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 92% for drying for 48 hours, and then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 80 ℃ and the relative humidity of 20% for drying for 12 hours; and after drying, machining the ceramic thread of M8 by using a lathe green body by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at the speed of 0.6 ℃/min, keeping the temperature for 1h, and heating to 1600 ℃ at the speed of 3 ℃/min, and keeping the temperature for 2 h.
The results showed that the ceramic rods with diameters of 15mm, 35mm and 40mm did not crack during drying and heat treatment, the sintered relative densities were 99%, 99% and 98%, respectively, and the ceramic rods with other diameters all cracked slightly after drying. The ceramic rods with the diameters of 15mm and 35mm are selected to be subjected to green body processing tests according to the processing conditions in the embodiment 1, and the results show that no corner collapse phenomenon occurs during thread processing, the damage to the cutter is less, and the processing performance is improved.
Example 6
Adding 10g of ceramic powder into a mixed solution of 100ml of ethanol and 4ml of water, dropwise adding 0.5g of polyvinylpyrrolidone (PVP) and 0.4g of ammonia water while stirring, then ultrasonically dispersing at room temperature, then adding 6ml of ethyl orthosilicate into the solution under the condition of continuous stirring, reacting at room temperature for 4-24 h, and centrifugally drying to obtain the silicon dioxide coated ceramic powder.
Weighing 3g N-hydroxymethyl acrylamide and 0.5g of PEGDAM, putting the weighed materials into a beaker, adding 20g of deionized water to fully dissolve the materials, then adding 2g of PAA and 2.6g of polyethylene glycol 200 to fully stir, adjusting the pH of a system to be 8-11 by using ammonia water, adding 0.8g of triethylene glycol acetate into the solution to stir uniformly, adding 100g of silicon dioxide coated ceramic powder, performing ultrasonic dispersion at room temperature for 30min, adding 0.3ml of 10% AZIP and 0.03g of TEMED, quickly stirring, and removing bubbles dissolved in ceramic slurry in vacuum; then carefully injecting the ceramic slurry into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water cooling the mould, demoulding to obtain wet ceramic rod blanks with diameters of 15mm, 35mm, 40mm, 43mm and 45mm respectively; soaking the ceramic rod wet blank into an ethanol water solution for 12 hours, then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 92% for drying for 48 hours, and then placing the ceramic rod wet blank into a constant-temperature constant-humidity drying box with the temperature of 80 ℃ and the relative humidity of 20% for drying for 12 hours; and after drying, machining the ceramic thread of M8 by using a lathe green body by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at the speed of 0.6 ℃/min, keeping the temperature for 1h, and heating to 1600 ℃ at the speed of 3 ℃/min, and keeping the temperature for 2 h.
The results showed that the ceramic rods with diameters of 15mm, 35mm and 40mm did not crack during drying and heat treatment, the sintered relative densities were 99%, 99% and 98%, respectively, and the ceramic rods with other diameters all cracked slightly after drying. The ceramic rods with the diameters of 15mm and 35mm are selected to be subjected to green body processing tests according to the processing conditions in the embodiment 1, and the results show that no corner collapse phenomenon occurs during thread processing, the damage to the cutter is less, and the processing performance is improved.
It should be understood that although the present invention has been described with reference to the preferred embodiments, it is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.

Claims (6)

1. The toughened ceramic gel injection molding method is characterized by comprising the following steps of:
(1) adding a ceramic raw material into a ball milling tank, grinding the ceramic raw material into ceramic powder of 0.1-1 mu m, adding the ceramic powder into a mixed solution of ethanol and water, dropwise adding polyvinylpyrrolidone (PVP) and ammonia water while stirring, then ultrasonically dispersing at room temperature, then adding ethyl orthosilicate into the solution under the condition of continuous stirring, reacting at room temperature for 4-24 h, and centrifugally drying to obtain silicon dioxide coated ceramic powder; the volume ratio of the ethanol to the water to the ethyl orthosilicate is (20-50): 1 (1-2), the volume ratio of the water to the ammonia water is (2-10): 1, the ceramic powder accounts for 1-10 wt% of the whole system, and the PVP accounts for 1-5 wt% of the ceramic powder;
(2) weighing an organic monomer and a crosslinking agent, putting the organic monomer and the crosslinking agent into a beaker, adding deionized water to fully dissolve the organic monomer and the crosslinking agent, then adding a dispersing agent and an aqueous cosolvent, fully stirring, adjusting the pH of the system to be 8-11 by using ammonia water, adding a plasticizer and an initiator into the solution, uniformly stirring, adding the silicon dioxide coated ceramic powder in the step (1), performing ultrasonic dispersion for 10-30 min at room temperature, adding a catalyst, rapidly stirring, and removing bubbles dissolved in ceramic slurry in vacuum; the ceramic slurry comprises 1-3 wt% of organic monomers, 1 (5-30) of a cross-linking agent and the organic monomers, 8-20 wt% of deionized water, 0.5-2 wt% of a dispersing agent, 0-10 wt% of a water-based cosolvent, 20-50 wt% of an organic monomer, 0.01-1 wt% of an initiator and 0.01-1 wt% of a catalyst, wherein the mass ratio of the cross-linking agent to the organic monomers is 1;
(3) carefully injecting the ceramic slurry in the step (2) into a mold, and placing the mold in a water bath kettle at 50-80 ℃ to heat for 5-15 min to obtain a solidified ceramic wet blank; water-cooling the mold, demolding to obtain a ceramic wet blank, immersing the ceramic wet blank into an ethanol water solution for 12 hours, then placing the ceramic wet blank in a constant-temperature and constant-humidity drying box with the temperature of 40 ℃ and the relative humidity of 92% for drying for 48 hours, and then placing the ceramic wet blank in a constant-temperature and constant-humidity drying box with the temperature of 80 ℃ and the relative humidity of 20% for drying for 12 hours; and after drying, machining the ceramic thread of M8 on a green body of the lathe by using a hard alloy cutter, degreasing the machined ceramic green body in a glue removing furnace, heating to 600 ℃ at a speed of 0.6 ℃/min, preserving heat for 1h, heating to 1600 ℃ at a speed of 3 ℃/min, preserving heat for 2h to obtain a ceramic product, and finally performing quality detection.
2. The method of claim 1, wherein the organic monomer is any one of acrylamide, N-methylolacrylamide, N-N' methylenebisacrylamide, methacrylamide, acrylic acid, methacrylic acid, and hydroxyethyl acrylate; the cross-linking agent is methylene bisacrylamide or poly (vinyl glycol) dimethylacrylic acid.
3. The method of claim 1, wherein the dispersant is any one of citric acid, ammonium citrate, hydroxymethyl cellulose, polyacrylic acid and its copolymer, and polyethyleneimine; the aqueous cosolvent is any one of ethanol, ethylene glycol, n-propanol, 1, 2-propylene glycol, n-butanol, 1, 4-butanediol, 1, 6-hexanediol, diethylene glycol, triethylene glycol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and glycerol.
4. The method of claim 1, wherein the plasticizer is selected from the group consisting of polyethylene glycol, polymethacrylamide, glycerol, and triethylene glycol acetate; the initiator is any one of ammonium persulfate, hydrogen peroxide and azo [ 2-imidazoline-2-propane ] hydrochloride.
5. The method of claim 1, wherein the catalyst is tetramethylethylenediamine.
6. The toughened ceramic gel injection molding method of claim 1 wherein said ceramic powder is alumina, zirconia, silicon nitride or aluminum titanate.
CN201710952306.0A 2017-10-12 2017-10-12 Toughened ceramic gel injection molding method Active CN107759230B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710952306.0A CN107759230B (en) 2017-10-12 2017-10-12 Toughened ceramic gel injection molding method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710952306.0A CN107759230B (en) 2017-10-12 2017-10-12 Toughened ceramic gel injection molding method

Publications (2)

Publication Number Publication Date
CN107759230A CN107759230A (en) 2018-03-06
CN107759230B true CN107759230B (en) 2020-09-01

Family

ID=61268067

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710952306.0A Active CN107759230B (en) 2017-10-12 2017-10-12 Toughened ceramic gel injection molding method

Country Status (1)

Country Link
CN (1) CN107759230B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109719829B (en) * 2019-01-23 2021-09-17 宁波多维时空智能设备有限公司 Method for manufacturing ceramic by using three-dimensional printing technology
CN112408949B (en) * 2020-10-28 2021-12-28 山东大学 Device and method for preparing alumina microfiber by using microfluidic chip and application
CN112521161B (en) * 2020-12-15 2022-08-30 无锡特科精细陶瓷有限公司 Gel injection molding method of aluminum oxide-zirconium dioxide complex phase ceramic
CN116023124B (en) * 2023-03-28 2023-07-25 成都超纯应用材料有限责任公司 Alumina ceramic based on injection molding and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9290409B2 (en) * 2012-12-23 2016-03-22 King Abdulazia City for Science and Technology (KACST) Glaze composition, method for manufacturing the glaze composition and methods of glazing

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1315754C (en) * 2004-11-16 2007-05-16 中国航空工业第一集团公司北京航空材料研究院 Method for precission shaping ceramic blank by semi-water-base injection-moulding gel process
US20080108496A1 (en) * 2006-11-07 2008-05-08 Gratson Gregory M Composition Used to Make a Transparent Ceramic Material and Method of Manufacturing the Same
CN101905974B (en) * 2010-02-05 2011-11-16 西安理工大学 Electrostatic spinning preparation method of ceramic nanometer composite fibers
CN103419268B (en) * 2013-06-28 2016-03-23 无锡特科精细陶瓷有限公司 A kind of structural ceramics water-base gel casting method
CN105314986A (en) * 2015-05-13 2016-02-10 洛阳名力科技开发有限公司 Silicon carbide ceramic body semi-aqueous gelcasting method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9290409B2 (en) * 2012-12-23 2016-03-22 King Abdulazia City for Science and Technology (KACST) Glaze composition, method for manufacturing the glaze composition and methods of glazing

Also Published As

Publication number Publication date
CN107759230A (en) 2018-03-06

Similar Documents

Publication Publication Date Title
CN107759230B (en) Toughened ceramic gel injection molding method
CN107500781B (en) Preparation method of porous ceramic
CN103419268B (en) A kind of structural ceramics water-base gel casting method
CN108748611B (en) Method for forming ceramic body
CN101323528B (en) Preparation of continuous hole graded ceramic tube
US10906840B2 (en) Cellulose nanocrystal-modified ceramic blank and preparation method thereof
CN111517770A (en) Production method of high-compactness fused quartz ceramic
CN101348376B (en) Double-component monomer system for ceramic material gel pouring moulding and use method thereof
CN102515776A (en) Solidification method for gel injection molding slurry
CN104211407B (en) A kind of moulding process of big-size complicated shape ceramics biscuits of carbonized bricks
CN109081685B (en) Alumina ceramic and preparation method thereof
CN111269011A (en) Preparation method of zirconia microspheres
CN101514108A (en) Simple and reliable multistep drying method for gelatin casting biscuit
CN110253735B (en) Ceramic body, ceramic product and corresponding preparation method
CN109809802B (en) Preparation method of alumina-titania-zirconia ceramic material
CN114538897A (en) Sintering method of gel-casting ceramic green body
CN114292101A (en) Preparation method of quartz ceramic revolving body
CN112456978A (en) Ceramic slurry and preparation method and application thereof
CN116023164B (en) Porous zirconia ceramic block for dental restoration and preparation method and application thereof
CN111548150A (en) Preparation process for preparing ceramic rear cover by gel casting
CN108997003B (en) Ceramic slurry, ceramic device and preparation method thereof
CN111774558B (en) Method for manufacturing tundish nozzle with excellent thermal shock stability for continuous casting
CN114736009B (en) Injection molding aluminum oxide-based ceramic part composite material and preparation method thereof
Wang et al. Alumina ceramics via gelcasting forming with low-toxicity system
CN110937895A (en) Preparation method of zirconia sheet ceramic

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