CN108178665A - A kind of method that ceramic glaze thin layer is prepared based on 3D printing - Google Patents

A kind of method that ceramic glaze thin layer is prepared based on 3D printing Download PDF

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CN108178665A
CN108178665A CN201810033280.4A CN201810033280A CN108178665A CN 108178665 A CN108178665 A CN 108178665A CN 201810033280 A CN201810033280 A CN 201810033280A CN 108178665 A CN108178665 A CN 108178665A
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ceramic
parts
ceramic glaze
thin layer
glaze
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不公告发明人
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Duan Yanling
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Duan Yanling
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y50/00—Data acquisition or data processing for additive manufacturing
    • B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/86—Glazes; Cold glazes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Producing Shaped Articles From Materials (AREA)

Abstract

The present invention relates to ceramic technology fields, disclose a kind of method that ceramic glaze thin layer is prepared based on 3D printing.The preparation method of the ceramic glaze thin layer is first is scanned to obtain three dimensional point cloud using spatial digitizer to molding ceramic idiosome outer contoured shape, three dimensional point cloud is inputted into computer, obtain ceramic idiosome model, then ceramic glaze 3D thin film models are built in the outer surface of ceramic idiosome model, again in ceramic glaze 3D thin film models data input 3D printer corollary equipment, print routine is set, then ceramic glaze slurry is added in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, it accumulates to form ceramic glaze thin layer in ceramic enamel surface, finally ceramic glaze thin layer is obtained through overbaking and sintering.The present invention makes ceramic glaze thickness of thin layer uniform using 3D printing ceramic glaze, and it is preferable to obtain ceramic glaze chromaticness.

Description

A kind of method that ceramic glaze thin layer is prepared based on 3D printing
Technical field
The present invention relates to ceramic technology field, more particularly, to a kind of method that ceramic glaze thin layer is prepared based on 3D printing.
Background technology
The quality of Ceramic glaze quality directly affects the performance and quality of glazed products, and the quality of glaze quality is removed and glaze Material formula, glaze slip preparation process and burning condition have also related with glazing process outside the Pass.With the continuous development of ceramics, glazing work Skill is also to high quality, and low energy consumption, the direction for being more suitable for modern production is developed.During ceramic idiosome glazing, glaze covering Ceramic idiosome surface, forms ceramic glaze thin layer, and the thickness of ceramic glaze thin layer has larger impact, the big pottery of thickness to the performance of ceramics The finish on its surface of enamel thin layer and lustrous and transparent humidity are higher, and the brightness of glaze paint is relatively low, and corner lines obscure.Synthesis is applied at home and abroad Glaze handicraft, existing enameling method mainly have：Glaze is smeared, glaze, brushing glazing is applied, pours glaze, leaching glaze, the glazing of electrostatic vacuum pipe, glazing by sufflation and spray Glaze.Although these glazing process can cover ceramic glaze thin layer on ceramic idiosome surface, the thickness of ceramic glaze thin layer is more difficult Control, after glazing, the ceramic glaze of ceramic idiosome surface some places covering is thicker, and the ceramic glaze of some places covering is relatively thin, this Sample can lead to the uneven thickness one of ceramic glaze thin layer, make the glaze paint brightness of ceramics, finish different with profit jade-like stone degree, influence ceramics The quality of product.In addition the brightness of different types of its needs of ceramics, finish and profit jade-like stone degree are different, that is, variety classes Its ceramic ceramic glaze thickness of thin layer it is different, art methods cannot be accurate to the thickness of ceramic glaze thin layer during glazing Control causes glaze paint brightness, finish and profit jade-like stone degree to be difficult to control, and needs to be fired a large amount of ceramics to select performance conjunction The ceramic of lattice wastes a large amount of manpower and raw material.
Invention content
The present invention is to overcome the problems, such as that prior art ceramic glaze thickness of thin layer is out of contior, and providing one kind can be accurate Control the preparation method of ceramic glaze thickness of thin layer and ceramic glaze thin layer in homogeneous thickness.
To achieve these goals, the present invention uses following technical scheme：One kind prepares ceramic glaze thin layer based on 3D printing Method, include the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 200~300 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, then to the glazed ceramics after baking Idiosome carries out high temperature sintering, is finally cooled to room temperature.
Brightness, finish and the pottery for moistening jade-like stone degree, only suitable thickness of the thickness effect Ceramic glaze of ceramic glaze thin layer Enamel thin layer can just prepare the ceramic glaze thin layer of high quality chromaticness.It is by ceramic embryo that conventional method, which prepares ceramic glaze thin layer method, External surface manually covers one layer of ceramic glaze, but the thickness of ceramic glaze thin layer not can determine that, can only be by adjusting ceramic glaze Viscosity size carry out the rough ceramic glaze thin layer for preparing different-thickness, then picked out from a large amount of ceramic product of good quality Ceramic, wastes raw material and manual labor.The present invention first passes through spatial digitizer, and ceramic idiosome exterior contour data are defeated Enter computer, ceramic idiosome model is shown in computer, then add certain thickness pottery automatically on ceramic idiosome model by computer Enamel thin film model, the size of ceramic glaze thin film model thickness can be manually entered adjusting, then input ceramic model data In 3D printer, 3D printer nozzle is controlled the certain thickness ceramic glaze of jet-stacking on ceramic idiosome material object by computer program Thin layer, the thickness of ceramic glaze thin layer is the entity ceramic glaze thin layer and the preset pottery of computer that print by computer preset in advance Enamel thickness of thin layer size is identical, and the ceramic glaze thin layer of different-thickness can be thus printed according to different types of ceramics, from And the higher ceramics of chromaticness are obtained, the present invention does not need to prepare a large amount of ceramic to be selected to carry out quality, is saved a large amount of Raw material does not need to artificial glazing, saves manpower；In addition the present invention can ensure ceramic glaze thin layer using 3D printing ceramic glaze thin layer Thickness is in the same size, greatly improves the uniformity of ceramic surface color and luster.
Preferably, glazed ceramics idiosome baking temperature is 60~70 DEG C in the step (3), baking time is 1~2h.
Preferably, in the step (3), the process that the ceramic idiosome after toasting is sintered is：First with 90~120 DEG C/heating rate of h rises to 850~900 DEG C from kiln roasting temperature and keeps the temperature 3~5h, then with the heating of 40~50 DEG C/h Speed rises to 1100~1250 DEG C and keeps the temperature 6~10h.
Preferably, ceramic glaze slurry is made of the raw material that following parts by weight match in the step (2)：
30~40 parts of nepheline syenite, 25~30 parts of potassium feldspar, 15~20 parts of kaolin, 2~3 parts of calcium phosphate, barium carbonate 1~3 Part, 2~5 parts of silicon carbide, 4~8 parts of compound binding agent, 1~3 part of antimony oxide, 2~5 part, nanometer two of dolomite micron particles 3~6 parts of silicon oxide particle.
Using nepheline syenite, potassium feldspar and kaolin as the basic ingredient of ceramic glaze dispensing, calcium phosphate is used for the present invention Component dispersibility in glaze is improved, barium carbonate is used to increase the glossiness of ceramic enamel surface, and compound binding agent is used for material It bonds, increases the intensity of ceramic glaze, antimony oxide is used to increase the heat resistance of ceramic glaze, ceramic glaze thin layer is prevented to be sintered Occurs Large Area Cracking phenomenon in the process.
Preferably, the dolomite micron particles size is 20~30 μm, the nanometer silicon dioxide particle size is 100~250nm.
Dolomite micron particles and nano SiO 2 particle are mixed into ceramic glaze by the present invention, and a part of dolomite is micro- Rice grain and nano SiO 2 particle are mixed in the inside of glaze thin layer, and dolomite micron particles can improve ceramic glaze thin layer Thermal stability, nano SiO 2 particle can improve the intensity and compactness of ceramic glaze thin layer, prevent moisture in air from entering Inside ceramic idiosome；In addition, a part of micron particles and nano particle are dispersed in the surface of ceramic glaze thin layer, micron particles and receive Rice grain forms micron particles and the alternate structure of nano particle in ceramic glaze thin layer surface, greatly promotes ceramic glaze thin layer surface Roughness, make ceramic glaze thin layer that there is ultra-hydrophobicity, when ceramics are stained with dust or dirt, ceramics made to become easily clear It washes.
Preferably, the dolomite micron particles, by pretreatment, preprocess method is：
2~3g calcium hydroxides are added in reaction kettle, then add in 50~60mL deionized waters, are heated to 50~60 DEG C, stirring 4~8g dolomite micron particles are added in after uniformly, 0.1~0.2g sodium pyrophosphates is added, is then at the uniform velocity passed through carbon dioxide, instead 1~2h is answered, carbon dioxide is passed through rate control in 3~5m3/ h, is finally putting into vacuum drying chamber, in 70~80 DEG C of condition 3~7h of lower drying, the dolomite micron particles pre-processed.
The present invention is anti-with carbon dioxide using calcium hydroxide in order to further improve the hydrophobic performance of ceramic glaze thin layer surface Precipitation of calcium carbonate should be generated, one layer of nano-calcium carbonate particles, this micron particles surface are coated on dolomite micron particles surface The structure of dispersing nanoparticles forms the bionic super-hydrophobic structure of similar lotus leaf microcosmic surface, greatly improves ceramic glaze thin layer surface Roughness, further increase the hydrophobic performance of ceramic glaze thin layer；In addition cium carbonate nanoparticles are conducive to improve ceramic glaze Curing rate, prevent ceramic glaze ink after ceramic idiosome surface is ejected into due to gravity caused by Glaze Slip drop position It moves, ceramic glaze thin layer surface is caused to form recess and protrusion, influences ceramic mass.
Preferably, the compound binding agent is made of the raw material that following parts by weight match：
30~35 parts of glycidyl ester epoxy resin, 50~60 parts of montmorillonite, 2~5 parts of calgon, vinyl trimethoxy 3~5 parts of 1~3 part of base silane, 5~10 parts of modified diethylenetriamine and silicon carbide.
For compound binding agent using glycidyl ester epoxy resin as bonding material, montmorillonite is compound binding agent in the present invention Filler, calgon increases the dispersibility between component, and vinyltrimethoxysilane improves the compatibility of component and affine Power, modified diethylenetriamine are the curing rate for promoting compound binding agent, and silicon carbide improves the thermal stability of binding agent.
Preferably, the modified vinyl triamine preparation method is：By 20~25mL diethylenetriamines and 80~100mL Acetone is added in four-hole boiling flask, then adds in 15~20ml allyl phenyl thioethers, and heating water bath is added to 50~60 DEG C 0.1~0.15g azodiisobutyronitriles react 4~5h, obtain modified diethylenetriamine.
Since the ceramic later stage will pass through high temperature sintering, compound binding agent must have certain heat resistance, otherwise can make Into the cracking of ceramic glaze thin layer surface, the present invention carries out graft modification to curing agent, is connect on diethylenetriamine curing agent molecule Branch improves its heat resistance containing phenyl ring skeleton；Glycidyl ester epoxy resin and modified diethylenetriamine at a certain temperature In primary amine reaction generation secondary amine, secondary amine continuation react to form crosslinked reticular structure with glycidyl ester epoxy resin, make Compound binding agent rapid curing further increases the heat resistance of compound binding agent.
Therefore, the present invention has the advantages that：(1) the ceramic glaze thin layer of ceramic idiosome surface covering can be controlled Thickness, so as to promote ceramic glaze chromaticness；(2) ceramic glaze thickness of thin layer is in the same size, and chromaticness is uniform；(3) raw material is saved, is reduced into This；(4) there is ultra-hydrophobicity, convenient for the cleaning of ceramic surface.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention is described further.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art, Method in embodiment is the conventional method of this field unless otherwise instructed.
Embodiment 1
A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 200 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 60 DEG C, during baking Between for 1h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 90 DEG C/h speed Degree rises to 850 DEG C from kiln roasting temperature and keeps the temperature 3h, then rises to 1100 DEG C with the heating rate of 40 DEG C/h and keeps the temperature 6h, most Postcooling is to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 30 parts of nepheline syenite, 25 parts of potassium feldspar, 15 parts of kaolin, 2 parts of calcium phosphate, 1 part of barium carbonate, 2 parts of silicon carbide, compound viscous 4 parts of agent of knot, 1 part of antimony oxide, particle size are the nanometer two that 20 μm of 2 parts of dolomite micron particles, particle sizes are 100nm 3 parts of silicon oxide particle.
Wherein, dolomite micron particles are by pretreatment, preprocess method：
2g calcium hydroxides are added in reaction kettle, 50mL deionized waters is then added in, is heated to 50 DEG C, is stirring evenly and then adding into 4g Dolomite micron particles add 0.1g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, react 1h, and carbon dioxide is passed through speed Rate is controlled in 3m3/ h, is finally putting into vacuum drying chamber, and dry 3h, the dolomite pre-processed are micro- under conditions of 70 DEG C Rice grain.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
30 parts of glycidyl ester epoxy resin, 50 parts of montmorillonite, 2 parts of calgon, 1 part of vinyltrimethoxysilane, It is modified 3 parts of 5 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：20mL diethylenetriamines and 80mL acetone are added in four-hole boiling flask, Then 15ml allyl phenyl thioethers are added in, heating water bath adds 0.1g azodiisobutyronitriles to 50 DEG C, reacts 4h, obtains Modified diethylenetriamine.
Embodiment 2
A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 220 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 63 DEG C, during baking Between for 1.2h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 100 DEG C/h Speed rises to 860 DEG C from kiln roasting temperature and keeps the temperature 3.5h, then rises to 1150 DEG C with the heating rate of 42 DEG C/h and keeps the temperature 7h is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 32 parts of nepheline syenite, 26 parts of potassium feldspar, 16 parts of kaolin, 2 parts of calcium phosphate, 1 part of barium carbonate, 3 parts of silicon carbide, compound viscous 5 parts of agent of knot, 1 part of antimony oxide, particle size are the nanometer two that 22 μm of 3 parts of dolomite micron particles, particle sizes are 150nm 4 parts of silicon oxide particle.
Wherein, dolomite micron particles are by pretreatment, preprocess method：
2.4g calcium hydroxides are added in reaction kettle, 53mL deionized waters is then added in, is heated to 52 DEG C, is stirring evenly and then adding into 5g dolomite micron particles, add 0.12g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, react 1.3h, and carbon dioxide leads to Enter rate control in 3.5m3/ h, is finally putting into vacuum drying chamber, and the dry 4h under conditions of 72 DEG C, what is pre-processed is white Marble micron particles.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
32 parts of glycidyl ester epoxy resin, 53 parts of montmorillonite, 3 parts of calgon, 1 part of vinyltrimethoxysilane, It is modified 3 parts of 6 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：22mL diethylenetriamines and 85mL acetone are added in four-hole boiling flask, Then 16ml allyl phenyl thioethers are added in, heating water bath adds 0.12g azodiisobutyronitriles to 52 DEG C, reacts 4.2h, obtains To modified diethylenetriamine.
Embodiment 3
A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 250 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 65 DEG C, during baking Between for 1.6h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 105 DEG C/h Speed rises to 870 DEG C from kiln roasting temperature and keeps the temperature 4h, then rises to 1180 DEG C with the heating rate of 45 DEG C/h and keeps the temperature 8h, It is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
35 parts of nepheline syenite, 18 parts of kaolin, 2.5 parts of calcium phosphate, 2 parts of barium carbonate, 3.5 parts of silicon carbide, is answered at 27 parts of potassium feldspar It is that 25 μm of 3.5 parts of dolomite micron particles, particle sizes are 200nm's to close 6 parts of binding agent, 2 parts of antimony oxide, particle size 4.5 parts of nanometer silicon dioxide particle.
Wherein, dolomite micron particles are by pretreatment, preprocess method：
2.6g calcium hydroxides are added in reaction kettle, 55mL deionized waters is then added in, is heated to 55 DEG C, is stirring evenly and then adding into 6g dolomite micron particles, add 0.15g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, react 1.5h, and carbon dioxide leads to Enter rate control in 4m3/ h, is finally putting into vacuum drying chamber, dry 5h, the white clouds pre-processed under conditions of 75 DEG C Stone micron particles.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
33 parts of glycidyl ester epoxy resin, 55 parts of montmorillonite, 3.5 parts of calgon, vinyltrimethoxysilane 2 4 parts of part, 7 parts of modified diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：23mL diethylenetriamines and 90mL acetone are added in four-hole boiling flask, Then 17ml allyl phenyl thioethers are added in, heating water bath adds 0.13g azodiisobutyronitriles to 55 DEG C, reacts 4.5h, obtains To modified diethylenetriamine.
Embodiment 4
A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 270 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 68 DEG C, during baking Between for 1.8h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 110 DEG C/h Speed rises to 880 DEG C from kiln roasting temperature and keeps the temperature 4.5h, then rises to 1200 DEG C with the heating rate of 48 DEG C/h and keeps the temperature 9h is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 38 parts of nepheline syenite, 28 parts of potassium feldspar, 19 parts of kaolin, 3 parts of calcium phosphate, 3 parts of barium carbonate, 4 parts of silicon carbide, compound viscous 7 parts of agent of knot, 3 parts of antimony oxide, particle size are the nanometer two that 27 μm of 4 parts of dolomite micron particles, particle sizes are 220nm 5 parts of silicon oxide particle.
Wherein, dolomite micron particles are by pretreatment, preprocess method：
2.8g calcium hydroxides are added in reaction kettle, 57mL deionized waters is then added in, is heated to 58 DEG C, is stirring evenly and then adding into 7g dolomite micron particles, add 0.18g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, react 1.8h, and carbon dioxide leads to Enter rate control in 4.5m3/ h, is finally putting into vacuum drying chamber, and the dry 6h under conditions of 78 DEG C, what is pre-processed is white Marble micron particles.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
34 parts of glycidyl ester epoxy resin, 58 parts of montmorillonite, 4 parts of calgon, 3 parts of vinyltrimethoxysilane, It is modified 5 parts of 8 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：24mL diethylenetriamines and 95mL acetone are added in four-hole boiling flask, Then 18ml allyl phenyl thioethers are added in, heating water bath adds 0.14g azodiisobutyronitriles to 58 DEG C, reacts 4.7h, obtains To modified diethylenetriamine.
Embodiment 5
A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 300 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 70 DEG C, during baking Between for 2h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 120 DEG C/h speed Degree rises to 900 DEG C from kiln roasting temperature and keeps the temperature 5h, then rises to 1250 DEG C with the heating rate of 50 DEG C/h and keeps the temperature 10h, It is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 40 parts of nepheline syenite, 30 parts of potassium feldspar, 20 parts of kaolin, 3 parts of calcium phosphate, 3 parts of barium carbonate, 5 parts of silicon carbide, compound viscous 8 parts of agent of knot, 3 parts of antimony oxide, particle size are the nanometer two that 30 μm of 5 parts of dolomite micron particles, particle sizes are 250nm 6 parts of silicon oxide particle.
Wherein, dolomite micron particles are by pretreatment, preprocess method：
3g calcium hydroxides are added in reaction kettle, 60mL deionized waters is then added in, is heated to 60 DEG C, is stirring evenly and then adding into 8g Dolomite micron particles add 0.2g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, react 2h, and carbon dioxide is passed through speed Rate is controlled in 5m3/ h, is finally putting into vacuum drying chamber, and dry 7h, the dolomite pre-processed are micro- under conditions of 80 DEG C Rice grain.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
35 parts of glycidyl ester epoxy resin, 60 parts of montmorillonite, 5 parts of calgon, 3 parts of vinyltrimethoxysilane, It is modified 5 parts of 10 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：25mL diethylenetriamines and 100mL acetone are added in four-hole boiling flask, Then 20ml allyl phenyl thioethers are added in, heating water bath adds 0.15g azodiisobutyronitriles to 60 DEG C, reacts 5h, obtains Modified diethylenetriamine.
Comparative example 1
Difference lies in nanometer silicon dioxide particle, specific preparation method are not contained in ceramic glaze slurry with embodiment 2 for comparative example 1 It is as follows：A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 220 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 63 DEG C, during baking Between for 1.2h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 100 DEG C/h Speed rises to 860 DEG C from kiln roasting temperature and keeps the temperature 3.5h, then rises to 1150 DEG C with the heating rate of 42 DEG C/h and keeps the temperature 7h is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 32 parts of nepheline syenite, 26 parts of potassium feldspar, 16 parts of kaolin, 2 parts of calcium phosphate, 1 part of barium carbonate, 3 parts of silicon carbide, compound viscous 5 parts of agent of knot, 1 part of antimony oxide, particle size are 22 μm of 3 parts of dolomite micron particles.
Wherein, dolomite micron particles are by pretreatment, preprocess method：
2.4g calcium hydroxides are added in reaction kettle, 53mL deionized waters is then added in, is heated to 52 DEG C, is stirring evenly and then adding into 5g dolomite micron particles, add 0.12g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, react 1.3h, and carbon dioxide leads to Enter rate control in 3.5m3/ h, is finally putting into vacuum drying chamber, and the dry 4h under conditions of 72 DEG C, what is pre-processed is white Marble micron particles.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
32 parts of glycidyl ester epoxy resin, 53 parts of montmorillonite, 3 parts of calgon, 1 part of vinyltrimethoxysilane, It is modified 3 parts of 6 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：22mL diethylenetriamines and 85mL acetone are added in four-hole boiling flask, Then 16ml allyl phenyl thioethers are added in, heating water bath adds 0.12g azodiisobutyronitriles to 52 DEG C, reacts 4.2h, obtains To modified diethylenetriamine.
Comparative example 2
Comparative example 2 is not with embodiment 2 difference lies in dolomite micron particles are contained in ceramic glaze slurry, specific preparation method is such as Under：A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 220 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 63 DEG C, during baking Between for 1.2h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 100 DEG C/h Speed rises to 860 DEG C from kiln roasting temperature and keeps the temperature 3.5h, then rises to 1150 DEG C with the heating rate of 42 DEG C/h and keeps the temperature 7h is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 32 parts of nepheline syenite, 26 parts of potassium feldspar, 16 parts of kaolin, 2 parts of calcium phosphate, 1 part of barium carbonate, 3 parts of silicon carbide, compound viscous Tie 5 parts of agent, 1 part of antimony oxide, 4 parts of the nanometer silicon dioxide particle that particle size is 150nm.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
32 parts of glycidyl ester epoxy resin, 53 parts of montmorillonite, 3 parts of calgon, 1 part of vinyltrimethoxysilane, It is modified 3 parts of 6 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：22mL diethylenetriamines and 85mL acetone are added in four-hole boiling flask, Then 16ml allyl phenyl thioethers are added in, heating water bath adds 0.12g azodiisobutyronitriles to 52 DEG C, reacts 4.2h, obtains To modified diethylenetriamine.
Comparative example 3
Difference lies in do not contain dolomite micron particles and silica nanometer in ceramic glaze slurry with embodiment 2 for comparative example 3 Particle, specific preparation method are as follows：
A kind of method that ceramic glaze thin layer is prepared based on 3D printing, is included the following steps：
(1) it models：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 220 μm；
(2) glazing：By in ceramic glaze 3D thin film models data input 3D printer corollary equipment in step (1), setting prints journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
(3) it is sintered：Ceramics after glazing are put into kiln and are toasted under cryogenic, baking temperature is 63 DEG C, during baking Between for 1.2h, high temperature sintering is then carried out to the glazed ceramics idiosome after baking, the process of sintering is first with the heating of 100 DEG C/h Speed rises to 860 DEG C from kiln roasting temperature and keeps the temperature 3.5h, then rises to 1150 DEG C with the heating rate of 42 DEG C/h and keeps the temperature 7h is finally cooled to room temperature.
Wherein, ceramic glaze slurry is made of the raw material that following parts by weight match：
It is 32 parts of nepheline syenite, 26 parts of potassium feldspar, 16 parts of kaolin, 2 parts of calcium phosphate, 1 part of barium carbonate, 3 parts of silicon carbide, compound viscous Tie 5 parts of agent, 1 part of antimony oxide.
Wherein, compound binding agent is made of the raw material that following parts by weight match：
32 parts of glycidyl ester epoxy resin, 53 parts of montmorillonite, 3 parts of calgon, 1 part of vinyltrimethoxysilane, It is modified 3 parts of 6 parts of diethylenetriamine and silicon carbide.
The preparation method of modified diethylenetriamine is：22mL diethylenetriamines and 85mL acetone are added in four-hole boiling flask, Then 16ml allyl phenyl thioethers are added in, heating water bath adds 0.12g azodiisobutyronitriles to 52 DEG C, reacts 4.2h, obtains To modified diethylenetriamine.
Using contact angle instrument to the static contact angle of 1~3 ceramic glaze thin layer surface of Examples 1 to 5 and comparative example into Row test, test result is as follows shown in table：
The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention, although this Invention is disclosed above with preferred embodiment, however is not limited to the present invention, any person skilled in the art, It does not depart from the range of technical solution of the present invention, when the technology contents using the disclosure above make a little change or are modified to equivalent The equivalent embodiment of variation, as long as being without departing from technical solution of the present invention content, technical spirit according to the present invention is to above real Any simple modification, equivalent change and modification that example is made is applied, in the range of still falling within technical solution of the present invention.

Claims (8)

  1. A kind of 1. method that ceramic glaze thin layer is prepared based on 3D printing, which is characterized in that include the following steps：
    （1）Modeling：Molding ceramic idiosome outer contoured shape is scanned to obtain three-dimensional point cloud number using spatial digitizer According to, three dimensional point cloud is inputted into computer, obtains ceramic idiosome model, then the outer surface of ceramic idiosome model build ceramics Glaze 3D thin film models, then ceramic glaze 3D thin film models are resolved into a series of two dimensional model that thickness are 200 ~ 300 μm；
    （2）Glazing：By step（1）In middle ceramic glaze 3D thin film models data input 3D printer corollary equipment, setting printing journey Then sequence adds in ceramic glaze slurry in 3D printer, 3D printer nozzle sprays ceramic glaze ink on ceramic idiosome surface, Ceramic enamel surface is accumulated to form ceramic glaze thin layer；
    （3）Sintering：Ceramics after glazing are put into kiln and are toasted under cryogenic, then to the glazed ceramics after baking Idiosome carries out high temperature sintering, is finally cooled to room temperature.
  2. A kind of 2. method that ceramic glaze thin layer is prepared based on 3D printing according to claim 1, which is characterized in that the step Suddenly（3）Middle glazed ceramics idiosome baking temperature is 60 ~ 70 DEG C, and baking time is 1 ~ 2h.
  3. A kind of 3. method that ceramic glaze thin layer is prepared based on 3D printing according to claim 1, which is characterized in that the step Suddenly（3）In, the process that the ceramic idiosome after toasting is sintered is：First dried with the heating rate of 90 ~ 120 DEG C/h from kiln Roasting temperature rises to 850 ~ 900 DEG C and keeps the temperature 3 ~ 5h, then rises to 1100 ~ 1250 DEG C with the heating rate of 40 ~ 50 DEG C/h and keeps the temperature 6~10h。
  4. 4. a kind of method that ceramic glaze thin layer is prepared based on 3D printing according to claim 1 ~ 3 any claim, It is characterized in that, the step（2）Middle ceramic glaze slurry is made of the raw material that following parts by weight match：
    30 ~ 40 parts of nepheline syenite, 25 ~ 30 parts of potassium feldspar, 15 ~ 20 parts of kaolin, 2 ~ 3 parts of calcium phosphate, 1 ~ 3 part of barium carbonate, carbon 2 ~ 5 parts of SiClx, 4 ~ 8 parts of compound binding agent, 1 ~ 3 part of antimony oxide, 2 ~ 5 parts of dolomite micron particles, nano silicon dioxide 3 ~ 6 parts of grain.
  5. 5. a kind of method that ceramic glaze thin layer is prepared based on 3D printing according to claim 4, which is characterized in that described white Marble micron particles size is 20 ~ 30 μm, and the nanometer silicon dioxide particle size is 100 ~ 250nm.
  6. 6. a kind of method that ceramic glaze thin layer is prepared based on 3D printing according to claim 5, which is characterized in that described white By pre-processing, preprocess method is marble micron particles：
    2 ~ 3g calcium hydroxides are added in reaction kettle, 50 ~ 60mL deionized waters is then added in, is heated to 50 ~ 60 DEG C, stirs evenly 4 ~ 8g dolomite micron particles are added in afterwards, add 0.1 ~ 0.2g sodium pyrophosphates, are then at the uniform velocity passed through carbon dioxide, reaction 1 ~ 2h, carbon dioxide are passed through rate control in 3 ~ 5m3/ h, is finally putting into vacuum drying chamber, dry 3 under conditions of 70 ~ 80 DEG C ~ 7h, the dolomite micron particles pre-processed.
  7. 7. a kind of method that ceramic glaze thin layer is prepared based on 3D printing according to claim 4, which is characterized in that described multiple Binding agent is closed to be made of the raw material that following parts by weight match：
    30 ~ 35 parts of glycidyl ester epoxy resin, 50 ~ 60 parts of montmorillonite, 2 ~ 5 parts of calgon, vinyl trimethoxy 3 ~ 5 parts of 1 ~ 3 part of silane, 5 ~ 10 parts of modified diethylenetriamine and silicon carbide.
  8. 8. a kind of method that ceramic glaze thin layer is prepared based on 3D printing according to claim 7, which is characterized in that described to change Sex ethylene base triamine preparation method is：20 ~ 25mL diethylenetriamines and 80 ~ 100mL acetone are added in four-hole boiling flask, Ran Houjia Entering 15 ~ 20ml allyl phenyl thioethers, heating water bath adds 0.1 ~ 0.15g azodiisobutyronitriles to 50 ~ 60 DEG C, reaction 4 ~ 5h obtains modified diethylenetriamine.
CN201810033280.4A 2018-01-14 2018-01-14 A kind of method that ceramic glaze thin layer is prepared based on 3D printing Withdrawn CN108178665A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110682395A (en) * 2018-07-05 2020-01-14 张伟 Method for preparing enamel coating on surface of photovoltaic cell by using 3D printing technology
CN110757631A (en) * 2019-10-30 2020-02-07 福建省佳美集团公司 Ceramic spraying device
CN110774428A (en) * 2019-10-30 2020-02-11 福建省佳美集团公司 Ceramic processing method
CN112408789A (en) * 2020-12-03 2021-02-26 马鞍山市三川机械制造有限公司 Preparation method of hydrophobic antifouling ground coat slurry
CN113754411A (en) * 2021-08-17 2021-12-07 南通大学 Preparation method of 3D printing red overglaze Ce: YAG fluorescent ceramic
CN113800952A (en) * 2021-09-24 2021-12-17 童心笛 Glazed tile with artistic effect and preparation method thereof
CN115745404A (en) * 2022-11-28 2023-03-07 浙江大学温州研究院 High-solid-content glaze suitable for direct-writing 3D printing and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110682395A (en) * 2018-07-05 2020-01-14 张伟 Method for preparing enamel coating on surface of photovoltaic cell by using 3D printing technology
CN110757631A (en) * 2019-10-30 2020-02-07 福建省佳美集团公司 Ceramic spraying device
CN110774428A (en) * 2019-10-30 2020-02-11 福建省佳美集团公司 Ceramic processing method
CN112408789A (en) * 2020-12-03 2021-02-26 马鞍山市三川机械制造有限公司 Preparation method of hydrophobic antifouling ground coat slurry
CN113754411A (en) * 2021-08-17 2021-12-07 南通大学 Preparation method of 3D printing red overglaze Ce: YAG fluorescent ceramic
CN113800952A (en) * 2021-09-24 2021-12-17 童心笛 Glazed tile with artistic effect and preparation method thereof
CN113800952B (en) * 2021-09-24 2022-12-23 童心笛 Glazed tile with artistic effect and preparation method thereof
CN115745404A (en) * 2022-11-28 2023-03-07 浙江大学温州研究院 High-solid-content glaze suitable for direct-writing 3D printing and preparation method thereof

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