CN110526696A - Digital light polymer-ceramic material and preparation method - Google Patents
Digital light polymer-ceramic material and preparation method Download PDFInfo
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- CN110526696A CN110526696A CN201910976999.6A CN201910976999A CN110526696A CN 110526696 A CN110526696 A CN 110526696A CN 201910976999 A CN201910976999 A CN 201910976999A CN 110526696 A CN110526696 A CN 110526696A
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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
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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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
- C04B35/62615—High energy or reactive ball milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/386—Boron nitrides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3865—Aluminium nitrides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
Abstract
The present invention provides a kind of digital light polymer-ceramic material, the raw material including following parts by weight: 45-65 parts of ceramic base material, 1-5 parts of polytetrafluoroethylene (PTFE), 1-2 parts of covering material, 25-50 parts of light-cured resin, 0.2-0.5 parts of compatilizer, 1-4 parts of photoinitiator.The present invention also provides preparation methods: ceramic base material and polytetrafluoroethylene (PTFE) being put into planetary ball mill, ball milling 30-60min obtains mixing ceramic base material；Covering material and compatilizer are put into batch mixer, after mixing evenly, point 5 batches are put into mixing ceramic base material, and temperature is 20-60 DEG C, mixing 30-60min；Light-cured resin will be entered into batch mixer, under nitrogen protection, after mixing is uniform, add photoinitiator, product is kept in dark place mixing 2-3h.Digital light polymer-ceramic material of the invention and preparation method thereof has the advantages that low in cost, simple process, better quality compared to the prior art, is more conducive to be mass produced.
Description
Technical field
The present invention relates to 3D printing ceramics consumptive material manufacturing field, in particular to a kind of digital light polymer-ceramic material and
Preparation method.
Background technique
Ceramic 3D printing has the characteristics that layer-by-layer printing shaping, and the sharpest edges compared to traditional ceramics manufacturing process are
Production precision is high, fabrication cycle is short, it is relatively low that personalized production, the diversity of making material and cost of manufacture can be achieved.
3D printing is alternatively referred to as increases material manufacturing technology, and the appearance of 3D printing becomes manufacture complex parts easily and quickly.Currently, comparing
Mature 3D printing technique mainly has " fuse deposition rapid forming ", and " quires layer rapid shaping ", " selective laser sintering is fast
Rapid-result type " and " stereolithography rapid shaping ".
Digital photopolymerization (DLP) 3D printing technique utilize photo-curing material the characteristics of, be by Digital Signals light source,
Promote light-sensitive material according to setting shape successively form, have structure it is simple and easy to control, it is at low cost, it is high-efficient the features such as.DLP printing
Technology is designed primarily directed to UV photo-curing material.Current ceramics DLP printing is usually by ceramic raw material and photocuring tree
Rouge is implemented printing manufacture again after being compounded.The viscosity of entire slurry becomes larger after photosensitive resin addition ceramic raw material, flows
Property be deteriorated, printing precision and speed decline.In addition for ceramic raw material in the system of light-cured resin and unstable, it is heavy easily to occur
It forms sediment, seriously affects the molding effect of printing green body, green body is caused to be easy to happen fracture and ceramic product in high-temperature molding
Standard cannot ensure.
Summary of the invention
It is an object of the invention to overcome the shortage of prior art, provide a kind of good with integrally formed property and controllability
Good, simple process, high mechanical properties 3D printing ceramic materials, still further provide the preparation method of this ceramic material.
The technical scheme is that
Digital light polymer-ceramic material, the raw material including following parts by weight: 45-65 parts of ceramic base material, polytetrafluoroethylene (PTFE) 1-5
Part, 15-20 parts of covering material, 25-50 parts of light-cured resin, 1-4 parts of compatilizer, 1-4 parts of photoinitiator.
Preferably, ceramic base material is silica, tetragonal zirconia polycrystal ceramic powders, silicon nitride ceramic powder, nitridation
Aluminium powder, boron nitride ceramics powder, the ceramic base material partial size are 0-200nm.
Preferably, the covering material is epoxy resin, methyl methacrylate.
Preferably, it includes Tricyclodecane Dimethanol diacrylate, dipentaerythritol that light-cured resin, which is esters of acrylic acid,
Five acrylate, the third oxidation glycerol triacrylate, 2- methyl-1,3-propanediol diacrylate, 2- butyl -2- ethyl -
1,3-propanediol diacrylate, ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, trihydroxy methyl third
Alkane trimethyl acrylic ester, pentaerythritol triacrylate, 1,6- hexanediyl ester, dipropylene glycol diacrylate,
Double Glycerin tetraacrylates, aliphatic acrylate, urethane acrylate, one kind of epoxy acrylate or several
Kind.
Preferably, photoinitiator is 2- hydroxy-2-methyl -1- phenyl -1- acetone, benzophenone, dimethoxybenzoin, chlorine
Change one or more of benzophenone.
Preferably, the compatilizer is copolymer-maleic anhydride grafted ethene-vinyl acetate copolymer, maleic anhydride
At least one of copolymer grafted ethylene-acrylate copolymer, maleic anhydride inoculated polypropylene.
The preparation method of digital light polymer-ceramic material, comprising the following steps:
Ceramic base material and polytetrafluoroethylene (PTFE) are put into planetary ball mill by S1, and ball milling 30-60min obtains mixing ceramic base material；
Covering material and compatilizer are put into batch mixer by S2, and after mixing evenly, point 5 batches are put into mixing ceramic base material, temperature
Degree is 20-60 DEG C, mixing 30-60min；
S3 will enter light-cured resin into batch mixer, under nitrogen protection, after mixing is uniform, add photoinitiator, mixing
Product is kept in dark place 2-3h.
The beneficial effects of the present invention are:
The digital light polymer-ceramic material, good fluidity is not stratified to have good shatter value, and photopolymerization prints degree height, beats
Green body after print maintains good sintering character, can use pressureless sintering, gas pressure sintering or hot pressed sintering.
The preparation method is that by a small amount of multiple dispensing of ceramic base material and teflon mixture to coating material
Material and compatilizer in, increase clad ratio, reduce covering material and compatilizer dosage, improve low price ceramic base material in raw material
Accounting reduces cost.After ball milling, polytetrafluoroethylene (PTFE) and ceramic base material formation are inlayed, and can preferably be distributed to oiliness
In solvent.Light-cured resin has oiliness property, is good polytetrafluoroethyldispersions dispersions.In addition using such as methyl in covering
The achievable polytetrafluoroethylene (PTFE) of methyl acrylate and ceramic base material it is pre-dispersed, the digital light polymer-ceramic material finally prepared
Stable system is suitble to the 3D printing of DLP.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment 1,
Digital light polymer-ceramic material, the raw material including following parts by weight: ceramic base material: 25 parts of SiO 2 powder, cubic oxygen
Change 10 parts of zirconium polycrystalline ceramics powder, 10 parts of silicon nitride ceramic powder, 10 parts of aluminium nitride powder, 10 parts of boron nitride ceramics powder.It is poly-
1 part of tetrafluoroethene, covering material: 1.5 parts of epoxy resin, the third 0.5 part of glycerol triacrylate of oxidation.Light-cured resin:
5 parts of Tricyclodecane Dimethanol diacrylate, 5 parts of Dipentaerythritol Pentaacrylate, the third oxidation glycerol triacrylate 5
Part, 2- methyl-1,5 parts of 3-propanediol diacrylate, ethyl -1 2- butyl -2-, 5 parts of 3-propanediol diacrylate, second
5 parts of diol dimethacrylate, compatilizer: copolymer-maleic anhydride grafted ethene -0.5 part of acrylate copolymer, hexichol
0.5 part of ketone, photoinitiator: 0.5 part of dimethoxybenzoin.
Embodiment 2,
Digital light polymer-ceramic material, the raw material including following parts by weight: ceramic base material: 35 parts of SiO 2 powder, cubic oxygen
Change 5 parts of zirconium polycrystalline ceramics powder, 5 parts of silicon nitride ceramic powder, 5 parts of aluminium nitride powder, 5 parts of boron nitride ceramics powder, polytetrafluoro
1 part of ethylene, covering material: 0.5 part of epoxy resin, 0.5 part of methyl methacrylate, light-cured resin: Tricyclodecane Dimethanol
5 parts of diacrylate, 5 parts of Dipentaerythritol Pentaacrylate, the third 5 parts of glycerol triacrylate of oxidation, 2- methyl-1,3-
5 parts of propylene glycol diacrylate, ethyl -1 2- butyl -2-, 5 parts of 3-propanediol diacrylate, ethyleneglycol dimethacrylate
5 parts of ester, compatilizer: copolymer-maleic anhydride grafted ethene -0.5 part of acrylate copolymer, photoinitiator: benzophenone 2
Part, 2 parts of dimethoxybenzoin.
Embodiment 3,
Digital light polymer-ceramic material, the raw material including following parts by weight: ceramic base material: 25 parts of SiO 2 powder, cubic oxygen
Change 10 parts of zirconium polycrystalline ceramics powder, 10 parts of silicon nitride ceramic powder, 10 parts of aluminium nitride powder, 10 parts of boron nitride ceramics powder, gathers
5 parts of tetrafluoroethene, covering material: 0.5 part of epoxy resin, 0.5 part of methyl methacrylate, light-cured resin: tristane
10 parts of Dimethanol Diacrylate, 10 parts of Dipentaerythritol Pentaacrylate, the third 5 parts of glycerol triacrylate of oxidation, 2- first
Base -1,10 parts of 3-propanediol diacrylate, ethyl -1 2- butyl -2-, 10 parts of 3-propanediol diacrylate, compatilizer:
5 parts of ethylene glycol dimethacrylate, copolymer-maleic anhydride grafted ethene -0.2 part of acrylate copolymer, photoinitiator:
2 parts of benzophenone, 2 parts of dimethoxybenzoin.
The preparation method of embodiment 1-3:
Ceramic base material and polytetrafluoroethylene (PTFE) are put into planetary ball mill by S1, and ball milling 30-60min obtains mixing ceramic base material；
Covering material and compatilizer are put into batch mixer by S2, and after mixing evenly, point 5 batches are put into mixing ceramic base material, temperature
Degree is 20-60 DEG C, mixing 30-60min；
S3 will enter light-cured resin into batch mixer, under nitrogen protection, after mixing is uniform, add photoinitiator, mixing
Product is kept in dark place 2-3h.
Compare 1 ceramic base material: 25 parts of SiO 2 powder, 10 parts of tetragonal zirconia polycrystal ceramic powders, silicon nitride pottery
10 parts of porcelain powder, 10 parts of aluminium nitride powder, 10 parts of boron nitride ceramics powder, 5 parts of polytetrafluoroethylene (PTFE), solidified resin: tristane
10 parts of Dimethanol Diacrylate, 10 parts of Dipentaerythritol Pentaacrylate, the third 5 parts of glycerol triacrylate of oxidation, 2- first
Base -1,10 parts of 3-propanediol diacrylate, ethyl -1 2- butyl -2-, 10 parts of 3-propanediol diacrylate, compatilizer:
5 parts of ethylene glycol dimethacrylate, copolymer-maleic anhydride grafted ethene -0.2 part of acrylate copolymer, photoinitiator:
2 parts of benzophenone, 2 parts of dimethoxybenzoin are mixed.
Digital light polymer-ceramic material made from above-described embodiment 1-3 and comparative example 1 carries out fluidity testing and quiet
Diaphragm density measurement is measured after setting 2 days, the result of test is classified as table:
Table 1,
| Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| mPa·s | 121 | 145 | 161 | 136 |
| Diaphragm density g/cm3 | 3.15 | 3.43 | 3.21 | 3.5 |
| Diaphragm appearance | Diaphragm irregular colour | Disperse excellent | Disperse excellent | Disperse excellent |
Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.The present invention is described in detail above, its object is to allow
The personage for being familiar with this field technology can understand the contents of the present invention and be implemented, and protection of the invention can not be limited with this
Range, and the invention is not restricted to the embodiments described, equivalent change or modification made by all Spirit Essences according to the present invention, all
It is covered by the protection scope of the present invention.
Claims (7)
1. digital light polymer-ceramic material, which is characterized in that the raw material including following parts by weight: 45-65 parts of ceramic base material gathers
1-5 parts of tetrafluoroethene, 1-2 parts of covering material, 25-50 parts of light-cured resin, 0.2-0.5 parts of compatilizer, photoinitiator 1-4
Part.
2. the digital light polymer-ceramic material according to claim 1, which is characterized in that the ceramic base material is titanium dioxide
Si powder, tetragonal zirconia polycrystal ceramic powders, silicon nitride ceramic powder, aluminium nitride powder, boron nitride ceramics powder, the pottery
Porcelain substrate partial size is 0-200nm.
3. the digital light polymer-ceramic material according to claim 1, which is characterized in that the covering material is asphalt mixtures modified by epoxy resin
Rouge, methyl methacrylate.
4. digital light polymer-ceramic material according to claim 1, which is characterized in that the light-cured resin is acrylic acid
Esters include Tricyclodecane Dimethanol diacrylate, and Dipentaerythritol Pentaacrylate, third aoxidizes glycerol triacrylate,
2- methyl-1,3-propanediol diacrylate, ethyl -1 2- butyl -2-, 3-propanediol diacrylate, ethylene glycol dimethyl
Acrylate, trimethylolpropane trimethacrylate, trimethylol-propane trimethacrylate, three acrylic acid of pentaerythrite
Ester, 1,6- hexanediyl ester, dipropylene glycol diacrylate, double Glycerin tetraacrylates, aliphatic propylene
Acid esters, urethane acrylate, the one or more of epoxy acrylate.
5. digital light polymer-ceramic material according to claim 1, which is characterized in that the photoinitiator is 2- hydroxyl-
One or more of 2- methyl-1-phenyl-1- acetone, benzophenone, dimethoxybenzoin, chlorinated diphenyl ketone.
6. digital light polymer-ceramic material according to claim 1, which is characterized in that the compatilizer is total for maleic anhydride
Polymers grafted ethene-vinyl acetate copolymer, copolymer-maleic anhydride grafted ethene-acrylate copolymer, maleic acid
At least one of acid anhydride graft polypropylene.
7. the preparation method of digital light polymer-ceramic material described in -6 any one according to claim 1, which is characterized in that including
Following steps:
Ceramic base material and polytetrafluoroethylene (PTFE) are put into planetary ball mill by S1, and ball milling 30-60min obtains mixing ceramic base material；
Covering material and compatilizer are put into batch mixer by S2, and after mixing evenly, point 5 batches are put into mixing ceramic base material, temperature
It is 20-60 DEG C, mixing 30-60min；
S3 will enter light-cured resin into batch mixer, under nitrogen protection, after mixing is uniform, add photoinitiator, mixing
Product is kept in dark place 2-3h.
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