CN109485381A - The method that a kind of ceramic slurry of high fluidity and 3D printing prepare ceramic mold - Google Patents
The method that a kind of ceramic slurry of high fluidity and 3D printing prepare ceramic mold Download PDFInfo
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Abstract
The present invention relates to ceramic 3D printing technique fields, a kind of method that ceramic slurry and 3D printing more particularly to high fluidity prepare ceramic mold, ceramic slurry includes nano ceramic powder, binder, light curing agent, photoinitiator, dispersing agent, more particles and solvent, wherein nano ceramic powder is the mixture that albite in powder, kaolin powder, alumina powder and zirconia powder 35~40:11 in mass ratio~16:19~23:15~17 are formed, binder is the amylose water solution of concentration 5wt%~7wt%, and more particles are MgSi particle.Realize that green body is fully cured using the ultraviolet light of two kinds of intensities of illumination, organic matter is discharged through 700~800 DEG C of calcinings, 1110~1150 DEG C melt MgSi particle sufficiently, it is warming up to 1500~1600 DEG C of calcinings, it decomposes polysiloxanes and generates SiC network structure, and blended with the MgSi phase of melting, it is densified inside mold after cooling, improves the intensity of calcined ceramic mold.
Description
Technical field
The present invention relates to ceramic 3D printing technique fields, and in particular to a kind of ceramic slurry and 3D printing system of high fluidity
The method of standby ceramics mold.
Background technique
3D printing technique is also referred to as increases material manufacturing technology or rapid shaping technique, is based on three-dimensional mathematical model data, passes through
The physical layer of practice is superimposed, and increases material successively to generate 3D solid.3D printing has compared with traditional materials processing technology
There is following advantage: (1) digitizing product structure by modeling software, realizes Digitized manufacturing；(2) it can be manufactured in principle
The structure of any complexity out fundamentally solves the conventionally manufactured defect for being limited by mold；(3) " from below to up " push away long-pending mode
Be conducive to the non-manufacture for causing material, functionally gradient device；(4) it may be implemented to customize manufacture.By above-mentioned advantage, in recent years
3D printing technique is fast-developing, obtains in fields such as product prototype, mold manufacture, jewelry manufacture, automobile, space flight and medical industries
It is widely applied, and there is huge development potentiality.Ceramics be in people's daily life and industry in relatively common article, it is main
If being kneaded, forming and calcining each of material obtained by crushing using natural clay and various natural minerals as primary raw material
Kind product.The production technology of ceramic tradition is complex, can only prepare simple three-dimensional ceramic product, and energy consumption and resource disappear
Loss-rate is larger, and fabrication cycle is long.It is existing that 3D printing technique is applied to the standby research of ceramic system.3D printing ceramics mainly will pottery
Porcelain powder, binder and additive are mixed and made into ceramic ink according to a certain percentage, are subsequently placed in 3D printing equipment and are printed as
Type, then through high-temperature calcination and etc. ceramics are made, there is high-precision, high-intensitive characteristic.And it is applied to the ceramics of 3D printing
Slurry or ceramic ink should have good mobility and low caking property, so that slurry is easy to spray from 3D printing equipment.
But existing ceramic slurry adds organic resinoid bond, the caking property glue of slurry is big, and mobility is low, and slurry is easy blocking
Nozzle, while curing rate is slow after slurry ejection, ceramics, which are easy to appear, to be collapsed, and organic binder is during later period ceramic roasting
Volatilization is decomposed, causes ceramic hole big, influences the intensity of ceramics.Chinese patent CN20161097803, a kind of ceramic base 3D printing
Material and preparation method thereof on November 8 2016 date of application, is disclosed by modified Nano ceramic powders, organic silicone oil, poly- third
Acrylamide, chitosan, graphene, nano aluminium oxide, salicylate ultraviolet absorbent, phenolic resin, calcium carbonate mixing system
Standby 3D printing ceramic slurry, wherein phenolic resin is binder, and after shaping through ultraviolet photo-curing, but phenolic resin
The higher mobility that will affect ceramic slurry of viscosity, while phenolic resin can go out lower decompose in high-temperature calcination and cause ceramic inner hole
Gap is larger, influences ceramics strength, and ceramics have certain thickness, and ceramic interior UV curing rate is slow.
Summary of the invention
Ceramic slurry mobility it is low, it is sticky high and aiming at the problem that influence printing shaping, it is an object of the invention to mention
For a kind of ceramic slurry of high fluidity, sticky low, the good fluidity of ceramic slurry, while the curing rate after printing shaping
Fastly, the structure of the ceramics after high-temperature calcination is finer and close, and ceramics strength is high.
Another object of the present invention is to provide prepare ceramic mold by the ceramic slurry 3D printing of above-mentioned high fluidity
Method.
The present invention provides the following technical solution:
A kind of ceramic slurry of high fluidity, including following parts by weight component: 60~80 parts of nano ceramic powder, binder 1.8
~2.6 parts, 3~5 parts of light curing agent, 0.03~0.08 part of photoinitiator, 0.3~0.6 part of dispersing agent, more particles 8~12
Part and 100 parts of solvent, wherein nano ceramic powder be albite in powder, kaolin powder, alumina powder and zirconia powder in mass ratio
The mixture that 35~40:11~16:19~23:15~17 is formed, binder are that the amylose of concentration 5wt%~7wt% is water-soluble
Liquid.
As an improvement of the present invention, solvent is ether solution, the aqueous acetone solution, ethanol water of 80wt%~90wt%
One of solution and dimethylformamide in water.
As an improvement of the present invention, light curing agent is to introduce light-initiated group modified polysiloxanes, light on side chain
Initiation group is one of vinyl ether, allyl, cyano, fluoroalkyl and styryl or a variety of.
As an improvement of the present invention, polysiloxanes is siloxanes phosphate, cyclomethicone and polymethyl-benzene base
One of siloxanes.
As an improvement of the present invention, photoinitiator is diaryl iodonium salt, 2,4,6- trimethyl benzoyl diphenyls
At least two in bis- (lignocaine) Benzophenones of base phosphine oxide, 4,4'- and 2- isopropyl thioxanthone.
As an improvement of the present invention, more particles are MgSi particle, the partial size of more particles is respectively 30~
40 μm, 60~80 μm, 100~120 μm, 140~160 μm and 200~220 μm, the mass particle ratio of each particle size range is followed successively by
1:0.8~1.0:0.6~0.8:0.4~0.6:0.2~0.3.
As an improvement of the present invention, more particles use after following procedure is handled: by nanometer titanium dioxide, yin from
Sub- surfactant, defoaming agent and water are uniformly mixed, and more particles are added in redisperse, are spray-dried after ultrasonic disperse, more
Diameter particle, nanometer titanium dioxide, anionic surfactant, defoaming agent and water quality ratio are followed successively by 1:2~3:0.1~0.3:0.1
~0.2:10.
As an improvement of the present invention, dispersing agent is sodium pyrophosphate, tertiary sodium phosphate, calgon, sorbierite alkyl
At least two in compound and lauryl sodium sulfate.
Ceramic slurry of the invention is by nano ceramic powder, binder, light curing agent, photoinitiator, dispersing agent, more partial sizes
Particle and solvent composition, by light curing agent solidifies under ultraviolet light after ceramic slurry printing shaping.Binder is concentration
The amylose water solution of 5wt%~7wt%, mobility with higher replace organic resin in the prior art, can be very big
Raising ceramic slurry mobility, reduce the viscosity of ceramic slurry.And amylose can carbonize after high temperature sintering,
The hole generated inside ceramics is small.Zirconium oxide and aluminium oxide in nano ceramic powder can provide ceramics higher intensity.
Selection side chain introduces the polysiloxanes of light-initiated group as light curing agent, and curing rate is fast under photoinitiator effect, ceramics
Green body curing molding effect is good, while polysiloxanes cracks in green body high-temperature sintering process and forms SiC network structure, greatly
Enhance the intensity of ceramics.And siloxanes phosphate, cyclomethicone and the polymethylphenylsiloxane selected have well
Surface lubrication effect, the mobility of ceramic slurry can be further enhanced.More particle size ranges are set in ceramic slurry
MgSi particle, the MgSi particle of these different-grain diameters can increase the intracorporal hole of ceramic blank in forming process, make ceramic blank
Body internally forms continuous ultraviolet optical channel from surface, accelerates the curing rate inside ceramic body, while these MgSi
Son is improved through anionic surfactant, nanometer titanium dioxide impregnation rear surface lubricity and whiteness, is on the one hand improved
On the other hand the mobility of ceramic slurry can increase the ultraviolet light diffusing scattering effect inside ceramic body, accelerate internal curing.
MgSi particle is melted when high temperature sintering temperature reaches 1100 DEG C or so, refills the gap between particle, and with it is poly-
The SiC network structure that siloxanes is formed mutually blends, and makes ceramic body inside solid after cooling, enhances the intensity of ceramics.It selects
Solvent be high concentration ether solution, aqueous acetone solution, ethanol water or dimethylformamide in water, evaporation rate
Fastly, it is evaporated rapidly in the Light Curing of ceramic body, accelerates curing proceeding.And it selects at least two photoinitiators and divides
Powder mixing is added in ceramic slurry, and the wave-length coverage that compound photoinitiator absorbs is wide, and it is fast to cause cured speed, addition
The good dispersion of the ceramic slurry of compound dispersing agent, system are more uniform.Ceramic slurry of the invention flowing with higher
Property and lesser caking property, while the forming and hardening speed of obtained ceramic body is fast, and ceramics after high temperature sintering
Compact structure, ceramics strength are high.
The method that the ceramic slurry 3D printing of above-mentioned high fluidity prepares ceramic mold, comprising the following steps:
(1) after ceramic powders, light curing agent, photoinitiator, more particles and dispersing agent being added into solvent under stirring condition
It stirs evenly, adds binder and stir to get uniform ceramic slurry；
(2) ceramic slurry is sprayed into sizing material forming through 3D printer and obtains green body, apply 320~400nm of wavelength in print procedure
Ultraviolet light, intensity of illumination be 8~10mw/cm2, kept for 35~40 DEG C of printing environment；
(3) molding green body 10~12s of rotary irradiation in 320~400nm ultraviolet light, 15~20mw/cm of intensity of illumination2；
(4) green body is put into sintering furnace, 700~800 DEG C of 6~12h of calcining under nitrogen atmosphere, then 5 DEG C/min rate heats up
To 1110~1150 DEG C of 3~4h of calcining, then 1 DEG C/min is warming up to cooling the ceramic blank afterwards of 1500~1600 DEG C of calcinings 20~for 24 hours
Tire.
The method of the present invention irradiates green body in forming process and after molding using the ultraviolet light of two kinds of intensities of illumination respectively, real
Existing green body is fully cured, then through 700~800 DEG C of calcinings discharge organic matters, after make MgSi particle at 1110~1150 DEG C
Sufficiently melting fills the gap inside green body, then heats to 1500~1600 DEG C of calcinings, decomposes polysiloxanes and generates SiC
Network structure, and blended with the MgSi phase of melting, it is densified inside green body after cooling, improves the strong of calcined ceramic mold
Degree.
Beneficial effects of the present invention are as follows:
Ceramic slurry of the invention selects amylose solution as binder, and the mobility of slurry is high, caking property is low, contains light
The polysiloxanes of initiation group rapid curing under the action of photoinitiator, the curing molding speed of ceramic body is fast, through MgSi
After particle forms continuous ultraviolet optical channel inside ceramic body, shaping speed is accelerated, while the MgSi and poly- silicon oxygen melted
The SiC network structure that alkane is decomposed to form mutually blends, and ceramic mold inside solid degree is high, and ceramics strength is high, to make this hair
It is bright that a kind of ceramic slurry of high fluidity is provided, and the structure of ceramics prepared therefrom is finer and close, intensity is high.
Specific embodiment
A specific embodiment of the invention is described further below.
Unless otherwise instructed, raw material employed in the present invention is commercially available or commonly used in the art, such as
Without special instruction, the method in following embodiments is the conventional method of this field.
Embodiment 1
A kind of ceramic slurry of high fluidity, including following component: the amylose water of nano ceramic powder 60g, concentration 5wt%
The ether solution of solution 1.8g, light curing agent 3g, photoinitiator 0.03g, dispersing agent 0.3g, MgSi particle 8g and 80wt%
100g, wherein nano ceramic powder by nanoscale albite in powder, kaolin powder, alumina powder and zirconia powder in mass ratio
35:11:19:15 composition, light curing agent are the siloxanes phosphate that vinyl ether is introduced on side chain, and photoinitiator is Diaryl iodonium
The mixture of salt and 2,4,6-trimethylbenzoyldiphenylphosphine oxide, the partial size of MgSi particle is respectively 30~40 μm,
60~80 μm, 100~120 μm, 140~160 μm and 200~220 μm, the mass particle ratio of each particle size range is followed successively by 1:0.8:
0.6:0.4:0.2, dispersing agent are the mixture of sodium pyrophosphate and sorbierite alkylates.
The method that above-mentioned ceramic slurry 3D printing prepares ceramic mold, comprising the following steps:
(1) after ceramic powders, light curing agent, photoinitiator, more particles and dispersing agent being added into solvent under stirring condition
It stirs evenly, adds binder and stir to get uniform ceramic slurry；
(2) ceramic slurry is sprayed into sizing material forming through 3D printer and obtains green body, apply the ultraviolet of wavelength 320nm in print procedure
Light irradiation, intensity of illumination 8mw/cm2, kept for 35 DEG C of printing environment；
(3) molding green body rotary irradiation 10s in 320nm ultraviolet light, intensity of illumination 15mw/cm2；
(4) green body is put into sintering furnace, the lower 700 DEG C of calcinings 6h of nitrogen atmosphere, then 5 DEG C/min rate is warming up to 1120 DEG C and forges
3h is burnt, then 1 DEG C/min is warming up to cool down after 1500 DEG C of calcining 20h and obtains ceramic mold.
The viscosity of above-mentioned ceramic slurry is 18.5cP, and the Vickers hardness of the ceramic mold of gained is 19.3GPa, fracture after calcining
Toughness is 4.1MPam1/2。
Embodiment 2
The method that a kind of ceramic slurry of high fluidity and 3D printing prepare ceramic mold, the difference with embodiment 1, MgSi
Particle uses after following procedure is handled: nanometer titanium dioxide, anionic surfactant, defoaming agent and water is uniformly mixed, then
MgSi particle is added in dispersion, and ultrasonic disperse is uniformly spray-dried afterwards, MgSi particle, nanometer titanium dioxide, anionic surfactant,
The mass ratio of defoaming agent and water is followed successively by 1:2:0.1:0.1:10.
The viscosity of above-mentioned ceramic slurry is 17.6cP, and the Vickers hardness of the ceramic mold of gained is 19.4GPa, fracture after calcining
Toughness is 4.2MPam1/2。
Embodiment 3
A kind of ceramic slurry of high fluidity, including following component: the amylose water of nano ceramic powder 70g, concentration 6wt%
The ether solution of solution 2.2g, light curing agent 4g, photoinitiator 0.055g, dispersing agent 0.45g, MgSi particle 10g and 85wt%
100g, wherein nano ceramic powder by nanoscale albite in powder, kaolin powder, alumina powder and zirconia powder in mass ratio
37:13:21:16 composition, light curing agent are the cyclomethicone that allyl is introduced on side chain, and photoinitiator is Diaryl iodonium
Salt and 4, the mixture of bis- (lignocaine) Benzophenones of 4'-, the partial size of MgSi particle is respectively 30~40 μm, 60~80 μm, 100
~120 μm, 140~160 μm and 200~220 μm, the mass particle ratio of each particle size range is followed successively by 1:0.9:0.7:0.5:
0.25, dispersing agent is the mixture of sodium pyrophosphate and lauryl sodium sulfate.
The method that above-mentioned ceramic slurry 3D printing prepares ceramic mold, comprising the following steps:
(1) after ceramic powders, light curing agent, photoinitiator, more particles and dispersing agent being added into solvent under stirring condition
It stirs evenly, adds binder and stir to get uniform ceramic slurry；
(2) ceramic slurry is sprayed into sizing material forming through 3D printer and obtains green body, apply the ultraviolet of wavelength 365nm in print procedure
Light irradiation, intensity of illumination 9mw/cm2, kept for 38 DEG C of printing environment；
(3) molding green body rotary irradiation 11s in 365nm ultraviolet light, intensity of illumination 17mw/cm2；
(4) green body is put into sintering furnace, the lower 750 DEG C of calcinings 9h of nitrogen atmosphere, then 5 DEG C/min rate is warming up to 1130 DEG C and forges
3.5h is burnt, then 1 DEG C/min is warming up to cool down after 1550 DEG C of calcining 22h and obtains ceramic mold.
The viscosity of above-mentioned ceramic slurry is 19.7cP, and the Vickers hardness of the ceramic mold of gained is 19.7GPa, fracture after calcining
Toughness is 4.5MPam1/2。
Embodiment 4
The method that a kind of ceramic slurry of high fluidity and 3D printing prepare ceramic mold, the difference with embodiment 3, MgSi
Particle uses after following procedure is handled: nanometer titanium dioxide, anionic surfactant, defoaming agent and water is uniformly mixed, then
MgSi particle is added in dispersion, and ultrasonic disperse is uniformly spray-dried afterwards, MgSi particle, nanometer titanium dioxide, anionic surfactant,
The mass ratio of defoaming agent and water is followed successively by 1:2.5:0.2:0.15:10.
The viscosity of above-mentioned ceramic slurry is 18.9cP, and the Vickers hardness of the ceramic mold of gained is 19.9GPa, fracture after calcining
Toughness is 4.6MPam1/2。
Embodiment 5
A kind of ceramic slurry of high fluidity, including following component: the amylose water of nano ceramic powder 80g, concentration 7wt%
Solution 2.6g, light curing agent 5g, photoinitiator 0.08g, dispersing agent 0.6g, MgSi particle 12g and 90wt% ether solution,
100g, wherein nano ceramic powder by nanoscale albite in powder, kaolin powder, alumina powder and zirconia powder in mass ratio
40:16:23:17 composition, light curing agent are the polymethylphenylsiloxane that fluoroalkyl is introduced on side chain, and photoinitiator is two virtues
The mixture of base salt compounded of iodine and 2- isopropyl thioxanthone, the partial size of MgSi particle are respectively 30~40 μm, 60~80 μm, 100
~120 μm, 140~160 μm and 200~220 μm, the mass particle ratio of each particle size range is followed successively by 1:1.0:0.8:0.6:0.3,
Dispersing agent is the mixture of sorbierite alkylates and lauryl sodium sulfate.
The method that above-mentioned ceramic slurry 3D printing prepares ceramic mold, comprising the following steps:
(1) after ceramic powders, light curing agent, photoinitiator, more particles and dispersing agent being added into solvent under stirring condition
It stirs evenly, adds binder and stir to get uniform ceramic slurry；
(2) ceramic slurry is sprayed into sizing material forming through 3D printer and obtains green body, apply the ultraviolet of wavelength 400nm in print procedure
Light irradiation, intensity of illumination 10mw/cm2, kept for 40 DEG C of printing environment；
(3) molding green body rotary irradiation 12s in 400nm ultraviolet light, intensity of illumination 20mw/cm2；
(4) green body is put into sintering furnace, the lower 800 DEG C of calcinings 12h of nitrogen atmosphere, then 5 DEG C/min rate is warming up to 1150 DEG C
Calcine 4h, then 1 DEG C/min be warming up to 1600 DEG C calcining for 24 hours afterwards cooling obtain ceramic mold.
The viscosity of above-mentioned ceramic slurry is 20.8cP, and the Vickers hardness of the ceramic mold of gained is 20.2GPa, fracture after calcining
Toughness is 4.8MPam1/2。
Embodiment 6
The method that a kind of ceramic slurry of high fluidity and 3D printing prepare ceramic mold, the difference with embodiment 5, MgSi
Particle uses after following procedure is handled: nanometer titanium dioxide, anionic surfactant, defoaming agent and water is uniformly mixed, then
Dispersion be added MgSi particle, ultrasonic disperse uniformly after evaporation drying, MgSi particle, nanometer titanium dioxide, anionic surfactant,
Ultrasonic disperse is uniform after the mass ratio of defoaming agent and water is followed successively by 1:3:0.3:0.2:10 mixing, is then spray-dried.
The viscosity of above-mentioned ceramic slurry is 20.1cP, and the Vickers hardness of the ceramic mold of gained is 20.3GPa, fracture after calcining
Toughness is 4.9MPam1/2。
It should be noted that in above-described embodiment 1~6 and being not limited to the above embodiments, solvent for use can be with 80wt%
One of aqueous acetone solution, ethanol water and dimethylformamide in water of~90wt% introduce on polysiloxanes side chain
Light-initiated group can also be one of cyano and styryl or vinyl ether, allyl, cyano, styryl with
Two or more functional groups in fluoroalkyl, photoinitiator can be 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 4,4'-
Two kinds of mixing or diaryl iodonium salt, 2,4,6- trimethyl in bis- (lignocaine) Benzophenones and 2- isopropyl thioxanthone
Three kinds or more in bis- (lignocaine) Benzophenones of benzoyl diphenyl phosphine oxide, 4,4'- and 2- isopropyl thioxanthone
Mixing, dispersing agent be sodium pyrophosphate, tertiary sodium phosphate, calgon, sorbierite alkylates and lauryl sodium sulfate in
At least two.
Claims (9)
1. a kind of ceramic slurry of high fluidity, which is characterized in that ceramic slurry includes the following parts by weight: nano ceramics
60~80 parts of powder, 1.8~2.6 parts of binder, 3~5 parts of light curing agent, 0.03~0.08 part of photoinitiator, dispersing agent 0.3~
0.6 part, 8~12 parts of more particles and 100 parts of solvent, wherein nano ceramic powder is nanoscale albite in powder, kaolin
The mixture of powder, alumina powder and zirconia powder 35~40:11 in mass ratio~16:19~23:15~17 composition, binder are
The amylose water solution of concentration 5wt%~7wt%.
2. ceramic slurry according to claim 1, which is characterized in that solvent be 80wt%~90wt% ether solution,
One of aqueous acetone solution, ethanol water and dimethylformamide in water.
3. ceramic slurry according to claim 1 or 2, which is characterized in that light curing agent is to introduce light-initiated base on side chain
The modified polysiloxanes of group, light-initiated group be one of vinyl ether, allyl, cyano, fluoroalkyl and styryl or
It is a variety of.
4. ceramic slurry according to claim 3, which is characterized in that polysiloxanes is siloxanes phosphate, cyclohexyl methyl silicon
One of oxygen alkane and polymethylphenylsiloxane.
5. ceramic slurry according to claim 1 or 2, which is characterized in that photoinitiator is diaryl iodonium salt, 2,4,6-
In bis- (lignocaine) Benzophenones of trimethyl benzoyl diphenyl base phosphine oxide, 4,4'- and 2- isopropyl thioxanthone at least
Two kinds.
6. ceramic slurry according to claim 1 or 2, which is characterized in that more particles are MgSi particle, more partial size grains
The partial size of son is respectively 30~40 μm, 60~80 μm, 100~120 μm, 140~160 μm and 200~220 μm, each particle size range
Mass particle ratio be followed successively by 1:0.8~1.0:0.6~0.8:0.4~0.6:0.2~0.3.
7. ceramic slurry according to claim 6, which is characterized in that more particles use after following procedure is handled:
Nanometer titanium dioxide, anionic surfactant, defoaming agent and water are uniformly mixed, more particles, ultrasound point is added in redisperse
Spray drying after dissipating uniformly, more particles, nanometer titanium dioxide, anionic surfactant, defoaming agent and water mass ratio according to
Secondary is 1:2~3:0.1~0.3:0.1~0.2:10.
8. ceramic slurry according to claim 1 or 2, which is characterized in that dispersing agent is sodium pyrophosphate, tertiary sodium phosphate, six
At least two in sodium metaphosphate, sorbierite alkylates and lauryl sodium sulfate.
9. the method that the ceramic slurry 3D printing as described in claim 1~8 prepares ceramic mold, comprising the following steps:
(1) nano ceramic powder, light curing agent, photoinitiator, more particles and dispersion is added under stirring condition into solvent
It is stirred evenly after agent, adds binder and stir to get uniform ceramic slurry；
(2) ceramic slurry is sprayed into molding through 3D printer and obtains green body, in print procedure to green body apply wavelength 320~
The ultraviolet light of 400nm, intensity of illumination are 8~10mw/cm2, kept for 35~40 DEG C of printing environment；
(3) molding green body 10~12s of rotary irradiation in 320~400nm ultraviolet light, 15~20mw/cm of intensity of illumination2；
(4) green body is put into sintering furnace, 700~800 DEG C of 6~12h of calcining, are warming up under nitrogen atmosphere with 5 DEG C/min rate
1120~1150 DEG C of 3~4h of calcining, then 1 DEG C/min are warming up to 1500~1600 DEG C of calcinings 20~for 24 hours, then cooling ceramic blank
Tire.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171952A (en) * | 2019-04-30 | 2019-08-27 | 广西陶匠智能科技有限公司 | A kind of clay formula that can improve Nixing pottery 3D printing speed |
| CN110668812A (en) * | 2019-09-18 | 2020-01-10 | 苏州炻原新材料科技有限公司 | Nano zirconium oxide spraying powder and preparation method thereof |
| CN111039680A (en) * | 2019-12-26 | 2020-04-21 | 西安铂力特增材技术股份有限公司 | Forming method of silicon-containing ceramic part |
| CN112321314A (en) * | 2020-11-18 | 2021-02-05 | 韩山师范学院 | Powder material and preparation method and application thereof |
| CN115252884A (en) * | 2022-07-11 | 2022-11-01 | 湖北工业大学 | Powder composition and application thereof in preparation of pet wound powder dressing |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100029801A1 (en) * | 2008-07-30 | 2010-02-04 | Ivoclar Vivadent Ag | Light-curing slips for the stereolithographic preparation of dental ceramics |
| CN105566860A (en) * | 2015-12-11 | 2016-05-11 | 上海联泰科技股份有限公司 | Ceramic material for 3D (three-dimensional) light curing forming printing and preparation method thereof |
| CN106396620A (en) * | 2016-09-07 | 2017-02-15 | 济南大学 | Preparation of rapid prototyping black pottery powder material used for 3DP (three-dimensional printing) process |
| CN106563763A (en) * | 2016-10-31 | 2017-04-19 | 宁夏共享模具有限公司 | Granular material used for 3D printing and casting model for 3D printing |
| CN106810215A (en) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | A kind of preparation of ceramic size and 3D printing Stereolithography method |
-
2018
- 2018-01-15 CN CN201810037031.2A patent/CN109485381A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100029801A1 (en) * | 2008-07-30 | 2010-02-04 | Ivoclar Vivadent Ag | Light-curing slips for the stereolithographic preparation of dental ceramics |
| CN105566860A (en) * | 2015-12-11 | 2016-05-11 | 上海联泰科技股份有限公司 | Ceramic material for 3D (three-dimensional) light curing forming printing and preparation method thereof |
| CN106396620A (en) * | 2016-09-07 | 2017-02-15 | 济南大学 | Preparation of rapid prototyping black pottery powder material used for 3DP (three-dimensional printing) process |
| CN106563763A (en) * | 2016-10-31 | 2017-04-19 | 宁夏共享模具有限公司 | Granular material used for 3D printing and casting model for 3D printing |
| CN106810215A (en) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | A kind of preparation of ceramic size and 3D printing Stereolithography method |
Non-Patent Citations (2)
| Title |
|---|
| 张旭之等: "《乙烯衍生物工学》", 31 July 1995, 北京：化学工业出版社 * |
| 王生杰等: "紫外光固化聚硅氧烷", 《化学通报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171952A (en) * | 2019-04-30 | 2019-08-27 | 广西陶匠智能科技有限公司 | A kind of clay formula that can improve Nixing pottery 3D printing speed |
| CN110668812A (en) * | 2019-09-18 | 2020-01-10 | 苏州炻原新材料科技有限公司 | Nano zirconium oxide spraying powder and preparation method thereof |
| CN110668813A (en) * | 2019-09-18 | 2020-01-10 | 苏州炻原新材料科技有限公司 | Preparation method of nano zirconia granulated powder |
| CN110845233A (en) * | 2019-09-18 | 2020-02-28 | 苏州炻原新材料科技有限公司 | Preparation method of superfine zirconia grinding ball |
| CN110668812B (en) * | 2019-09-18 | 2021-10-26 | 苏州炻原新材料科技有限公司 | Nano zirconium oxide spraying powder and preparation method thereof |
| CN111039680A (en) * | 2019-12-26 | 2020-04-21 | 西安铂力特增材技术股份有限公司 | Forming method of silicon-containing ceramic part |
| CN112321314A (en) * | 2020-11-18 | 2021-02-05 | 韩山师范学院 | Powder material and preparation method and application thereof |
| CN115252884A (en) * | 2022-07-11 | 2022-11-01 | 湖北工业大学 | Powder composition and application thereof in preparation of pet wound powder dressing |
| CN115252884B (en) * | 2022-07-11 | 2023-07-14 | 湖北工业大学 | Powder composition and application thereof in preparation of pet wound powder dressing |
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