CN105198449B - A kind of preparation method of the high ceramic of compact of Stereolithography - Google Patents
A kind of preparation method of the high ceramic of compact of Stereolithography Download PDFInfo
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- CN105198449B CN105198449B CN201510590675.0A CN201510590675A CN105198449B CN 105198449 B CN105198449 B CN 105198449B CN 201510590675 A CN201510590675 A CN 201510590675A CN 105198449 B CN105198449 B CN 105198449B
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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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The present invention relates to field of ceramic preparation technology, the preparation method of the high ceramic of compact of specially a kind of Stereolithography.Component and proportioning of the invention by optimizing slurry, slurry is applied to the 3D printing of complex-shaped high ceramic of compact shaped piece base substrate and prepare, without being especially tailored corresponding mould.And the base substrate for making high ceramic of compact is remained to when the solid content of the slurry of the present invention is less than 40vol%, the relative density of final obtained high ceramic of compact still may be up to more than 99%.Base substrate is dried using liquid drying mode so that the present invention is suitable to the base substrate for making complicated and accurate high ceramic of compact.The present invention carries out dumping using two step degreasing methods of vacuum/atmosphere protection dumping and air dumping, the defects of blank deformation, cracking, foaming can be reduced problem.For the relative density for the high ceramic of compact being prepared by the method for the present invention more than 90%, Vickers hardness is respectively less than 0.5wt% in more than 12GPa, residual carbon content.
Description
Technical field
The present invention relates to field of ceramic preparation technology, more particularly to a kind of preparation side of the high ceramic of compact of Stereolithography
Method.
Background technology
Special ceramic material is due to high intensity, high rigidity, corrosion-resistant, wear-resistant, chemical stability and bio-compatible
Property well wait excellent properties, obtained in fields such as the energy, aviation, machinery, chemical industry, electronics, semiconductor, medical science it is more and more should
With.When complicated technique outfit, making be present due to manufacturing complex-shaped accurate special cermacis with traditional ceramic process
Between it is long, cost of manufacture is high the problems such as, preparing special cermacis by traditional ceramic process can not keep up with now to special type
The growing research and development of ceramic product and use demand.Especially for high ceramic of compact, it has hardness height, chemical stability
Well, the advantages that high-temperature behavior is excellent, but shaping and processing of these advantages simultaneously to high ceramic of compact part bring very big be stranded
Disturb, particularly complex-shaped high ceramic of compact shaped piece, it usually needs it is molded using the mould of complexity, and complicated mould
Production cost and period is added, is unsuitable for the small lot production or experimental production of high ceramic of compact part.It is although international at present
On developed various new shaping method of ceramics, such as injection, curtain coating, gel injection-moulding, Direct Coagulation Casting etc., but nothing
By being these novel methods, or traditional slip casting, it is dry-pressing formed the methods of, can not all break away from system of the mould to ceramics manufacture
About.In addition, for high ceramic of compact part, in addition to the problem of blank forming, the drying process in traditional ceramic preparation technology
Base substrate can be made to produce larger deformation quantity, complex-shaped accurate ceramic shaped piece can not be made, binder removal can not also meet
Fire the requirement of high ceramic of compact.
In view of above-mentioned situation, the quick mould-free forming technology of the research and extension ceramic industry more backward to China as early as possible comes
It is imperative to say.3D printing technique used in the present invention is Stereolithography technology (Stereo lithography
Appearance, abridge SLA), its principle as shown in figure 1, by computer control laser beam be scanned in x-y faces, make pottery
Porcelain slurry selectivity solidifies, and forms individual layer section；Subsequent lifting platform declines a certain distance, and scraper is inswept, on cured layer
Uniformly one layer of ceramic slurry of coating, then the scanning in x-y faces is carried out, another layer cross section is formed, and bond together with preceding layer；Such as
This circulation, obtains photocuring ceramic body.
The content of the invention
The present invention is directed to need to first be made again with high ceramic of compact of the existing ceramic preparation manufacture with labyrinth
Miscellaneous mould, causes the problem of production cost is high and the production cycle is long, and is answered because the deformation quantity of base substrate is difficult to manufacture shape greatly
A kind of the problem of miscellaneous, accurate ceramics, there is provided the preparation method of high ceramic of compact with Stereolithography.
To achieve the above object, the present invention uses following technical solution：
S1 prepares slurry：Each component is weighed by following mass percent and is well mixed, 30-80% ceramic powders, 15-
65% premixed liquid, 0.01-2% light trigger, 0.04-3% dispersant, obtain slurry.
The premixed liquid is made up of organic solute and solvent, and the quality of the solvent is the 0-90% of the quality of premixed liquid；
The organic solute is acrylamide, N-N ' methylene-bisacrylamides, 1,6 hexanediol diacrylate and trihydroxy methyl third
At least one of alkane triacrylate.Preferably, organic solute by acrylamide and N-N ' methylene-bisacrylamides with matter
Amount compares 9-29：1 is combined.
Preferably, the quality of the solvent is the 60-90% of the quality of premixed liquid.
Preferably, solvent is at least one of deionized water, glycerine, absolute ethyl alcohol and acetone.It is it is furthermore preferred that described molten
Agent is made up of deionized water and glycerine, and the quality of glycerine is the 5-20% of the quality of premixed liquid.
Preferably, the ceramic powders are aluminum oxide, zirconium oxide, lead zirconate titanate, silicon nitride, aluminium nitride, carborundum, carbonization
At least one of boron, titanium carbonitride, titanium carbide, titanium oxide and silica.It is furthermore preferred that the average grain diameter of the ceramic powders
Less than or equal to 10 μm, the purity of ceramic powders is more than or equal to 99.9%.
The light trigger is 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxycyclohexyl phenyl ketones and 2- hydroxyls
At least one of base -4'- (2- hydroxy ethoxies) -2- methyl phenyl ketones.
The dispersant is at least one in ammonium citrate, polyvinylpyrrolidone, calgon and ammonium polyacrylate
Kind.
Preferably, it is described to prepare comprising the concrete steps that for slurry：Organic solute is well mixed with solvent first, forms premix
Liquid, dispersant is then added into premixed liquid and is well mixed, ceramic powders and ball milling 0.1- are then added into premixed liquid
50h, obtain just slurry；Followed by de-bubble technique：By first slurry be placed under subnormal ambient and stir just slurry 1-120min with except
Bubble is removed, light trigger is added in most backward centrotheca material and is well mixed, slurry is made.
S2 is molded：Slurry is placed in Stereolithography equipment, made by Stereolithography method (wavelength X≤405nm used)
It is standby go out base substrate.
Preferably, after Stereolithography legal system goes out base substrate, cleaning removes the uncured slurry of billet surface.
S3：Then, base substrate passes through the processing of S31 drying steps, S32 dumpings step and S33 sintering steps successively, and phase is made
It is more than or equal to 90% to density, Vickers hardness is more than or equal to 12GPa, and residual carbon content is less than or equal to 0.5wt% pottery
Porcelain.
Preferably, the S31 drying steps are：Base substrate is placed in liquid desiccant and dries 1-72h.Preferably, it is described
Liquid desiccant is the polyethylene glycol that molecular weight is 200-600.
Preferably, after body drying 1-72h, the liquid desiccant of billet surface is cleaned up with cleaning fluid；Specifically may be used
To be that the base substrate is placed in ethanol, cleaned with ultrasonic wave.Then with ultraviolet light base substrate to reinforce base substrate；Specifically can be with
It is that base substrate is placed under uviol lamp (λ≤405nm), with ultra violet lamp base substrate.
Preferably, the S32 dumpings step is：Vacuum dumping is first carried out to base substrate or atmosphere protection dumping is handled, then it is right
Base substrate carries out air dumping processing.
The heating rate of organic matter in base substrate can be reduced using vacuum dumping or atmosphere protection dumping, is gone out so as to reduce base substrate
The defects of now ftractureing, bubbling.It can be removed in base substrate by air dumping because vacuum dumping or atmosphere protection dumping are and the carbon that remains.
It is furthermore preferred that the condition of the vacuum dumping or atmosphere protection dumping is：Base substrate is placed in the draft glue discharging furnace of negative pressure
Or inert gas/N2In the draft glue discharging furnace of protection, it is warming up to 300-1000 DEG C with 0.1-10 DEG C/min speed and is incubated 2-6h, and
In temperature-rise period 0-60min is incubated every 50-150 DEG C；Then, base substrate is in the draft glue discharging furnace of negative pressure or inert gas/N2Protection
Draft glue discharging furnace in be cooled to room temperature.It is further preferred that the vacuum that the draft glue discharging furnace of the negative pressure refers in draft glue discharging furnace be more than or
Equal to 0.09MPa.
It is furthermore preferred that the condition of the air dumping is：Base substrate is placed in the draft glue discharging furnace of air atmosphere, with 1-10 DEG C/
Min speed is warming up to 400-700 DEG C and is incubated 0.5-10h；Then base substrate cools to room temperature with the furnace.It is further preferred that base
After body insulation 0.5-10h, it is warming up to 800-1100 DEG C with 2-15 DEG C/min speed and is incubated 10-60min, then base substrate is with stove
It is cooled to room temperature.
Preferably, the condition of the S33 sintering steps is：Base substrate is placed in sintering furnace, with 5-30 DEG C/min speed
It is warming up to 1200-2200 DEG C and is incubated 1-8h, ceramics is made.It is further preferred that base substrate is in air/N2/ inert gas atmosphere
Sintering furnace in sinter, or sintered in the sintering furnace of negative pressure.
Compared with prior art, the beneficial effects of the invention are as follows：Component and proportioning of the invention by optimizing slurry, make slurry
Material is prepared suitable for the 3D printing of complex-shaped high ceramic of compact shaped piece base substrate so for preparing high ceramic of compact shaped piece
During need not be especially tailored corresponding mould, reduce high ceramic of compact shaped piece production cost and generation the cycle.And
The base substrate for making high ceramic of compact is remained to when the solid content of the slurry of the present invention is less than 40vol%, it is final obtained high
The relative density of ceramic of compact still may be up to more than 99%, overcome in the prior art must use solid content 40vol% with
On slurry make the limitation of high ceramic of compact.Base substrate is dried using liquid drying mode, makes each equal to shrinking of base substrate
It is even, effectively reduce the deformation quantity of base substrate so that and the present invention is suitable to the base substrate for making complicated and accurate high ceramic of compact,
Solves the problems, such as the insurmountable blank deformation of traditional natural drying process.The present invention using vacuum/atmosphere protection dumping with
Two step degreasing methods of air dumping carry out dumping, can reduce base substrate due to a step degreasing heating rate is too fast or base substrate in it is organic
The defects of deforming, ftracture caused by thing heating rate is too fast, bubbling problem, and air is combined after vacuum/atmosphere protection dumping
Dumping, the carbon remained in base substrate by vacuum/atmosphere protection dumping can be discharged.The high ceramic of compact being prepared by the method for the present invention
Relative density more than 90%, Vickers hardness is respectively less than 0.5wt% in more than 12GPa, residual carbon content.
Brief description of the drawings
Fig. 1 is the operation principle schematic diagram of Stereolithography equipment；
Fig. 2 is the schematic diagram of the object construction of high dense product in each embodiment；
Fig. 3 is the base substrate after liquid drying process in embodiment 1；
Fig. 4 is high ceramic of compact finished figure prepared by embodiment 1；
Fig. 5 is the SEM figures of high ceramic of compact prepared by embodiment 1；
Fig. 6 is the base substrate after natural drying in comparative example 1.
Embodiment
In order to more fully understand the technology contents of the present invention, with reference to specific embodiment to technical scheme
It is described further and illustrates.
In following examples, before high ceramic of compact is made, base substrate is made in slurry especially by Stereolithography method
Before, the rapid shaping data for meeting object construction for Stereolithography equipment are produced according to prior art, and will be quick
Forming data file is imported in the control program of Stereolithography equipment, stand-by.Specifically：3D solid is carried out using software UG
Modeling, obtains ceramic shaped piece model；The model is imported into generation support in rapid shaping auxiliary software Magics and cut
Piece processing, rapid shaping data file is then exported, and rapid shaping data file is imported to the control of Stereolithography equipment
In program.The object construction of high ceramic of compact finished product prepared by following examples is that the length of side is 16mm, and a height of 5mm triangle is made pottery
There are the circular perforations of an a diameter of 4mm porcelain cutter, the centre of triangle sintex, and in the upper following table of triangle sintex
Face, three chip-breakers are provided with along outside, as shown in Figure 2.In other embodiments, can be according to the high dense product of reality
The corresponding rapid shaping data of structure fabrication, the structure of high dense product is not limited to the structure shown in following embodiments.
Using fine ceramics density and apparent porosity test method (national standard：GB/T 25995-2010) the following implementation of test
The relative density of high ceramic of compact prepared by example, using fine ceramics room temperature hardness test method (national standard：GB/T 16534-
2009) hardness of high ceramic of compact prepared by following examples is tested.
Embodiment 1
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
Premixed liquid processed：665g deionized waters and 160g glycerine are weighed respectively as solvent (account for premixed liquid quality 75%)；
247.5g acrylamides are weighed respectively and 27.5g N-N ' methylene-bisacrylamides (account for premixed liquid quality as organic solute
25%).Organic solute is well mixed with solvent, organic solute is all dissolved, obtains the slightly yellow transparent premixed liquids of 1100g.
Slurrying material：Take above-mentioned premixed liquid (38.85%), and weigh respectively 30g polyethylene pyrrole networks alkanone (dispersant,
1.06%), 1700g Alpha-aluminas (ceramic powders, 60%；Particle diameter≤0.2 μm, purity 99.99%), 1.5g 2- hydroxyls -2-
Methyl isophthalic acid-phenyl -1- acetone (light trigger 1173,0.05%).Add and dispersant and be well mixed into premixed liquid, then to
Ceramic powders and ball milling 8h are added in premixed liquid, obtains just slurry；First slurry is placed under subnormal ambient and stirs just slurry
30min adds light trigger to remove bubble, in most backward centrotheca material and stirred, and slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 400 and dries 48h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Through the dried base substrate of liquid as shown in figure 3, the structure of base substrate and
Size is consistent with object construction.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to add
Gu base substrate.Then, base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 600 DEG C with 2 DEG C/min speed and is incubated 4h, and 20min is incubated every 100 DEG C in temperature-rise period；Keep dumping
The vacuum of stove, base substrate are cooled to room temperature with draft glue discharging furnace.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 2 DEG C/min speed
To 600 DEG C and it is incubated 4h；Then 1000 DEG C are warming up to 15 DEG C/min speed again and are incubated 30min, then base substrate is cold with stove
But to room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of air atmosphere, 1650 DEG C is warming up to 15 DEG C/min speed and is incubated 1h, is made
Obtain high ceramic of compact.
The solid content of the slurry of the present embodiment is 30vol%, and the relative density of prepared high ceramic of compact is 99.5%,
Vickers hardness is 17.5GPa, residual carbon content 0.1wt%.Structure such as Fig. 4 institutes of high ceramic of compact manufactured in the present embodiment
Show, the structure snd size of high ceramic of compact are basically identical with object construction, and deformation quantity is very small, can be neglected, do not influence into
The quality of product.Shown in microstructure such as Fig. 5 (SEM figures) of high ceramic of compact manufactured in the present embodiment, crystal grain can be observed by Fig. 5
Size between 1-15 μm, the prepared ceramic porosity is very low.
Embodiment 2
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
Premixed liquid processed：930g deionized waters and 60g glycerine are weighed respectively as solvent (account for premixed liquid quality 90%)；Point
Also known as 104.5g acrylamides and 5.5g N-N ' methylene-bisacrylamides is taken (to account for premixed liquid quality as organic solute
10%).Organic solute is well mixed with solvent, organic solute is all dissolved, obtains the slightly yellow transparent premixed liquids of 1100g.
Slurrying material：Take above-mentioned premixed liquid (23.26%), and weigh respectively 100g ammonium citrates (dispersant, 2.1%),
3500g Alpha-aluminas (ceramic powders, 74%；Particle diameter≤0.5 μm, purity 99.99%), 30g 2- hydroxy-2-methyl -1- benzene
Base -1- acetone (light trigger 1173,0.63%).Dispersant is added into premixed liquid and is well mixed, then into premixed liquid
Ceramic powders and ball milling 48h are added, obtains just slurry；By first slurry be placed under subnormal ambient and stir just slurry 10min with except
Bubble is removed, light trigger is added in most backward centrotheca material and is stirred, slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 600 and dries 72h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Structure snd size and object construction through the dried base substrate of liquid
Unanimously.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to reinforce base substrate.Then, will
Base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 900 DEG C with 3 DEG C/min speed and is incubated 2h, and 10min is incubated every 100 DEG C in temperature-rise period；Keep dumping
The vacuum of stove, base substrate are cooled to room temperature with draft glue discharging furnace.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 3 DEG C/min speed
To 700 DEG C and it is incubated 2h；Then 1100 DEG C are warming up to 10 DEG C/min speed again and are incubated 10min, then base substrate is cold with stove
But to room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of air atmosphere, 1400 DEG C is warming up to 10 DEG C/min speed and is incubated 3h, is made
Obtain high ceramic of compact.
The relative density of high ceramic of compact prepared by the present embodiment is 99.7%, and Vickers hardness is 18.5GPa, remaining
Carbon content is 0.1wt%.The structure snd size and object construction of high ceramic of compact manufactured in the present embodiment are basically identical, deformation quantity
It is very small, it can be neglected, not influence the quality of finished product.
Embodiment 3
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
Premixed liquid processed：440g deionized waters and 220g glycerine are weighed respectively as solvent (account for premixed liquid quality 60%)；
425.3g acrylamides are weighed respectively and 14.7g N-N ' methylene-bisacrylamides (account for premixed liquid quality as organic solute
40%).Organic solute is well mixed with solvent, organic solute is all dissolved, obtains the slightly yellow transparent premixed liquids of 1100g.
Slurrying material：Take above-mentioned premixed liquid (59.46%), and weigh respectively 1g ammonium citrates (dispersant, 0.05%),
734g Alpha-aluminas (ceramic powders, 39.68%；Particle diameter≤0.1 μm, purity 99.99%), 15g 2- hydroxy-2-methyls -1-
Phenyl -1- acetone (light trigger 1173,0.81%).Dispersant is added into premixed liquid and is well mixed, then to premixed liquid
Middle addition ceramic powders and ball milling 3h, obtain just slurry；By first slurry be placed under subnormal ambient and stir just slurry 60min with except
Bubble is removed, light trigger is added in most backward centrotheca material and is stirred, slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 200 and dries 3h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Structure snd size and object construction through the dried base substrate of liquid
Unanimously.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to reinforce base substrate.Then, will
Base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 500 DEG C with 0.2 DEG C/min speed and is incubated 6h, and 60min is incubated every 100 DEG C in temperature-rise period；The row of holding
The vacuum of glue stove, base substrate are cooled to room temperature with draft glue discharging furnace.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 1 DEG C/min speed
To 400 DEG C and it is incubated 6h；Then 800 DEG C are warming up to 5 DEG C/min speed again and are incubated 60min, then base substrate furnace cooling
To room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of air atmosphere, 1700 DEG C is warming up to 5 DEG C/min speed and is incubated 1h, is made
High ceramic of compact.
The relative density of high ceramic of compact prepared by the present embodiment is 96.2%, and Vickers hardness is 16.3GPa, remaining
Carbon content is 0.3wt%.The structure snd size and object construction of high ceramic of compact manufactured in the present embodiment are basically identical, deformation quantity
It is very small, it can be neglected, not influence the quality of finished product.
Embodiment 4
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
Premixed liquid processed：528g deionized waters and 132g glycerine are weighed respectively as solvent (account for premixed liquid quality 60%)；
396g acrylamides are weighed respectively and 44g N-N ' methylene-bisacrylamides (account for premixed liquid quality as organic solute
40%).Organic solute is well mixed with solvent, organic solute is all dissolved, obtains the slightly yellow transparent premixed liquids of 1100g.
Slurrying material：Take above-mentioned premixed liquid (65%), and weigh respectively 0.68g ammonium citrates (dispersant, 0.04%),
591g Alpha-aluminas (ceramic powders, 34.95%；Particle diameter≤0.1 μm, purity 99.99%), 0.17g 2- hydroxyl -4'- (2-
Hydroxy ethoxy) -2- methyl phenyl ketones (light trigger 2959,0.01%).Dispersant is added into premixed liquid and is well mixed, is connect
And ceramic powders and ball milling 1h are added into premixed liquid, obtain just slurry；First slurry is placed under subnormal ambient and stirs centrotheca
120min is expected to remove bubble, and light trigger is added in most backward centrotheca material and is stirred, slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 200 and dries 1h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Structure snd size and object construction through the dried base substrate of liquid
Unanimously.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to reinforce base substrate.Then, will
Base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 300 DEG C with 0.1 DEG C/min speed and is incubated 6h；The vacuum of draft glue discharging furnace is kept, base substrate is cooled to draft glue discharging furnace
Room temperature.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 5 DEG C/min speed
To 600 DEG C and it is incubated 0.5h；Then 800 DEG C are warming up to 2 DEG C/min speed again and are incubated 60min, then base substrate is cold with stove
But to room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of air atmosphere, 1700 DEG C is warming up to 10 DEG C/min speed and is incubated 1h, is made
Obtain high ceramic of compact.
The relative density of high ceramic of compact prepared by the present embodiment is 95.1%, and Vickers hardness is 15.8GPa, remaining
Carbon content is 0.3wt%.The structure snd size and object construction of high ceramic of compact manufactured in the present embodiment are basically identical, deformation quantity
It is very small, it can be neglected, not influence the quality of finished product.
Embodiment 5
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
Premixed liquid processed：605g deionized waters and 55g glycerine are weighed respectively as solvent (account for premixed liquid quality 60%)；Point
Also known as 425g acrylamides and 15g N-N ' methylene-bisacrylamides are taken as organic solute (account for premixed liquid quality 40%).
Organic solute is well mixed with solvent, organic solute is all dissolved, obtains the slightly yellow transparent premixed liquids of 1100g.
Slurrying material：Above-mentioned premixed liquid (15%) is taken, and weighs 220g ammonium citrates (dispersant, 3%), 5866g respectively
Alpha-alumina (ceramic powders, 80%；Particle diameter≤0.1 μm, purity 99.99%), 147g 1- hydroxycyclohexyl phenyl ketones
(light trigger 184,2%).Dispersant is added into premixed liquid and is well mixed, then adds ceramic powders simultaneously into premixed liquid
Ball milling 50h, obtain just slurry；First slurry is placed under subnormal ambient and stirs first slurry 1min to remove bubble, it is most backward first
Light trigger is added in slurry and is stirred, slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 200 and dries 50h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Structure snd size and object construction through the dried base substrate of liquid
Unanimously.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to reinforce base substrate.Then, will
Base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 1000 DEG C with 10 DEG C/min speed and is incubated 2h, and 60min is incubated every 150 DEG C in temperature-rise period；The row of holding
The vacuum of glue stove, base substrate are cooled to room temperature with draft glue discharging furnace.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, with 10 DEG C/min speed liter
Temperature is to 600 DEG C and is incubated 10h；Then 1100 DEG C are warming up to 10 DEG C/min speed again and are incubated 40min, then base substrate is with stove
It is cooled to room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of air atmosphere, 1300 DEG C is warming up to 15 DEG C/min speed and is incubated 8h, is made
Obtain high ceramic of compact.
The relative density of high ceramic of compact prepared by the present embodiment is 93.8%, and Vickers hardness is 14.1GPa, remaining
Carbon content is 0.2wt%.The structure snd size and object construction of high ceramic of compact manufactured in the present embodiment are basically identical, deformation quantity
It is very small, it can be neglected, not influence the quality of finished product.
Embodiment 6
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
Premixed liquid processed：605g deionized waters and 55g glycerine are weighed respectively as solvent (account for premixed liquid quality 60%)；Point
Also known as 425g acrylamides and 15g N-N ' methylene-bisacrylamides are taken as organic solute (account for premixed liquid quality 40%).
Organic solute is well mixed with solvent, organic solute is all dissolved, obtains the slightly yellow transparent premixed liquids of 1100g.
Slurrying material：Take above-mentioned premixed liquid (69.95%), and weigh respectively 0.63g ammonium citrates (dispersant,
0.04%), 471g Alpha-aluminas (ceramic powders, 30%；Particle diameter≤0.1 μm, purity 99.99%), 0.16g 1- hydroxyl rings
Hexyl phenyl ketone (light trigger 184,0.01%).Dispersant is added into premixed liquid and is well mixed, then to premixed liquid
Middle addition ceramic powders and ball milling 30h, obtain just slurry；By first slurry be placed under subnormal ambient and stir just slurry 20min with
Bubble is removed, light trigger is added in most backward centrotheca material and is stirred, slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 500 and dries 60h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Structure snd size and object construction through the dried base substrate of liquid
Unanimously.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to reinforce base substrate.Then, will
Base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 1000 DEG C with 5 DEG C/min speed and is incubated 3h, and 60min is incubated every 150 DEG C in temperature-rise period；The row of holding
The vacuum of glue stove, base substrate are cooled to room temperature with draft glue discharging furnace.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 5 DEG C/min speed
To 600 DEG C and it is incubated 5h；Then 1100 DEG C are warming up to 10 DEG C/min speed again and are incubated 40min, then base substrate is cold with stove
But to room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of argon gas atmosphere, 1700 DEG C is warming up to 10 DEG C/min speed and is incubated 7h, is made
Obtain high ceramic of compact.
The relative density of high ceramic of compact prepared by the present embodiment is 91.7%, and Vickers hardness is 12.8GPa, remaining
Carbon content is 0.5wt%.The structure snd size and object construction of high ceramic of compact manufactured in the present embodiment are basically identical, deformation quantity
It is very small, it can be neglected, not influence the quality of finished product.
Embodiment 7
The present embodiment provides a kind of preparation method of the high ceramic of compact of Stereolithography, comprises the following steps that：
(1) slurry is prepared
1100g 1 is weighed, 6- hexanediyl esters weigh 100g lemons respectively as premixed liquid (23.26%)
Sour ammonium (dispersant, 2.1%), 3500g Alpha-aluminas (ceramic powders, 74%；Particle diameter≤0.5 μm, purity 99.99%), 30g
2- hydroxy-2-methyl -1- phenyl -1- acetone (light trigger 1173,0.63%).Dispersant is added into premixed liquid and is mixed equal
It is even, ceramic powders and ball milling 48h are then added into premixed liquid, obtains just slurry；First slurry is placed under subnormal ambient and stirred
Mix just slurry 10min to add light trigger to remove bubble, in most backward centrotheca material and stir, slurry is made.
(2) it is molded
Slurry is placed in Stereolithography equipment, base substrate is prepared by Stereolithography method (wavelength 355nm).Then
Take out base substrate and clean up the uncured slurry of billet surface.
(3) dry
Base substrate is placed in the polyethylene glycol that molecular weight is 600 and dries 72h, then base substrate is placed in absolute ethyl alcohol and carried out
Ultrasonic wave is cleaned to remove the liquid desiccant of billet surface.Structure snd size and object construction through the dried base substrate of liquid
Unanimously.Then, base substrate is placed under wavelength≤405nm uviol lamp, with ultra violet lamp base substrate to reinforce base substrate.Then, will
Base substrate is placed in baking oven and dried.
(4) dumping
Vacuum dumping or atmosphere protection dumping first are carried out to base substrate：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace
It is interior, it is warming up to 900 DEG C with 3 DEG C/min speed and is incubated 2h, and 10min is incubated every 100 DEG C in temperature-rise period；Keep dumping
The vacuum of stove, base substrate are cooled to room temperature with draft glue discharging furnace.
Air dumping is carried out to base substrate again：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 3 DEG C/min speed
To 700 DEG C and it is incubated 2h；Then 1100 DEG C are warming up to 10 DEG C/min speed again and are incubated 10min, then base substrate is cold with stove
But to room temperature.
(5) sinter
Base substrate is placed in the sintering furnace of air atmosphere, 1400 DEG C is warming up to 10 DEG C/min speed and is incubated 3h, is made
Obtain high ceramic of compact.
The relative density of high ceramic of compact prepared by the present embodiment is 99.6%, and Vickers hardness is 18.1GPa, remaining
Carbon content is 0.1wt%.The structure snd size and object construction of high ceramic of compact manufactured in the present embodiment are basically identical, deformation quantity
It is very small, it can be neglected, not influence the quality of finished product.
Comparative example 1
This comparative example provides a kind of ceramic preparation method, includes preparing slurry stage, forming step successively, dries step
Suddenly, dumping step, sintering step.Slurry used in this comparative example is identical with the slurry used in embodiment 1, preparation slurry stage,
Forming step, dumping step and sintering step are also identical with embodiment 1, and difference is drying steps.This comparative example
Drying steps are as follows：Base substrate stands 48h at room temperature.The shape of the base substrate after 48h is stood as shown in fig. 6, the deformation quantity of base substrate
It is very big, do not meet generation and require.
It is 93% as the ceramic relative density prepared by this comparative example, Vickers hardness is 14.3GPa, residual carbon content
For 0.5wt%.But the deformation quantity of ceramics is big, does not meet the requirement of target product.
Comparative example 2
This comparative example provides a kind of ceramic preparation method, includes preparing slurry stage, forming step successively, dries step
Suddenly, dumping step, sintering step.Slurry used in this comparative example is identical with the slurry used in embodiment 1, preparation slurry stage,
Forming step, drying steps and sintering step are also identical with embodiment 1, and difference is dumping step, and this comparative example is only
Carry out vacuum dumping.The dumping step of this comparative example is as follows：Base substrate is placed in vacuum >=0.09MPa draft glue discharging furnace, with 2
DEG C/min speed is warming up to 600 DEG C and is incubated 4h, and be incubated 20min every 100 DEG C in temperature-rise period；Keep the true of draft glue discharging furnace
Reciprocal of duty cycle, base substrate are cooled to room temperature with draft glue discharging furnace.
There is obvious crack as the ceramics prepared by this comparative example, do not meet product requirement.
Comparative example 3
This comparative example provides a kind of ceramic preparation method, includes preparing slurry stage, forming step successively, dries step
Suddenly, dumping step, sintering step.Slurry used in this comparative example is identical with the slurry used in embodiment 1, preparation slurry stage,
Forming step, drying steps and sintering step are also identical with embodiment 1, and difference is dumping step, and this comparative example is only
Carry out air dumping.The dumping step of this comparative example is as follows：Base substrate is placed in the draft glue discharging furnace of air atmosphere, with 2 DEG C/min's
Speed is warming up to 600 DEG C and is incubated 4h；Then 1000 DEG C are warming up to 15 DEG C/min speed again and are incubated 30min, then base
Body cools to room temperature with the furnace.
There is obviously crack as the ceramics prepared by this comparative example, do not meet product requirement.
In other embodiments, the organic solute for forming premixed liquid can also be acrylamide, N-N ' di-2-ethylhexylphosphine oxides third
At least one of acrylamide, 1,6 hexanediol diacrylate, trimethylolpropane trimethacrylate.Form the molten of premixed liquid
Agent can also be at least one of deionized water, glycerine, absolute ethyl alcohol, acetone.
In other embodiments, ceramic powders can also be aluminum oxide, zirconium oxide, lead zirconate titanate, silicon nitride, nitridation
At least one of aluminium, carborundum, boron carbide, titanium carbonitride, titanium carbide, titanium oxide and silica.The average grain of ceramic powders
Footpath is less than or equal to 10 μm, and the purity of ceramic powders is more than or equal to 99.9%.
In other embodiments, light trigger can also be 2- hydroxy-2-methyl -1- phenyl -1- acetone (light triggers
1173), 1- hydroxycyclohexyl phenyl ketones (light trigger 184), 2- hydroxyls -4'- (2- hydroxy ethoxies) -2- methyl phenyl ketones
At least one of (light trigger 2959)；Dispersant can also be ammonium citrate, polyvinylpyrrolidone, calgon,
At least one of ammonium polyacrylate.
In other embodiments, in dumping step, inert gas atmosphere protection dumping substitution vacuum dumping can be also used,
Or using N2Atmosphere protection dumping substitution vacuum dumping, dumping effect are consistent with the effect of vacuum dumping.In curing schedule, light is solid
Chemical conversion type use up can be λ≤405nm ultraviolet, be not limited to wavelength be 405nm ultraviolet.
The technology contents described above that the present invention is only further illustrated with embodiment, in order to which reader is easier to understand,
But embodiments of the present invention are not represented and are only limitted to this, any technology done according to the present invention extends or recreation, is sent out by this
Bright protection.
Claims (7)
1. the preparation method of the high ceramic of compact of a kind of Stereolithography, it is characterised in that comprise the following steps：
S1 prepares slurry：Each component is weighed by following mass percent and is well mixed, 30-80% ceramic powders, 15-65%
Premixed liquid, 0.01-2% light trigger, 0.04-3% dispersant, obtain slurry；
The premixed liquid is made up of organic solute and solvent, and the quality of the solvent is the 0-90% of the quality of premixed liquid, and not
Take 0；The organic solute is acrylamide, N-N ' methylene-bisacrylamides, 1,6 hexanediol diacrylate and three hydroxyl first
At least one of base propane triacrylate；
S2 is molded：Slurry is placed in Stereolithography equipment, base substrate is prepared out by Stereolithography method；
Then, base substrate passes through the processing of drying steps, dumping step and sintering step successively, and obtained relative density is more than or is equal to
90%, Vickers hardness is more than or equal to 12GPa, and residual carbon content is less than or equal to 0.5wt% ceramics；
The dumping step is：Vacuum dumping is first carried out to base substrate or atmosphere protection dumping is handled, then air row is carried out to base substrate
Glue processing；
The condition of the vacuum dumping or atmosphere protection dumping is：Base substrate is placed in the draft glue discharging furnace of negative pressure or inert gas shielding
Draft glue discharging furnace in, be warming up to 300-1000 DEG C with 0.1-10 DEG C/min speed and be incubated 2-6h, and every 50- in temperature-rise period
150 DEG C of insulation 0-60min；Then, base substrate is cooled to room temperature in the draft glue discharging furnace of negative pressure or in the draft glue discharging furnace of inert gas shielding；
The condition of the air dumping is：Base substrate is placed in the draft glue discharging furnace of air atmosphere, heated up with 1-10 DEG C/min speed
To 400-700 DEG C and it is incubated 0.5-10h；Then base substrate cools to room temperature with the furnace.
2. the preparation method of the high ceramic of compact of a kind of Stereolithography according to claim 1, it is characterised in that described dry
Dry step is：Base substrate is placed in liquid desiccant and dries 1-72h.
3. the preparation method of the high ceramic of compact of a kind of Stereolithography according to claim 1, it is characterised in that described negative
The draft glue discharging furnace of pressure refers to that the vacuum in draft glue discharging furnace is more than or equal to 0.09MPa.
A kind of 4. preparation method of the high ceramic of compact of Stereolithography according to claim 1, it is characterised in that the sky
In gas dumping step, after base substrate insulation 0.5-10h, it is warming up to 800-1100 DEG C with 2-15 DEG C/min speed and is incubated 10-
60min, then base substrate cool to room temperature with the furnace.
A kind of 5. preparation method of the high ceramic of compact of Stereolithography according to claim 1, it is characterised in that the burning
Tying the condition of step is：Base substrate is placed in sintering furnace, 1200-2200 DEG C is warming up to 5-30 DEG C/min speed and is incubated 1-
8h, ceramics are made.
A kind of 6. preparation method of the high ceramic of compact of Stereolithography according to claim 1, it is characterised in that the system
In standby slurry stage：Organic solute is well mixed with solvent first, premixed liquid is formed, dispersant is then added into premixed liquid
And be well mixed, ceramic powders and ball milling 0.1-50h are then added into premixed liquid, obtains just slurry；First slurry is placed in negative
Under pressure ring border and the first slurry 1-120min of stirring adds light trigger to remove bubble, in most backward centrotheca material and is well mixed,
Slurry is made.
A kind of 7. preparation method of the high ceramic of compact of Stereolithography according to claim 1, it is characterised in that the pottery
Porcelain powder is aluminum oxide, zirconium oxide, lead zirconate titanate, silicon nitride, aluminium nitride, carborundum, boron carbide, titanium carbonitride, titanium carbide, oxygen
Change at least one of titanium and silica.
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| PCT/CN2015/089961 WO2017045191A1 (en) | 2015-09-16 | 2015-09-18 | Method for preparing photocuring-formed high-density ceramic |
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| CN116425535A (en) * | 2023-03-16 | 2023-07-14 | 深圳奇遇科技有限公司 | Lead zirconate titanate slurry for photocuring forming, preparation method thereof and finished product |
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| CN101148360B (en) * | 2007-08-14 | 2010-05-19 | 西安交通大学 | Customized forming method for gradient porous structure ceramic |
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