CN110372398A - A kind of quick degreasing sintered method of Stereolithography ceramic body - Google Patents
A kind of quick degreasing sintered method of Stereolithography ceramic body Download PDFInfo
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Abstract
The present invention relates to a kind of quick degreasing sintered methods of vacuum-air-vacuum of Stereolithography ceramic body, and Stereolithography ceramic body is placed in being transferred in vacuum drying oven in foamed alumina ceramic platform, 1 × 10‑3~5 × 10‑1Under the vacuum condition of Pa, 550~650 DEG C are raised the temperature to the interruption heat preservation in the heating rate and temperature-rise period of 0.5~2 DEG C/min and keeps the temperature 1~2h；The temperature of vacuum drying oven is naturally cooling to 300~400 DEG C after the completion of ceramic body carbonization and keeps the temperature 1~2h, close vacuum pump, air is slowly passed through into vacuum drying oven with the rate of 0.1~1L/min, remaining carbon in ceramic body is set to generate carbon dioxide with oxygen slow reaction and escape, it completes to open vacuum pump to soaking time, the sintering temperature of ceramics is raised the temperature to the rate of 3~5 DEG C/min and is kept the temperature, and the air oxidation after vacuum carburization prevents influence of the remaining a small amount of charcoal to ceramic performance after sintering.
Description
Technical field
The invention belongs to material increasing fields, and in particular to a kind of quick degreasing sintered side of Stereolithography ceramic body
Method.
Background technique
Ceramic material due to its hardness with higher, intensity, good wearability, thermal stability, chemical stability and
A series of excellent performances such as biocompatibility, are widely used in the fields such as aerospace, machinery, electronics, semiconductor.Tradition
Process for preparing ceramic be mainly gel injection-moulding, it is dry-pressing formed, these manufacturing methods are required to manufacture elaborate using mold
Ceramic when mold manufacture it is difficult and the manufacturing cycle is longer, be unable to satisfy the personalized production of small lot.With increasing material system
The development of technology is made, 3D printing technique such as laser 3D printing, photocuring 3D printing is used to prepare ceramics.In recent years, this technology
Hot spot be photocuring ceramic printer equipment design and high solid loading, low viscosity ceramic slurry development in terms of.
3D printing technique can forming shape complexity, fine structure, accurate size and excellent surface ceramic body, still
Final ceramic product in order to obtain needs to carry out degreasing and sintering step.For example, CN106316369A is using Muffle furnace in sky
Degreasing and sintering are carried out under gas atmosphere；CN106316369B using raw material identical with ceramic body and powder to ceramic body into
Segmentation dumping is carried out after row embedding and filling in air atmosphere, and is being lower than 300 DEG C of ceramic sintering temperature or so progress pre-burnings
Tie and take out the sintering that ceramic body avoids green body and buried powder after degreasing.However, conventional degreasing side in air atmosphere
Method can be with a series of physical chemical reaction (fusing, evaporation, oxidation and the decomposition of such as organic binder), and organic matter is fused into
Liquid will lead to the expansion of volume, and temperature further increases organic matter and evaporates rapidly, 0.2-1 DEG C/min's of degreasing heating rate
In the case of be also easy under the bigger air atmosphere of volume for leading to the cracking and ceramic body of ceramic body under degreasing occur cracking,
The defect of layering is bigger.Temperature setting and soaking time in skimming processes need the TGA-DSC curve according to binder
It designs, skimming temp setting difference is larger in the binder of different formulations, does not have general applicability.
Degreasing is a vital step in the post-processing of photocuring 3D molded ceramic blank, the fine fisssure occurred in skimming processes
The defects of line, hole, layering, can be amplified during the sintering process, directly determine the quality of forming ceramic.According to photocuring 3D
The ceramming process for printing aluminium oxide ceramics green body needs degreasing to remove the large amount of organic contained in ceramic body, however
It is one of major technology bottleneck in ceramming process by going on smoothly for control skimming processes, existing skimming processes are main
It is arranged with the heating rate of 0.2~1 DEG C/min and uninterrupted soaking time, process is very long, completes degreasing and generally requires 50-
100h。
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of photocuring in view of the deficiency of the prior art
The quick degreasing sintered method of molded ceramic blank can make ceramic degreasing blank keep certain intensity quick, flawless de-
Most of organic matter in ceramic body out avoids needing the TGA-DSC heat according to organic binder in air thermal degreasing process
Degreasing characteristic carries out the specific setting of heating rate and soaking time slowly, complicated, and universality is good.
The present invention be solve the problems, such as it is set forth above used by technical solution are as follows:
A kind of quick degreasing sintered method of Stereolithography ceramic body, steps are as follows:
(1) vacuum degreasing: Stereolithography ceramic body is placed on Alumina Foam platform and is transferred to vacuum drying oven
In, 1 × 10-3~5 × 10-1Vacuum condition under, in the heating rate of 0.5~2 DEG C/min and temperature-rise period be interrupted heat preservation
It raises the temperature to 550~650 DEG C and keeps the temperature 1~2h, the organic matter in ceramic body is made to decompose volatilization and carbonization, removal ceramics
Most organic in green body；
(2) air oxidation carbon removal: vacuum pump is closed simultaneously when the vacuum drying oven in step (1) is naturally cooling to 300~400 DEG C
Keep the temperature 1~2h in this temperature range, be passed through in this insulating process into vacuum drying oven air make in ceramic body remaining carbon with
Oxygen slow reaction generates carbon dioxide and escapes；
(3) vacuum-sintering: after in step 2 keep the temperature after the completion of, reopen the vacuum pump of vacuum drying oven, then with 3~5 DEG C/
The temperature of vacuum drying oven is increased to the sintering temperature of ceramics and kept the temperature by the rate of min, and last vacuum drying oven naturally cools to room
Temperature obtains excellent surface quality, no cracking, the high-compactness ceramic without layering.
According to the above scheme, Stereolithography ceramic body the preparation method is as follows: by photosensitive resin, dispersing agent and nanometer,
The ceramic powders mixing and ball milling of submicron order, obtains photocuring ceramic slurry；Then the photocuring ceramic slurry passes through photocuring
3D printing molding, obtained Stereolithography ceramic body.
According to the above scheme, the photosensitive resin is mixed by the reactive diluent and photoinitiator of low viscosity, and activity is dilute
Releasing agent can be new for 2- phenoxyethyl acrylate, tetrahydrofuran acrylate, 1,6 hexanediol diacrylate, the third oxidation
One of Diacrylate, trimethylolpropane trimethacrylate, ethoxyquin pentaerythritol tetraacrylate etc. or
It is a variety of；Photoinitiator can be one of TPO, BPO etc..
According to the above scheme, the volume fraction of ceramic powder is not less than 40% in the photocuring ceramic slurry.
According to the above scheme, in step (1), interruption heat preservation are as follows: often reach interruption heat preservation when hundred temperature in temperature-rise period
0.5-2h, that is, when being warming up to 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C etc. whole hundred DEG C, respectively in temperature 0.5-
2h。
According to the above scheme, in step (2), air is passed through into vacuum drying oven in insulating process, makes the oxygen in vacuum drying oven
Volume fraction in the range of 15-20%.0.1~1L/min may be selected in the rate for being generally passed through air.
According to the above scheme, in step (3), the vacuum pump for reopening vacuum drying oven makes vacuum degree in vacuum drying oven be in 1 × 10-3
~5 × 10-1In the range of Pa.
According to the above scheme, in step (3), when ceramics are aluminium oxide, 1600-1650 DEG C of sintering temperature is simultaneously protected at this temperature
Warm 1-2h.
Major technique design of the invention is as follows: firstly, ceramic body after first step vacuum degreasing to vacuum drying oven oneself
It is so cooled to 300~400 DEG C and keeps the temperature 1~2h.The purpose in this stage is to make the most organic in ceramic body
Carbonization is decomposed under oxygen-free environment, and gaseous state is become from solid-state under high vacuum state and is volatilized rapidly, and organic matter is in anaerobic
Remaining carbon coating ceramic powders are decomposed under state can make ceramic body keep certain intensity in skimming processes again, avoid
There is the defects of cracking, layering, blistering in skimming processes in ceramic body, ensure that the dimensional accuracy and surface matter of ceramic body
Amount.Then, vacuum pump is closed, air is passed through into vacuum drying oven slowly with the rate of 0.1~1L/min, is made residual in ceramic body
The charcoal stayed generates carbon dioxide with oxygen slow reaction and escapes.This process is directly reacted in a vacuum furnace, avoids base
Body, which is transferred in Muffle furnace, to be damaged in structure and directly carries out carbon removal using the temperature of vacuum drying oven, is conducive to energy saving.Then,
Soaking time to carbon removal is completed to close and open vacuum pump for the valve for being passed through air one end, will be warm with the rate of 3~5 DEG C/min
Degree is increased to the sintering temperature of ceramics and is kept the temperature, and is conducive to the densification of ceramic.
Compared with prior art, the quick degreasing sintered method of a kind of Stereolithography ceramic body proposed by the present invention.
Compared with the thermal debinding under air atmosphere, the thermal debinding of ceramic body under vacuum conditions in the method for the invention has drop
The decomposition rate of low organic matter, in skimming processes organic binder directly by it is solid state transformed be gaseous state, avoid solid-state and be fused into
Influence of the volume expansion to ceramics bad body intensity when liquid, and the thermal debinding of ceramic body is inwardly carried out from surface, vacuum environment
Under thermal debinding facilitate the volatilization of internal organic binder, organic matter under oxygen-free environment in the stomata that ceramic body surface leaves
Carbonization also ceramic body can be made to remain certain intensity in skimming processes.It has the beneficial effect that:
Firstly, the present invention, by vacuum condition, low heating rate, low skimming temp can make ceramic degreasing blank in carbon residue
Cladding keeps that certain intensity is quick, most of organic matter in flawless abjection ceramic body.
Secondly, the present invention can be to avoid the TGA-DSC thermal debinding needed in air thermal degreasing process according to organic binder
Characteristic carries out the specific setting of heating rate and soaking time slowly, complicated, has certain general applicability.
Furthermore the present invention can obtain the ceramic of high-compactness using vacuum degreasing, sintering, be conducive to improve its
Mechanical performance.
Detailed description of the invention
Fig. 1 is the pictorial diagram of sample obtained by 1 step of embodiment (1)；
Fig. 2 is sample object figure obtained by 1 step of embodiment (2)；
Fig. 3 is sample object figure obtained by 1 step of embodiment (3).
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
In following embodiments, the preparation method of Stereolithography ceramic body can be such that by photosensitive resin, dispersing agent and
Nanometer, the ceramic powders mixing and ball milling of submicron order, obtain photocuring ceramic slurry；Then the photocuring ceramic slurry passes through light
Solidify 3D printing molding, obtained Stereolithography ceramic body.
Specifically, for the Stereolithography ceramic body of embodiment 1, specifically the preparation method comprises the following steps: by isobomyl acrylate
Ester (IBOA), 1,6- hexanediyl ester (HDDA), trimethylolpropane trimethacrylate (TMPTA) are with the body of 2:4:2
Product adds the photoinitiator 2 of the 1wt% of three's gross mass than mixing, 4,6- trimethylbenzoy-dipheny phosphine oxides
(TPO) 30min is mixed on magnetic stirring apparatus to be uniformly mixed, obtain photosensitive resin mixture；By photosensitive resin mixture and receive
The ball-aluminium oxide powder of meter level mixes, and adds the phosphate of alumina powder mass fraction 3% as dispersing agent, to aoxidize
Aluminium: zirconium oxide=1:1 quality is added mill ball and on planetary ball mill for 24 hours with 120r/min ball milling is configured to volume fraction
40% aluminium oxide ceramics slurry；The ceramic slurry of ball milling is poured into the resin storage tank of photocuring ceramic printer with printing
The rectangle of 40*10*3mm and the small column of Φ 20*3mm are printed in the setting of thickness 50um respectively.
Embodiment 1
A kind of quick degreasing sintered method of Stereolithography ceramic body, steps are as follows:
(1) vacuum degreasing: aluminium oxide ceramics cuboid green body is placed on aluminium oxide ceramics platform and is transferred to vacuum
In furnace, 1 × 10-3~5 × 10-1Under the vacuum condition of Pa, often to reach hundred in the heating rate of 1 DEG C/min and temperature-rise period
1h ((when being warming up to 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, keeping the temperature 1h respectively) heat preservation, by temperature liter when the temperature of position
Up to 600 DEG C and keep the temperature 1h；
(2) vacuum pump and herein air oxidation carbon removal: is closed when the vacuum drying oven in step (1) is naturally cooling to 350 DEG C
At a temperature of keep the temperature 2h, in this insulating process, in this insulating process, be passed through with the rate of 0.1~1L/min into vacuum drying oven
Air makes the volume fraction of the oxygen in vacuum drying oven in the range of 15-20%；
(3) vacuum-sintering: after the completion of keeping the temperature in step 2, the vacuum pump for reopening vacuum drying oven makes vacuum in vacuum drying oven
Degree is in 5 × 10-2Under the vacuum condition of Pa, the temperature of vacuum drying oven is then increased to by aluminium oxide ceramics with the rate of 5 DEG C/min
1600 DEG C of sintering temperature and keep the temperature 1h at this temperature, last vacuum drying oven cooled to room temperature, obtain excellent surface quality,
High-compactness ceramic without cracking, layering.After magnifying glass amplifies 20 times, observation ceramic surface still presents excellent
Quality, it is no cracking and layering.
In above procedure, the purpose of step (1) is to come the organic matter in ceramic body directly with solid-state to gaseous state transformation
Slowly volatilization, while the anaerobic decomposition carbon residue coating function of organic matter can also make ceramic body keep certain in skimming processes
Intensity can obtain excellent surface quality, the grey ceramic body without cracking layering, effectively after the completion of most of organic matter degreasing
The quick nondestructive skimming processes for having pushed photocuring 3D printing molded ceramic blank, by experiment measure by this vacuum degreasing
The quality of treated greyish black ceramic body accounts for the 71.59% of former ceramic body quality.The purpose of step (2) is to make ceramic body
It is cooled to the ignition point of charcoal, prevents the too fast formation micro-damage of carbon residue high-temperature oxydation rate in ceramic body.Also, keep vacuum de-
The carbon residue in ceramic body after rouge slowly aoxidizes under air environment, and the carbon residue in green body is discharged, prevents it to follow-up sintering
The influence of product properties, measures air carbon removal treated that quality accounts for the 69.68% of former ceramic body sample quality by experiment.
The purpose of step (3) is the ceramic body vacuum Fast Sintering after making air carbon removal, obtains high-compactness ceramic, passes through matter
Measure aluminium oxide ceramics density be 3.953g/cm3, consistency is theoretical density 3.98g/cm399.3216%, after sintering
Cuboid ceramics three-point bending strength be 236Mpa, it can thus be appreciated that by the method can get high-compactness ceramic system
Product.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to of the invention
Protection scope.
Claims (9)
1. a kind of quick degreasing sintered method of Stereolithography ceramic body, it is characterised in that steps are as follows:
(1) vacuum degreasing: Stereolithography ceramic body being placed on Alumina Foam platform and is transferred in vacuum drying oven,
1×10-3~5 × 10-1Vacuum condition under, in the heating rate of 0.5~2 DEG C/min and temperature-rise period be interrupted heat preservation will be warm
Degree is increased to 550~650 DEG C and keeps the temperature 1~2h；
(2) vacuum pump and herein air oxidation carbon removal: is closed when the vacuum drying oven in step (1) is naturally cooling to 300~400 DEG C
Temperature range keeps the temperature 1~2h, and air is passed through into vacuum drying oven in this insulating process；
(3) vacuum-sintering: after the completion of heat preservation in step (2), the vacuum pump of vacuum drying oven is reopened, then with 3~5 DEG C/min
Rate by the temperature of vacuum drying oven be increased to ceramics sintering temperature and keep the temperature, last vacuum drying oven cooled to room temperature,
Obtain high-compactness ceramic.
2. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 1, it is characterised in that
Stereolithography ceramic body the preparation method is as follows: the ceramic powders of photosensitive resin, dispersing agent and nanometer, submicron order are mixed
Ball milling is closed, photocuring ceramic slurry is obtained；Then the photocuring ceramic slurry is formed by photocuring 3D printing, and obtained light is solid
Change molded ceramic blank.
3. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 2, it is characterised in that
The photosensitive resin is mixed by the reactive diluent and photoinitiator of low viscosity；Wherein, reactive diluent is 2- phenoxy group
Ethyl propylene acid esters, tetrahydrofuran acrylate, 1,6 hexanediol diacrylate, third oxidation neopentylglycol diacrylate,
One of trimethylolpropane trimethacrylate, ethoxyquin pentaerythritol tetraacrylate are a variety of；Photoinitiator be TPO,
One of BPO.
4. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 2, it is characterised in that
The volume fraction of ceramic powder is not less than 40% in the photocuring ceramic slurry.
5. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 1, it is characterised in that
In step (1), interruption heat preservation are as follows: often reach interruption heat preservation 0.5-2h when hundred temperature in temperature-rise period.
6. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 1, it is characterised in that
In step (2), air is passed through into vacuum drying oven in insulating process, makes the volume fraction of the oxygen in vacuum drying oven in 15-20%
In the range of.
7. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 6, it is characterised in that
The rate for being passed through air selects 0.1~1L/min.
8. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 1, it is characterised in that
In step (3), the vacuum pump for reopening vacuum drying oven makes vacuum degree in vacuum drying oven be in 1 × 10-3~5 × 10-1The range of Pa
It is interior.
9. a kind of quick degreasing sintered method of Stereolithography ceramic body according to claim 1, it is characterised in that
In step (3), when ceramics are aluminium oxide, 1600-1650 DEG C of sintering temperature simultaneously keeps the temperature 1-2h at this temperature.
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| CN112851339A (en) * | 2021-01-29 | 2021-05-28 | 华南师范大学 | Ceramic slurry for photocuring 3D printing and preparation method of ceramic device thereof |
| CN113208750A (en) * | 2021-05-15 | 2021-08-06 | 江苏京科智镕新材料科技有限公司 | Light-transmission gradual-change dental crown based on stereolithography 3D printing and preparation method |
| CN113860889A (en) * | 2021-09-26 | 2021-12-31 | 深圳技术大学 | Low-temperature rapid degreasing sintering method for alumina ceramic biscuit |
| CN113956023A (en) * | 2021-11-16 | 2022-01-21 | 中国人民解放军国防科技大学 | Method for preparing aluminum oxide ceramic based on sinking type DLP photocuring 3D printing |
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| CN113956023B (en) * | 2021-11-16 | 2022-08-19 | 中国人民解放军国防科技大学 | Method for preparing aluminum oxide ceramic based on sunken DLP photocuring 3D printing |
| CN113956023A (en) * | 2021-11-16 | 2022-01-21 | 中国人民解放军国防科技大学 | Method for preparing aluminum oxide ceramic based on sinking type DLP photocuring 3D printing |
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| CN116135818A (en) * | 2023-03-03 | 2023-05-19 | 上海科技大学 | Ceramic blank glue discharging method and ceramic workpiece preparation method |
| CN118239685A (en) * | 2024-03-28 | 2024-06-25 | 江南大学 | Method for manufacturing high-permeability lithium disilicate glass ceramic by photo-curing additive |
| CN118270984A (en) * | 2024-03-28 | 2024-07-02 | 江南大学 | Method for manufacturing gradient lithium disilicate glass ceramic by photo-curing additive |
| CN118239685B (en) * | 2024-03-28 | 2024-10-18 | 江南大学 | Method for manufacturing high-permeability lithium disilicate glass ceramic by photo-curing additive |
| CN118270984B (en) * | 2024-03-28 | 2024-10-25 | 江南大学 | Method for manufacturing gradient lithium disilicate glass ceramic by photo-curing additive |
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