CN106316369B - A kind of dumping and sintering process of 3D printing ceramic body - Google Patents
A kind of dumping and sintering process of 3D printing ceramic body Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- 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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- 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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- C04B35/64—Burning or sintering processes
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- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
Abstract
The present invention relates to the dumpings and sintering process of a kind of 3D printing ceramic body, it include: that the ceramic body that the solid content of 3D printing is 20~95wt.% is put into crucible by (1), and use raw material powder identical with ceramic body ingredient is embedded and filled to ceramic body；(2) crucible for being placed with ceramic body is put into Muffle furnace, segmentation dumping is carried out under air atmosphere；(3) sintering temperature is warming up to 1~3 DEG C/min of heating rate, sintering time 1~12 hour；Wherein, the densification temperature is 300~1000 DEG C lower than the sintering temperature of the ceramic body.Green body is embedded and is filled using raw material powder identical with ceramic body ingredient by the present invention.Raw material powder not only needs to wrap ceramic body, but also needs to insert the hollow structures such as the hole in green body, it is therefore an objective to be heated evenly ceramic body, slowly, prevent the cataclysm of temperature, avoid generating internal stress inside green body, reduce the probability of collapsing.
Description
Technical field
The invention belongs to increases material manufacturing technology field, in particular to a kind of the dumping and agglomerant of 3D printing ceramic body
Skill.
Background technique
Since ceramic material has many advantages, such as corrosion-resistant, high temperature resistant, environmental-friendly, high mechanical strength, in energy-saving and emission-reduction function
Energy devices field is widely used, and the material that energy-saving and emission-reduction field generallys use at present.However, due to ceramics
The features such as high temperature of material itself, brittleness, traditional molding methods are difficult to prepare complex-shaped, thin wall hollow ceramic component.3D
Printing has the characteristics that the manufacturing cycle is short, is suitble to single-piece individual character manufacturing, one-pass molding, saves raw material, therefore, large-scale in manufacture
There is greater advantage in terms of the difficult processing such as ceramic thin-wall part, honeycomb complexity ceramic structure, titanium alloy, easy thermoformed parts.3D
Printing technique refers to be superimposed by continuous physical layer, increases material successively to generate the technology of 3D solid.With it is conventionally manufactured
The removal material processing method of industry is different, and what 3D printing followed is addition rule, i.e., in kind to be formed by stacking for powder layer by layer, so
Also referred to as increase material technology.Traditional ceramic preparation method is a many and diverse process, from the burning of initial Raw material processing to the end
It is all linked with one another at needing tens procedures, it is indispensable.And the 3D printing technique of ceramics can greatly save the time, make technique
Simplify, and saves a large amount of labor cost and raw material, energy consumption.
Traditional ceramics raw material generally can be divided into plasticity, four major class of lean property, solvent borne and functional raw material according to operational characteristic,
Wherein, plastic raw material mainly plays plasticizing and combination in production, is the molding key of ceramics, assigns blank plasticity and note
Processability is starched, mechanical strength, thermal stability, the chemical stability etc. after guaranteeing dry body strength and firing, including it is kaolin, swollen
Moisten soil, china clay, kieselguhr, Suzhou soil etc., is clay matter ceramics into porcelain basis.But due to clay mineral complex genesis, group
At unevenness, show as that the nature differences such as plasticity, thixotropy, associativity, shrinkage, refractoriness are larger, and therefore, each ceramics produce
There are difference for the ceramic batch formula and technique in area.Since clay itself is a kind of permanent adhesives, so matching in ceramic batch
Fang Zhong adds other adhesives again seldom to improve the plasticity of ingredient.
However, formed using 3D printing technique to ceramics, the requirement to the performance and process of pug is completely not
Equally.The plastic pug of tradition needs to be prepared by the techniques such as broken, ball milling, filters pressing, pugging, aging, if beaten using 3D
Print technology forms pug, then fineness, mobility, in terms of have tightened up requirement.Common 3D printing
The raw material that ceramic technology is utilized is generally the suspended nitride of as a form of gel or high solid volume fraction.It is good in order to have pug
Good rheological property, does not need only rely upon the adhesive attraction power of clay itself, it is necessary to a large amount of binder and plasticiser are added,
Make pug that there is good mobility by the modified function of these additives, and generate cementation power between particles, rises
To the effect for reducing viscosity, increasing mobility, improving inter-layer bonding force, finally ensure being normally carried out for 3D printing process.It is common
Binder have the high-molecular organic materials such as starch, dextrin, CMC, gum arabic, resin, gel-like.These additives are being burnt
During knot, main component will be decomposed volatilization, will not be embodied in final ceramic.Due to being added in ceramic material
A large amount of binders enable 3D printing technique to form lowplastcity raw material even non-plastic raw material, the selectivity of ceramic raw material
It is more extensive.
3D printing technique can forming shape complexity, precise structure, accurate in size ceramic body, the later period dumping burn
During knot, since containing high-molecular organic materials such as a large amount of binders, acutely contraction and weightlessness can occur for ceramic body, such as
What passes through the design effectively of dumping sintering process, makes ceramic body uniform shrinkage during dumping, does not deform, and keeps one
Fixed intensity, during the sintering process, ceramic member can have very high surface smoothness, reach preferable consistency, and intensity is excellent
It is good, there is lesser internal stress, accurate size, these are all the technology bottles that 3D printing ceramic technology obtains that application has to overcome
Neck, and the 3D printing technique of limitation ceramics obtain the main problem applied.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of dumping and sintering process suitable for 3D printing ceramic body, it is real
The densification for having showed 3D printing ceramic body (high-glue content ceramic body) breaches the molding technical bottleneck of ceramic 3D printing.
For this purpose, one aspect of the present invention provides the dumping and sintering process of a kind of 3D printing ceramic body, which is characterized in that
Include:
(1) ceramic body that the solid content of 3D printing is 20~95wt.% is put into crucible, and use and ceramic body
The identical raw material powder of ingredient is embedded and is filled to ceramic body；
(2) crucible for being placed with ceramic body is put into Muffle furnace, segmentation dumping, the segmentation row is carried out under air atmosphere
Glue includes heat preservation 2 hours or less first with 0.3~0.6 DEG C/min of heating rate from room temperature to 200 DEG C；Again with 0.4~
0.7 DEG C/min of heating rate is warming up to 500 DEG C, heat preservation 3 hours or less from 200 DEG C；Again with 0.4~0.7 DEG C/min of liter
Warm rate is warming up to densification temperature from 500 DEG C, keeps the temperature 2~6 hours, cools to room temperature with the furnace；
(3) sintering temperature is warming up to 1~3 DEG C/min of heating rate, sintering time 1~12 hour；
Wherein, the densification temperature is 300~1000 DEG C lower than the sintering temperature of the ceramic body.
Green body is embedded and is filled using raw material powder identical with ceramic body ingredient by the present invention.Raw material powder not only needs
Ceramic body is wrapped, and needs to insert the hollow structures such as the hole in green body, it is therefore an objective to be heated evenly ceramic body,
Slowly, the cataclysm for preventing temperature avoids generating internal stress inside green body, reduces the probability of collapsing.The present invention will be loaded with 3D again and beat
The crucible of print ceramic body (high-glue content, solid content are 20~95wt.%) is put into Muffle furnace, starts to carry out dumping process.
Wherein binder removal are as follows: with the heating rate of 0.3~0.6 DEG C/min, be warming up to 200 DEG C of 0~2h of heat preservation, the purpose of this stage is row
Except moisture such as free water, crystallization waters in green body.Again with the heating rate of 0.4~0.7 DEG C/min be warming up to 500 DEG C heat preservation 0~
3h, this stage purpose make the organic matter in green body decompose volatilization.Densification is risen to the heating rate of 0.4~0.7 DEG C/min again
2~6h of temperature, by this process, ceramic body can generate certain intensity, be unlikely to collapse.Densification temperature is general
It lower than 300~1000 DEG C of the ceramic sintering temperature, avoids raw material powder and ceramic body that sintering process occurs, is raw material powder
It removes and convenience is provided.
Preferably, the ceramic body is the ceramic body prepared by oxide, the oxide is Al2O3、TiO2、
ZrO2、SiO2, at least one of spinelle and mullite.
Preferably, the purity of the raw material powder is pure not less than analyzing, particle size is lower than 6 microns.
Dumping and sintering process of the invention can effectively handle the ceramic body containing a large amount of organic adhesives, especially
It is suitable for the molding ceramic members of 3D printing.This binder removal can not only effectively remove organic matter and water in ceramic body
Point, additionally it is possible to guarantee that ceramic body generates uniform shrinkage during dumping, phenomena such as not deforming, collapse, by dumping
After process, ceramic body also has certain intensity, the operation for being conducive to the removing of raw material powder and re-sintering.
3D printing technique in catalysis reaction carriers, is started due to that can prepare the special ceramics device such as abnormity, hollow and thin-walled
The fields such as machine jet pipe have a good application prospect.Dumping and sintering process through the invention, can not only effectively exclude
Organic matter in green body, additionally it is possible to obtain that dimensional contraction is uniform, surface quality is good, the ceramic member of good mechanical performance, be 3D
Application of the printing technique in ceramic system is standby provides solid foundation.
Detailed description of the invention
Fig. 1 a is the alumina ceramic tube green body illustraton of model of 3D printing；
Fig. 1 b is boat-shaped alumina ceramic crucible illustraton of model；
Fig. 2 is the illustraton of model that ceramic body is embedded to after alumina powder.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
According to the prior art, 3D printing has been able to realize the molding of ceramics, however, ceramic body obtained contains greatly
The organic gel of amount, this just brings huge difficulty to dumping sintering process and 3D printing ceramics realize the important skill of application
Art bottleneck.
The present invention is made pottery using the 3D printing techniques such as stereolithography apparatus (SLA) or selective sintering molding (SLS)
The printing of porcelain billet body.Wherein the solid content of ceramic body can be 20%~95wt.%, preferably 50~80wt.%.As above-mentioned
The ingredient of 3D printing ceramic body can be Al2O3、TiO2、ZrO2、SiO2, spinelle, the oxides such as mullite, can be above
The mixing of one or more oxides forms.
The present invention is that the ceramic body for obtaining 3D printing weighs, measures size, takes pictures, then ceramic body is put into especially
In the crucible of design, and green body is embedded and filled using raw material powder identical with ceramic body ingredient.Raw material powder is not only
It needs to wrap ceramic body, and needs to insert the hollow structures such as the hole in green body.The purity of raw material powder, which is not less than, divides
Analyse pure, particle size is less than 6 microns.
The crucible for being loaded with ceramic body is put into the position in Muffle furnace close to thermocouple, starts to carry out dumping process.Row
Adhesive process can are as follows: with the heating rate of 0.3~0.6 DEG C/min, is warming up to 200 DEG C of 0~2h of heat preservation, excludes the freedom in green body
The moisture such as water, the crystallization water.500 DEG C of 0~3h of heat preservation are warming up to the heating rate of 0.4~0.7 DEG C/min again, make having in green body
Machine object decomposes volatilization.Densification temperature is risen to the heating rate of 0.4~0.7 DEG C/min again and keeps the temperature 2~6h, by this process,
Ceramic body can generate certain intensity, be unlikely to collapse.Densification temperature be generally below the ceramic sintering temperature 300~
It 1000 DEG C, avoids raw material powder and ceramic body that sintering process occurs, provides convenience for the removing of raw material powder.The type of cooling is
Furnace is cold, and atmosphere is air atmosphere.By binder removal, the moisture and organic matter in green body are not only removed, also obtains green body
Uniform shrinkage realizes certain densification, volume contraction 4-30%, weightless 20-50%.
It is to be cooled to after room temperature, the crucible for being loaded with ceramic body is taken out from Muffle furnace.With hairbrush by billet surface or/
It is cleaned out with internal raw material powder, and wind leaching is carried out to green body with hair dryer, it is ensured that no raw material powder sticks in green body
Surface.
The ceramic body for completing binder removal is weighed, measured size and taken pictures.In conjunction with dumping pre-ceramic green body
Measurement data calculates weightlessness and dimensional contraction rate of the ceramic body during dumping.
The clean ceramic body of dumping is placed again into Muffle furnace, burning is warming up under the heating rate of 1~3 DEG C/min
Junction temperature keeps the temperature 1~12h, and atmosphere is air, then cools to room temperature with the furnace, takes out ceramic product.
The present invention carries out dumping to the ceramic body of high-glue content and sintering, obtained ceramic member are able to maintain good
Shape, intensity, surface smoothness and consistency have effectively pushed application of the 3D printing technique in ceramic forming field.It is right
The ceramic member for completing sintering process is weighed, measured size and is taken pictures.In conjunction with the measurement data of dumping pre-ceramic green body, calculate
The weightlessness and dimensional contraction rate of ceramic member during the sintering process.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Alumina ceramic tube is printed using Stereo Lithography technology, the solid content of ceramic body is 60%, the ruler of ceramic tube
It is very little be outer diameter 12mm, internal diameter 8mm, long 60mm, as shown in Figure 1a.Unbodied alumina powder is selected, in boat-shaped alumina crucible
(as shown in Figure 1 b) bottom spreads one layer of alumina powder, then ceramic tube green body is put into crucible, and aluminium oxide is filled up in ceramic tube
Powder, then ceramic tube green body is wholly embedded into alumina powder, as shown in Figure 2.Boat-shaped alumina crucible is put into Muffle furnace, is leaned on
The position of nearly stove thermocouple.200 DEG C are warming up within 7 hours, then was warming up to 500 DEG C with 10 hours and keeps the temperature 1 hour, then with 20 hours
It is warming up to 1100 DEG C and keeps the temperature 4 hours, last furnace cooling, atmosphere is air atmosphere.After being cooled to room temperature, crucible, cleaning are taken out
Alumina powder on ceramic tube green body is cleaned down the powder on surface with hairbrush, and with hair dryer further by remaining oxidation
Aluminium powder removing finishes.The alumina ceramic tube green body that dumping has been got well is put into Muffle furnace again and is sintered, was warming up to 15 hours
1700 DEG C keep the temperature 2 hours, furnace cooling, air atmosphere.After being cooled to room temperature, alumina ceramic tube is taken out, completes 3D printing oxygen
Change the dumping sintering process of aluminium ceramic tube.
Claims (2)
1. a kind of dumping and sintering process of 3D printing ceramic body characterized by comprising
(1) ceramic body that the solid content of 3D printing is 20~60wt.% is put into crucible, and use and ceramic body ingredient
Identical raw material powder embed and be filled the hollow structure in ceramic body, the ceramic body to ceramic body
For the ceramic body prepared by oxide, the oxide is Al2O3、TiO2、ZrO2、SiO2, in spinelle and mullite one
Kind；
(2) crucible for being placed with ceramic body is put into Muffle furnace, segmentation dumping, the segmentation dumping packet is carried out under air atmosphere
It includes first with 0.3~0.6 DEG C/min of heating rate from room temperature to 200 DEG C, heat preservation 2 hours or less；Again with 0.4~0.7
DEG C/min heating rate be warming up to 500 DEG C from 200 DEG C, heat preservation 3 hours or less；Again with 0.4~0.7 DEG C/min of heating speed
Rate is warming up to densification temperature from 500 DEG C, keeps the temperature 2~6 hours, cools to room temperature with the furnace；
(3) sintering temperature is warming up to 1~3 DEG C/min of heating rate, sintering time 1~12 hour；
Wherein, the densification temperature is 300~1000 DEG C lower than the sintering temperature of the ceramic body.
2. technique according to claim 1, which is characterized in that the purity of the raw material powder is not less than pure, the particle of analysis
Size is lower than 6 microns.
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| CN106810215B (en) * | 2017-01-18 | 2022-08-16 | 重庆摩方科技有限公司 | Preparation of ceramic slurry and 3D printing photocuring forming method |
| CN109485395A (en) * | 2018-01-15 | 2019-03-19 | 杭州创屹机电科技有限公司 | A kind of method of 3D printing high-strength ceramic mold |
| CN108424134B (en) * | 2018-02-13 | 2020-09-25 | 西安理工大学 | Garnet type solid solution magneto-dielectric functional dielectric ceramic material and preparation method thereof |
| CN112089103A (en) * | 2019-06-17 | 2020-12-18 | 深圳市卓力能电子有限公司 | Atomizer heating body and manufacturing method thereof |
| CN111302772A (en) * | 2020-02-23 | 2020-06-19 | 西北工业大学 | Argon atmosphere sintering method for 3D printing ceramic core |
| CN112479687A (en) * | 2020-12-16 | 2021-03-12 | 集美大学 | Ceramic 3D printed product and degreasing and roasting integrated process method thereof |
| CN115141023B (en) * | 2022-04-06 | 2024-01-05 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic |
| CN116063083A (en) * | 2022-12-19 | 2023-05-05 | 江西金石三维智能制造科技有限公司 | Rapid degreasing method for photo-curing slurry |
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| CN103817767A (en) * | 2014-03-14 | 2014-05-28 | 邓湘凌 | Method for manufacturing ceramic products with 3D printing technology |
| CN104591231A (en) * | 2013-10-31 | 2015-05-06 | 中国科学院上海硅酸盐研究所 | Fluorine-containing garnet-structure lithium ion oxide ceramic |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104591231A (en) * | 2013-10-31 | 2015-05-06 | 中国科学院上海硅酸盐研究所 | Fluorine-containing garnet-structure lithium ion oxide ceramic |
| CN103817767A (en) * | 2014-03-14 | 2014-05-28 | 邓湘凌 | Method for manufacturing ceramic products with 3D printing technology |
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