CN104526838B - Method for 3D ceramic printing forming - Google Patents

Method for 3D ceramic printing forming Download PDF

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Publication number
CN104526838B
CN104526838B CN201410840236.6A CN201410840236A CN104526838B CN 104526838 B CN104526838 B CN 104526838B CN 201410840236 A CN201410840236 A CN 201410840236A CN 104526838 B CN104526838 B CN 104526838B
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ceramic
pottery
shaping
printing shaping
ceramics
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CN201410840236.6A
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Chinese (zh)
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CN104526838A (en
Inventor
邬国平
李妙妙
谢方民
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宁波伏尔肯陶瓷科技有限公司
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS, SLAG, OR MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • 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

Abstract

The invention discloses a method for 3D ceramic printing forming. The method comprises the following steps that (1) a 3D model of a target part is established; (2) layering processing is performed, and layered data are imported into a manufacturing program; (3) ceramic slurry is prepared; (4) the prepared ceramic slurry is added into a 3D printer to be made into a ceramic green body quickly formed; (5) the green body is cured at curing temperature for 10 min-60 min and then is placed in a drying oven for drying; (6) the dried green body is dewaxed and sintered to be made into the target part. The method is simple in technology and low in equipment cost; the distance between powder particles in the ceramic slurry can be reduced in the extrusion process, and therefore density is high; besides, the method is not limited by the type of ceramic particles and the shape of the part and is suitable for manufacturing ceramic products made of various ceramic materials and in various complex shapes.

Description

The method of pottery 3D printing shaping

Technical field

A kind of method that the present invention relates to pottery 3D printing shaping.

Background technology

Ceramic material has mechanical property (high intensity, high rigidity, high-wearing feature), thermal property (high temperature resistant, low thermal coefficient of expansion and thermal shock resistance) and the chemical stability of excellence, is widely used in the industrial circles such as petrochemical industry, Ferrous Metallurgy, mechano-electronic, Aero-Space, energy environment protection, nuclear energy, automobile, high temperature kiln.At present ceramic forming material method mainly has: extruded, injection moulding, isostatic pressing, flow casting molding etc., when these techniques prepare component, the mould with respective shapes need to be prepared according to the shape of component, if the structure of component varies slightly, it is accomplished by again preparing mould or needing sample is carried out machining, thus increases preparation cost.And limited by mould, these techniques are suitable for preparing the goods of simple shape.Along with industrial expansion, these conventional molding process can not meet the requirement of some special dimension.Rapid shaping technique (RP) is a kind of novel forming technology fast-developing in recent years, this technology utilization computer CAD software designed component, discrete and the numerical control molding system by software hierarchy, utilize the mode such as laser beam, hot melt nozzle that the special materials such as metal dust, ceramic powders, plastics, histiocyte are successively piled up bonding, final superposition molding, produces entity products.This technique, compared with traditional molding methods, has the following characteristics that (1) can prepare complex-shaped goods；(2) participating in without any mould or model in forming process, make process more integrated, the manufacturing cycle shortens, and production efficiency is high；(3) molded body geometry and size can be changed at any time by software processing system, it is not necessary to wait manufacturing and designing of mould, be greatly shortened the new product development time；(4) advantages such as the small electronic ceramics goods of structure can be prepared.Therefore, rapid shaping technique is paid close attention to widely in recent years.

Rapid shaping technique mainly has stereolithography technology (SLA), selective laser sintering (SLS), layer separated growth (LOM), 3 D-printing (3DP) etc. at present.The most existing report about ceramic material rapid shaping, as " quick manufacturing process of a kind of complicated ceramic part " of patent No. CN101391896A uses, ceramic powders and liquid photosensitive resin are uniformly mixed with ceramic size, in Stereolithography machine, then enter rapid shaping prepare biscuit of ceramics (SLA).Low-temperature reinforcement agent is mixed homogeneously by patent No. CN101890480 " a kind of ceramic core quick forming fabri-cation method " with ceramic powder, obtain the ceramic post sintering powder for SLS rapid shaping, carry out SLS rapid shaping with ceramic post sintering powder and obtain ceramic core green compact, and green compact are strengthened front pretreatment, defat, pre-burning, sintering obtain ceramic core (SLS).The patent No. CN101391896A quick manufacturing process of ceramic part " a kind of complicated " with scribble high polymer binder ceramic membrane as raw material, the ceramic part of shaped three dimensional just base on rapid prototyping system is manufactured at lamella material's layer, isostatic cool pressing process is carried out after first for ceramic part base is covered with jacket, finally carry out defat, sintering, post processing, obtain ceramic part (LOM).Patent No. CN1368386A " composite manufacturing method of Artificial bioactive bone bone based on rapid shaping " makes one on rapidform machine and adds heat container with controlled heating system, container bottom is opened the material of a 0.2mm and is extruded hole, emulsifying sugar addition pressurizing vessel is realized Layered manufacturing, obtains emulsifying sugar artificial bone transoid (3DP).

Stereolithography technology (SLA) prepares ceramic material owing to liquid photosensitive resin cost used is high, selectable range is little, resin has certain toxicity, apparatus expensive etc. not to be used widely；Existing selective laser sintering (SLS), 3 D-printing (3DP) are prepared ceramic material to there is between ceramic powder particle spacing big, and green density is low, in high-temperature sintering process cannot densification, the affected problem of ceramic performance；Layer separated growth (LOM) technology requires that to ceramic substrate difficulty removed by high, redundance material.

Summary of the invention

The technical problem to be solved is, the shortcoming overcoming above prior art: technique is simple, equipment cost is low to provide one, the spacing of powder particle in ceramic size can be reduced in extrusion, consistency is high, and do not limited by ceramic particle kind and part shape, the method being suitable for preparing the ceramic 3D printing shaping of the ceramic of various ceramic material, various complicated shape.

The technical solution of the present invention is as follows: a kind of method of pottery 3D printing shaping, comprises the following steps:

(1) build the threedimensional model of target part, be STL formatted file by data model translation；

(2) by the delamination software of rapidform machine, STL formatted file is carried out layered shaping, then individual-layer data is imported in fabrication schedule；

(3) by ceramic powders, deionized water, dispersant, defoamer and firming agent mix homogeneously ball milling 1～8h；Then the slurry after ball milling is carried out in froth in vacuum machine froth in vacuum 10～60min and is prepared as ceramic size；

(4) ceramic size of preparation is joined in the barrel of 3D printer, barrel temperature is heated to 50～250 DEG C, be incubated 5～30min；The shower nozzle of 3D printer is under the control of fabrication schedule, become extrusion silk according to the individual-layer data extruded ceramic slurry in step (2) and print cross section thin layers, firming agent in extrusion silk starts solidification at curing temperatures, the entity of Formation cross-section thin layer, by piling up layer by layer, prepare the base substrate of pottery rapid shaping；

(5), after base substrate being solidified 10～60min at curing temperatures, it is placed in baking oven and is dried 10～60min in 40～80 DEG C；

(6) carry out dried base substrate dewaxing, sintering prepared target part.

As optimization, described in step (3) in ceramic size, the content of ceramic powders is 10～95 wt%；Curing agent content is 0.1～20wt%；The content of dispersant is 0.1～10wt%；The content of defoamer is 0.1～10wt%；Surplus is deionized water.

Described ceramic powders is one or more in oxide ceramics (such as aluminium oxide ceramics, zirconia ceramics, magnesia ceramics), carbide ceramics (such as reaction silicon carbide ceramics, without pressure silicon carbide ceramics, boron carbide ceramics, titanium carbide ceramic, zirconium carbide ceramics), nitride ceramics (silicon nitride ceramics, boron nitride ceramics, aluminium nitride ceramics, titanium nitride ceramic), bioceramic, glass ceramics.

As preferably, described ceramic powders is the one in aluminium oxide ceramics, zirconia ceramics, reaction silicon carbide ceramics, nothing pressure silicon carbide ceramics, boron carbide ceramics.

The mean diameter of described ceramic powders is 0.5～100 μm.

Described firming agent is water solublity colloidal sol (such as gelatin, Ludox, sodium alginate, agarose), organic monomer (such as acrylamide) and cross-linking agent (methylene-bisacrylamide), thermoplastic (such as thermoplastic resins such as paraffin and polyethylene, polypropylene, polybutene, polystyrene).

As optimization, described firming agent is water solublity colloidal sol.

As optimizing further, described water solublity colloidal sol is the one in gelatin, Ludox, sodium alginate, agarose.

As optimization, described water solublity colloidal sol is agarose.

The injection diameter of described shower nozzle is 60 μm～5mm, and barrel heating-up temperature is 50～250 DEG C, and after extrusion, solidification temperature is-30 DEG C～120 DEG C, and ceramic size extruded velocity is 0.5～100mm/s, and the spacing between extrusion silk and silk is 0.01～10mm.

Described dispersant is the one in ammonia, Tetramethylammonium hydroxide, citrate, polyacrylate, six phosphorus meta-acid sodium, Polyetherimide, Radix Acaciae senegalis, sodium tripolyphosphate, Polyethylene Glycol, waterglass, triethanolamine, polycarboxylic acids ammonium salt, polymine (PEI).

Described defoamer is the one in n-octyl alcohol, n-butyl alcohol, tributyl phosphate, alkyl-silicone oil, ethylene glycol.

3D printing technique is combined the curing characteristics of water-soluable gel by the present invention first, is applied to the quick manufacturing process of ceramic material, is not limited by ceramic material and parts shape, can go out, with rapid shaping, the ceramic material that precision is high, relative density is high.Preparation for complicated shape ceramic material provides new process, greatly reduces R&D cycle and the cost of complicated shape ceramic part, it is achieved that the quick Non-mould shaping of ceramic material.

The invention has the beneficial effects as follows: the present invention utilizes the curing characteristics of water-soluable gel, aqueous-based ceramic slurry adds a certain amount of firming agent, utilize 3D printing shaping technique to prepare the ceramic component of variously-shaped complexity.Present invention process is simple, equipment cost is low, the spacing of powder particle in ceramic size can be reduced in extrusion, consistency is high, and do not limited by ceramic particle kind and part shape, being suitable for preparing various ceramic material, the ceramic of various complicated shape, the rapid shaping for ceramic part provides a kind of new method.

Accompanying drawing explanation

The process chart of the method for Fig. 1 pottery of the present invention 3D printing shaping.

Detailed description of the invention

With specific embodiment, the present invention is described in further details below, but the present invention is not only limited to specific examples below.

Embodiment one

As it is shown in figure 1, the process step of the invention includes:

1) foundation of threedimensional model.According to the actual requirements, with the threedimensional model of Pro/E or AutoCAD software construction part, and three-dimensional modeling data is converted to STL formatted file；

2) using the delamination software of rapidform machine that threedimensional model is carried out layered shaping, the data after layering import in fabrication schedule；

3) take 250g reaction bonded sic raw material powder (powdered carbon and α-SiC are 1 4～99 to mix with mass ratio), after 0.306g ammonia, 40g deionized water stirring 30min, add 1.8g tributyl phosphate, 1.5g gelatin, ball milling 2h in high speed ball mill；

4) by the slurry after ball milling in froth in vacuum machine under-0.08MPa vacuum de-bubble 10min；

5) being placed in by the slurry after de-bubble in the barrel of rapidform machine (preferably motor pushing microinjection formula 3D printer), begin to warm up barrel, arranging barrel heating-up temperature is 70～100 DEG C；After insulation 20min, the shower nozzle of rapidform machine is under the control of fabrication schedule, become extrusion silk according to the individual-layer data extruded ceramic slurry in step (2) and print cross section thin layers, extrusion silk solidifies under room temperature (25 DEG C), the entity of Formation cross-section thin layer, by piling up layer by layer, prepare the biscuit of pottery rapid shaping；Described extrusion filament diameter is 60 μm～5mm, and ceramic size extruded velocity is 0.5～100mm/s, and the spacing between extrusion silk and silk is 0.01～10mm.

6) biscuit of curing molding is dried at 60 DEG C 30min, at 80 DEG C, is then dried 30min, makes biscuit be completely dried；

7) dried biscuit dewaxes.Dewaxing temperature curve is: be incubated 1h from room temperature to 160 DEG C, then heats to 600 DEG C of insulation 1h, is then warming up to 850 DEG C of insulation 2h；

8) reaction-sintered.Biscuit after dewaxing is embedded in Si grain, carries out reaction-sintered under vacuo；Sintering temperature curve is: from room temperature to 600 DEG C, then heats to 1000 DEG C, is then warming up to 1550 DEG C of insulation 2h, and sintered density reaches 3.05g/cm3Above.

Embodiment two

The present embodiment is unlike embodiment one, the ceramic powders used in step 3) is alumina ceramic powder, firming agent is agarose, step 8) is sintered to: from room temperature with the ramp of 2 DEG C/min to 500 DEG C, then with the ramp of 10 DEG C/min to 800 DEG C, then being incubated 2h with the ramp of 8 DEG C/min to 1700 DEG C, the Alumina Ceramics Sintering density obtained is 3.85 g/cm3Above.

Embodiment three

The present embodiment is unlike embodiment one, the ceramic powders used in step 3) is zirconia ceramics powder, firming agent is organic monomer acrylamide and cross-linking agent methylene-bisacrylamide, step 8) is sintered to: from room temperature with the ramp of 2 DEG C/min to 500 DEG C, then with the ramp of 10 DEG C/min to 800 DEG C, then being incubated 3h with the ramp of 8 DEG C/min to 1460 DEG C, the sintered density obtaining zirconia ceramics is 5.55 g/cm3Above.

The present invention prepares the process of ceramic part based on 3D printing shaping technology, by adding firming agent, rapid shaping in 3D printer in aqueous-based ceramic slurry, obtains the ceramic material of required form by being dried, dewax, sintering.Its general principles is the gel solidification characteristic utilizing water-soluable gel material, a certain amount of gel solidification agent is added in aqueous-based ceramic slurry, ball milling mixing final vacuum de-bubble, gained ceramic size is placed in 3D printer (preferably motor pushing microinjection formula 3D printer) barrel, by barrel heating being improved viscosity and the mobility of slurry, ceramic size is extruded from syringe needle under stepper promotes, after extrusion silk solidifies at a certain temperature, it is complex parts biscuit by the rapid shaping that is layering.Ceramic part is obtained finally by being dried, dewax, sintering.The method can be with the ceramic body of the various complicated shape of molding, it is not necessary to mould, it is not necessary to the later stage goes material to process, and technique is simple, low cost.

Below it is only that inventive feature implements example, scope is not constituted any limitation.The technical scheme that all employings exchange on an equal basis or equivalence is replaced and formed, within the scope of all falling within rights protection of the present invention.

Claims (7)

1. the method for a ceramic 3D printing shaping, it is characterised in that: comprise the following steps:
(1) build the threedimensional model of target part, be STL formatted file by data model translation；
(2) by the delamination software of rapidform machine, STL formatted file is carried out layered shaping, then will layering Data import in fabrication schedule；
(3) by ceramic powders, deionized water, dispersant, defoamer and firming agent mix homogeneously ball milling 1～ 8h, then carries out the slurry after ball milling froth in vacuum 10～60min in froth in vacuum machine and is prepared as ceramic slurry Material；
(4) ceramic size of preparation is joined in the barrel of 3D printer, barrel temperature is heated to 50～ 250 DEG C, it is incubated 5～30min；The shower nozzle of 3D printer is under the control of fabrication schedule, according to step (2) In individual-layer data extruded ceramic slurry become extrusion silk print cross section thin layers, the firming agent in extrusion silk is solid Start solidification, the entity of Formation cross-section thin layer at a temperature of change, by piling up layer by layer, prepare pottery rapid shaping Base substrate；
(5), after base substrate being solidified 10～60min at curing temperatures, it is placed in baking oven and is dried in 40～80 DEG C 10～60min；
(6) carry out dried base substrate dewaxing, sintering prepared target part；
Described in step (3) in ceramic size, the content of ceramic powders is 10～95wt%；Curing agent content It is 0.1～20wt%；The content of dispersant is 0.1～10wt%；The content of defoamer is 0.1～10wt%；Remaining Amount is deionized water；
Described firming agent is water solublity colloidal sol；Described water solublity colloidal sol be gelatin, Ludox, sodium alginate, One in agarose.
The method of pottery 3D printing shaping the most according to claim 1, it is characterised in that: described Ceramic powders is aluminium oxide ceramics, zirconia ceramics, reaction silicon carbide ceramics, nothing pressure silicon carbide ceramics, carbonization One in boron pottery.
The method of pottery 3D printing shaping the most according to claim 1, it is characterised in that: described pottery The mean diameter of porcelain powder is 0.5～100 μm.
The method of pottery 3D printing shaping the most according to claim 1, it is characterised in that: described water Dissolubility colloidal sol is agarose.
The method of pottery 3D printing shaping the most according to claim 1, it is characterised in that: described spray The injection diameter of head is 60 μm～5mm, and barrel heating-up temperature is 50～250 DEG C, and after extrusion, solidification temperature is -30 DEG C～120 DEG C, ceramic size extruded velocity is 0.5～100mm/s, and the spacing between extrusion silk and silk is 0.01～10mm.
The method of pottery 3D printing shaping the most according to claim 1, it is characterised in that: described Dispersant is ammonia, Tetramethylammonium hydroxide, citrate, polyacrylate, six phosphorus meta-acid sodium, polyethers acyl Imines, Radix Acaciae senegalis, sodium tripolyphosphate, Polyethylene Glycol, waterglass, triethanolamine, polycarboxylic acids ammonium salt, One in polymine (PEI).
The method of pottery 3D printing shaping the most according to claim 1, it is characterised in that: described Defoamer is the one in n-octyl alcohol, n-butyl alcohol, tributyl phosphate, alkyl-silicone oil, ethylene glycol.
CN201410840236.6A 2014-12-30 2014-12-30 Method for 3D ceramic printing forming CN104526838B (en)

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