CN103936428B - Preparation method of rapid molding powder material used for three dimensional printing - Google Patents
Preparation method of rapid molding powder material used for three dimensional printing Download PDFInfo
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- CN103936428B CN103936428B CN201410092122.8A CN201410092122A CN103936428B CN 103936428 B CN103936428 B CN 103936428B CN 201410092122 A CN201410092122 A CN 201410092122A CN 103936428 B CN103936428 B CN 103936428B
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Abstract
The invention discloses a preparation method of a rapid molding powder material used for three dimensional printing. The method is characterized in that the method comprises the following steps: 1, powder material pretreatment: mixing 88-96% of a powder material with 4-12% of 3-aminopropyltriethoxysilane, and grinding at a rotating speed of 500-1000rpm for 2-6h to obtain a pretreated powder material; and 2, molding material preparation: adding 50-70% by mass of water, adding 0.5-1.0% of polyethylene glycol monooleyl ether, stirring for dissolving, adding 2-10% of polyvinyl alcohol, heating for dissolving, adding 25-40% of the pretreated powder material, stirring for uniform mixing, putting the obtained mixture in a grinder, carrying out normal temperature mixing grinding for 10-15h, and carrying out spray drying to obtain the rapid molding powder material. The rapid molding powder material can be directly molded at a temperature of 85-100DEG C under a pressure of 1-10MPa without sprinkling a binder, and has the advantages of simple preparation technology, easy condition control, low production cost and easy industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method for rapid three dimensional printing forming powdered material, belong to the Material Field of rapid shaping, particularly a kind of preparation technology for rapid three dimensional printing forming aluminum oxide, silicon carbide, ceramic powder material.
Background technology
Rapid Prototyping technique is also known as rapid prototype manufacturing (Rapid Prototyping Manufacturing, be called for short RPM) technology, being born in the later stage eighties 20th century, is the high-new manufacturing technology of one based on bing area method, is considered to the great achievement manufacturing field in recent years.It integrates mechanical engineering, CAD, reverse Engineering Technology, Layered Manufacturing Technology, Numeric Control Technology, Materials science, laser technology, automatically can change the prototype or direct finished parts with certain function, directly, quickly and accurately by design philosophy into, thus be the realization rate that the aspects such as the verification of part prototype, newly design philosophy provide a kind of high efficiency, low cost.That is, Rapid Prototyping technique is exactly the data utilizing three-dimensional CAD, by rapidform machine, material stacking is from level to level become physical prototypes.
3 D-printing (Three Dimonsion Printing, be called for short 3DP) be a kind of rapid shaping technique, the three-dimensional modeling data of Computer Design can be divided into synusia model data, specific raw materials in layer be piled up shaping until complete the structure of whole entity.3DP is shaping has the advantages such as cost is low, working process is pollution-free, shaping speed is fast.
3D printing technique has 3DP technology, FDM fusion stacking forming technique, SLA stereolithography techniques, SLS precinct laser sintering, DLP laser formation technology and UV ultraviolet forming technique, the different material therefor of technology is then completely different, the most often FDM3D printing technique applied with our the general population and family, this technology can enter into family, simple to operate, material therefor is generally easy to get, this technology prints product also close to our daily necessities, material used is environmental protection macromolecule material mainly, as: PLA, PCL PHA PBS PA ABS PC PS POM PVC, because this technology is generally print on the table, the smell that the macromolecular material of melting produces or decompose and produce objectionable impurities and directly contact with our people, easily cause safety problem.The product that industrial part etc. need some strength function can select the material adapted.
In existing formed material field, because SLS rapid shaping technique has the advantages such as raw material sources various and structure time that is part is shorter, therefore have in rapid shaping field and apply more widely.A kind of nylon powder material for laser sintering and moulding goods is disclosed in Chinese invention patent CN1379061A, by the improvement of chemosynthesis and technique, the surface of nylon powder material is processed, obtain sintering character excellent, moulded products intensity is high, the product of good toughness, simplifies the preparation technology of laser sintered nylon material, reduces cost.But SLS technique also exists many deficiencies and seriously limits the further application of SLS and popularize; Thus also make to be restricted based on SLS technological forming materials'use.
3DP technique and SLS technique similar, all adopt powdered material constituency shaping, difference is the powdered material of 3DP technique is not coupled together by the sintering layer by layer of laser, but under the effect of shower nozzle, with caking agent (as silica gel) by the cross section information " printing " of part on powdered material.Because 3DP is shaping by sprinkler caking agent, avoid the use cost of the agglomerating plant using the complex and expensive such as laser, be beneficial to using and promoting of rapid shaping technique.Disclosing a kind of preparation method for rapid three dimensional printing forming material in Chinese invention patent CN102093646 B, is powdered material is carried out a series of modification obtain modified powder materials A, modified powder materials A and caking agent B adapted during use.
Because the particle diameter of 3DP rapid prototyping material powder is comparatively large, make thin-walled parts not easy-formation, the formed precision of micro parts is not high enough, and surface exists obvious harsh feeling; In addition, because binding agent is firm not, there is the low grade of profiled member intensity not enough.In addition, the 3DP technological forming material that Vehicles Collected from Market is sold substantially monopolize by offshore company, price is high, serious restriction 3DP forming technique popularizing in China.
The present invention, by carrying out Dispersion on surface modification to powdered material, obtains ultra-fine powder materials and can reach submicron order even nano level, and the powdered material of uniform particle diameter; Start with from the formula of powder modification, the powdered material obtained under certain temperature and pressure can straight forming, does not need to spray caking agent, greatly simplifies and just does program.Not only intensity is high for institute's product that obtains, and also makes the realization be molded on 3DP rapidform machine of thin-walled micro parts become possibility; In addition, the method that this patent provides is simple, and cost is low.
Summary of the invention
Order of the present invention is to provide a kind of preparation method for rapid three dimensional printing forming powdered material, and rapid shaping powder does not need to spray binding agent can straight forming;
Object of the present invention is achieved through the following technical solutions.
For a preparation method for rapid three dimensional printing forming powdered material, be characterised in that the method has following processing step:
(1) powdered material pre-treatment: in shredder, the APTES of 4% ~ 12% is added by mass percentage concentration, add the powdered material of 88% ~ 96%, each component sum is absolutely, open shredder rotating speed at 500 ~ 1000 revs/min, grinding at room temperature 2 ~ 6 h, obtains pre-treatment powdered material;
(2) rapid shaping powdered material preparation: in the reactor, 50% ~ 70% water is added by mass percentage concentration, add the polyoxyethylene laurel ether of 0.5% ~ 1.0%, stirring and dissolving, add the polyvinyl alcohol of 2% ~ 10% again, after heating makes it dissolve, add the pre-treatment powdered material of 25% ~ 40%, each component sum is absolutely, is uniformly mixed, puts into shredder, normal temperature mixed grinding 10 ~ 15 h, then spraying dry, obtains rapid shaping powdered material, and the particle diameter of the rapid shaping powdered material obtained is within the scope of 200 ~ 600nm;
Powdered material described is in step (1) alchlor, silicon carbide, zirconium dioxide, ceramics powder, and the particle diameter of its powdered material is within the scope of 100 ~ 500nm;
In the spraying dry described in step (2), inlet temperature controls within the scope of 120 ~ 180 DEG C.
Particle size test method of the present invention is the granularity equivalent diameter size adopting laser particle analyzer to record.
Another object of the present invention is to provide a kind of application shaping on three-dimensional printer for rapid three dimensional printing forming powdered material, feature is: get rapid shaping powdered material and be placed on rapid three dimensional printing forming machine, on the horizontal plane X sprawling uniform rapid shaping powdered material and Y-direction (X and Y-direction represent the horizontal and vertical of horizontal plane respectively), then decline certain altitude in the vertical Z-direction of plane.Carry out sprawling of rapid shaping powdered material to lower one deck again, so repeat, after all having fed in raw material, temperature has been raised within the scope of 85 ~ 100 DEG C, and pressure can straight forming in the scope of 1MPa ~ 10MPa.
Compared with the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention obtains rapid shaping powdered material, does not need to spray binding agent heating 85 ~ 100 DEG C, and pressure can straight forming in the scope of 1MPa ~ 10MPa.
(2) the present invention obtains rapid shaping powdered material, and particle can reach submicron order even nano level, has meso-position radius grain little, the feature that particle size distribution is narrow, stable in properties; Can manufacture thin-walled model or small component by this rapid shaping powdered material, producing product, to have surface gloss high, and intensity is good, precision high.
(3) the present invention obtains rapid shaping powdered material, has preparation technology simple, and condition is easy to control, and production cost is low, is easy to suitability for industrialized production.
(4) the present invention obtains rapid shaping powdered material, can effective rapid shaping on three-dimensional printer, can be applicable to the three-dimensional printer of multiple different model.
Embodiment
Embodiment 1
(1) silicon carbide powder pretreatment: in shredder, adds the APTES of 7g, adds the silicon carbide of 93g, and open shredder rotating speed at 1000 revs/min, grinding at room temperature 4 h, obtains pre-treatment carborundum powder powder material;
(2) rapid shaping carborundum powder powder material preparation: in the reactor, add 60g water, add the polyoxyethylene laurel ether of 0.8g, stirring and dissolving, add the polyvinyl alcohol of 6g again, after heating makes it dissolve, add the pre-treatment carborundum powder powder material of 33.2g, be uniformly mixed, put into shredder, normal temperature mixed grinding 12 h, then spraying dry, obtains rapid shaping carborundum powder powder material.
Embodiment 2
(1) silicon carbide powder pretreatment: in shredder, adds the APTES of 12g, adds the silicon carbide of 88g, and open shredder rotating speed at 500 revs/min, grinding at room temperature 6h, obtains pre-treatment carborundum powder powder material;
(2) rapid shaping carborundum powder powder material preparation: in the reactor, add 66.5g water, add the polyoxyethylene laurel ether of 0.5g, stirring and dissolving, add the polyvinyl alcohol of 8g again, after heating makes it dissolve, add the pre-treatment carborundum powder powder material of 25g, be uniformly mixed, put into shredder, normal temperature mixed grinding 10 h, then spraying dry, obtains rapid shaping carborundum powder powder material.
Embodiment 3
(1) silicon carbide powder pretreatment: in shredder, adds the APTES of 4g, adds the silicon carbide of 96g, and open shredder rotating speed at 800 revs/min, grinding at room temperature 5h, obtains pre-treatment carborundum powder powder material;
(2) rapid shaping carborundum powder powder material preparation: in the reactor, add 50g water, add the polyoxyethylene laurel ether of 1.0g, stirring and dissolving, add the polyvinyl alcohol of 10g again, after heating makes it dissolve, add the pre-treatment carborundum powder powder material of 39g, be uniformly mixed, put into shredder, normal temperature mixed grinding 15 h, then spraying dry, obtains rapid shaping carborundum powder powder material.
Embodiment 4
(1) silicon carbide powder pretreatment: in shredder, adds the APTES of 10g, adds the silicon carbide of 90g, and open shredder rotating speed at 1000 revs/min, grinding at room temperature 2 h, obtains pre-treatment carborundum powder powder material;
(2) rapid shaping carborundum powder powder material preparation: in the reactor, add 70g water, add the polyoxyethylene laurel ether of 1.0g, stirring and dissolving, add the polyvinyl alcohol of 2g again, after heating makes it dissolve, add the pre-treatment carborundum powder powder material of 27g, be uniformly mixed, put into shredder, normal temperature mixed grinding 14 h, then spraying dry, obtains rapid shaping carborundum powder powder material.
Embodiment 5
(1) aluminium sesquioxide powdered material pre-treatment: in shredder, add the APTES of 7g, add the aluminium sesquioxide of 93g, open shredder rotating speed at 500 revs/min, grinding at room temperature 4 h, obtains pre-treatment aluminium sesquioxide powdered material;
(2) rapid shaping aluminium sesquioxide powdered material preparation: in the reactor, add 60g water, add the polyoxyethylene laurel ether of 0.8g, stirring and dissolving, add the polyvinyl alcohol of 6g again, after heating makes it dissolve, add the pre-treatment aluminium sesquioxide powdered material of 33.2g, be uniformly mixed, put into shredder, normal temperature mixed grinding 12 h, then spraying dry, obtains rapid shaping aluminium sesquioxide powdered material.
Embodiment 6
(1) aluminium sesquioxide powdered material pre-treatment: in shredder, add the APTES of 10g, add the aluminium sesquioxide of 90g, open shredder rotating speed at 800 revs/min, grinding at room temperature 3 h, obtains pre-treatment aluminium sesquioxide powdered material;
(2) rapid shaping aluminium sesquioxide powdered material preparation: in the reactor, add 55g water, add the polyoxyethylene laurel ether of 1.0g, stirring and dissolving, add the polyvinyl alcohol of 4g again, after heating makes it dissolve, add the pre-treatment aluminium sesquioxide powdered material of 40g, be uniformly mixed, put into shredder, normal temperature mixed grinding 11 h, then spraying dry, obtains rapid shaping aluminium sesquioxide powdered material.
Embodiment 7
(1) Zirconium dioxide powder pretreatment: in shredder, adds the APTES of 7g, adds the zirconium dioxide of 93g, and open shredder rotating speed at 1000 revs/min, grinding at room temperature 4 h, obtains pre-treatment Zirconium dioxide powder material;
(2) rapid shaping Zirconium dioxide powder material preparation: in the reactor, add 60g water, add the polyoxyethylene laurel ether of 0.8g, stirring and dissolving, add the polyvinyl alcohol of 6g again, after heating makes it dissolve, add the pre-treatment Zirconium dioxide powder material of 33.2g, be uniformly mixed, put into shredder, normal temperature mixed grinding 12 h, then spraying dry, obtains rapid shaping Zirconium dioxide powder material.
Embodiment 8
(1) Zirconium dioxide powder pretreatment: in shredder, adds the APTES of 9g, adds the zirconium dioxide of 91g, and open shredder rotating speed at 500 revs/min, grinding at room temperature 5 h, obtains pre-treatment Zirconium dioxide powder material;
(2) rapid shaping Zirconium dioxide powder material preparation: in the reactor, add 65g water, add the polyoxyethylene laurel ether of 0.5g, stirring and dissolving, add the polyvinyl alcohol of 5g again, after heating makes it dissolve, add the pre-treatment Zirconium dioxide powder material of 29.5g, be uniformly mixed, put into shredder, normal temperature mixed grinding 13 h, then spraying dry, obtains rapid shaping Zirconium dioxide powder material.
Embodiment 9
(1) ceramic powder material pre-treatment: in shredder, adds the APTES of 7g, adds the ceramics powder of 93g, and open shredder rotating speed at 800 revs/min, grinding at room temperature 4 h, obtains pre-treatment ceramic powder material;
(2) fast formed ceramic powdered material preparation: in the reactor, add 60g water, add the polyoxyethylene laurel ether of 0.8g, stirring and dissolving, add the polyvinyl alcohol of 6g again, after heating makes it dissolve, add the pre-treatment ceramic powder material of 33.2g, be uniformly mixed, put into shredder, normal temperature mixed grinding 12 h, then spraying dry, obtains fast formed ceramic powdered material.
Embodiment 10
(1) ceramic powder material pre-treatment: in shredder, adds the APTES of 11g, adds the ceramics powder of 89g, and open shredder rotating speed at 1000 revs/min, grinding at room temperature 2 h, obtains pre-treatment ceramic powder material;
(2) fast formed ceramic powdered material preparation: in the reactor, add 65g water, add the polyoxyethylene laurel ether of 0.5g, stirring and dissolving, add the polyvinyl alcohol of 4.5g again, after heating makes it dissolve, add the pre-treatment ceramic powder material of 30g, be uniformly mixed, put into shredder, normal temperature mixed grinding 15h, then spraying dry, obtains fast formed ceramic powdered material.
Using method: the rapid shaping powdered material synthesized in Example is placed on rapid three dimensional printing forming machine, on the horizontal plane X sprawling uniform rapid shaping powdered material and Y-direction (X and Y-direction represent the horizontal and vertical of horizontal plane respectively), then decline certain altitude in the vertical Z-direction of plane.Carry out sprawling of rapid shaping powdered material to lower one deck again, so repeat, after all having fed in raw material, temperature has been raised within the scope of 85 ~ 100 DEG C, and pressure can straight forming in the scope of 1MPa ~ 10MPa.The product obtained has higher crushing resistance, glossiness good.
Claims (5)
1. for a preparation method for rapid three dimensional printing forming powdered material, it is characterized in that, the method has following processing step:
(1) powdered material pre-treatment: in shredder, add the APTES of 4% ~ 12% by mass percentage, add the powdered material of 88% ~ 96%, each component sum is absolutely, open shredder rotating speed at 500 ~ 1000 revs/min, grinding at room temperature 2 ~ 6h, obtains pre-treatment powdered material;
(2) rapid shaping powdered material preparation: in the reactor, add 50% ~ 70% water by mass percentage, add the polyoxyethylene laurel ether of 0.5% ~ 1.0%, stirring and dissolving, add the polyvinyl alcohol of 2% ~ 10% again, after heating makes it dissolve, add the pre-treatment powdered material of 25% ~ 40%, each component sum is absolutely, is uniformly mixed, puts into shredder, normal temperature mixed grinding 10 ~ 15h, then spraying dry, obtains rapid shaping powdered material, and the particle diameter of the rapid shaping powdered material obtained is within the scope of 200 ~ 600nm.
2. a kind of preparation method for rapid three dimensional printing forming powdered material according to claim 1, is characterized in that: described powdered material is aluminum oxide, silicon carbide, zirconium dioxide.
3. a kind of preparation method for rapid three dimensional printing forming powdered material according to claim 1, is characterized in that: the particle diameter of described powdered material is within the scope of 100 ~ 500nm.
4. a kind of preparation method for rapid three dimensional printing forming powdered material according to claim 1, is characterized in that: in the spraying dry described in step (2), inlet temperature controls within the scope of 120 ~ 180 DEG C.
5. the application during the rapid shaping powdered material prepared by method according to claim 1 is shaping on three-dimensional printer.
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| CN104446393A (en) * | 2014-12-01 | 2015-03-25 | 青岛麦特瑞欧新材料技术有限公司 | Yttrium-doped inorganic nanocomposite material for 3D printing and preparation method of yttrium-doped inorganic nanocomposite material |
| CN104448744B (en) * | 2014-12-03 | 2016-06-08 | 谢宝军 | A kind of raw material for rapid shaping and corresponding three-dimensional fast shaping method |
| CN104944962B (en) * | 2015-03-23 | 2017-08-15 | 济南大学 | A kind of preparation of laser sintering rapid forming silicon nitride ceramic powder |
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| EP2233449B1 (en) * | 2009-03-27 | 2014-12-17 | Ivoclar Vivadent AG | Use of a slip for the production of dental ceramics with hot melt inkjet printing methods |
| CN102093646B (en) * | 2010-10-29 | 2012-07-18 | 华南理工大学 | Material for rapid three dimensional printing forming and preparation method thereof |
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