CN107434417A - Make the ceramic powder slurry and direct write shaped three dimensional structure preparation method that base substrate is conformal - Google Patents
Make the ceramic powder slurry and direct write shaped three dimensional structure preparation method that base substrate is conformal Download PDFInfo
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Abstract
The invention belongs to 3D printing field shaping technique, more particularly to making the conformal ceramic powder slurry of base substrate and direct write shaped three dimensional structure preparation method, a certain proportion of water, ceramic powder and dispersant are mixed, the slurry of suitable viscosity and solid content is made, then soluble long-chain organic matter is added in the ceramic powder slurry of direct write shaping, powder granule is fixed using its long-chain characteristic, so as to realize the indeformable purpose of molding blank.
Description
Technical field
The present invention relates to 3D printing field shaping technique, and in particular to makes the ceramic powder slurry and direct write shaped three dimensional structure preparation method that base substrate is conformal.
Background technology
Direct write forming technique（Direct
Ink Writing）It is a kind of new ceramic material 3D printing forming technique【J
A Lewis. Colloidal processing of ceramics. Journal of the American Ceramic Society,
2000, 83(10): 2341-2359.】.The technology is first by area of computer aided（CAD）The pattern of the three-dimensional structure of design, then the ceramic powder slurry conveying device being made up of syringe and pin mouth on Z axis is arranged on by computer controlled automatic, slurry in syringe is extruded to the line style fluid of accurate dimension out of pin mouth, X-Y axles move according to the track of program setting simultaneously, by line style fluid deposition on the moving platform, the first Rotating fields are obtained.After completing the first formable layer, Z axis motor drives slurry conveying device to be moved to the height that organization plan determines exactly up, and the second formable layer will be carried out on the first Rotating fields.Then, by way of being successively superimposed, the complex three-dimensional stereochemical structure that can not be prepared with traditional moulding process is obtained.
In direct write forming process, the phenomenon that " cross flow " etc. changes blank shape can usually occur after pin mouth extrusion for ceramic powder slurry, therefore direct write molding blank is kept shape invariance is the key that can shaping be carried out and can dimensional accuracy ensure.To solve this problem, the solid volume fraction of researchers' generally use increase slurry or increasing the mode of content of organic matter dispersant makes the molding blank conformal【J III Cesarano, T A Baer, P Calvert.
Recent developments in freeform fabrication of dense ceramics from slurry
deposition. Albuquerque, NM: Sandia National Labs., 1997.】.But usually there is printhead and blocks the situation that pin etc. makes direct write shaping not continue in such case.
The content of the invention
In order to solve the above technical problems, we have proposed a kind of novel, easy and can realize that molding blank is indeformable and make the conformal ceramic powder slurry of base substrate and direct write shaped three dimensional structure preparation method.
To reach above-mentioned purpose, the invention provides a kind of ceramic powder slurry preparation method for making base substrate conformal, it comprises the following steps：
1）A certain proportion of water, ceramic powder, sintering aid and dispersant are subjected to ball milling, slurry is made；
2）One or more of soluble long-chain organic matters are added in the slurry and continue ball milling；
Wherein, the solid content of powder is 0.01% ~ 99%；The addition of dispersant is the 0.001% ~ 10% of powder quality.
Preferably, the ceramic powder is one kind in alumina powder, beta-silicon nitride powder, Zirconium powder, aluminium nitride powder.
Preferably, the sintering aid is one or more in yittrium oxide, lanthana, magnesia.
Preferably, the dispersant is one kind in anionic dispersing agent, cationic dispersing agent.
Preferably, the anionic dispersing agent is one or more in polyacrylic, poly class, polystyrene sulphuric acid class, polyphenyl sulphonic acids, polyvinyl sulfonic acid class, polyvinyl class.
Preferably, it is one or more in the cationic dispersing agent polyethyleneimine amine hydrochlorate class, polyvinyl pyridine class, polyethylene amine.
Preferably, the abrading-ball that the ball milling uses is a kind of in zirconia ball, alumina balls.
Preferably, the soluble long-chain organic matter is one or more of compositions in polyacrylamide, polyvinyl alcohol or cellulose, and molecular weight is all higher than 100,000.
Present invention also offers a kind of preparation method using ceramic powder slurry direct write shaped three dimensional structure, it comprises the following steps：
1）Ceramic powder slurry is carried out to be stirred under vacuum degasification 5min ~ 30min；
2）Ceramic powder slurry is loaded into direct write former, under control of a computer program, by way of being successively superimposed, prepares 3-D solid structure；
Wherein, process parameter control scope during slurry progress direct write shaping is：Pressure limit is 10 ~ 2000PSI；Printhead translational speed is 0.01 ~ 600mm/sec；Forming temperature scope is 20 ~ 40 DEG C；Shaping humidity range is ＞ 40%.
Preferably, the ceramic powder slurry is prepared by the above-mentioned ceramic powder slurry preparation method for making base substrate conformal.
Pass through above-mentioned technical proposal, the base substrate that the present invention is molded direct write using the method for adding soluble long-chain organic matter in ceramic powder slurry is indeformable, the advantage is that：
First, direct write shaping ceramic powder slurry need to only control the order of addition of soluble long-chain organic matter and addition to obtain；
When the 2nd, carrying out direct write shaping using ceramic powder slurry proposed by the present invention, it is not easy to phenomena such as gaging somebody, beneficial to the control of direct write moulding process；
3rd, the present invention's has a wide range of application, the control of shape when being molded available for a variety of ceramic powder slurry direct writes.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made belongs to the scope of protection of the invention.
The embodiment of the present invention is described in further detail below.
Embodiment 1. uses polyacrylamide to prepare ZrO for soluble long-chain organic matter23-D solid structure, its is specific as follows：
By 3g dispersants Sodium Polyacrylate and Y2O3Stable 180g ZrO2Powder（D50 is 0.8 μm）It is added in 10mL deionized waters and carries out ball milling, then adds concentration 10%, 2g polyacrylamide solutions（M.W. 1,000,000）, continue ball milling 1 hour, obtain ZrO2 slurries, wherein, abrading-ball is 200g zirconia ball, and ball milling speed is 50 rad/min；
By the ZrO of acquisition2Slurry is carried out after being stirred under vacuum degasification 5min, then carries out direct write shaping, obtains crisscross 3-D solid structure, and temperature control is 32 DEG C or so, and humid control 41%, direct write briquetting pressure is 60PSI, and printhead translational speed is 8mm/sec.
Example 2, polyacrylamide is used to prepare Si for soluble long-chain organic matter3N43-D solid structure, its is specific as follows：
First by 8g polyethylene of dispersing agent imines and 820g Si3N4Powder（D50 is 11 μm）, 5g sintering aids Y2O3With 2g La2O3It is added in 50mL deionized waters and carries out ball milling 13 hours, then adds concentration 5%, 2g polyacrylamide solutions（M.W. 1,200,000）, continue ball milling 0.5 hour, obtain Si3N4Slurry, wherein, abrading-ball is 800g zirconia ball, and ball milling speed is 60 rad/min；
By the Si of acquisition3N4Slurry is carried out after being stirred under vacuum degasification 8min, then carries out direct write shaping, obtains the tubulose 3-D solid structure that 30 stackings add, temperature control is 22 DEG C or so, and humid control 61%, direct write briquetting pressure is 30PSI；Printhead translational speed is 5mm/sec.
Example 3, polyvinyl alcohol is used to prepare Al for soluble long-chain organic matter2O33-D solid structure, its is specific as follows：
By 6g dispersants polyacrylic acid and 310g Al2O3Powder（D50 is 1.5 μm）, 3.1g sintering aids MgO be added in 50mL deionized waters and carry out ball milling 20 hours, then add concentration 10%, 1g polyvinyl alcohol water solutions（M.W. 800,000）, continue ball milling 2 hours, obtain Al2O3Slurry, wherein, abrading-ball is 320g alumina balls, and ball milling speed is 10 rad/min；
By the Al of acquisition2O3Slurry is carried out after being stirred under vacuum degasification 5min, then carries out direct write shaping, obtains 3-D solid structure, and temperature control is 32 DEG C or so, and humid control 42%, direct write briquetting pressure is 40PSI, and printhead translational speed is 10mm/sec.
Example 4, polyvinyl alcohol is used to prepare AlN 3-D solid structures for soluble long-chain organic matter, its is specific as follows：
By 16g dispersants ammonium polyacrylates and 350g AlN powders（D50 is 2.8 μm）2 g sintering aids Y2O3 and 3.2g La2O3, which is added in 38mL deionized waters, carries out ball milling 22 hours, then adds concentration 5%, 2g polyvinyl alcohol water solutions（M.W.
1000000）, continue ball milling 1.6 hours, obtain AlN slurries, wherein, abrading-ball is 420g zirconia ball, and ball milling speed is 32 rad/min；
The AlN slurries of acquisition are carried out after being stirred under vacuum degasification 6min, then carry out direct write shaping, obtain crisscross 3-D solid structure.Temperature control is 30 DEG C or so, and humid control 72%, direct write briquetting pressure is 90PSI, and printhead translational speed is 100mm/sec.
Example 5, cellulose is used to prepare ZrO for soluble long-chain organic matter23-D solid structure, its is specific as follows：
By 4g dispersants Sodium Polyacrylate and Y2O3Stable 310g ZrO2 powders（D50 is 0.8 μm）It is added in 10mL deionized waters and carries out ball milling, then adds concentration 5%, 1g cellulose aqueous solutions（M.W. 150,000）, continue ball milling 2 hours, obtain ZrO2Slurry, wherein, abrading-ball is 350g zirconia ball, and ball milling speed is 22 rad/min；
By the ZrO of acquisition2Slurry is carried out after being stirred under vacuum degasification 12min, then carries out direct write shaping, obtains crisscross 3-D solid structure, and temperature control is 32 DEG C or so, and humid control 50%, direct write briquetting pressure is 90PSI, and printhead translational speed is 28mm/sec.
Example 6, cellulose is used to prepare Si for soluble long-chain organic matter3N43-D solid structure, its is specific as follows：
First by 6g dispersants TMAH and 600g Si3N4Powder（D50 is 15 μm）, 3g sintering aid Y2O3With 2g La2O3It is added in 60mL deionized waters and carries out ball milling 15 hours, then adds concentration 10%, 1g cellulose aqueous solutions（M.W. 100,000）, continue ball milling 1 hour, obtain Si3N4Slurry, wherein, abrading-ball is 800g zirconia ball, and ball milling speed is 50 rad/min；
By the Si of acquisition3N4Slurry is carried out after being stirred under vacuum degasification 8min, then carries out direct write shaping, obtains crisscross 3-D solid structure, and temperature control is 28 DEG C or so, and humid control 60%, direct write briquetting pressure is 30PSI, and printhead translational speed is 25mm/sec.
Above-described is only the preferred embodiment of the present invention, it is noted that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to protection scope of the present invention.
Claims (10)
1. a kind of ceramic powder slurry preparation method for making base substrate conformal, it is characterised in that it comprises the following steps：
1）A certain proportion of water, ceramic powder, sintering aid and dispersant are subjected to ball milling, slurry is made；
2）One or more of soluble long-chain organic matters are added in the slurry and continue ball milling；
Wherein, the solid content of powder is 0.01% ~ 99%；The addition of dispersant is the 0.001% ~ 10% of powder quality.
2. a kind of ceramic powder slurry preparation method for making base substrate conformal according to claim 1, it is characterised in that the ceramic powder is one kind in alumina powder, beta-silicon nitride powder, Zirconium powder, aluminium nitride powder.
3. a kind of ceramic powder slurry preparation method for making base substrate conformal according to claim 1, it is characterised in that the sintering aid is one or more in yittrium oxide, lanthana, magnesia.
4. a kind of ceramic powder slurry preparation method for making base substrate conformal according to claim 1, it is characterised in that the dispersant is one kind in anionic dispersing agent, cationic dispersing agent.
A kind of 5. ceramic powder slurry preparation method for making base substrate conformal according to claim 4, characterized in that, the anionic dispersing agent is one or more in polyacrylic, poly class, polystyrene sulphuric acid class, polyphenyl sulphonic acids, polyvinyl sulfonic acid class, polyvinyl class.
6. a kind of ceramic powder slurry preparation method for making base substrate conformal according to claim 4, it is characterised in that one or more in the cationic dispersing agent polyethyleneimine amine hydrochlorate class, polyvinyl pyridine class, polyethylene amine.
7. a kind of ceramic powder slurry preparation method for making base substrate conformal according to claim 1, it is characterised in that the abrading-ball that the ball milling uses is a kind of in zirconia ball, alumina balls.
A kind of 8. ceramic powder slurry preparation method for making base substrate conformal according to claim 1, it is characterized in that, the soluble long-chain organic matter is one or more of compositions in polyacrylamide, polyvinyl alcohol or cellulose, and molecular weight is all higher than 100,000.
9. a kind of preparation method using ceramic powder slurry direct write shaped three dimensional structure, it is characterised in that it comprises the following steps：
1）Ceramic powder slurry is carried out to be stirred under vacuum degasification 5min ~ 30min；
2）Ceramic powder slurry is loaded into direct write former, under control of a computer program, by way of being successively superimposed, prepares 3-D solid structure；
Wherein, process parameter control scope during slurry progress direct write shaping is：Pressure limit is 10 ~ 2000PSI；Printhead translational speed is 0.01 ~ 600mm/sec；Forming temperature scope is 20 ~ 40 DEG C；Shaping humidity range is ＞ 40%.
A kind of 10. preparation method using ceramic powder slurry direct write shaped three dimensional structure according to claim 9, characterized in that, the ceramic powder slurry is prepared by the ceramic powder slurry preparation method for making base substrate conformal any one of claim 1 ~ 8.
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Cited By (10)
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|---|---|---|---|---|
| CN108069706A (en) * | 2017-12-15 | 2018-05-25 | 天津大学 | A kind of forming method of the fiber reinforced ceramic thin-wall part based on 3D printing technique |
| CN108298965A (en) * | 2018-01-10 | 2018-07-20 | 苏州拜博机电科技有限公司 | A method of multilevel hole material is prepared using direct write forming technique |
| CN108455972A (en) * | 2018-01-10 | 2018-08-28 | 苏州拜博机电科技有限公司 | A method of regulation and control direct write molding sizing material forming performance |
| CN108811307A (en) * | 2018-06-29 | 2018-11-13 | 华中科技大学 | A kind of three-dimensional ceramic circuit board and preparation method thereof |
| CN109095918A (en) * | 2018-08-29 | 2018-12-28 | 济南大学 | A kind of preparation method of 3DP moulding process strontium bismuth titanate dielectric ceramic powder |
| CN109761621A (en) * | 2019-03-18 | 2019-05-17 | 哈尔滨工业大学 | A kind of method preparing big-size complicated shape silicon nitride ceramics |
| CN110228996A (en) * | 2019-06-26 | 2019-09-13 | 陕西博鼎快速精铸科技有限责任公司 | One kind being based on the molding ceramic core preparation method of slurry direct write |
| CN111848141A (en) * | 2020-07-24 | 2020-10-30 | 江苏师范大学 | Preparation method of ceramic paste for 3D printing by direct-writing forming of slurry |
| CN112390651A (en) * | 2020-11-16 | 2021-02-23 | 中国工程物理研究院材料研究所 | AlN ceramic powder preparation method based on 3D printing molding |
| CN115432998A (en) * | 2021-06-03 | 2022-12-06 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent ceramic slurry for direct writing |
Citations (4)
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| CN108069706A (en) * | 2017-12-15 | 2018-05-25 | 天津大学 | A kind of forming method of the fiber reinforced ceramic thin-wall part based on 3D printing technique |
| CN108298965A (en) * | 2018-01-10 | 2018-07-20 | 苏州拜博机电科技有限公司 | A method of multilevel hole material is prepared using direct write forming technique |
| CN108455972A (en) * | 2018-01-10 | 2018-08-28 | 苏州拜博机电科技有限公司 | A method of regulation and control direct write molding sizing material forming performance |
| CN108298965B (en) * | 2018-01-10 | 2021-01-26 | 苏州拜博机电科技有限公司 | Method for preparing hierarchical porous material by adopting direct-writing forming technology |
| CN108811307A (en) * | 2018-06-29 | 2018-11-13 | 华中科技大学 | A kind of three-dimensional ceramic circuit board and preparation method thereof |
| CN109095918A (en) * | 2018-08-29 | 2018-12-28 | 济南大学 | A kind of preparation method of 3DP moulding process strontium bismuth titanate dielectric ceramic powder |
| CN109761621A (en) * | 2019-03-18 | 2019-05-17 | 哈尔滨工业大学 | A kind of method preparing big-size complicated shape silicon nitride ceramics |
| CN110228996A (en) * | 2019-06-26 | 2019-09-13 | 陕西博鼎快速精铸科技有限责任公司 | One kind being based on the molding ceramic core preparation method of slurry direct write |
| CN110228996B (en) * | 2019-06-26 | 2022-02-08 | 陕西博鼎快速精铸科技有限责任公司 | Ceramic core preparation method based on slurry direct-writing forming |
| CN111848141A (en) * | 2020-07-24 | 2020-10-30 | 江苏师范大学 | Preparation method of ceramic paste for 3D printing by direct-writing forming of slurry |
| CN112390651A (en) * | 2020-11-16 | 2021-02-23 | 中国工程物理研究院材料研究所 | AlN ceramic powder preparation method based on 3D printing molding |
| CN115432998A (en) * | 2021-06-03 | 2022-12-06 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent ceramic slurry for direct writing |
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