CN111960809B - Spherical Al for photocuring 3D printing2O3Method for preparing powder - Google Patents
Spherical Al for photocuring 3D printing2O3Method for preparing powder 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention relates to photocuring 3D printing, belongs to the technical field of ceramic powder, and particularly relates to spherical Al for photocuring 3D printing2O3The preparation method of the powder comprises the following steps: 1) preparing a metal aluminum salt solution; 2) according to the formula with Al3+Weighing an alkali source according to a certain molar ratio, and dissolving the alkali source in the metal aluminum salt solution obtained in the step 1); 3) carrying out ultrasonic treatment on the mixed solution obtained in the step 2) for 5-10 min; 4) carrying out hydrothermal reaction; 5) filtering the hydrothermal product to obtain white powder, and washing the obtained white powder; 6) adding ethanol to the washed product, and then carrying out ultrasonic treatment; 7) drying; 8) firing to obtain Al2O3Ceramic powder. Al prepared by the invention2O3The powder has high sphericity, superfine granularity, good dispersity, uniform granularity and narrow granularity distribution, and can well meet the requirements of Al for photocuring 3D printing2O3The requirement of ceramic slurry fluidity.
Description
Technical Field
The invention relates to photocuring 3D printing, belongs to the technical field of ceramic powder, and particularly relates to spherical Al for photocuring 3D printing2O3A method for preparing powder.
Background
The ceramic photocuring 3D printing technology is characterized in that light with specific wavelength is controlled by a computer, selectively irradiates on photosensitive resin containing ceramic powder, is cured to form a single-layer profile, then the photosensitive resin is recoated on the surface by moving a working platform, the next layer of curing is continued, the process is circulated until a final solid green body is obtained, and then the formed green body is subjected to glue removal and sintering to prepare a high-density ceramic device. The ceramic photocuring 3D printing technology can be classified into a stereo photocuring modeling (SLA) technology and a Digital Light Processing (DLP) technology according to the kind of a Light source. The ceramic photocuring 3D printing technology can fully combine the excellent performance of ceramic materials and the advantages of rapid and precise manufacturing of 3D printing, does not need a special die, and has obvious advantages in the aspect of preparing ceramic parts with complex structures and high precision. Ceramic photocuring 3D printing technology The key point of the technology lies in the preparation of ceramic slurry with high solid content, high stability and low viscosity, and the ceramic powder commonly used for preparing ceramic photocuring 3D printing slurry at present is Al2O3、ZrO2、SiO2、Ca5(PO4)3(OH)、Si3N4And the sphericity, particle size distribution, dispersibility and homogeneity of the ceramic powder have significant influence on slurry performance and final product quality.
Al2O3As one of ceramic materials with the widest application, ceramics are the hot spots for researching the ultrafine spherical ceramic powder for photocuring 3D printing. At present, ultrafine spherical Al2O3The preparation method of the powder generally comprises a physical method and a wet chemical method. For example, the Chinese invention patent "preparation method of micron-sized spherical alumina carrier" (CN104163446A) introduces a physical method, which uses industrial-grade alumina with the particle size of less than 50mm as a raw material to prepare alumina powder by high-energy ball milling, and the particle size of the obtained powder is more than 10 μm. Document "High-precision dispersese alpha-Al2O3nanoparticules synthesized by high-energy ball milling (Advanced Powder Technology, Volume 29, Issue 9, September 2018, Pages 2194-2O3The superfine powder prepared by the method has uniform granularity, irregular blocky appearance and agglomeration. The requirements for preparing high-precision ceramic products by the photocuring 3D printing technology cannot be met.
Preparation of Al by sol-gel method2O3Superfine powder (proceedings of Henan university of science and technology, Nature science edition, 14 th 2011) A wet chemistry method is reported, wherein Al is prepared by taking aluminum nitrate as a raw material and citric acid as a complexing agent by adopting a sol-gel method2O3The prepared superfine powder has wider particle size distribution, agglomeration and insufficient sphericity. Document "Low temperature Synthesis of ultra alpha-Al2O3powder by a simple aqueous sol-gel Process (Ceramics International, Volume 32, Issue 5,2006, Pages 587-The chemical method is that aluminum nitrate and lemon acid are used as raw materials to synthesize Al by a sol-gel method2O3The superfine powder prepared by the method also has the problems of irregular shape, serious agglomeration and nonuniform particle size distribution. The requirements for preparing high-precision ceramic products by the photocuring 3D printing technology cannot be met.
Disclosure of Invention
The invention aims to provide a spherical Al for photocuring 3D printing2O3Preparation method of powder and prepared ultrafine spherical Al2O3Compared with the traditional method, the powder ball has the characteristics of high sphericity, superfine property, good dispersibility, uniform granularity, short preparation time and low cost.
The scheme adopted by the invention for realizing the purpose is as follows: photocuring 3D prints and uses superfine spherical Al2O3The preparation method of the powder comprises the following steps:
1) preparing a metal aluminum salt solution: weighing metal aluminum salt, dissolving the metal aluminum salt in water, and preparing a metal aluminum salt solution with a certain concentration;
2) preparing a mixed solution: according to the formula with Al3+Weighing an alkali source according to a certain molar ratio, dissolving the alkali source in the metal aluminum salt solution obtained in the step (1), and uniformly stirring to obtain a mixed solution;
3) ultrasonic: carrying out ultrasonic treatment on the mixed solution obtained in the step (2) at room temperature for 5-10 min;
4) hydrothermal reaction: carrying out heat treatment on the solution obtained in the step (3) at a certain temperature for a certain time;
5) suction filtration and washing: filtering the liquid of the hydrothermal product after the supernatant is removed to obtain white powder, and washing the obtained white powder;
6) ultrasonic: adding ethanol into the washing product, and then carrying out ultrasonic treatment for 10-20 min;
7) drying: drying the liquid subjected to the ultrasonic treatment in the step (6) to obtain Al2O3A precursor;
8) and (3) firing: drying the Al2O3Grinding the precursor, and then sintering at a certain temperature to obtain Al2O3Ceramic powder.
Preferably, in the step 1), the concentration of the metal aluminum salt solution is 0.05-0.15 mol/L.
Preferably, in the step 1), the metal aluminum salt is NH 4Al(SO4)2、Al2(SO4)3·18H2O and (NH)4)2SO4A mixture mixed according to a molar ratio of (3: 4) - (4: 2).
Preferably, in the step 2), the alkali source is urea and Al3+The molar ratio of the urea to the urea is 1: 0.5-1: 8.
Preferably, in the step 4), the heat treatment is carried out at 110-130 ℃ for 1.5-2.5 h.
Preferably, in the step 5), the white powder is washed with absolute ethyl alcohol and distilled water alternately for a plurality of times.
Preferably, in the step 7), the drying temperature is 80-100 ℃.
Preferably, in the step 8), the firing temperature is 1200-1250 ℃.
The invention has the following advantages and beneficial effects:
al prepared by the invention2O3The powder has high sphericity, superfine performance, high dispersivity and homogeneous granularity. Al prepared by traditional physical method and wet chemical method2O3The ceramic powder has irregular appearance, serious agglomeration and wide particle size distribution. The invention firstly synthesizes a spherical precursor by accurately controlling a wet chemical formula and a preparation process, and carries out heat treatment on the precursor to prepare the Al2O3The ceramic powder has extremely high sphericity, uniform dispersion without agglomeration and narrow particle size distribution, and can well meet the requirements of Al for photocuring 3D printing2O3The requirement of ceramic slurry fluidity.
Al of the invention2O3The powder preparation time is short and the cost is low. Preparation of Al by conventional physical and wet-chemical methods 2O3The preparation time of the ceramic powder is usually as long as more than 8 hours, the process is complicated, and the cost is high. The invention directly synthesizes the spherical precursor through the hydrothermal reaction of the raw materials, and the spherical Al can be obtained by heat treatment of the precursor2O3The ceramic powder is prepared by mixing a ceramic powder,the reaction time is shortened by more than 5h, thereby reducing the cost by more than 40 percent.
The ultrafine spherical Al for photocuring 3D printing prepared by the method2O3High sphericity of powder, uniform size, Al2O3Powder d501.91 mu m, meets the requirements of special Al for photocuring 3D printing2O3Ceramic powder and the technical requirements for preparing high-precision ceramic products.
Drawings
FIG. 1 shows Al in example 1 of the present invention2O3SEM image of precursor (500 x magnification);
FIG. 2 shows Al in example 1 of the present invention2O3SEM image (500 times magnification) of ceramic powder;
FIG. 3 shows Al in example 1 of the present invention2O3The particle size distribution of the ceramic powder.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1:
photocuring 3D prints and uses superfine spherical Al2O3The preparation method of the powder comprises the following steps:
1) preparing a metal aluminum salt solution: weighing analytically pure metal aluminum salt, dissolving in distilled water to prepare solution with concentration of 0.05mol/L, wherein the metal aluminum salt is NH 4Al(SO4)2、Al2(SO4)3·18H2O and (NH)4)2SO4The mixture has a molar ratio of 3.5: 3;
2) preparing a mixed solution: according to Al3+And CH4N2Weighing CH according to the molar ratio of O to 1:14N2Dissolving O in the aluminum salt solution, and continuously stirring for 30min at the stirring speed of 600 r/min;
3) ultrasonic: putting the mixed solution into a numerical control ultrasonic cleaner for ultrasonic treatment at room temperature for 5 min;
4) hydrothermal reaction: adding the solution into a high-pressure reaction kettle with a polytetrafluoroethylene inner container, carrying out heat treatment at 120 ℃ for 1.5h, wherein the filling degree is 70%;
5) suction filtration and washing: filtering the liquid of the hydrothermal product after supernatant liquid is removed by a Buchner funnel to obtain white powder, and alternately and respectively washing the obtained white powder for 3 times by using water and ethanol;
6) ultrasonic: adding 10ml of ethanol into the washing product, and then putting the washing product into a numerical control ultrasonic cleaner for ultrasonic treatment for 10min at room temperature;
7) drying: pouring the liquid after ultrasonic treatment into an evaporation pan; putting the evaporating dish into an oven, and drying at 80 ℃ to obtain Al2O3A precursor;
8) and (3) firing: drying the Al2O3Grinding the precursor, placing the ground precursor into a crucible, placing the crucible into a silicon-carbon furnace, and sintering at 1200 ℃ to obtain Al2O3Ceramic powder.
Through testing, the ultra-fine spherical Al for photocuring 3D printing prepared in the embodiment2O3High crystallinity of powder, high sphericity, uniform granularity and Al 2O3The median particle diameter of the powder is d501.82 mu m, meets the requirements on the market and is used for photocuring 3D printing2O3Technical requirements for ceramic powders.
FIG. 1 shows Al in this example2O3SEM image (500 x magnification) of the precursor, from which it can be seen: al prepared in this example2O3The precursor powder has high shape sphericity and no agglomeration.
FIG. 2 shows Al in the present example2O3SEM image (500 times magnification) of the ceramic powder, from which it can be seen that: al prepared in this example2O3The ceramic powder has high sphericity and no agglomeration.
FIG. 3 shows Al in this example2O3The particle size distribution diagram of the ceramic powder can be seen from the figure: al prepared in this example2O3The ceramic powder has narrow particle size distribution.
Example 2:
photocuring 3D prints and uses superfine spherical Al2O3The preparation method of the powder comprises the following steps:
1) preparing a metal aluminum salt solution: weighing analytically pure metal aluminum salt, dissolving in distilled water to prepare solution with concentration of 0.10mol/L, wherein the metal aluminum salt is NH4Al(SO4)2、Al2(SO4)3·18H2O and (NH)4)2SO4The mixture has a molar ratio of 3: 4;
2) preparing a mixed solution: according to Al3+And CH4N2Weighing CH according to the molar ratio of O to the CH of 1:24N2Dissolving O in the aluminum salt solution, and continuously stirring for 30min at the stirring speed of 800 r/min;
3) ultrasonic: putting the mixed solution into a numerical control ultrasonic cleaner for ultrasonic treatment at room temperature for 7 min;
4) Hydrothermal reaction: adding the solution into a high-pressure reaction kettle with a polytetrafluoroethylene inner container, carrying out heat treatment at 110 ℃ for 2h, wherein the filling degree is 75%;
5) suction filtration and washing: filtering the liquid of the hydrothermal product after supernatant liquid is removed by a Buchner funnel to obtain white powder, and alternately and respectively washing the obtained white powder for 4 times by using water and ethanol;
6) ultrasonic treatment: adding 10ml ethanol into the washed product, and performing ultrasonic treatment in a numerical control ultrasonic cleaner for 15min at room temperature
7) And (3) drying: pouring the liquid after ultrasonic treatment into an evaporation pan; putting the evaporating dish into an oven, and drying at 90 ℃ to obtain Al2O3A precursor;
8) and (3) firing: drying the Al2O3Grinding the precursor, placing the ground precursor into a crucible, placing the crucible into a silicon-carbon furnace, and sintering at 1230 ℃ to obtain Al2O3Ceramic powder.
Through testing, the ultra-fine spherical Al for photocuring 3D printing of the embodiment2O3High crystallinity of powder, high sphericity, uniform granularity and Al2O3The median particle diameter of the powder is d501.92 mu m, meets the requirements on the market and is used for photocuring 3D printing2O3The technical requirements of ceramic powder.
Example 3:
photocuring 3D prints and uses superfine spherical Al2O3The preparation method of the powder comprises the following steps:
1) preparing a metal aluminum salt solution: weighing analytically pure metal aluminum salt, dissolving in distilled water to prepare solution with concentration of 0.15mol/L, wherein the metal aluminum salt is NH 4Al(SO4)2、Al2(SO4)3·18H2O and (NH)4)2SO4Mixture (4: 2);
2) preparing a mixed solution: according to Al3+And CH4N2Weighing CH according to the molar ratio of O to 44N2Dissolving O in the aluminum salt solution, and continuously stirring for 30min at the stirring speed of 600 r/min;
3) ultrasonic: putting the mixed solution into a numerical control ultrasonic cleaner for ultrasonic treatment at room temperature for 10 min;
4) hydrothermal reaction: adding the solution into a high-pressure reaction kettle with a polytetrafluoroethylene inner container, performing heat treatment at 130 ℃ for 2.5 hours, wherein the filling degree is 80%;
5) suction filtration and washing: filtering the liquid of the hydrothermal product after supernatant is removed by a Buchner funnel to obtain white powder, and alternately and respectively washing the obtained white powder for 5 times by using water and ethanol;
6) ultrasonic: adding 10ml ethanol into the washed product, and performing ultrasonic treatment in a numerical control ultrasonic cleaner at room temperature for 20min
7) Drying: pouring the liquid after ultrasonic treatment into an evaporation pan; putting the evaporating dish into an oven, and drying at 100 ℃ to obtain Al2O3A precursor;
8) and (3) firing: drying the Al2O3Grinding the precursor, putting the ground precursor into a crucible, putting the crucible into a silicon-carbon furnace, and sintering at 1250 ℃; to obtain Al2O3Ceramic powder.
Through testing, the ultra-fine spherical Al for photocuring 3D printing of the embodiment2O3High crystallinity of powder, high sphericity, uniform granularity and Al 2O3The median particle diameter of the powder is d50The particle size of the particles was 2.19. mu.m,photocuring 3D printing Al meeting market requirements2O3The technical requirements of ceramic powder.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (6)
1. Photocuring 3D prints and uses superfine spherical Al2O3The preparation method of the powder is characterized by comprising the following steps:
1) preparing a metal aluminum salt solution: weighing metal aluminum salt, dissolving the metal aluminum salt in water, and preparing a metal aluminum salt solution with a certain concentration;
2) preparing a mixed solution: according to the formula with Al3+Weighing an alkali source according to a certain molar ratio, dissolving the alkali source in the metal aluminum salt solution obtained in the step (1), and uniformly stirring to obtain a mixed solution;
3) ultrasonic: carrying out ultrasonic treatment on the mixed solution obtained in the step (2) at room temperature for 5-10 min;
4) hydrothermal reaction: carrying out heat treatment on the solution obtained in the step (3) at a certain temperature for a certain time;
5) suction filtration and washing: filtering the liquid of the hydrothermal product after the supernatant is removed to obtain white powder, and washing the obtained white powder;
6) Ultrasonic treatment: adding ethanol into the washing product, and then carrying out ultrasonic treatment for 10-20 min;
7) and (3) drying: drying the liquid subjected to the ultrasonic treatment in the step (6) to obtain Al2O3A precursor;
8) and (3) firing: drying the Al2O3Grinding the precursor, and then sintering at a certain temperature to obtain Al2O3Ceramic powder;
in the step 1), the metal aluminum salt is NH4Al(SO4)2、Al2(SO4)3·18H2O and (NH)4)2SO4Mixing the components according to the mol ratio of (3: 4) to (4: 2); in the step 2), the alkali source is urea and Al3+The molar ratio of the urea to the urea is 1: 0.5-1: 8.
2. Spherical Al for photocuring 3D printing according to claim 12O3The preparation method of the powder is characterized by comprising the following steps: in the step 1), the concentration of the metal aluminum salt solution is 0.05-0.15 mol/L.
3. Spherical Al for photocuring 3D printing according to claim 12O3The preparation method of the powder is characterized by comprising the following steps: in the step 4), heat treatment is carried out at 110-130 ℃ for 1.5-2.5 h.
4. Spherical Al for photocuring 3D printing according to claim 12O3The preparation method of the powder is characterized by comprising the following steps: in the step 5), the white powder is washed by adopting absolute ethyl alcohol and distilled water alternately for multiple times.
5. Spherical Al for photocuring 3D printing according to claim 1 2O3The preparation method of the powder is characterized by comprising the following steps: in the step 7), the drying temperature is 80-100 ℃.
6. Spherical Al for photocuring 3D printing according to claim 12O3The preparation method of the powder is characterized by comprising the following steps: in the step 8), the firing temperature is 1200-1250 ℃.
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| US3855172A (en) * | 1972-04-07 | 1974-12-17 | Du Pont | Uniform oxide microspheres and a process for their manufacture |
| CN1962447A (en) * | 2005-11-10 | 2007-05-16 | 中国科学院电工研究所 | Method for preparing nanometer alumina powder |
| CN101164888A (en) * | 2007-09-17 | 2008-04-23 | 南京工业大学 | Method for preparing single grain diameter spherical ultra-fine Al2O3 powder |
| CN108483474A (en) * | 2018-04-10 | 2018-09-04 | 河南科技大学 | A kind of preparation method of nano-level sphere aluminium oxide |
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| US3027234A (en) * | 1959-09-08 | 1962-03-27 | Universal Oil Prod Co | Manufacture of spheroidal alumina particles from aluminum sulfate |
| US3183194A (en) * | 1961-03-31 | 1965-05-11 | Mizusawa Industrial Chem | Method of preparing spherical active alumina gel and spherical active alumina-silica gel |
| US7422730B2 (en) * | 2003-04-02 | 2008-09-09 | Saint-Gobain Ceramics & Plastics, Inc. | Nanoporous ultrafine α-alumina powders and sol-gel process of preparing same |
| WO2018110384A1 (en) * | 2016-12-12 | 2018-06-21 | 多木化学株式会社 | Alumina powder |
| CN107188210A (en) * | 2017-07-25 | 2017-09-22 | 山东非金属材料研究所 | A kind of preparation method of high-purity alpha alumina powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3855172A (en) * | 1972-04-07 | 1974-12-17 | Du Pont | Uniform oxide microspheres and a process for their manufacture |
| CN1962447A (en) * | 2005-11-10 | 2007-05-16 | 中国科学院电工研究所 | Method for preparing nanometer alumina powder |
| CN101164888A (en) * | 2007-09-17 | 2008-04-23 | 南京工业大学 | Method for preparing single grain diameter spherical ultra-fine Al2O3 powder |
| CN108483474A (en) * | 2018-04-10 | 2018-09-04 | 河南科技大学 | A kind of preparation method of nano-level sphere aluminium oxide |
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