CN113548882B - Cordierite ceramic device and preparation method and application thereof - Google Patents
Cordierite ceramic device and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses a cordierite ceramic device and a preparation method and application thereof, wherein the method comprises the following steps: mixing Al 2 O 3 Mixing the powder with photosensitive resin to obtain photosensitive slurry; preparing the photosensitive paste into Al based on a 3D printing process 2 O 3 A skeleton preform; for the Al 2 O 3 The framework preform is subjected to debonding treatment to obtain Al 2 O 3 A framework; adding the Al 2 O 3 Skeleton, mgO powder and SiO 2 Sintering the powder to obtain the cordierite ceramic device. The method solves the problems that the prior cordierite ceramic is difficult to realize the preparation of complex shape, large in energy consumption, low in strength and the like.
Description
Technical Field
The application relates to a cordierite ceramic device with a complex shape and a preparation method and application thereof, belonging to the field of ceramics.
Background
3D printing technology (3D printing technology) is also called Additive manufacturing technology (Additive manufacturing), which was born in the 80's of the 20 th century and is a technology of interdisciplinary development of multiple disciplines such as computers, machinery, and lasers. Based on the principle of 'discrete-stacking', the 3D printing technology stacks the powder material with high solid content layer by layer until the whole target object is constructed. New equipment and new materials developed on the basis of a 3D printing technology are applied to the industries such as aerospace, automobile parts, building materials and the like, the production and research and development costs can be greatly reduced, and the process of industrial application is accelerated.
The cordierite ceramic has the characteristics of low thermal expansion coefficient, high thermal stability, excellent thermal shock resistance and the like, and is widely applied to the fields of tail gas treatment, sewage purification and the like. At present, cordierite ceramic devices are generally prepared in an extrusion molding mode, so that the cordierite ceramic devices have the defects of simple structure, large energy consumption of a preparation process, low thermal conductivity and the like.
Disclosure of Invention
According to the first aspect of the application, a method for preparing a cordierite ceramic device is provided, which solves the problems that the existing cordierite ceramic is difficult to prepare in a complex shape, large in energy consumption, low in strength and the like.
A method for preparing a cordierite ceramic device at least comprises the following steps:
(1) Mixing Al 2 O 3 Mixing the powder with photosensitive resin to obtain photosensitive slurry;
(2) Preparing the photosensitive paste into Al based on a 3D printing process 2 O 3 A framework preform;
(3) For the Al 2 O 3 The skeleton preform is subjected to a debinding treatment to remove organic matter, thereby obtaining Al 2 O 3 A framework;
(4) Adding the Al 2 O 3 Skeleton, mgO powder and SiO 2 Sintering the powder to obtain the cordierite ceramic device.
Al 2 O 3 The high-temperature-resistant three-dimensional printing method has the advantages of being strong in heat conduction capability, high in mechanical strength, excellent in high-temperature-resistant performance and the like, and meanwhile, the 3D printing technology is mature, and the preparation of high-precision devices with complex shapes can be achieved. By printing Al in 3D 2 O 3 The ceramic is used as a framework, the design and the molding of a complex shape are realized, and the cordierite ceramic is generated by utilizing a solid phase reaction, so that the purpose of obtaining the cordierite ceramic with the complex shape is realized.
In the present application, the cordierite ceramic device may be a ceramic device containing only a cordierite phase, or may be a ceramic device containing cordierite and Al 2 O 3 The two-phase ceramic device may further contain MgO, cordierite and Al 2 O 3 A three-phase ceramic device; the corresponding ceramic material can be obtained by controlling the reactant proportion, the reaction condition and the like according to the requirementAnd (3) a material device.
In the present application, the ceramic device is preferably a hollow tube array structure or a three-dimensional lattice structure.
In the application, a model in the 3D printing process is obtained by modeling according to the three-dimensional structure of a device; the 3D printing process parameters can be selected from Al according to the device structure 2 O 3 Selecting the conventional 3D printing process conditions of the material, and the application is not limited; al (Al) 2 O 3 、MgO、SiO 2 The specific technological parameters for preparing cordierite material by reaction can be determined from the existing method for preparing cordierite by oxide high-temperature solid-phase reaction according to the requirements on the components of cordierite devices.
Preferably, the specific conditions of the 3D printing process include: the exposure power is 6-120 mW/cm 2 The exposure time of the single layer is 1-100 s, and the set layer thickness of the single layer is 10-100 μm.
Alternatively, al described in step (1) 2 O 3 The grain diameter of the powder is 0.2-50 mu m;
preferably, said Al 2 O 3 The particle size of the powder is 0.2-2 μm.
Optionally, the photosensitive resin is an ultraviolet light curing resin;
the ultraviolet curing resin is cured under ultraviolet light wavelength of 395nm or 405 nm;
the resin cured under the ultraviolet light wavelength of 395nm or 405nm is at least one of epoxy photosensitive resin, acrylic photosensitive resin, polyester photosensitive resin, polyurethane photosensitive resin and thiol-ene photosensitive resin.
Optionally, al in the photosensitive paste of step (1) 2 O 3 The volume content of the powder is 5-80 vol%.
Optionally, the photosensitive slurry in the step (1) is mixed by a planetary ball mill, and the mixed photosensitive slurry is subjected to vibration and vacuum environment to remove bubbles in the slurry; preferably, the rotation speed of the planetary ball mill is 300r/min.
Optionally, specific conditions of the debonding treatment in step (3) include:
the treatment temperature is 400-1000 ℃;
the treatment time is 0.5-10 h;
the atmosphere is oxygen-containing atmosphere; wherein the oxygen-containing atmosphere is an atmosphere containing oxygen, such as air, oxygen, a mixture of oxygen and an inert gas, or the like.
Preferably, the temperature rise rate of the debonding treatment is 1 to 10 ℃/min, more preferably 2 ℃/min;
preferably, the cooling rate of the de-binding treatment is 1 to 10 ℃/min, more preferably 2 ℃/min.
Optionally, siO in step (4) 2 Powder and MgO powder are coated on the Al 2 O 3 Surface of skeleton of said Al 2 O 3 Skeleton, siO 2 The mass ratio of the powder to the MgO powder is 1:0.5 to 5:0.5 to 5.
The Al is 2 O 3 The skeletal surface includes both an outer surface and an inner surface;
in an alternative embodiment, the SiO is formed by mixing 2 Mixing the powder with MgO powder to obtain mixed powder, and adding Al 2 O 3 The skeleton is embedded in the mixed powder to realize Al-to-Al conversion 2 O 3 And (5) coating the surface of the framework.
In another alternative embodiment, by mixing SiO 2 Dispersing the powder and MgO powder in a certain amount of dispersant to obtain a uniform jelly, and applying the jelly to the Al 2 O 3 Skeleton surface, realize to Al 2 O 3 And (5) coating the surface of the framework. Wherein the dispersant may be ethanol.
Optionally, specific conditions of the sintering reaction in step (4) include:
the sintering temperature is 1200-1600 ℃;
the sintering time is 0.5-8 h;
the sintering atmosphere is oxygen-containing atmosphere;
preferably, the temperature rise rate of the sintering reaction is 2-30 ℃/min;
preferably, the temperature reduction rate of the sintering reaction is 2-30 ℃/min.
In one embodiment, a 3D printing method for producing cordierite/Al 2 O 3 A method of complex phase ceramic devices comprising:
(1) Mixing Al 2 O 3 Mixing with photosensitive resin to obtain photosensitive slurry;
(2) Programming according to the well-modeled three-dimensional structure model, and realizing Al by adopting 3D printing technology 2 O 3 Preliminary molding of the skeleton, curing the device under ultraviolet light, cleaning and drying to remove organic matters and the like to obtain the Al 2 O 3 A framework;
(3) Mixing the obtained Al 2 O 3 Stent warp mixed with MgO and SiO 2 Reaction and sintering to obtain the cordierite/Al 2 O 3 A complex phase ceramic device.
In the present application, the cordierite/Al 2 O 3 The complex phase ceramic device at least contains cordierite and Al 2 O 3 Two-phase cordierite ceramic devices.
In a second aspect of the present application, there is provided a cordierite ceramic device produced by any of the methods described above.
Optionally, cordierite and Al are contained 2 O 3 Two phases or MgO, cordierite and Al 2 O 3 Three phases.
In a third aspect of the application, the application of the cordierite ceramic device prepared by the method in the fields of tail gas treatment and sewage purification is provided
The beneficial effect that this application can produce includes:
in the invention, 3D printing is adopted to print three-dimensional Al 2 O 3 The framework has the advantages of complex structure designability, high precision, high efficiency and the like. 3D printing three-dimensional Al 2 O 3 The skeleton preform can be directly debonded and carbonized to obtain any three-dimensional structure, so that the limit of mold forming is broken through. Because the steps of the process flow are less, the time consumption of a single step is short, the preparation time of the ceramic is greatly shortened, and because Al 2 O 3 The ceramic has the functions of toughening fibers and directional heat transmission, and the ceramic prepared by subsequent reaction sintering has good mechanical property and thermal property.
Drawings
FIG. 1 is a 3-dimensional porous structure model provided in example 1;
fig. 2 is a 3-dimensional square grid structure model obtained in example 2.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
Unless otherwise specified, the raw materials in the examples of the present application were all purchased commercially.
Wherein, al 2 O 3 The powder was a TM-DAR model purchased from DAMING;
SiO 2 flour was model S116482 from alatin corporation;
MgO powder is model M103940 from Aladdin corporation;
the UV curable resin was purchased from DSM-AGI model of Shanghai light chemical company, inc.
In this disclosure, photo-curing Al is used for the first time 2 O 3 Preparation of photo-cured Al for the skeleton 2 O 3 And (3) preparing a preform, combining with a solid-phase reaction, and sintering to prepare a cordierite ceramic device, wherein the structure and the components of the obtained cordierite ceramic device can be regulated and controlled by the method.
Al printed in 3D 2 O 3 As a molding framework, air high-temperature sintering is utilized to get rid of the constraint of a mold on a material green body, and a cordierite material device with a complex structure can be prepared. The preparation method has the characteristics of simple preparation process, high blank forming efficiency, high precision of formed devices and the like, and can shorten the preparation period of cordierite ceramic devices. The following is an exemplary description of Al provided by the present invention 2 O 3 A method of making a cordierite device for a preform.
Example 1
21.27vol％Al 2 O 3 78.73vol% ultraviolet curing resin, and Al 2 O 3 The balls are used as grinding media and are ball-milled for 30min on a 300r/s planetary ball mill. Pressure reduction by vacuum deviceAnd degassing for 2min to prepare 3D printing photo-curing paste (photosensitive paste). Using the designed 3-dimensional porous structure model (a hollow tube array structure as shown in FIG. 1, in which the tube wall thickness is 0.5mm and the hollow diameter is 1 mm), the parameters of 3D printing were set, in which the exposure power was set to 78.00mW/cm 2 The exposure time was selected to be 30s. After printing, placing the obtained sample in ultraviolet light for irradiation and curing for 5min, after curing, placing the sample in an ultrasonic cleaning instrument for ultrasonic cleaning for 5min, and then drying in an oven at 60 ℃ for 1h to obtain Al 2 O 3 And (5) prefabricating a body. Mixing Al 2 O 3 The prefabricated body is subjected to debonding treatment for 1h at 800 ℃ in air atmosphere to obtain three-dimensional Al 2 O 3 Support (i.e. Al) 2 O 3 A backbone). Adding three-dimensional Al 2 O 3 The stent is placed on Al coated with boron nitride 2 O 3 In the crucible, al is distributed according to three dimensions 2 O 3 A support: siO 2 2 Powder: mgO powder mass ratio =2:2:5 weighing the required materials, and weighing the weighed SiO 2 Uniformly mixing the powder and MgO powder, and filling the mixture in the Al 2 O 3 Holes and peripheries of the brackets are made of Al 2 O 3 The bracket is embedded in the mixed powder. And carrying out vacuum solid-phase reaction at 1350 ℃, keeping the temperature for 1h to realize densification, cooling to room temperature in an air environment, and removing MgO on the surface to obtain the porous cordierite ceramic with the structure shown in figure 1.
Example 2
21.27vol％Al 2 O 3 78.73vol% ultraviolet curing resin, and Al 2 O 3 The balls are used as grinding media and are ball-milled for 30min on a planetary ball mill of 300 r/s. And (4) decompressing by using a vacuum device, degassing for 2min, and preparing the 3D printing photocuring slurry. Using the designed 3-dimensional square grid structure model (wall thickness 0.5mm, individual squares 2mm on side as shown in FIG. 2), the parameters for 3D printing were set with the exposure power set to 78.00mW/cm 2 The exposure time was selected to be 30s. After printing, placing the obtained sample in ultraviolet light for irradiation and curing for 5min, after curing, placing the sample in an ultrasonic cleaning instrument for ultrasonic cleaning for 5min, and then drying in an oven at 60 ℃ for 1h to obtain Al 2 O 3 And (4) prefabricating. Mixing Al 2 O 3 The prefabricated body is subjected to debonding treatment at 800 ℃ in air atmosphere to obtain three-dimensional Al 2 O 3 And (4) a bracket. Mixing three-dimensional Al 2 O 3 The stent is placed on Al coated with boron nitride 2 O 3 In the crucible, al is distributed according to three dimensions 2 O 3 A support: siO 2 2 Powder: mgO powder mass ratio =3:2:6 weighing the required materials according to the proportion, and weighing the weighed SiO 2 Uniformly mixing the powder and MgO powder, and filling the mixture in the Al 2 O 3 Holes and peripheries of the brackets are made of Al 2 O 3 The bracket is embedded in the mixed powder. Vacuum solid-phase reaction at 1350 deg.C, maintaining for 1 hr to achieve densification, cooling to room temperature in air environment, removing MgO on the surface to obtain cordierite/Al shown in FIG. 2 2 O 3 A ceramic composite material.
Although the present invention has been described with reference to a few preferred embodiments, it should be understood that various changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (14)
1. A method for producing a cordierite ceramic device, comprising at least the steps of:
(1) Mixing Al 2 O 3 Mixing the powder with photosensitive resin to obtain photosensitive slurry;
(2) Preparing the photosensitive paste into Al based on a 3D printing process 2 O 3 A skeleton preform;
(3) For the Al 2 O 3 The skeleton preform is subjected to debonding treatment to obtain Al 2 O 3 A framework;
(4) Mixing the Al 2 O 3 Skeleton, mgO powder and SiO 2 Sintering the powder to obtain a cordierite ceramic device;
the cordierite ceramic device contains cordierite and Al 2 O 3 Two phases or containing MgOCordierite and Al 2 O 3 Three phases.
2. The method according to claim 1, wherein Al in the step (1) 2 O 3 The particle size of the powder is 0.2-50 μm.
3. The method according to claim 1, wherein the Al is 2 O 3 The particle size of the powder is 0.2 to 2 μm.
4. The production method according to claim 1, wherein the photosensitive resin is an ultraviolet-curable resin;
the ultraviolet light curing resin is cured under the ultraviolet light wavelength of 395nm or 405 nm;
the resin cured under the ultraviolet light wavelength of 395nm or 405nm is at least one of epoxy photosensitive resin, acrylic photosensitive resin, polyester photosensitive resin, polyurethane photosensitive resin and thiol-ene photosensitive resin.
5. The method according to claim 1, wherein Al is contained in the photosensitive paste of the step (1) 2 O 3 The volume content of the powder is 5-80 vol%.
6. The production method according to claim 1, wherein the specific conditions of the debinding treatment of step (3) include:
the processing temperature is 400 to 1000 ℃;
the processing time is 0.5 to 10h;
the atmosphere is an oxygen-containing atmosphere.
7. The method according to claim 1, wherein the temperature increase rate of the de-binding treatment is 1 to 10 ℃/min.
8. The method according to claim 1, wherein the temperature decrease rate of the de-binding treatment is 1 to 10 ℃/min.
9. The method according to claim 1, wherein SiO in step (4) 2 Powder and MgO powder are coated on the Al 2 O 3 A surface of the skeleton;
the Al is 2 O 3 Skeleton, siO 2 The mass ratio of the powder to the MgO powder is 1:0.5 to 5:0.5 to 5.
10. The preparation method according to claim 1, wherein the specific conditions of the sintering reaction in step (4) include:
the sintering temperature is 1200-1600 ℃;
the sintering time is 0.5-8 h;
the sintering atmosphere is an oxygen-containing atmosphere.
11. The method according to claim 1, wherein the sintering reaction temperature rise rate is 2 to 30 ℃/min.
12. The method according to claim 1, wherein the temperature reduction rate of the sintering reaction is 2 to 30 ℃/min.
13. A cordierite ceramic device produced by the method of any one of claims 1 to 12.
14. The cordierite ceramic device prepared by the method of any one of claims 1 to 12 is used in the fields of tail gas treatment and sewage purification.
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