CN113816758B - Photocuring 3D printing dehumidifying ceramic material and preparation method thereof - Google Patents

Photocuring 3D printing dehumidifying ceramic material and preparation method thereof Download PDF

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CN113816758B
CN113816758B CN202111288841.3A CN202111288841A CN113816758B CN 113816758 B CN113816758 B CN 113816758B CN 202111288841 A CN202111288841 A CN 202111288841A CN 113816758 B CN113816758 B CN 113816758B
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printing
photocuring
dehumidifying
ceramic material
ceramic
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CN113816758A (en
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李金国
李乔磊
梁静静
周亦胄
孙晓峰
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Institute of Metal Research of CAS
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Abstract

The invention relates to a photocuring 3D printing dehumidifying ceramic material and a preparation method thereof, and the technical scheme is mainly adopted as follows: the preparation method of the photocuring 3D printing dehumidifying ceramic material comprises the following steps: mixing a 3D printing dehumidifying ceramic solid-phase raw material and a 3D printing liquid phase solvent to obtain photocuring 3D printing dehumidifying ceramic slurry; wherein, by weight, the photocuring 3D printing dehumidification ceramic slurry comprises: 35-50 parts of reinforcing agent, 1-25 parts of condensation agent, 1-15 parts of hydrophobic agent and 30-50 parts of 3D printing liquid phase solvent; carrying out photocuring 3D printing treatment on the photocuring 3D printing dehumidification ceramic slurry to obtain a photocuring 3D printing dehumidification ceramic biscuit; and (4) degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain the photocuring 3D printing dehumidification ceramic material. The invention is mainly used for preparing the dehumidifying ceramic material which has large moisture absorption amount, wide dehumidifying range and stable chemical property and can realize rapid recycling.

Description

Photocuring 3D printing dehumidification ceramic material and preparation method thereof
Technical Field
The invention relates to the technical field of additive manufacturing ceramic materials, in particular to a photocuring 3D printing dehumidification ceramic material and a preparation method thereof.
Background
The method has very obvious significance for controlling the environmental humidity in the fields of life, article storage, industrial production and the like of people; for example, for people's life, people are suitable for an environment with a relative humidity of 40-70%, and if the relative humidity exceeds the humidity range, people feel uncomfortable, so that the indoor air humidity needs to be controlled; in addition, if the humidity of the indoor environment is excessively high for a long time, the indoor objects may be mildewed or rusted.
At present, a large number of electric appliances and equipment with a dehumidifying function are emerging in the field of household appliances to ensure the humidity of environments sensitive to moisture, such as domestic living environments, specific environments of factories and precision equipment, medicines and the like. Therefore, the dehumidifying material has wide application market, and the research and innovation of the dehumidifying material have very important significance.
The traditional solid dehumidifying material comprises molecular sieve, calcium chloride, silica gel and the like, but the dehumidifying material has limited service life and cannot be regenerated at low temperature.
With the development of porous ceramic materials, porous ceramic dehumidifying materials have gradually appeared in recent years. The porous ceramic dehumidifying material at the present stage adopts a material with an adsorption effect to adsorb water molecules in the ambient air needing to be dehumidified; however, the adsorbed water molecules are adhered to the porous ceramic dehumidifying material and are easily brought back to the ambient air to be dehumidified by the air flow; therefore, the existing porous ceramic dehumidifying material has the problem of poor dehumidifying effect.
Disclosure of Invention
In view of the above, the invention provides a photocuring 3D printing dehumidifying ceramic material and a preparation method thereof, and mainly aims to prepare a dehumidifying ceramic material which can be rapidly recycled and has a good dehumidifying effect.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, an embodiment of the present invention provides a method for preparing a photocuring 3D printing dehumidification ceramic material, including the following steps:
preparing photocuring 3D printing dehumidifying ceramic slurry: mixing a 3D printing dehumidifying ceramic solid-phase raw material and a 3D printing liquid phase solvent to obtain photocuring 3D printing dehumidifying ceramic slurry; wherein the photocuring 3D printing dehumidifying ceramic slurry comprises the following components in parts by weight: 35-50 parts of reinforcing agent, 1-25 parts of condensation agent, 1-15 parts of hydrophobic agent and 30-50 parts of 3D printing liquid phase solvent;
and (3) photocuring 3D printing: carrying out photocuring 3D printing treatment on the photocuring 3D printing dehumidification ceramic slurry to obtain a photocuring 3D printing dehumidification ceramic biscuit;
degreasing and sintering treatment: and degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain the photocuring 3D printing dehumidification ceramic material.
Preferably, the condensing agent is ceramic particle powder with a sharp angle shape; preferably, the component of the condensation agent is Al2O3、TiO2、SiO2One or more of the above; preferably, the condensing agent is diamond-shaped ceramic particle powder; preferably, the particle size of the dew condensation agent is 10-50 μm.
Preferably, the reinforcer is one or more of quartz powder, corundum powder, feldspar powder, biotite powder and kaolinite powder; preferably, the grain size of the enhancer is 50-200 μm; preferably, the reinforcing agent is spherical or ellipsoidal particle powder.
Preferably, the hydrophobic agent is nano SiO2Nano Al2O3Nano ZrO 22One or more of; preferably, the particle size of the hydrophobic agent is 10-80 nm; preferably, the hydrophobic agent is spherical or ellipsoidal particle powder.
Preferably, the photocuring 3D printing dehumidifying ceramic slurry further comprises 5-9 parts by weight of an adsorbent; preferably, the adsorbent is clay mineral powder, hydromica powder or SiO2·nH2One or more of O and alunite. Preferably, the particle size of the adsorbent is 100nm to 50 μm.
Preferably, the 3D printing liquid phase solvent includes a photosensitive resin and a diluent; wherein, the volume fraction of the photosensitive resin is 70-80%; the volume fraction of the diluent is 20-30%; preferably, the photosensitive resin is one or more of 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate and trimethylolpropane triacrylate; preferably, the diluent is one or two of deionized water and silica sol.
Preferably, the step of preparing the photocuring 3D printing dehumidifying ceramic slurry includes: mixing the 3D printing dehumidifying ceramic solid-phase raw materials, mixing the mixture with a 3D printing liquid phase solvent, and stirring the mixture at a heat preservation state to obtain photocuring 3D printing dehumidifying ceramic slurry; preferably, the temperature for heat preservation is 80-180 ℃, and the stirring time is 2-12 h.
Preferably, the photocuring 3D printing step includes:
designing a three-dimensional model through software, slicing the three-dimensional model, and exporting a 3D printing STL file;
importing the 3D printing STL file into a photocuring 3D printer, setting 3D printing parameters, and curing the photocuring 3D printing dehumidifying ceramic slurry according to the three-dimensional model to obtain a photocuring 3D printing dehumidifying ceramic biscuit;
preferably, the 3D printing process parameters are: the curing thickness is 100-300 mu m, and the curing power is 25-50nW/cm2The single layer curing time is 10-30 s.
In the step of degreasing treatment: the degreasing temperature is 550-; preferably, the heating rate is 40-60 ℃/h, and the cooling rate is 40-60 ℃/h.
In the step of the sintering treatment: the sintering treatment temperature is 1200-1700 ℃, and the heat preservation time at the sintering treatment temperature is 180-600 min; preferably, the temperature rise rate is 180 ℃/h within 120-.
In another aspect, an embodiment of the present invention provides a photocuring 3D printing dehumidification ceramic material, wherein the photocuring 3D printing dehumidification ceramic material comprises the following components in parts by weight: 35-50 parts of reinforcing agent, 1-25 parts of condensation agent and 1-15 parts of hydrophobing agent;
preferably, the condensation agent is ceramic particles with sharp corners; preferably, the component of the condensation agent is Al2O3、TiO2、SiO2One or more of the above; preferably, the condensation agent is diamond-shapedThe ceramic particles of (a); preferably, the particle size of the dew condensation agent is 10-50 μm.
Preferably, the hydrophobic agent is nano SiO2Nano Al2O3Nano ZrO 22One or more of;
preferably, the light-cured 3D printing dehumidifying ceramic material further comprises 5-9 parts by weight of an adsorbent;
preferably, the photocuring 3D printing dehumidifying ceramic material has a lamellar structure, and gaps are formed between lamellae of the lamellar structure to form penetrating interlayer air holes;
preferably, an arc-shaped convex structure is formed on the surface of an airflow channel of the photocuring 3D printing dehumidification ceramic material;
preferably, the photocuring 3D printing dehumidifying material is prepared by any one of the preparation methods of the photocuring 3D printing dehumidifying ceramic material.
Compared with the prior art, the photocuring 3D printing dehumidification ceramic material and the preparation method thereof have at least the following beneficial effects:
according to the photocuring 3D printing dehumidifying ceramic material and the preparation method thereof provided by the embodiment of the invention, as the photocuring 3D printing ceramic material belongs to porous ceramic and has the characteristic of porosity, the photocuring 3D printing ceramic material has an adsorption effect on water molecules in air, on the basis, by introducing a condensation agent and a hydrophobic agent, after air flow entering a porous ceramic structure meets the condensation agent, the water molecules can be condensed to form small droplets, and the hydrophobic agent further enables the small droplets to form water flow to flow out without being adhered to the porous ceramic, so that the photocuring 3D printing dehumidifying ceramic material is rapidly recycled, and the dehumidifying efficiency is improved; meanwhile, the problem that ' adsorbed water molecules are easily brought back to the ambient air needing dehumidification ' of the existing porous ceramic dehumidification material by air flow ' is solved by the scheme, so that the photocuring 3D printing dehumidification ceramic material prepared by the embodiment of the invention further has an excellent dehumidification effect.
Further, the embodiment of the invention provides a photocuring 3D printing dehumidifying ceramic material and a preparation method thereofThe method further comprises introducing adsorbent, i.e. clay mineral, hydromica powder, SiO2·nH2One or more of O and alunite, the adsorbent has a plurality of transverse small air holes and can adhere to small molecules in the air; the condensation agent and the adsorbent have double dehumidification effects, so that the dehumidification humidity range of the material can be widened, and the dehumidification effect and the dehumidification efficiency of the material are further improved.
In addition, the ceramic material that photocuring 3D printing technology was prepared appears lamellar structure and the structure of horizontal intercommunication gas pocket between the layer easily, makes the water that the condensation formed can not taken away by the air current like this, and can obtain quick storage and discharge to realize dehumidifying material's quick cycle and use. In addition, in the preparation process of the photocuring 3D printing ceramic material, the lamella is easy to form an arc-shaped convex structure on the surface of an airflow channel of the porous ceramic material due to refraction of curing light, and the convex structure enables airflow flowing into the dehumidifying material to form turbulent flow or vortex flow, so that air is fully contacted with a condensation agent and an adsorbent in the dehumidifying ceramic material, the dehumidifying humidity range of the material is widened, and the dehumidifying efficiency is improved. Therefore, the synergistic effect among the condensation agent (preferably, the adsorption agent), the hydrophobic agent and the photocuring 3D printing ceramic material structure widens the dehumidification humidity range of the material, and improves the dehumidification effect and the dehumidification efficiency of the material.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is an SEM photograph of cross-sectional lamellar structure and interlayer transverse communication pore structure of a photocured 3D printed dehumidifying ceramic material prepared in example 1;
FIG. 2 is an SEM photograph of a surface arc-shaped convex structure of the photocuring 3D printing dehumidification ceramic material prepared in example 1;
FIG. 3 is a three-dimensional model of the design of example 1;
fig. 4 is a physical diagram of the photocurable 3D printing dehumidifying ceramic material prepared in example 1.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
At present, the gradually mature photocuring 3D printing ceramic technology has high forming precision and high forming speed and can realize the forming of ceramic materials with complex porous or topological structures. In addition, the photocuring 3D printing ceramic material is easy to have a lamellar structure and a structure with transversely communicated air holes between layers, and the convex boundary structure caused by mis-curing in the lamellar printing process can better change the flowing mode of air flow in ceramic air; the inventors of the present invention have found that these characteristics provide convenient preparation conditions for the preparation of the dehumidifying ceramic material.
On one hand, the embodiment of the invention provides a preparation method of a photocuring 3D printing dehumidification ceramic material, which comprises the following steps:
1) preparing photocuring 3D printing dehumidifying ceramic slurry: mixing a 3D printing dehumidifying ceramic solid-phase raw material and a 3D printing liquid phase solvent to obtain photocuring 3D printing dehumidifying ceramic slurry; wherein, by weight, the photocuring 3D printing dehumidification ceramic slurry comprises: 35-50 parts of reinforcer, 1-25 parts of dew condensation agent, 1-15 parts of hydrophobic agent and 30-50 parts of 3D printing liquid phase solvent. Preferably, the photocuring 3D printing dehumidification ceramic slurry further comprises 5-9 parts by weight of an adsorbent.
Preferably, the steps are specifically: mechanically stirring 3D printing dehumidifying ceramic solid phase raw materials (including a reinforcing agent, a condensation agent and a hydrophobic agent, preferably also including an adsorbent); and adding the 3D printing dehumidifying ceramic solid-phase raw material into the 3D printing liquid phase solvent for heat preservation and stirring to obtain the photocuring 3D printing dehumidifying ceramic slurry.
Wherein the dewing agent is selected from angular ceramic particle powder with particle diameter of 10-50 μm, preferably diamond-shaped ceramic particle powder. The ceramic particles with sharp horniness (especially rhombus shape) are similar to camel beard and have excellent condensation effect. The condensing agent is Al2O3、TiO2、SiO2One or more of them.
Wherein the reinforcer is one or more of quartz powder, corundum powder, feldspar powder, biotite powder and kaolinite powder. Preferably, the enhancer is spherical or ellipsoidal powder with a particle size of 50-200 μm. It should be noted here that: the reinforcing agent has the function of promoting the sintering reinforcement of the condensation agent and has better reinforcing effect on the strength of the sintered material. The above-mentioned grain size and shape of the reinforcing agent have a significant influence on the accelerating action during sintering.
Wherein the hydrophobic agent is nano SiO2Nano Al2O3Nano ZrO 22One or more of; preferably, the hydrophobic agent is spherical or ellipsoidal particle powder with the particle size of 10-80 nm. Here, it should be noted that: the hydrophobic agent is a nano spherical or ellipsoidal material to form a lotus-like hydrophobic structure.
Wherein the adsorbent is selected from clay mineral powder, hydromica powder, and SiO2·nH2One or more of O and alunite. The particle size of the adsorbent is 100nm-50 mu m.
Wherein the 3D printing liquid phase solvent comprises photosensitive resin and a diluent; wherein, the volume fraction of the photosensitive resin is 70-80%; the volume fraction of the diluent is 20-30%. Wherein the photosensitive resin is one or more of 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate and trimethylolpropane triacrylate. The diluent is one or two of deionized water and silica sol.
2) And (3) photocuring 3D printing: and carrying out photocuring 3D printing treatment on the photocuring 3D printing dehumidification ceramic slurry to obtain a photocuring 3D printing dehumidification ceramic biscuit.
Designing a three-dimensional model through design software such as UG (Unigraphics) and Solidworks, slicing the three-dimensional model, and exporting a 3D (three-dimensional) printing STL (Standard template library) file; and importing the STL file into a photocuring 3D printer, setting 3D printing parameters, and curing the photocuring 3D printing dehumidifying ceramic slurry according to a three-dimensional model to obtain a photocuring 3D printing dehumidifying ceramic biscuit.
In this step, the photocuring 3D printing process parameters are designed as: the curing thickness is 100-300 mu m, and the curing power is 25-50nW/cm2The single layer curing time is 10-30 s.
3) Degreasing and sintering treatment: and (4) degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain the photocuring 3D printing dehumidification ceramic material.
In the step of degreasing treatment: the degreasing treatment temperature is 550-600 ℃, and the heat preservation time at the degreasing treatment temperature is 300-360 min. Preferably, the temperature is raised to the degreasing temperature at a heating rate of 40-60 ℃/h, and the temperature is lowered at a cooling rate of 40-60 ℃/h after the temperature is maintained for 360 min.
In the step of sintering treatment: the sintering treatment temperature is 1200-1700 ℃, and the heat preservation time at the sintering treatment temperature is 180-600 min; preferably, the temperature is raised to the sintering treatment temperature at the temperature raising rate of 120-180 ℃/h, and the temperature is lowered at the temperature lowering rate of 120-180 ℃/h after the temperature is maintained for 600 min.
On the other hand, the embodiment of the invention also provides a photocuring 3D printing dehumidifying ceramic material, which comprises the following components in parts by weight: 35-50 parts of reinforcing agent, 1-25 parts of condensation agent and 1-15 parts of hydrophobing agent. The condensing agent is ceramic particles with sharp corners; preferably, the component of the condensation agent is Al2O3、TiO2、SiO2One or more of the above; preferably, the condensation agent is rhombus-shaped ceramic particles; preferably, the particle size of the dewing agent is 10-50 μm. The hydrophobic agent is nano SiO2Nano Al2O3Nano ZrO 22One or more of (a). The light-cured 3D printing dehumidifying ceramic material also comprises 5-9 parts by weight of an adsorbent. Preferably, the photocuring 3D printing dehumidifying ceramic material has a lamellar structure, and gaps are formed between lamellae of the lamellar structure to form through interlayer air holes (see fig. 1)Shown). An arc-shaped convex structure is formed on the surface of the airflow channel of the photocuring 3D printing dehumidification ceramic material (see figure 2). The photocuring 3D printing dehumidifying material is prepared by the preparation method of the photocuring 3D printing dehumidifying ceramic material.
In conclusion, the scheme of the invention realizes double dehumidification by using condensation of the condensation agent with a sharp-horn shape (preferably a rhombus shape) and adsorption of the adsorbent, which are added in the material, and widens the dehumidification humidity range and the dehumidification efficiency of the material. Meanwhile, liquid drops formed by condensation can be quickly discharged without being attached by using a hydrophobing agent, so that the quick cyclic utilization of the dehumidifying material is realized, and the dehumidifying effect and efficiency of the photocuring 3D printing dehumidifying material are improved. In addition, the embodiment of the invention utilizes the photocuring 3D printing ceramic material to easily generate a lamellar structure and a structure of transversely communicated air holes between layers, so that water formed by condensation can be timely stored and discharged, and the rapid recycling of the dehumidifying material is realized. In addition, because the lamella is easy to form curved protruding structure on porous material airflow channel surface because of solidification light refraction in photocuring 3D printing ceramic technology preparation in-process lamella, this protruding structure makes the air current that flows into among the dehumidification material form the random flow or vortex, makes the air fully contact with condensation agent and adsorbent among the dehumidification pottery to widen the humidity range of material dehumidification, improve dehumidification effect and the dehumidification efficiency of material.
The following are further detailed by specific experimental examples as follows:
example 1
The embodiment prepares a photocuring 3D printing dehumidifying ceramic material; the raw materials and the parts by weight are as follows: 40 parts of reinforcer, 20 parts of condensation agent, 5 parts of hydrophobic agent, 5 parts of adsorbent and 30 parts of 3D printing liquid phase solvent (wherein in the 3D printing liquid phase solvent, the volume ratio of the photosensitive resin to the diluent is 21: 9).
Wherein the reinforcer is prepared by mixing quartz powder, corundum powder and feldspar powder according to the mass ratio of 3:1: 1. The reinforcing agent has a particle size of 100 μm, and the powder particles are ellipsoidal. The condensing agent is Al2O3And TiO2According toThe mass ratio of the components is 6: 4. The particle size of the dewing agent is 50 μm, and the powder particle shape is rhombic. The hydrophobing agent being SiO2And Al2O3The water repellent agent is mixed according to the mass ratio of 1:1, the particle size of the water repellent agent is 10nm, and the powder particles are spherical. The adsorbent is clay mineral powder and SiO2·nH2O is mixed according to the mass ratio of 1:3, and the particle size of the adsorbent is 50 μm. The photosensitive resin is 1, 6-hexanediol diacrylate, and the diluent is formed by mixing deionized water and silica sol according to the volume ratio of 7: 3.
The preparation method comprises the following specific steps:
1) preparing photocuring 3D printing dehumidifying ceramic slurry: and mechanically stirring and uniformly mixing the enhancer, the condensation agent, the hydrophobic agent and the adsorbent to obtain the 3D printing dehumidifying ceramic solid-phase raw material. Mixing the 3D printing dehumidifying ceramic solid-phase raw material with the 3D printing liquid phase solvent, and stirring for 90 minutes at the temperature of 80 ℃ to obtain the photocuring 3D printing dehumidifying ceramic slurry.
2) And (3) photocuring 3D printing: and designing a three-dimensional model (wherein the three-dimensional model is shown in figure 3) by adopting software UG, slicing the three-dimensional model, and exporting a 3D printing STL file. The STL file was imported into a photocuring 3D printer, and 3D printing parameters were set (wherein the curing thickness was set to 200 μm and the curing power was set to 40 nW/cm)2The monolayer cure time was set to 10 s). And curing the photocuring 3D printing dehumidification ceramic slurry according to the three-dimensional model to obtain a photocuring 3D printing dehumidification ceramic biscuit.
3) Degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain a photocuring 3D printing dehumidification ceramic material; wherein, the degreasing treatment conditions are as follows: heating to 600 ℃ at the heating rate of 40 ℃/h, preserving heat for 360min, and then cooling at the cooling rate of 40 ℃/h; the conditions of the sintering treatment are as follows: heating to 1300 ℃ at the heating rate of 120 ℃/h, preserving the heat for 600min, and then cooling at the cooling rate of 120 ℃/h.
Fig. 1 is an SEM detection photograph of a lamellar structure and an interlayer transverse communication pore structure of a cross section of the photocuring 3D printing dehumidification ceramic material obtained in the present embodiment. As can be seen from fig. 1: obvious lamellar structure can be observed after the cross section is polished, and a large number of communicated air holes are formed between layers; in the dehumidification process, a large number of communicating air holes between layers play a role in storing and discharging liquid water, so that the dehumidification ceramic material can continuously condense and discharge water molecules in the air, and the dehumidification efficiency and the recycling speed are improved.
Fig. 2 is an SEM detection photograph of the surface arc-shaped protrusion structure of the photocuring 3D-printed dehumidifying ceramic material prepared in this embodiment. By observing the surface microstructure of the photocuring 3D printed dehumidifying ceramic material, it can be found that: because the slurry refracts ultraviolet light in the photocuring process, the surface of the sheet layer has an arc-shaped protruding structure, and the high protruding structure enables air flowing into the dehumidifying ceramic to be in turbulent flow or vortex flow, so that the air is fully contacted with a condensing agent and an adsorbent in the dehumidifying ceramic, and the dehumidifying humidity range and dehumidifying efficiency of the material are widened.
Fig. 3 is a physical diagram of the photocuring 3D printing dehumidification ceramic material prepared in example 1.
Example 2
The embodiment prepares a photocuring 3D printing dehumidification ceramic material; the raw materials and the parts by weight are as follows: 35 parts of reinforcer, 25 parts of dewing agent, 1 part of hydrophobic agent, 9 parts of adsorbent and 30 parts of 3D printing liquid phase solvent (wherein in the 3D printing liquid phase solvent, the volume ratio of the photosensitive resin to the diluent is 24: 6).
Wherein the enhancer is prepared by mixing feldspar powder, biotite powder and kaolin powder according to the mass ratio of 4:2: 1. The reinforcing agent has a particle size of 200 μm and the powder particles are spherical. The condensing agent is Al2O3And SiO2The components are mixed according to the mass ratio of 2: 1. The particle size of the dewing agent is 10 μm, and the powder particle shape is rhombic. The hydrophobic agent being ellipsoidal ZrO2Particle powder, and the particle diameter of the hydrophobic agent is 10 nm. The adsorbent is formed by mixing hydromica powder and bauxite according to the mass ratio of 2: 5; the particle size of the adsorbent was 30 μm. The photosensitive resin is prepared from tripropylene glycol diacrylate and trimethylolpropane triacrylateThe diluent is prepared by mixing deionized water and silica sol according to the volume ratio of 4: 1.
The preparation method comprises the following specific steps:
1) preparing photocuring 3D printing dehumidifying ceramic slurry: and mechanically stirring and uniformly mixing the enhancer, the condensation agent, the hydrophobic agent and the adsorbent to obtain the 3D printing dehumidifying ceramic solid-phase raw material. Mixing the 3D printing dehumidifying ceramic solid-phase raw material with the 3D printing liquid phase solvent, and stirring for 60 minutes at the temperature of 120 ℃ to obtain the photocuring 3D printing dehumidifying ceramic slurry.
2) And (3) photocuring 3D printing: a three-dimensional model (as shown in fig. 3) is designed by using software UG, and the three-dimensional model is sliced to derive a 3D print STL file. The STL file was directed to a photocuring 3D printer, and the 3D printing parameters were set (where the curing thickness was set to 300 μm and the curing power was set to 35 nW/cm)2The monolayer cure time was set at 15 s). And curing the photocuring 3D printing dehumidifying ceramic slurry according to the three-dimensional model to obtain a photocuring 3D printing dehumidifying ceramic biscuit.
3) Degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain a photocuring 3D printing dehumidification ceramic material; wherein, the degreasing treatment conditions are as follows: heating to 550 ℃ at a heating rate of 60 ℃/h, preserving heat for 300min, and then cooling at a cooling rate of 60 ℃/h; the conditions of the sintering treatment are as follows: heating to 1350 ℃ at the heating rate of 180 ℃/h, preserving heat for 540min, and then cooling at the cooling rate of 180 ℃/h.
Example 3
The embodiment prepares a photocuring 3D printing dehumidifying ceramic material; the raw materials and the parts by weight thereof are as follows: 35 parts of reinforcer, 11 parts of condensation agent, 15 parts of hydrophobic agent, 9 parts of adsorbent and 30 parts of 3D printing liquid phase solvent (wherein, in the 3D printing liquid phase solvent, the volume ratio of the photosensitive resin to the diluent is 24: 6).
The reinforcer is prepared by mixing quartz powder, feldspar powder and biotite powder according to the mass ratio of 3:1: 1. The reinforcing agent had a particle size of 150 μm, and the powder particles were spherical. Coagulation of waterThe distillate is Al2O3And SiO2The components are mixed according to the mass ratio of 3: 1. The particle size of the dewing agent is 10 μm, and the powder particle shape is rhombic. The hydrophobic agent being ellipsoidal ZrO2Particle powder, and the particle diameter of the hydrophobic agent is 10 nm. The adsorbent is formed by mixing hydromica powder and bauxite according to the mass ratio of 2: 5; the particle size of the adsorbent was 100 nm. The photosensitive resin is prepared by mixing tripropylene glycol diacrylate and trimethylolpropane triacrylate according to the volume ratio of 3:2, and the diluent is prepared by mixing deionized water and silica sol according to the volume ratio of 4: 1.
The preparation method comprises the following specific steps:
1) preparing photocuring 3D printing dehumidifying ceramic slurry: and mechanically stirring and uniformly mixing the enhancer, the condensing agent, the hydrophobic agent and the adsorbent to obtain the 3D printing dehumidifying ceramic solid-phase raw material. Mixing the 3D printing dehumidifying ceramic solid-phase raw material and the 3D printing liquid-phase solvent, and stirring at 120 ℃ for 60 minutes to obtain the photocuring 3D printing dehumidifying ceramic slurry.
2) And (3) photocuring 3D printing: and designing a three-dimensional model (as shown in fig. 3) by using software UG, slicing the three-dimensional model, and exporting a 3D printing STL file. The STL file was directed to a photocuring 3D printer, and 3D printing parameters were set (where the curing thickness was set to 200 μm and the curing power was set to 35 nW/cm)2The monolayer cure time was set at 12 s). And curing the photocuring 3D printing dehumidifying ceramic slurry according to the three-dimensional model to obtain a photocuring 3D printing dehumidifying ceramic biscuit.
3) Degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain a photocuring 3D printing dehumidification ceramic material; wherein, the degreasing treatment conditions are as follows: heating to 550 ℃ at a heating rate of 60 ℃/h, preserving heat for 300min, and then cooling at a cooling rate of 60 ℃/h; the conditions of the sintering treatment are as follows: heating to 1350 ℃ at the heating rate of 180 ℃/h, preserving heat for 540min, and then cooling at the cooling rate of 180 ℃/h.
Example 4
The embodiment prepares a photocuring 3D printing dehumidifying ceramic material; the present embodiment is different from embodiment 1 in that: the adsorbent except 5 parts by weight was replaced with 5 parts by weight of an ellipsoidal quartz powder having a particle size of 100 μm (corresponding to an increase in the amount of the reinforcing agent).
The other raw materials and procedures were identical to those of example 1.
Comparative example 1
Comparative example 1 a dehumidifying ceramic material was prepared, which differs from example 1 in that: replacing the 3D printing solution phase solvent and other qualities with paraffin, and replacing the forming process with the traditional hot-pressing injection process; the rest of the formulation, preparation of the dehumidifying ceramic model and the degreasing and sintering processes are completely the same as those of example 1.
Comparative example 2
Comparative example 2 a photocurable 3D-printed dehumidifying ceramic material was prepared, which differs from example 1 in that: no dew condensation agent and hydrophobic agent are added into the photocuring 3D printing ceramic dehumidifying slurry; the formula, the forming process, the preparation of the dehumidifying ceramic model and the degreasing and sintering processes are completely consistent with those of the embodiment 1.
For the test data of indexes such as porosity, moisture absorption amount, controllable humidity range and the like of the ceramic dehumidifying materials prepared in the above examples 1 to 4, comparative example 1 and comparative example 2 and the conventional preparation method, the test data is shown in table 1.
TABLE 1
Detecting items Porosity of the alloy Amount of moisture absorption Controllable humidity range
Example 1 96％ 31wt.％ 5-95％RH
Example 2 97％ 29wt.％ 8-92％RH
Example 3 98％ 30wt.％ 7-90％RH
Example 4 95％ 23wt.％ 15-85％RH
Comparative example 1 85％ 12wt.％ 20-80％RH
Comparative example 2 80％ 9.5wt.％ 23-78％RH
As can be seen from the data in table 1:
(1) compared with comparative examples 1 and 2, the photocuring 3D printing dehumidifying ceramic material prepared in the embodiment of the invention has high porosity, larger moisture absorption amount and wider dehumidification range, so that the photocuring 3D printing dehumidifying ceramic material prepared in the embodiment of the invention has excellent dehumidification effect.
In addition, the dehumidification efficiency of the ceramic material is mainly related to the moisture absorption amount (the moisture absorption amount is the ratio of the weight of moisture absorbed by the dehumidification material per unit weight), the recovery of the water removal material inside the dehumidification material and the circulation speed, so that the photocuring 3D printing dehumidification ceramic material prepared by the embodiment of the invention has high dehumidification efficiency.
(2) As can be seen by comparing the data of example 1 and example 4: through condensation and adsorption synergistic dehumidification, the dehumidification effect of the photocuring 3D printing dehumidification ceramic material is more obvious.
(3) As can be seen by comparing the data of example 1 and comparative example 1: the condensation agent, the hydrophobic agent and the adsorbent in the slurry have a synergistic effect with the photocuring 3D printing technology, and the porosity, the moisture absorption amount and the dehumidification range of the dehumidification ceramic material can be improved.
Wherein, the theory of cooperation is: utilize photocuring 3D to print ceramic material and appear lamellar structure and the structure of horizontal intercommunication gas pocket between the layer easily, the hydroenergy that makes the condensation form obtains timely storage and discharge, realizes dehumidifying material's quick cycle and uses. The photocuring 3D printing ceramic technology is characterized in that a cambered protruding structure is easily formed on the surface of a porous material airflow channel due to refraction of curing light rays in a preparation process of a lamella, airflow flowing into a dehumidifying material forms turbulent flow or vortex by the aid of the protruding structure, and air is fully contacted with a condensation agent and an adsorbent in the dehumidifying ceramic, so that the dehumidifying humidity range, the dehumidifying effect and the dehumidifying efficiency of the material are widened.
In summary, the embodiment of the invention provides the photocuring 3D printing dehumidifying ceramic material which has the technical characteristic that transverse through air holes are easily formed between photocuring 3D printing laminated structures and sheets, and realizes efficient, stable and wide-range removal of water in gas by combining material formula and synergistic regulation and control of particle size and morphology of raw materials.
The above embodiments are only part of the application examples of the present invention, but the present invention is not limited to the above embodiments, and any method or process similar to the above embodiments may be used to achieve the technical effects of the present invention.

Claims (33)

1. A preparation method of a photocuring 3D printing dehumidification ceramic material is characterized by comprising the following steps:
preparing photocuring 3D printing dehumidifying ceramic slurry: mixing a 3D printing dehumidifying ceramic solid-phase raw material and a 3D printing liquid phase solvent to obtain photocuring 3D printing dehumidifying ceramic slurry; wherein the photocuring 3D printing dehumidifying ceramic slurry comprises the following components in parts by weight: 35-50 parts of reinforcing agent, 1-25 parts of condensation agent, 1-15 parts of hydrophobic agent and 30-50 parts of 3D printing liquid phase solvent; wherein the condensing agent is ceramic particle powder with a sharp angle shape;
and (3) photocuring 3D printing: carrying out photocuring 3D printing treatment on the photocuring 3D printing dehumidification ceramic slurry to obtain a photocuring 3D printing dehumidification ceramic biscuit;
degreasing and sintering treatment: and degreasing and sintering the photocuring 3D printing dehumidification ceramic biscuit to obtain the photocuring 3D printing dehumidification ceramic material.
2. The preparation method of the photocuring 3D printing dehumidification ceramic material as set forth in claim 1, wherein the dewing agent is a diamond-shaped ceramic particle powder.
3. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 1, wherein the component of the dewetting agent is Al2O3、TiO2、SiO2One or more of them.
4. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 1, wherein the particle size of the dewing agent is 10-50 μm.
5. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 1, wherein the reinforcer is one or more of quartz powder, corundum powder, feldspar powder, biotite powder and kaolin powder.
6. The preparation method of the photocuring 3D printing dehumidification ceramic material as set forth in claim 5, wherein the hardening agent has a particle size of 50-200 μm.
7. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 5, wherein the enhancer is spherical or ellipsoidal granular powder.
8. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 1, wherein the water repellent agent is nano SiO2Nano Al2O3Nano ZrO 22One or more of (a).
9. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 8, wherein the particle size of the hydrophobizing agent is 10-80 nm.
10. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 8, wherein the hydrophobizing agent is spherical or ellipsoidal granular powder.
11. The method for preparing a photocurable 3D printing dehumidifying ceramic material according to any one of claims 1-10, wherein the photocurable 3D printing dehumidifying ceramic paste further comprises 5-9 parts by weight of an adsorbent.
12. The method for preparing the photocuring 3D printing dehumidification ceramic material of claim 11, wherein the adsorbent is clay mineral powder, hydromica powder, SiO2·nH2One or more of O and alunite.
13. The method for preparing the photocuring 3D-printed dehumidifying ceramic material of claim 11, wherein the particle size of the adsorbent is 100nm to 50 μm.
14. The method for preparing the photocuring 3D printing dehumidification ceramic material according to any one of claims 1 to 10, wherein the 3D printing liquid phase solvent comprises a photosensitive resin and a diluent; wherein, the volume fraction of the photosensitive resin is 70-80%; the volume fraction of the diluent is 20-30%.
15. The method for preparing the photocuring 3D printing dehumidifying ceramic material of claim 14, wherein the photosensitive resin is one or more of 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate and trimethylolpropane triacrylate.
16. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in claim 14, wherein the diluent is one or both of deionized water and silica sol.
17. The method for preparing a photocurable 3D printed dehumidifying ceramic material as claimed in any one of claims 1-10, wherein the step of formulating a photocurable 3D printed dehumidifying ceramic paste comprises:
mixing the 3D printing dehumidifying ceramic solid-phase raw materials, mixing the 3D printing dehumidifying ceramic solid-phase raw materials with a 3D printing liquid phase solvent, and stirring the mixture at a heat preservation state to obtain the photocuring 3D printing dehumidifying ceramic slurry.
18. The method for preparing a photocurable 3D-printed dehumidifying ceramic material as claimed in claim 17, wherein in the step of formulating a photocurable 3D-printed dehumidifying ceramic paste: the temperature of the heat preservation is 80-180 ℃, and the stirring time is 2-12 h.
19. The method for preparing the photocured 3D printed dehumidifying ceramic material of any one of claims 1-10, wherein the photocuring 3D printing step comprises:
designing a three-dimensional model through software, then slicing the three-dimensional model, and exporting a 3D printing STL file;
and leading the 3D printing STL file into a photocuring 3D printer, setting 3D printing parameters, and curing the photocuring 3D printing dehumidifying ceramic slurry according to the three-dimensional model to obtain a photocuring 3D printing dehumidifying ceramic biscuit.
20. The method for preparing the photocuring 3D printing dehumidifying ceramic material as claimed in claim 19, wherein the 3D printing process parameters are as follows: the curing thickness is 100-300 mu m, and the curing power is 25-50nW/cm2The single layer curing time is 10-30 s.
21. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in any one of claims 1 to 10,
in the step of degreasing treatment: the degreasing temperature is 550-.
22. The method for preparing a photocurable 3D-printing dehumidifying ceramic material according to claim 21, wherein in the step of degreasing treatment: the heating rate is 40-60 ℃/h, and the cooling rate is 40-60 ℃/h.
23. The preparation method of the photocuring 3D printing dehumidification ceramic material as claimed in any one of claims 1 to 10,
in the step of the sintering treatment: the sintering treatment temperature is 1200-1700 ℃, and the heat preservation time at the sintering treatment temperature is 180-600 min.
24. The method for preparing a photocurable 3D-printing dehumidifying ceramic material as claimed in claim 23, wherein in the step of sintering treatment:
the heating rate is 180 ℃/h along with 120-.
25. The photocuring 3D printing dehumidifying ceramic material is characterized by comprising the following components in parts by weight: 35-50 parts of reinforcing agent, 1-25 parts of condensation agent and 1-15 parts of hydrophobing agent;
wherein the condensing agent is ceramic particles with sharp corners.
26. The photocurable 3D printing dehumidifying ceramic material of claim 25,
the component of the dew condensation agent is Al2O3、TiO2、SiO2One or more of them.
27. The photocurable 3D printing dehumidifying ceramic material of claim 25,
the condensing agent is diamond-shaped ceramic particles.
28. The photocurable 3D printing dehumidifying ceramic material of claim 25,
the grain diameter of the dew condensation agent is 10-50 μm.
29. The photocurable 3D printing dehumidifying ceramic material of claim 25,
the hydrophobic agent is nano SiO2Nano Al2O3Nano ZrO 22One or more of (a).
30. The photocurable 3D printing dehumidifying ceramic material of claim 25,
the light-cured 3D printing dehumidifying ceramic material further comprises 5-9 parts by weight of an adsorbent.
31. The photocurable 3D printing dehumidifying ceramic material of claim 25,
the photocuring 3D printing dehumidifying ceramic material has a lamellar structure, gaps are formed among lamellae of the lamellar structure, and penetrating interlayer air holes are formed.
32. The light-cured 3D printed dehumidifying ceramic material of claim 25,
an arc-shaped convex structure is formed on the surface of an airflow channel of the photocuring 3D printing dehumidification ceramic material.
33. The photocurable 3D printing dehumidifying ceramic material of any one of claims 25-32,
the photocuring 3D printing dehumidifying material is prepared by the preparation method of the photocuring 3D printing dehumidifying ceramic material as claimed in any one of claims 1 to 24.
CN202111288841.3A 2021-11-02 2021-11-02 Photocuring 3D printing dehumidifying ceramic material and preparation method thereof Active CN113816758B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5702508A (en) * 1996-01-25 1997-12-30 Moratalla; Jose Ceramic desiccant device
CN109210646A (en) * 2017-06-29 2019-01-15 有限会社科技新领域 Dehumidify humidifying rotor
US10570065B1 (en) * 2018-10-08 2020-02-25 Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. Method of fabricating green desiccant wheel
CN112430103A (en) * 2020-11-19 2021-03-02 中国科学院金属研究所 Photocuring 3D printing hierarchical pore ceramic material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5702508A (en) * 1996-01-25 1997-12-30 Moratalla; Jose Ceramic desiccant device
CN109210646A (en) * 2017-06-29 2019-01-15 有限会社科技新领域 Dehumidify humidifying rotor
US10570065B1 (en) * 2018-10-08 2020-02-25 Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. Method of fabricating green desiccant wheel
CN112430103A (en) * 2020-11-19 2021-03-02 中国科学院金属研究所 Photocuring 3D printing hierarchical pore ceramic material and preparation method thereof

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