CN112960991A - Ceramic polymer composite material and preparation method thereof - Google Patents
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Abstract
The invention provides a ceramic polymer composite material, which takes inverse opal structure ceramic as a main body, wherein the inverse opal structure ceramic is provided with air holes, a zirconium oxide seed crystal layer is formed in the air holes, zirconium oxide nanowires are formed on the zirconium oxide seed crystal layer, and gaps among the zirconium oxide nanowires are filled with organic polymer materials. The thickness of the zirconium oxide seed crystal layer is 5-10nm, and the length-diameter ratio of the zirconium oxide nanowire is 8-12. Also provides a method for preparing the ceramic polymer composite material, which comprises the following steps: s1, providing a main body structure; s2, forming a zirconium oxide seed crystal layer; s3, forming zirconium oxide nanowires; s4, filling organic polymer material. According to the ceramic polymer composite material and the preparation method thereof, the inverse opal structure is combined with organic matters more tightly, the comprehensive performance is excellent, the ceramic polymer composite material is not easy to damage under the action of external force, and the service life of the ceramic is effectively prolonged.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a ceramic polymer composite material and a preparation method thereof.
Background
In the prior art, because the combination between the air holes and the organic matters of the inverse opal structure ceramic is not firm enough, the organic matters are easy to slide and fall off at the interface combination position. And the comprehensive performance is poor, when the ceramic is subjected to external force, the stress is uneven, the local damage and even the integral damage of the ceramic are easily caused, and the service life of the ceramic is short.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a ceramic polymer composite material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a ceramic polymer composite material takes inverse opal structure ceramic as a main body, the inverse opal structure ceramic is provided with air holes, a zirconia seed crystal layer is formed on the air holes, zirconia nanowires are formed on the zirconia seed crystal layer, and organic polymer materials are filled in gaps among the zirconia nanowires.
The further improvement of the technical scheme is as follows:
the thickness of the zirconium oxide seed crystal layer is 5-10nm, and the length-diameter ratio of the zirconium oxide nanowire is 8-12.
The inverse opal structure ceramic is an alumina inverse opal structure ceramic.
The invention also provides a method for preparing the ceramic polymer composite material, which comprises the following steps:
s1, the main structure provides: providing an alumina inverse opal structure ceramic having air pores;
s2, forming a zirconium oxide seed crystal layer: depositing a zirconia seed layer on the air holes;
s3, forming the zirconium oxide nanowire: growing zirconia nanowires on the zirconia seed crystal layer to obtain alumina inverse opal structural ceramics with a zirconia nanowire structure;
s4, filling organic polymer material: filling organic polymer materials in the gaps between the zirconia nanowires prepared in step S3, and simultaneously curing the organic polymer materials by using a curing agent in a matching manner.
The further improvement of the technical scheme is as follows:
the alumina inverse opal structure ceramic in the step S1 is prepared by the following method:
spherical particles of silicon dioxide, polystyrene and PMMA are self-assembled to form a template, alumina is filled in the pores of the template, and then the template is removed to obtain the alumina inverse opal structure ceramic.
The zirconia seed layer in step S2 is prepared by the following method:
opening corresponding atomic layer deposition valve and introducingZirconium tetramethylamino; removing excess tetramethylamino zirconium and reaction by-products by a purging process; opening corresponding atomic layer deposition valve and introducing H2O; removal of excess H by a purge process2O and reaction by-products;
the above operations are repeated until the zirconia seed layer reaches the desired thickness.
The zirconia nanowires in step S3 were prepared by the following method:
s3.1, preparing a reaction mother solution: ZrOCl2·6H2O、Y(NO3)3·6H2Dissolving O and citric acid in deionized water to form a solution, and stirring and reacting at the temperature of 60-80 ℃ to form white sol;
adding ethylenediamine or ammonia water into the white sol, uniformly stirring, and finely adjusting the pH value to 7.5-8.5 to obtain reaction mother liquor;
s3.2, generating the zirconium oxide nanowire: and controlling the temperature of the reaction mother liquor to be between 90 and 100 ℃, soaking the zirconium oxide seed crystal layer into the reaction mother liquor, standing for 1 to 3 hours, taking out the zirconium oxide seed crystal layer, and growing a zirconium oxide nanowire on the zirconium oxide seed crystal layer.
ZrOCl as described in step S3.12·6H2O、Y(NO3)3·6H2The molar ratio of O to citric acid is 92-94: 6-8: 92-94.
In the step S3.1, the total concentration of the solute in the solution is not more than 0.4mol/L, and the stirring reaction time is 2-3 h.
The specific method of step S4 is as follows:
s4.1, filling: heating and vacuumizing the alumina inverse opal structure ceramic prepared in the step S3 in a glue injection machine, and filling an organic high polymer material and a curing agent into gaps among the zirconia nanowires under the action of atmospheric pressure;
s4.2, curing: placing the alumina inverse opal structure ceramic filled with the organic polymer material and the curing agent in an oven for curing for 3-4h, and weighing after curing;
s4.3, circulating: and (4) repeating the steps S4.1 and S4.2, and when the weight difference between the weight weighed in the step S4.3 and the weight weighed in the step S4.2 is less than 0.01g, terminating the operation to obtain the ceramic polymer composite material.
According to the technical scheme of the invention, the ceramic polymer composite material takes the inverse opal structure ceramic as a main body, the zirconia seed crystal layer is formed on the air hole of the inverse opal structure ceramic, the zirconia nanowires are formed on the zirconia seed crystal layer, the organic polymer material is filled in the gaps among the zirconia nanowires, the zirconia nanowires have various orientations in the inverse opal structure ceramic, a large number of zirconia nanowires are like 'claws' growing on the alumina inverse opal structure ceramic in various postures, and the claws firmly grasp the polymer organic matter to ensure that the ceramic and the organic matter do not slide or fall off relatively at the interface. And because the zirconia nano wire has elasticity and toughness, when the zirconia nano wire is acted by an external force, the stress can be evenly transmitted to the whole structure, so that the ceramic is stressed uniformly, the local damage and even the whole damage caused by the overlarge local stress are avoided, the deformation of the ceramic caused by the overlarge stress can be recovered to the original shape due to the elasticity of the zirconia nano wire, and the working efficiency and the accuracy of the ceramic are ensured. Because the inverse opal structure ceramic is a three-dimensional porous ceramic framework and has a continuous ceramic material distribution network, the organic matter filled in the framework structure is also in a network structure, and the ceramic material and the organic matter are uniformly distributed on the whole, thereby greatly improving the comprehensive performance of the ceramic polymer composite material.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a ceramic polymer composite according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In example 1, the ceramic polymer composite material of this embodiment mainly includes an aluminum oxide inverse opal structure ceramic, in which spherical or spheroidal air holes are formed, a zirconia seed layer is formed on the air holes, zirconia nanowires are formed on the zirconia seed layer, and gaps between the zirconia nanowires are filled with an organic polymer material, which may be a resin or the like.
Wherein the thickness of the zirconium oxide seed crystal layer is 5-10nm, and the length-diameter ratio of the zirconium oxide nano wire is 8-12.
The alumina inverse opal structure ceramic is formed into a template by self-assembling small spheres of silicon dioxide, polystyrene and PMMA (polymethyl methacrylate), wherein the particle size of the small spheres is 200nm-300 nm; filling pores of the template with alumina by a sol-gel method, nano particles or Atomic Layer Deposition (ALD), and removing the initial template formed by the silica polystyrene and the PMMA by methods such as calcination, chemical corrosion, solvent dissolution and the like to obtain the alumina inverse opal structure ceramic with the air pore structure.
As shown in fig. 1, the preparation method of the ceramic polymer composite material comprises the following steps:
s1, the main structure provides: the method for providing the alumina inverse opal structure ceramic with the air holes comprises the following steps:
self-assembling spherical particles of silicon dioxide, polystyrene and PMMA to form a template, wherein the particle size of the spherical particles is 200nm-300 nm; filling pores of the template with alumina by a sol-gel method, nano particles or Atomic Layer Deposition (ALD), and removing the initial template formed by the silica polystyrene and the PMMA by methods such as calcination, chemical corrosion, solvent dissolution and the like to obtain the alumina inverse opal structure ceramic with regularly arranged spherical or sphere-like air pores.
S2, forming a zirconium oxide seed crystal layer: and depositing a zirconium oxide seed crystal layer with the thickness of 5-10nm on the air hole, wherein the specific method comprises the following steps:
s2.1, opening a corresponding Atomic Layer Deposition (ALD) valve for 5S-10S, and introducing tetramethyl amino zirconium (TDMAZr).
S2.2, maintaining the exposure process for 60-120S to promote the reaction to fully progress.
S2.3, maintaining a purging process of 120S-180S to remove the excess TDMAZr and reaction by-products.
S2.4, opening the corresponding ALD valve for 5-10S, and introducing H2O。
S2.5, maintaining the exposure process for 60-120S to promote the reaction to fully progress.
S2.6, maintaining a 180S-240S purge process to remove excess H2O and reaction by-products.
And repeating the steps S2.1-S2.6 until the thickness of the zirconia seed crystal layer reaches 5-10 nm.
S3, forming the zirconium oxide nanowire: and (3) growing the zirconia nanowires on the zirconia seed crystal layer by adopting a hydrothermal method to obtain the alumina inverse opal structural ceramic with the zirconia nanowire structure.
S3.1, preparing a reaction mother solution: proportionally mixing 92-94 mol of ZrOCl2·6H2O, 6 to 8 mol of Y (NO)3)3·6H2Dissolving O and 92-94 mol of citric acid in deionized water to form a solution, wherein the total concentration of solutes in the solution is not more than 0.4mol/L, and stirring and reacting for 2-3h at the temperature of 60-80 ℃ to form white sol.
And adding ethylenediamine or ammonia water into the white sol, stirring for 25-30 min until the mixture is uniformly mixed, and finely adjusting the pH value of the mixture to 7.5-8.5 to obtain reaction mother liquor.
S3.2, generating the zirconium oxide nanowire: and controlling the temperature of the reaction mother liquor to be between 90 and 100 ℃, immersing the zirconium oxide seed crystal layer into the reaction mother liquor, standing for 1 to 3 hours, taking out, naturally cooling, washing the zirconium oxide seed crystal layer with deionized water, drying the zirconium oxide seed crystal layer by blowing, and growing a zirconium oxide nanowire on the zirconium oxide seed crystal layer. The length-diameter ratio of the zirconia nanowire is 8-12.
S4, filling organic polymer material: and (4) filling an organic polymer material in the air holes of the alumina inverse opal structure ceramic prepared in the step (S3), and simultaneously curing the organic polymer material by using a curing agent in a matching manner. The organic polymer material may be a resin or the like.
S4.1, filling: and (4) vacuumizing the alumina inverse opal structure ceramic prepared in the step (S3) at the temperature of 220-250 ℃ in a glue injection machine, and filling the organic polymer material and the curing agent into gaps among the zirconia nanowires under the action of atmospheric pressure.
S4.2, curing: placing the alumina inverse opal structure ceramic filled with the organic polymer material and the curing agent in an oven, curing at the temperature of 70-80 ℃ for 3-4h, and weighing after curing.
S4.3, circulating: and (4) repeating the steps S4.1 and S4.2, and when the weight difference between the weight weighed in the step S4.3 and the weight weighed in the step S4.2 is less than 0.01g, terminating the operation to obtain the ceramic polymer composite material.
To prove that the ceramic polymer composite material prepared in the embodiment has better comprehensive performance, sampling detection is carried out on the ceramic polymer composite material prepared by adopting different TDMAZr exposure time, different total solute concentration and different pH values, the existing material only filled with organic resin in the inverse opal structure ceramic is taken as a comparative example, comparison is carried out, and the detection and comparison results are shown in table 1:
TABLE 1
From the above data, the ceramic polymer composite material prepared by the method of the present embodiment has a lower dielectric constant, a lower density, and a higher fracture toughness than the ceramic polymer composite material prepared by the prior art, and the comprehensive properties thereof are effectively improved.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only express preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A ceramic polymer composite material is characterized in that: the method comprises the following steps of taking inverse opal structure ceramic as a main body, wherein the inverse opal structure ceramic is provided with air holes, a zirconia seed crystal layer is formed on the air holes, zirconia nanowires are formed on the zirconia seed crystal layer, and organic polymer materials are filled in gaps among the zirconia nanowires.
2. The ceramic polymer composite according to claim 1, wherein: the thickness of the zirconium oxide seed crystal layer is 5-10nm, and the length-diameter ratio of the zirconium oxide nanowire is 8-12.
3. The ceramic polymer composite according to claim 1, wherein: the inverse opal structure ceramic is an alumina inverse opal structure ceramic.
4. A method of preparing the ceramic polymer composite of any one of claims 1 to 3, characterized in that: the method comprises the following steps:
s1, the main structure provides: providing an alumina inverse opal structure ceramic having air pores;
s2, forming a zirconium oxide seed crystal layer: depositing a zirconia seed layer on the air holes;
s3, forming the zirconium oxide nanowire: growing zirconia nanowires on the zirconia seed crystal layer to obtain alumina inverse opal structural ceramics with a zirconia nanowire structure;
s4, filling organic polymer material: filling organic polymer materials in gaps among the zirconia nanowires of the alumina inverse opal structure ceramic prepared in step S3, and simultaneously curing the organic polymer materials by using a curing agent in a matching manner.
5. The method of claim 4, wherein: the alumina inverse opal structure ceramic in the step S1 is prepared by the following method:
spherical particles of silicon dioxide, polystyrene and PMMA are self-assembled to form a template, alumina is filled in the pores of the template, and then the template is removed to obtain the alumina inverse opal structure ceramic.
6. The method of claim 4, wherein: the zirconia seed layer in step S2 is prepared by the following method:
opening a corresponding atomic layer deposition valve, and introducing tetramethyl amino zirconium; removing excess tetramethylamino zirconium and reaction by-products by a purging process; opening corresponding atomic layer deposition valve and introducing H2O; removal of excess H by a purge process2O and reaction by-products;
the above operations are repeated until the zirconia seed layer reaches the desired thickness.
7. The method of claim 4, wherein: the zirconia nanowires in step S3 were prepared by the following method:
s3.1, preparing a reaction mother solution: ZrOCl2·6H2O、Y(NO3)3·6H2Dissolving O and citric acid in deionized water to form a solution, and stirring and reacting at the temperature of 60-80 ℃ to form white sol;
adding ethylenediamine or ammonia water into the white sol, uniformly stirring, and adjusting the pH value to 7.5-8.5 to obtain reaction mother liquor;
s3.2, generating the zirconium oxide nanowire: and controlling the temperature of the reaction mother liquor to be between 90 and 100 ℃, soaking the zirconium oxide seed crystal layer into the reaction mother liquor, standing for 1 to 3 hours, taking out the zirconium oxide seed crystal layer, and growing a zirconium oxide nanowire on the zirconium oxide seed crystal layer.
8. The method of claim 7, wherein: ZrOCl as described in step S3.12·6H2O、Y(NO3)3·6H2The molar ratio of O to citric acid is 92-94: 6-8: 92-94.
9. The method of claim 7, wherein: in the step S3.1, the total concentration of the solute in the solution is not more than 0.4mol/L, and the stirring reaction time is 2-3 h.
10. The method of claim 4, wherein: the specific method of step S4 is as follows:
s4.1, filling: heating and vacuumizing the alumina inverse opal structure ceramic prepared in the step S3 in a glue injection machine, and filling an organic high polymer material and a curing agent into gaps among the zirconia nanowires under the action of atmospheric pressure;
s4.2, curing: placing the alumina inverse opal structure ceramic filled with the organic polymer material and the curing agent in an oven for curing for 3-4h, and weighing after curing;
s4.3, circulating: and (4) repeating the steps S4.1 and S4.2, and when the weight difference between the weight weighed in the step S4.3 and the weight weighed in the step S4.2 is less than 0.01g, terminating the operation to obtain the ceramic polymer composite material.
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| 周菲迟等: "籽晶层制备方式对氧化锌纳米棒阵列的影响", 《无机化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116003162A (en) * | 2022-12-14 | 2023-04-25 | 萍乡学院 | Electroceramics semiconductor glaze and preparation method thereof |
| CN116003162B (en) * | 2022-12-14 | 2023-08-08 | 萍乡学院 | Electroceramics semiconductor glaze and preparation method thereof |
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| CN112960991B (en) | 2022-05-31 |
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