CN114804885B - Preparation method of bucky paper/fly ash wear-resistant ceramic patch - Google Patents
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Abstract
A method for preparing a balsa paper/fly ash wear-resistant ceramic patch comprises the steps of conventionally carboxylating balsa paper, soaking the balsa paper in a dopamine aluminum nitrate solution, and carrying out ultrasonic treatment; preparing colloidal body by using n-butyl silicate, alumina sol and micro-nano fly ash, then coating the colloidal body on the bottom layer of a steel mould plate, then flatly paving the obtained bucky paper on the colloidal body, and repeating for 3-5 times to form a fly ash/bucky paper interlayer material; extruding and forming the interlayer material, and drying to obtain a blank. And sintering the blank in a high-temperature vacuum environment or an inert gas protection environment, and cooling to room temperature along with the furnace to obtain the bucky paper/fly ash wear-resistant ceramic patch. The invention has the advantages of simplicity, safety, easy operation, controllability and the like. Compared with the traditional chemical plating, the prepared ceramic patch has more advantages in interface adhesion; the hard and brittle performance of the ceramic wear-resistant sheet can be improved; the customizability of the shape of the ceramic wear-resistant patch is easier to realize.
Description
Technical Field
The invention belongs to the technical field of material preparation.
Background
Mullite is used as a high-quality aluminosilicate raw material, has excellent thermal stability, mechanical strength, electrical and optical properties, and is widely applied to the field of functional ceramics. The fly ash is used as an industrial waste, and the main components of the fly ash are alumina and silicon oxide which are suitable for mullite synthesis raw materials. Partial academic papers show that the components of the composite material are reasonably utilized, and the wear resistance, the mechanics performance and other various performances of the composite material can be obviously improved. However, the disadvantage is also evident, the pure ceramic structure being indicative of an extremely poor toughness, which is hard and brittle without optimization. Limiting its application in the field of surface wear resistant materials. On the other hand, the bucky paper has excellent breaking strength and toughness. Besides the better wear-resisting property, the material can also be used as a material structure support. But are difficult to use directly in composites due to low density and performance stability.
At present, the main stream wear-resistant ceramic paster in the market is zirconia and alumina, compared with the fly ash raw material, in daily use, the cost performance is relatively low besides the problem of extremely high requirement on the installation and fitting degree of a workpiece caused by hard brittleness. If the fly ash and the Baji paper are organically combined by adopting a new technology, the defects of each other can be complemented and a novel wear-resistant paster can be prepared. The invention is in accordance with the theme of energy conservation and environmental protection, effectively solves the problem of environmental pollution caused by the accumulation of the fly ash, reduces the raw material cost of the mullite material, and realizes the high-value resource utilization of the fly ash.
Disclosure of Invention
The invention aims to provide a preparation method of a bucky paper/fly ash wear-resistant ceramic patch, which is characterized in that a flaky bucky paper/fly ash sandwich structure is utilized to prepare the wear-resistant patch. According to the invention, the interlayer sintering is combined through an interface modification method, a viscosity layer is coated on the basepaper, and the viscosity layer and the basepaper layer are promoted to generate micro reaction, so that the optimization of the interface layer with the fly ash ceramic is finally achieved, and the combination effect is increased. And because the Basa paper can be bent, the Basa paper has an obvious shape customization, and is suitable for the performance reinforcement of various complex parts. In addition, the existence of the bucky paper can effectively reduce the hard and brittle defects of the ceramic, so that the toughness of the material can be obviously improved.
The invention is realized by the following technical scheme.
The invention relates to a preparation method of a bucky paper/fly ash wear-resistant ceramic patch, which comprises the following steps.
(1) The buckypaper is conventionally carboxylated. The thickness of the chosen paper is controlled within 0.15 to 0.2mm, and the purity is 95 to 99.9 percent.
(2) And (2) adding the carboxylated bucky paper obtained in the step (1) into an aluminum nitrate solution with the concentration of 15-25wt.% for ultrasonic treatment for 10-15 min, wherein the ultrasonic power is more than or equal to 150W.
(3) And (3) adding dopamine into the aluminum nitrate solution obtained in the step (2) according to the mass ratio of the aluminum nitrate solution to the dopamine of 0.2-0.1.
(4) And (3) adding a TRIS (hydroxymethyl) aminomethane (TRIS) buffer into the solution obtained in the step (3), adjusting the pH value to 8~9, continuously performing ultrasonic treatment for 3h to 5h, taking out the Bas paper, and drying in the air.
(5) Mixing 10 to 15vol.% of ethyl orthosilicate or butyl orthosilicate, 5 to 10vol.% of alumina sol (the content of alumina is 21 to 23wt.%), and 75 to 85vol.% of micro-nano fly ash, and performing ultrasonic vibration for 10 to 30min to obtain a fly ash colloid.
(6) Uniformly spreading the fly ash colloid obtained in the step (5) in a steel mould with the thickness of 1-3 mm, spreading the bucky paper obtained in the step (4) on the fly ash colloid in the steel mould, and repeating the steps for many times to form the sandwich material sandwiched with more than 3 layers of bucky paper.
(7) And (4) extruding and forming the interlayer material obtained in the step (6) in a mould under the pressure of 20 to 100MPa, taking out the interlayer material and drying the interlayer material at the temperature of below 90 ℃ to obtain the Bakeba paper/fly ash ceramic paster blank.
(8) Sintering the bucky paper/fly ash ceramic paster blank obtained in the step (7) in vacuum or inert gas atmosphere, wherein the vacuum degree is less than or equal to 10 -3 the sintering temperature is 1100 to 1500 ℃, and the heat preservation time is 2h to 4h. Wherein the temperature rising speed from room temperature to 250 to 350 ℃ is 1~3 ℃/min, the temperature rising speed from 250 to 350 ℃ to 850 to 1000 ℃ is 3 to 10 ℃/min, and the temperature rising speed from 850 to 1000 ℃ to the sintering temperature is 1~3 ℃/min. And obtaining the bucky paper/fly ash ceramic paster.
The main reaction equation generated in the sintering process of the invention is as follows:
SiO 2 +3C=SiC+2CO （1）；
2SiO 2 +3Al 2 O 3 = 3Al 2 O 3 ·2SiO 2 （2）。
compared with the prior art, the invention has the following technical effects: (1) The reactivity of silicon oxide and carbon is utilized to form a reaction transition layer. Compared with the traditional chemical plating, the interface adhesion is more advantageous. (2) The Baji paper has better toughness, so that the hard brittleness of the ceramic wear-resistant sheet can be improved. (3) The customizability of the shape of the ceramic wear-resistant paster is easier to realize by utilizing the foldability of the bucky paper. Therefore, the novel bucky paper/fly ash wear-resistant ceramic patch has wider applicability.
Drawings
FIG. 1 is an SEM micro-topography of a buckypaper/fly ash abrasion resistant ceramic patch made in example 1 of the present invention.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1.
(1) Putting the bucky paper with the purity of 99% and the thickness of 0.2mm into a mixed solution of concentrated nitric acid and concentrated sulfuric acid with the volume ratio of 1:3, and carrying out reflux reaction at 80 ℃ for 4h to obtain the carboxylated bucky paper.
(2) And (2) adding the carboxylated bucky paper obtained in the step (1) into an aluminum nitrate solution with the concentration of 15wt.% for ultrasonic treatment for 15min, wherein the ultrasonic power is 160W.
(3) Adding dopamine into the aluminum nitrate solution obtained in the step (2) according to the mass ratio of the aluminum nitrate solution to the dopamine of 0.15.
(4) And (4) adding a TRIS buffer into the solution obtained in the step (3) to adjust the pH value to 8, continuously carrying out ultrasonic treatment for 4 hours, taking out the buckyband paper, and airing.
(5) Mixing 10vol.% of ethyl orthosilicate, 10vol.% of alumina sol (the content of alumina is 22 wt.%), and 80vol.% of micro-nano fly ash into a gel, and performing ultrasonic treatment for 30min.
(6) And (3) uniformly spreading the fly ash colloid obtained in the step (5) in a steel mould, wherein the thickness of the fly ash colloid is 2mm, spreading the bucky paper obtained in the step (4) on the fly ash colloid in the steel mould, and repeating the steps for multiple times to form the interlayer material sandwiched with 4 layers of bucky paper.
(7) And (5) applying 40MPa pressure to the interlayer material obtained in the step (6) in a steel mould for forming, taking out the interlayer material, and drying at 80 ℃ to obtain the bucky paper/fly ash ceramic paster blank.
(8) Putting the Baji paper/fly ash ceramic paster blank obtained in the step (7) into a vacuum sintering furnace for heating and sintering, wherein the vacuum degree is 10 -3 torr, sintering temperature 1300 ℃, and heat preservation time 2h. Wherein the temperature rising speed from room temperature to 250 ℃ is 2 ℃/min, the temperature rising speed from 250 ℃ to 900 ℃ is 5 ℃/min, and the temperature rising speed from 900 ℃ to 1300 ℃ is 2 ℃/min. And obtaining the bucky paper/fly ash ceramic paster.
Example 2.
(1) Putting the bucky paper with the purity of 99% and the thickness of 0.15mm into a mixed solution of concentrated nitric acid and concentrated sulfuric acid with the volume ratio of 1:3, and carrying out reflux reaction at 80 ℃ for 4h to obtain the carboxylated bucky paper.
(2) Adding the carboxylated bucky paper obtained in the step (1) into an aluminum nitrate solution with the concentration of 20wt.% for ultrasonic treatment for 15min, wherein the ultrasonic power is 150W.
(3) And (3) adding dopamine into the aluminum nitrate solution obtained in the step (2) according to the mass ratio of the aluminum nitrate solution to the dopamine of 0.2.
(4) And (3) adding a TRIS buffer into the solution obtained in the step (3) to adjust the pH value to 9, continuously carrying out ultrasonic treatment for 3h, taking out the Bass paper, and airing.
(5) 15vol.% of ethyl orthosilicate, 10vol.% of alumina sol (the content of alumina is 23 wt.%), and 75vol.% of micro-nano fly ash are mixed into a gel, and ultrasonic treatment is carried out for 30min.
(6) And (3) uniformly spreading the fly ash colloid obtained in the step (5) in a steel mould, wherein the thickness of the fly ash colloid is 2mm, spreading the bucky paper obtained in the step (4) on the fly ash colloid in the steel mould, and repeating the steps for multiple times to form the interlayer material sandwiched with 4 layers of bucky paper.
(7) And (5) applying 60MPa pressure to the interlayer material obtained in the step (6) in a steel mould for forming, taking out the interlayer material, and drying at 80 ℃ to obtain the bucky paper/fly ash ceramic paster blank.
(8) Will step withPutting the Baji paper/fly ash ceramic paster blank obtained in the step (7) into a vacuum sintering furnace for heating and sintering, wherein the vacuum degree is 10 -3 torr, sintering temperature 1100 ℃, and holding time 4h. Wherein the temperature rising speed from room temperature to 300 ℃ is 2 ℃/min, the temperature rising speed from 250 ℃ to 850 ℃ is 5 ℃/min, and the temperature rising speed from 850 ℃ to 1100 ℃ is 2 ℃/min. And obtaining the bucky paper/fly ash ceramic paster.
Example 3.
(1) Putting the bucky paper with the purity of 99% and the thickness of 0.2mm into a mixed solution of concentrated nitric acid and concentrated sulfuric acid with the volume ratio of 1:3, and carrying out reflux reaction at 80 ℃ for 4h to obtain the carboxylated bucky paper.
(2) Adding the carboxylated bucky paper obtained in the step (1) into an aluminum nitrate solution with the concentration of 25wt.% for ultrasonic treatment for 15min, wherein the ultrasonic power is 170W.
(3) And (3) adding dopamine into the aluminum nitrate solution obtained in the step (2) according to the mass ratio of the aluminum nitrate solution to the dopamine of 0.1, and then continuing ultrasound for 25min at the ultrasound power of 170W.
(4) And (3) adding a TRIS buffer into the solution obtained in the step (3) to adjust the pH value to 9, continuously carrying out ultrasonic treatment for 5h, taking out the Bass paper, and airing.
(5) 5vol.% of ethyl orthosilicate, 10vol.% of alumina sol (the content of alumina is 21 wt.%), and 85vol.% of micro-nano fly ash are mixed into a gel, and ultrasonic treatment is carried out for 30min.
(6) And (3) uniformly spreading the fly ash colloid obtained in the step (5) in a steel mould, wherein the thickness of the fly ash colloid is 2mm, spreading the bucky paper obtained in the step (4) on the fly ash colloid in the steel mould, and repeating the steps for multiple times to form the interlayer material sandwiched with 4 layers of bucky paper.
(7) And (4) applying 80MPa pressure to the interlayer material obtained in the step (6) in a steel mould for forming, taking out and drying at 80 ℃ to obtain the Baji paper/fly ash ceramic paster blank.
(8) Putting the Baji paper/fly ash ceramic paster blank obtained in the step (7) into a vacuum sintering furnace for heating and sintering, wherein the vacuum degree is 10 -3 torr, sintering temperature 1500 ℃, and holding time 2h. Wherein the temperature rising speed from room temperature to 350 ℃ is 2 ℃/min, the temperature rising speed from 350 ℃ to 1000 ℃ is 5 ℃/min and 1000The temperature rise speed is 2 ℃/min from the temperature of DEG C to 1500 ℃. And obtaining the bucky paper/fly ash ceramic paster.
TABLE 1 Basa paper/fly ash abrasion resistant ceramic Patch Properties
Claims (1)
1. A preparation method of a balsa paper/fly ash wear-resistant ceramic paster is characterized by comprising the following steps:
(1) Conventionally carboxylating the bucky paper, wherein the thickness of the chosen bucky paper is controlled to be 0.15 to 0.2mm, and the purity is 95 to 99.9 percent;
(2) Adding the carboxylated bucky paper obtained in the step (1) into an aluminum nitrate solution with the concentration of 15-25wt.% for ultrasonic treatment for 10-15 min, wherein the ultrasonic power is more than or equal to 150W;
(3) Adding dopamine into the aluminum nitrate solution obtained in the step (2) according to the mass ratio of the aluminum nitrate solution to the dopamine of 0.2-0.1;
(4) Adding a trihydroxymethyl aminomethane buffering agent into the solution obtained in the step (3) to adjust the pH value to 8~9, continuously performing ultrasonic treatment for 3h to 5h, taking out the Bass paper and drying in the air;
(5) Mixing 10-15 vol.% of ethyl orthosilicate or butyl orthosilicate and 5-10vol.% of alumina sol, wherein the content of alumina is 21-23wt.%, and 75-85 vol.% of micro-nano fly ash is subjected to ultrasonic treatment for 10-30min to obtain a fly ash colloid;
(6) Uniformly spreading the fly ash colloid obtained in the step (5) in a steel mould, wherein the thickness of the fly ash colloid is 1-3 mm, then spreading the bucky paper obtained in the step (4) on the fly ash colloid in the steel mould, and repeating the steps for many times to form an interlayer material in which more than 3 layers of bucky paper are sandwiched;
(7) Extruding and forming the interlayer material obtained in the step (6) in a die, wherein the pressure is 20 to 100MPa, taking out the interlayer material, and drying the interlayer material at the temperature of below 90 ℃ to obtain a bucky paper/fly ash ceramic paster blank;
(8) The bucky paper/fly ash ceramic paster blank obtained in the step (7)Sintering the body in vacuum or inert gas atmosphere with vacuum degree less than or equal to 10 -3 the sintering temperature is 1100 to 1500 ℃, and the heat preservation time is 2h to 4h; wherein the temperature rising speed from room temperature to 250-350 ℃ is 1~3 ℃/min, the temperature rising speed from 250-350 ℃ to 850-1000 ℃ is 3-10 ℃/min, and the temperature rising speed from 850-1000 ℃ to sintering temperature is 1~3 ℃/min, so that the bucky paper/fly ash ceramic patch is obtained.
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| CN107935543A (en) * | 2017-10-12 | 2018-04-20 | 潘正龙 | A kind of wear-resisting composite ceramic mud of scratch resistance and preparation method thereof |
| CN109210319A (en) * | 2018-11-12 | 2019-01-15 | 中研信源（北京）节能科技有限公司 | A kind of aerogel vacuum thermal insulation plate and its core material with and preparation method thereof |
| CN110156442A (en) * | 2019-04-08 | 2019-08-23 | 启东市聚旺铸造有限公司 | Use the light-weight refractory aggregate and preparation method thereof of model casting antiquated sand |
| WO2020218631A1 (en) * | 2019-04-23 | 2020-10-29 | 원경에프에이비(주) | Board for building finishing and manufacturing method therefor |
| KR102157335B1 (en) * | 2019-12-27 | 2020-09-18 | 변경호 | Eco-Friendly Functional Clay Bricks |
| CN113773110A (en) * | 2021-09-30 | 2021-12-10 | 东北大学 | Preparation method of carbon nano tube/leucite porous ceramic composite material converted from alkali-activated fly ash |
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