CN115432957B - Method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering - Google Patents
Method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering Download PDFInfo
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Abstract
The invention discloses a method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering, which comprises the steps of ball milling and mixing ZnO powder and PTFE powder to obtain ZnO-PTFE composite powder; adding a cold sintering aid into the ZnO-PTFE composite powder, and fully and uniformly grinding to obtain powder to be sintered; and pouring the powder to be sintered into a mould, applying pressure, and naturally cooling by adopting common cold sintering or plasma sintering to obtain the ZnO-PTFE composite ceramic. The ZnO-polytetrafluoroethylene composite ceramic sheet with high density is obtained by adopting a cold sintering mode, the relative density is higher than 98 percent, the super-hydrophobic ceramic sheet has super-hydrophobic characteristic, and the hydrophobic angle can reach 160 degrees.
Description
Technical Field
The invention relates to a preparation method of ZnO composite ceramic, in particular to a method for preparing ZnO-Polytetrafluoroethylene (PTFE) composite ceramic with super-hydrophobic property based on cold sintering.
Background
ZnO has a narrow forbidden bandwidth of about 3.37eV, has a large number of point defects such as zinc gap filling and oxygen vacancies, is a typical N-type semiconductor, and is widely studied as a base material for pressure-sensitive, gas-sensitive, thermoelectric, optical and other devices. In general, in order to make ZnO ceramics have high density and certain mechanical properties, the sintering temperature needs to be above 1000 ℃, so that the temperature characteristics of polymers and ceramics are greatly different, and how to cofire ceramics and polymer materials is always a difficult point in industry, and cold sintering can well solve the problem. By adopting cold sintering, the ceramic grain boundary is regulated and controlled by a polymer phase, the mechanical toughness of the ceramic is expected to be improved, and other excellent performances of co-firing the ceramic and the organic polymer, such as super-hydrophobic property, can be found.
The super-hydrophobic material is a material with repellency to water, and water drops cannot slide and spread on the surface of the material to keep a ball rolling shape, so that the rolling self-cleaning effect is achieved. Wettability is one of the important properties of a solid material surface, and key factors that determine the wettability of a material surface include the chemical composition of the material surface and the microscopic geometry of the surface. Therefore, the scholars refer to a surface with a static water contact angle of more than 150 ° and a rolling angle of less than 10 ° as a superhydrophobic surface. The super-hydrophobic material is usually a chemical substance with a micro-nano composite coarse structure and low surface energy, which is also a precondition for becoming the super-hydrophobic material.
The super-hydrophobic surface has excellent characteristics of self-cleaning, oil-water separation, corrosion resistance, ice resistance, fog resistance and the like, and is a hot spot for domestic research in recent years. At present, the method for preparing the super-hydrophobic material has the following advantages and disadvantages: (1) The template method has the advantages of easy operation and simple process, but the durability of the surface is often poor; (2) The powder spraying method is convenient and quick, is easy to operate, but has poor wear resistance, unstable interface and easy corrosion; (3) The chemical deposition method has high speed, but chemical reagents are easy to cause environmental pollution, and the wear resistance of the deposition surface is often poor; (4) The electrochemical deposition method has the advantages of simple process, low cost, high efficiency and easy control, but the electrolytic polishing is easy to cause the problem of environmental pollution, and the prepared coating has poor strength and wear resistance; (5) By laser etching, parameters such as spacing and the like can be accurately controlled, the surface stability is good, but the manufacturing cost is high, and the cooling time is too long. (6) The chemical etching method has low cost, is controllable and corrosion-resistant, but the problems of environmental pollution and poor strength are difficult to solve. Although the technology for preparing the super-hydrophobic material is complete, a plurality of defects and problems still exist and need to be solved. The invention provides a ceramic-polymer composite super-hydrophobic material prepared by cold sintering, which has the characteristics of simple preparation process, economy, rapidness and the like.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to solve the technical problems that: the ZnO-PTFE composite material with the superhydrophobic property is good in wear resistance, simple in process, low in cost, high in efficiency and low in carbon, and the ZnO-PTFE composite material with the superhydrophobic property is rapidly prepared.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering comprises the following steps:
s1: ball milling and mixing ZnO powder and PTFE powder to obtain ZnO-PTFE composite powder, wherein the addition amount of the PTFE powder is 0-80vol%; specifically, absolute ethyl alcohol is used as a medium during ball milling and mixing, ball milling is carried out for 12 hours, and then drying is carried out at 70 ℃; wherein the mass ratio of the anhydrous ethanol to the added ZnO powder and PTFE powder is 1.5, and the ZnO powder and PTFE powder adopt analytical purity of 99.5 percent.
S2: adding a cold sintering aid into the ZnO-PTFE composite powder in the step S1, and fully and uniformly grinding the cold sintering aid in an agate mortar to obtain powder to be sintered;
s3: pouring powder to be sintered into a steel mold, applying pressure of 50MPa-500MPa, and naturally cooling by adopting common cold sintering or plasma sintering to obtain ZnO-PTFE composite ceramic;
the sintering temperature of the common cold sintering is 120-300 ℃, the heating rate is 5-20 ℃/min, and the heat preservation time is 1-10 h;
the sintering temperature of the plasma sintering is 100-300 ℃, the heating rate is 10-100 ℃/min, and the heat preservation time is 5-30 min.
Preferably, the particle size of the ZnO powder in the S1 is 10 nanometers to 20 micrometers, and the particle size of the PTFE powder is 0.1 to 100 micrometers.
Preferably, the cold sintering aid in S2 is one or more of acetic acid solution, zinc acetate dihydrate powder or zinc acetate solution;
when the cold sintering aid is one of acetic acid solution, zinc acetate dihydrate powder or zinc acetate solution:
the concentration of the acetic acid solution is 0.5-5mol/L, and the mass ratio of the acetic acid solution to the ZnO-PTFE composite powder is 1-25 wt%; the mass ratio of the zinc acetate dihydrate powder to the ZnO-PTFE composite powder is 0.5-20wt%; the concentration of the zinc acetate solution is 0.2-3mol/L, and the mass ratio of the zinc acetate solution to the ZnO-PTFE composite powder is 1-20wt%.
When the cold sintering aid is acetic acid solution or zinc acetate dihydrate powder or zinc acetate solution, the cold sintering aid is a plurality of the following materials:
the addition amount of the cold sintering additive is 2-20wt%, and the dosage ratio of the acetic acid solution, the zinc acetate dihydrate powder and the zinc acetate solution is 1:0.5:1, wherein the concentration of the acetic acid solution is 0.5-5mol/L, and the concentration of the zinc acetate solution is 0.2-3mol/L.
Preferably, the mass ratio of the zinc acetate powder to the ZnO-PTFE composite powder in the S2 is 3-6wt%.
Preferably, the concentration of the zinc acetate solution in S2 is 0.5-2mol%.
Preferably, the volume ratio of the PTFE powder to the ZnO powder in the S1 is 0-70%.
Preferably, the hydrophobic angle of the ZnO-PTFE composite ceramic obtained by the S3 can reach more than 160 degrees.
Compared with the prior art, the invention has at least the following advantages:
the invention adopts a cold sintering mode, and has the following great influence on the method:
1) Compared with the traditional method for preparing the superhydrophobic ceramic or glass surface by high-temperature sintering, the energy consumption for preparing the ceramic-polymer superhydrophobic material by cold sintering is greatly reduced, which is about 1/100 of that of the traditional sintering method, and the superhydrophobic material has the advantage of low carbon.
2) The method is characterized in that the cold-sintered ZnO-PTFE composite ceramic is adopted, and the composite ceramic with super-hydrophobic performance is prepared by utilizing the low surface energy property of PTFE and the surface roughness property of pure ZnO ceramic, so that the preparation process is simple and the economic cost is low.
3) By adopting cold sintering, the prepared ZnO-PTFE composite ceramic has super-hydrophobic performance (the hydrophobic angle can reach 160 degrees) as a whole, and the abrasion resistance of the sample material is good.
Drawings
FIG. 1 shows the results of hydrophobic angle test of the cold-sintered ZnO-PTFE composite ceramic.
FIGS. 2 (a) and (b) show the microstructure of the ZnO-PTFE ceramic cross section and surface, respectively.
FIG. 3 shows the surface roughness test results of ZnO-PTFE.
FIG. 4 shows the abrasion resistance test results of ZnO-PTFE composite ceramic samples.
Fig. 5 is a graph showing the energy consumption comparison result of the cold sintering and the conventional sintering process.
Detailed Description
The present invention will be described in further detail below.
The patent adopts cold sintering to co-sinter ZnO-PTFE, and discovers that ZnO-PTFE ceramic has hydrophobic property.
The adopted cold sintering realizes the low-temperature sintering of the ZnO-PTFE composite ceramic, and the sintering technology can realize the densification of the ZnO-PTFE ceramic in a few minutes to a few tens of minutes at extremely low temperature (less than or equal to 300 ℃), and the sintering energy consumption is less than 1/100 of that of the traditional solid-phase sintering. The main mechanism of the sintering technology is that a proper amount of liquid phase is added in the process of preparing ZnO-PTFE composite powder to carry out local wetting dissolution, so that the ZnO-PTFE powder is in a supersaturated state, and then the cold sintering is combined, the temperature is raised and the pressure sintering is carried out, so that chemical driving force is provided for the ceramic forming of a sample, and the compact ZnO-PTFE composite ceramic can be sintered in a short time at extremely low temperature. Along with the increase of the volume fraction of PTFE, the hydrophobic angle of the surface of the sample is in a rule of ascending and then descending, the hydrophobic angle is 161 degrees at most, and the definition of super-hydrophobic is achieved, namely the hydrophobic angle is more than 150 degrees. According to analysis of a sample section morphology graph, along with the increase of the volume fraction of PTFE, the size of ZnO crystal grains is gradually reduced, meanwhile, a spider-like net structure is formed in the composite ceramic, along with the increase of the content of PTFE, the phenomenon of ZnO-PTFE particle agglomeration gradually occurs. Meanwhile, according to a sample surface topography diagram, through analysis of results, PTFE and ZnO particles are distributed more and more uniformly between 0-56 vol% of PTFE content, and after 56-100 vol% of PTFE content is too high, the ZnO particles of the sample are almost covered by PTFE. As the volume fraction of PTFE increases, the roughness Rq value of the ZnO-PTFE composite surface increases and then decreases.
As shown in figure 1, the contact angle test result of the ZnO-PTFE composite powder shows that the maximum static contact angle can reach 161 degrees, because the surface energy of PTFE is low, and a certain amount of PTFE is added, the prepared ZnO-PTFE composite ceramic has a grain boundary structure with micro-nano roughness, and the surface energy of the ZnO-PTFE composite material is effectively reduced, so that the ZnO-PTFE composite material has hydrophobic property.
Example 1: the method for preparing ZnO ceramic based on cold sintering comprises the following steps: adopting prepared ZnO-PTFE (0%) composite powder and adopting ZnO powder with the particle size of 10 nanometers, wherein the particle size of the ZnO powder is 99.5% of that of the ZnO powder; adding cold sintering aid acetic acid (1 mol/L, 20wt%) solution, fully and uniformly grinding the powder material, and pouring into a steel mould; and (3) applying 50MPa pressure, maintaining the pressure for 5min, heating to 120 ℃ at a speed of 5 ℃/min, and preserving the temperature for 1h to obtain ZnO ceramic, namely a sample 1.
Example 2: the method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering comprises the following steps: the prepared ZnO-PTFE (24%) composite powder adopts analytically pure ZnO powder with the particle size of 100 nanometers and PTFE powder with the particle size of 0.1 micrometer, wherein the particle size of 99.5 percent; adding cold sintering aid acetic acid (0.5 mol/L, 10 wt%) solution, fully and uniformly grinding the powder material, and pouring into a steel mould; and (3) applying 300MPa pressure, maintaining the pressure for 5min, heating to 200 ℃ at a speed of 10 ℃/min, and preserving the temperature for 3h to obtain the ZnO-PTFE composite ceramic, namely a sample 2.
Examples 3-42 were prepared by cold sintering in the same steps as examples 1 and 2, except that the cold sintering aid, znO particle size, PTFE powder particle size, raw material ratio, sintering temperature, rate of rise, holding time and sintering pressure were selected, wherein examples 3-18 were prepared by conventional cold sintering and examples 19-42 were prepared by plasma cold sintering, as shown in table 1.
TABLE 1
Performance testing was performed on some of the ZnO ceramic samples of the resulting examples:
1. hydrophobic Angle test
FIG. 1 shows the result of measuring the volume fraction of PTFE at a hydrophobic angle of 56% and the size of water droplets at 6. Mu.L. As can be seen from the graph, the hydrophobic angle of the sample can reach 161 degrees, and the definition of superhydrophobicity, namely the hydrophobic angle is larger than 150 degrees, is achieved.
The samples prepared by the preparation technology of the super-hydrophobic materials reported at present have the characteristic of poor wear resistance, and the patent adopts a method of cold sintering co-fired ceramic-polymer, so that the whole material has the super-hydrophobic characteristic, as shown in figure 4, the ZnO-PTFE composite ceramic is polished on 400-mesh sand paper, and after the ZnO-PTFE composite ceramic is polished to different thicknesses, the hydrophobic angle can still reach more than 150 degrees. The ZnO-PTFE composite ceramic prepared by cold sintering has good wear resistance.
As can be seen from fig. 5, the energy consumption of cold sintering of pure ZnO ceramic is only about 1% of the energy consumption of conventional solid phase sintering, and thus the energy saving and environmental protection purposes can be achieved to a great extent by adopting cold sintering.
Analysis of microstructure of ZnO-PTFE composite ceramic the cross-sectional morphology of the sample is observed by an environmental Scanning Electron Microscope (SEM) as shown in figures 2 (a) and 2 (b), and the inside of the composite ceramic is found to form a spider-web-like structure, thus providing microscopic conditions for sample superhydrophobicity. The surface roughness of the sample is shown in fig. 2 (b), and the analysis results show that at the PTFE content of 56vol%, PTFE and ZnO particles are uniformly distributed, and meanwhile, the surface topography of the optimal sample is shown in fig. 3 together with an Atomic Force Microscope (AFM), and the roughness is rq= 70.47nm.
In summary, key factors that determine the wettability of a material surface include the chemical composition of the material surface and the microscopic geometry of the surface.
The study shows that cold sintering can co-sinter ceramic-polymer, and new properties can be studied by combining the respective characteristics. Key factors determining the wettability of a material surface include the chemical composition of the material surface and the microscopic geometry of the surface. Although the more PTFE content, the lower the surface energy of the ZnO-PTFE composite, the hydrophobicity is limited by simply lowering the surface energy, thus the surface morphology is seen to play a critical role in the sample surface static water contact angle being able to meet the superhydrophobic contact angle requirement (> 150 °).
Claims (6)
1. The method for preparing the ZnO-PTFE super-hydrophobic composite ceramic by cold sintering is characterized by comprising the following steps of:
s1: ball milling and mixing ZnO powder and PTFE powder to obtain ZnO-PTFE composite powder, wherein the volume doping amount of the PTFE powder is 48-80vol% of the composite powder, and the PTFE powder is polytetrafluoroethylene powder;
s2: adding a cold sintering aid into the ZnO-PTFE composite powder in the step S1, and fully and uniformly grinding to obtain powder to be sintered;
s3: pouring powder to be sintered into a die, applying pressure of 50-500 MPa, and naturally cooling by adopting common cold sintering or plasma sintering to obtain ZnO-PTFE composite ceramic;
the sintering temperature of the common cold sintering is 120-300 ℃, the heating rate is 5-20 ℃/min, and the heat preservation time is 1-10 h;
the sintering temperature of the plasma sintering is 100-300 ℃, the heating rate is 10-100 ℃/min, and the heat preservation time is 5-30 min.
2. The method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering according to claim 1, which is characterized in that: the particle size of the ZnO powder in the S1 is 10 nanometers-20 micrometers, and the particle size of the PTFE powder is 0.1-100 micrometers.
3. The method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering according to claim 1, which is characterized in that: the cold sintering aid in the step S2 is one or more of acetic acid solution, zinc acetate dihydrate powder or zinc acetate solution;
when the cold sintering aid is one of acetic acid solution, zinc acetate dihydrate powder or zinc acetate solution:
the concentration of the acetic acid solution is 0.5-5mol/L, and the mass ratio of the acetic acid solution to the ZnO-PTFE composite powder is 1-25 wt%; the mass ratio of the zinc acetate dihydrate powder to the ZnO-PTFE composite powder is 0.5-20wt%; the concentration of the zinc acetate solution is 0.2-3mol/L, and the mass ratio of the zinc acetate solution to the ZnO-PTFE composite powder is 1-20wt%;
when the cold sintering aid is acetic acid solution or zinc acetate dihydrate powder or zinc acetate solution, the cold sintering aid is a plurality of the following materials:
the addition amount of the cold sintering additive is 2-20wt%, and the dosage ratio of the acetic acid solution, the zinc acetate dihydrate powder and the zinc acetate solution is 1:0.5:1, wherein the concentration of the acetic acid solution is 0.5-5mol/L, and the concentration of the zinc acetate solution is 0.2-3mol/L.
4. The method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering according to claim 3, wherein the method comprises the following steps: the mass ratio of the zinc acetate powder to the ZnO-PTFE composite powder in the S2 is 3-6wt%.
5. The method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering according to claim 3, wherein the method comprises the following steps: the concentration of the zinc acetate solution in the S2 is 0.5-2mol percent.
6. The method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering according to claim 1, which is characterized in that: the hydrophobic angle of the ZnO-PTFE composite ceramic obtained by the step S3 can reach more than 160 degrees.
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