CN113215445B - Graphene oxide reinforced zinc-based composite material and preparation method thereof - Google Patents
Graphene oxide reinforced zinc-based composite material and preparation method thereof Download PDFInfo
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- CN113215445B CN113215445B CN202110506482.8A CN202110506482A CN113215445B CN 113215445 B CN113215445 B CN 113215445B CN 202110506482 A CN202110506482 A CN 202110506482A CN 113215445 B CN113215445 B CN 113215445B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
Abstract
The invention discloses a graphene oxide reinforced zinc-based composite material and a preparation method thereof. The graphene oxide reinforced zinc-based composite material comprises 0.3-0.7 wt% of graphene oxide and 99.3-99.7 wt% of zinc powder, and the preparation method comprises the following steps: adding graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a graphene oxide solution; adding zinc powder into deionized water, stirring, and gradually adding a cationic surfactant during stirring to obtain a zinc powder modifying solution; adding the graphene oxide solution into the zinc powder modifying solution, uniformly stirring, filtering and drying to obtain mixed powder; and carrying out vacuum hot-pressing sintering on the mixed powder to obtain the graphene oxide reinforced zinc-based composite material. The invention provides a method for preparing a graphene oxide reinforced zinc-based composite material by means of electrostatic adsorption and vacuum hot-pressing sintering, and the obtained material has excellent mechanical properties.
Description
Technical Field
The invention relates to the technical field of zinc-based composite materials, in particular to a graphene oxide reinforced zinc-based composite material and a preparation method thereof.
Background
The zinc has good biocompatibility, so that the zinc has great application potential in the field of biomedical materials. The standard electrode potential (-0.763V) of Zn is between Mg (-2.372V) and Fe (-0.447V), so Zn and Zn alloys show a suitable degradation rate from the viewpoint of corrosion resistance. Therefore, the zinc-based alloy is expected to become a new generation of biomedical degradable short-term implant material after being combined with magnesium-based alloy and iron-based alloy.
The as-cast zinc has poor room temperature combination properties. The metal can be prepared into a Metal Matrix Composite (MMC) material to improve the comprehensive mechanical property of the metal. The strength and plasticity of the metal matrix composite material can be effectively improved by selecting a proper reinforcement and a preparation method.
However, no report is found in the current research on the combination of graphene and derivatives thereof with zinc-based composite materials.
Disclosure of Invention
The invention aims to provide a graphene oxide reinforced zinc-based composite material and a preparation method thereof. The invention provides a method for preparing a graphene oxide reinforced zinc-based composite material by means of electrostatic adsorption and vacuum hot-pressing sintering, and the obtained material has excellent mechanical properties.
The technical scheme of the invention is as follows: the raw materials of the graphene oxide reinforced zinc-based composite material comprise 0.3-0.7 wt% of graphene oxide and 99.3-99.7 wt% of zinc powder.
In the graphene oxide reinforced zinc-based composite material, the raw material of the material comprises 0.7wt% of graphene oxide.
A preparation method of the graphene oxide reinforced zinc-based composite material comprises the following steps:
(1) Adding graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a graphene oxide solution;
(2) Adding zinc powder into deionized water, stirring, and gradually adding a cationic surfactant during stirring to obtain a zinc powder modifying solution;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring, filtering, and drying to obtain mixed powder;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the graphene oxide reinforced zinc-based composite material.
In the preparation method of the graphene oxide reinforced zinc-based composite material, the cationic surfactant is one or a combination of any one of polyvinylpyrrolidone, cetyl trimethyl ammonium bromide and/or octadecyl dimethyl benzyl ammonium chloride.
In the preparation method of the graphene oxide reinforced zinc-based composite material, the concentration of the cationic surfactant in the zinc powder modifying solution is 0.5 mg/mL-1.0 mg/mL.
In the preparation method of the graphene oxide reinforced zinc-based composite material, the stirring time in the step (3) is 90-120 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the method comprises the steps of adding graphene oxide into absolute ethyl alcohol, carrying out ultrasonic treatment to obtain a uniform graphene oxide solution, enabling the graphene oxide solution to be negative, adding zinc powder into deionized water, stirring, gradually adding a cationic surfactant to obtain a positive zinc powder modifying solution, mixing and stirring the negative graphene oxide solution and the positive zinc powder modifying solution, carrying out electrostatic self-assembly in the process in an electrostatic adsorption mode, effectively solving the problem of dispersion of graphene in a matrix, filtering and drying to obtain mixed powder, and carrying out vacuum hot-pressing sintering to obtain the graphene oxide reinforced zinc-based composite material.
2. In the graphene oxide reinforced zinc-based composite material prepared by the invention, if the content of the graphene oxide is too low (lower than 0.3 wt%) and the reinforcing effect on a zinc matrix is not obvious, and if the content of the graphene oxide is too high (higher than 0.7 wt%), the agglomeration phenomenon of the graphene oxide in the zinc matrix can be increased, so that the performance of the composite material is deteriorated, according to the invention, the content of the graphene oxide is controlled within the range of 0.3wt% -0.7 wt%, the content of the graphene oxide is in positive correlation with the tensile strength of the matrix, the effect is optimal when the 0.7wt% of the graphene oxide is added, the tensile strength of the graphene oxide reaches 254MPa, the tensile strength of the matrix is improved by 126.7% compared with that of pure zinc (112 MPa), and the plasticity of the graphene oxide reinforced zinc-based composite material is approximately equal to that of the pure zinc. The invention has the advantage of excellent mechanical property.
3. The concentration of the cationic surfactant is mainly determined according to the addition amount of the graphene oxide, 0.7wt% of the graphene oxide is added, and the adsorption effect is optimal when the concentration of the corresponding cationic surfactant is 1.0mg/mL. After the positive and negative charges are adsorbed in the concentration range of 0.5 mg/mL-1.0 mg/m of the cationic surfactant in the zinc powder modifying solution, the mixed turbid solution of the graphene oxide and the zinc powder approaches to electric neutrality, and the function of the mixed turbid solution is to tightly connect the sheet layer of the graphene oxide with zinc particles (micro spheres).
4. The electrostatic adsorption time, namely the stirring time for adding the graphene oxide solution into the zinc powder modifying solution, is mainly determined according to the addition amount of the graphene oxide, 0.7wt% of the graphene oxide is added, and the effect is optimal when the graphene oxide is selectively adsorbed for 120min. In the adsorption time range of 90min-120min, the adsorption effect can be ensured, and if the adsorption time is too short, the contact between the graphene oxide and the zinc particles with the cationic surface activated is insufficient, so that effective adsorption cannot be formed. Too long an adsorption time may cause the successfully adsorbed graphene oxide to be separated from the zinc particles, resulting in unsuccessful adsorption.
Drawings
FIG. 1 is a scanning electron microscope image of zinc electrostatic adsorption by graphene oxide;
FIG. 2 is an EDS diagram at the graphene oxide zinc-based composite block;
fig. 3 is a tensile stress-strain graph of examples 1 and 2.
Fig. 1 shows a scanning electron micrograph of graphene oxide and zinc particles after electrostatic adsorption, and it can be seen that a substance having adhesiveness exists between the zinc particles. EDS analysis (fig. 2) was performed on the substance, and it was found that the main component of the binder substance was carbon element, which was determined to be graphene oxide. This demonstrates that the graphene oxide and the cationic surface-treated zinc particles can successfully perform electrostatic adsorption.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1. A graphene oxide reinforced zinc-based composite material and a preparation method thereof are disclosed, wherein 0.3wt% of graphene oxide/zinc-based composite material is prepared by the following steps:
(1) Adding 60mg of graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a uniform graphene oxide solution;
(2) Adding 120g of zinc powder into deionized water, stirring under the action of a constant-temperature magnetic stirrer, and gradually adding 80mg of polyvinylpyrrolidone during stirring to obtain a zinc powder modifying solution; the concentration of the polyvinylpyrrolidone is 0.5mg/mL;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring under the action of a constant-temperature magnetic stirrer, and carrying out electrostatic self-assembly in the process for 90min; filtering and drying to obtain mixed powder of graphene oxide and zinc;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the bulk graphene oxide reinforced zinc-based composite material.
The obtained 0.3wt% graphene oxide/zinc-based composite material is detected, and the detection result is shown in figure 3, wherein the tensile strength of the material is 187MPa, and is improved by 66.9% compared with pure zinc (112 MPa).
Example 2. A graphene oxide reinforced zinc-based composite material and a preparation method thereof are used for preparing 0.7wt% of graphene oxide/zinc-based composite material, and the preparation steps are as follows:
(1) Adding 0.7wt% of graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a uniform graphene oxide solution;
(2) Adding 99.3wt% of zinc powder into deionized water, stirring, and gradually adding polyvinylpyrrolidone during stirring to obtain a zinc powder modification solution; the concentration of polyvinylpyrrolidone in the zinc powder modifying solution is 1.0mg/mL;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring, and carrying out electrostatic self-assembly in the process for 120min; filtering and drying to obtain mixed powder of graphene oxide and zinc;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the bulk graphene oxide reinforced zinc-based composite material.
The obtained 0.7wt% graphene oxide/zinc-based composite material is detected, and the detection result is shown in figure 3, wherein the tensile strength of the material is 254MPa, and is improved by 125.6% compared with pure zinc (112 MPa).
Example 3. A graphene oxide reinforced zinc-based composite material and a preparation method thereof,
the raw material of the material is 0.4wt% of graphene oxide, and the balance is zinc powder; the preparation steps are as follows:
(1) Adding 0.4wt% of graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a uniform graphene oxide solution;
(2) Adding 99.6wt% of zinc powder into deionized water, stirring, and gradually adding hexadecyl trimethyl ammonium bromide during stirring to obtain a zinc powder modifying solution; the concentration of hexadecyl trimethyl ammonium bromide in the zinc powder modifying solution is 0.6mg/mL;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring, and carrying out electrostatic self-assembly in the process for 95min; filtering and drying to obtain mixed powder of graphene oxide and zinc;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the bulk graphene oxide reinforced zinc-based composite material.
Example 4. A graphene oxide reinforced zinc-based composite material and a preparation method thereof,
the raw material of the material is 0.5wt% of graphene oxide, and the balance is zinc powder; the preparation steps are as follows:
(1) Adding 0.5wt% of graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a uniform graphene oxide solution;
(2) Adding 99.5wt% of zinc powder into deionized water, stirring, and gradually adding octadecyl dimethyl benzyl ammonium chloride during stirring to obtain a zinc powder modifying solution; the concentration of octadecyl dimethyl benzyl ammonium chloride in the zinc powder modifying solution is 0.7mg/mL;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring, and carrying out electrostatic self-assembly in the process for 100min; filtering and drying to obtain mixed powder of graphene oxide and zinc;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the bulk graphene oxide reinforced zinc-based composite material.
Example 5. A graphene oxide reinforced zinc-based composite material and a preparation method thereof,
the raw material of the material is 0.6wt% of graphene oxide, and the balance is zinc powder; the preparation steps are as follows:
(1) Adding 0.6wt% of graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a uniform graphene oxide solution;
(2) Adding 99.4wt% of zinc powder into deionized water, stirring, and gradually adding polyvinylpyrrolidone during stirring to obtain a zinc powder modification solution; the concentration of polyvinylpyrrolidone in the zinc powder modifying solution is 0.9mg/mL;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring, and carrying out electrostatic self-assembly in the process for 115min; filtering and drying to obtain mixed powder of graphene oxide and zinc;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the bulk graphene oxide reinforced zinc-based composite material.
In the embodiment, the vacuum hot-pressing sintering is used, powder mixing of the mixed powder is realized by adopting a variable speed ball milling method, and then the bulk graphene oxide reinforced zinc-based composite material is prepared by adopting a vacuum hot-pressing sintering method; the vacuum hot-pressing sintering method has the following vacuum hot-pressing sintering parameter ranges: heating rate of 10-15 deg.c/min and vacuum degree of 1 x 10 -2 ～9×10 -2 Pa, sintering temperature of 360-390 ℃, sintering pressure of 30-40 MPa, sintering time of 30-45 min, and furnace cooling after sintering.
Claims (3)
1. A preparation method of a graphene oxide reinforced zinc-based composite material is characterized by comprising the following steps: the raw materials of the material comprise 0.3-0.7 wt% of graphene oxide and 99.3-99.7 wt% of zinc powder; the preparation method of the graphene oxide reinforced zinc-based composite material comprises the following steps:
(1) Adding graphene oxide into absolute ethyl alcohol, and performing ultrasonic treatment to obtain a graphene oxide solution;
(2) Adding zinc powder into deionized water, stirring, and gradually adding a cationic surfactant during stirring to obtain a zinc powder modifying solution; the concentration of the cationic surfactant in the zinc powder modifying solution is 0.5 mg/mL-1.0 mg/mL;
(3) Adding the graphene oxide solution obtained in the step (1) into the zinc powder modifying solution obtained in the step (2), uniformly stirring, filtering, and drying to obtain mixed powder; the stirring time is 90min-120 min;
(4) And carrying out vacuum hot-pressing sintering on the mixed powder to obtain the graphene oxide reinforced zinc-based composite material.
2. The method for preparing the graphene oxide reinforced zinc-based composite material according to claim 1, characterized in that: the raw material of the material comprises 0.7wt% of graphene oxide.
3. The method of preparing a graphene oxide reinforced zinc-based composite material according to claim 1, wherein: the cationic surfactant is one or a composition of any more of polyvinylpyrrolidone, cetyl trimethyl ammonium bromide or/and octadecyl dimethyl benzyl ammonium chloride.
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