CN108164268B - Preparation method of graphene composite silicon-carbon-nitrogen precursor ceramic - Google Patents

Preparation method of graphene composite silicon-carbon-nitrogen precursor ceramic Download PDF

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CN108164268B
CN108164268B CN201711483578.7A CN201711483578A CN108164268B CN 108164268 B CN108164268 B CN 108164268B CN 201711483578 A CN201711483578 A CN 201711483578A CN 108164268 B CN108164268 B CN 108164268B
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龚红宇
冯玉润
张玉军
郭学
刘玉
林骁
毛俊杰
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Shandong University
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Abstract

The invention relates to preparation of graphene composite silicon carbon nitrogen precursor ceramicThe method comprises the following steps: (1) in N2Stirring Polysilazane (PSZ) and graphene uniformly under the atmosphere to obtain a mixed solution; (2) heating the mixed solution obtained in the step (1) from room temperature to 300-800 ℃ at a heating rate of 3-5 ℃/min, and curing for 1-8 h; (3) crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving the material with a 100-200-mesh sieve; (4) pressing and forming the powder obtained in the step (3) under the pressure of 5-15 MPa, carrying out cold isostatic pressing at 150-250 MPa, and maintaining the pressure for 200-400 s to obtain a green body; (5) putting the green body obtained in the step (4) in N2And carrying out heat treatment at the temperature of 1000-1300 ℃ under the protection of atmosphere, and keeping the temperature for 2-6 h to obtain the product. According to the invention, the graphene material is introduced in the preparation process of the precursor, the real part and the imaginary part of the relative complex dielectric constant of the ceramic material obtained by heat treatment are increased, the loss factor is increased, and the reflection loss of the material is improved.

Description

Preparation method of graphene composite silicon-carbon-nitrogen precursor ceramic
(I) technical field
The invention relates to a preparation method of graphene composite silicon carbon nitrogen precursor ceramic, and belongs to the field of microwave absorption.
(II) background of the invention
The traditional electromagnetic wave absorbing material has high density, low absorbing capacity and poor impedance matching characteristic. The novel wave-absorbing material is developing towards the direction of composite wave-absorbing materials, namely, the electromagnetic parameters of the material are adjusted by compounding and simultaneously utilizing the advantages of two types of wave-absorbing media, so that the impedance matching property is improved, and the absorption frequency band is widened.
The preparation of ceramics (PDCs) by a precursor conversion method is a great technical breakthrough in the history of ceramic preparation, and replaces the traditional method for preparing ceramics by high-temperature sintering, thereby preparing a novel preparation method of ceramics at a lower temperature. The existence of unique nanostructures in precursor ceramics gives the ceramics many specificitiesExamples of the dielectric layer include a semiconductor layer, a piezoelectric layer, and a dielectric layer. The precursor ceramic has high relative complex dielectric constant real and imaginary parts and dielectric loss tangent, so that the potential capability of electromagnetic wave absorption in a high frequency band attracts a great deal of attention. In recent years, the electromagnetic wave absorption characteristics of precursor ceramics have been developed. The silicon carbon nitrogen precursor ceramic (PDCs-SiCN) is a light ceramic with a unique amorphous structure, has uniform structure, high thermal stability and good creep resistance, and has the theoretical density of only 2g cm-3On the left and right sides, free carbon is gradually precipitated from the amorphous structure by the PDCs-SiCN ceramic in the heat treatment process, so that the PDCs-SiCN ceramic has special dielectric property and is considered to have certain potential in the wave-absorbing property. Graphene is a novel two-dimensional carbon material, and due to unique electrical properties, graphene can gradually replace other traditional materials in a plurality of scientific research fields. And the graphene also gradually arouses wide research interest as a wave-absorbing material.
Many documents and patents have been reported on silicon carbon nitrogen precursor ceramics. Xue Guo et al (Ceramics International 43(2017)16866-16871) describe the cross-linking curing behavior of polysilazane polymer precursors, indicating that: the chemical bond change of the thermal polymerization reaction in the process of crosslinking and curing the polymer precursor, the polymer precursor forms a SiCN framework network structure mainly comprising Si-C, Si-N, C-C after the crosslinking temperature exceeds 600 ℃ through double bond addition, hydrosilylation reaction, dehydrogenation coupling reaction, transamination reaction and the like, and the conversion from organic matters to inorganic matters is completed.
Quan Li et al (Journal of the European Ceramic Society 34(2014) 589-598) describe that the carbon-rich PDCs-SiCN Ceramic prepared at high temperature has high thermal stability, small dielectric constant, high loss and better wave-absorbing performance, but the Ceramic has large skin depth, lower electromagnetic shielding efficiency, higher reflection loss and poorer electromagnetic wave absorption capability.
The PDCs-SiCN Ceramic prepared by Xue Guo et al (Journal of the European Ceramic Society, Accepted 16 October 2017) at the low temperature of 1100 ℃ also has the problem of high reflection loss, and simultaneously, the dielectric loss of the prepared Ceramic is poor due to the low free carbon content at the low temperature, and the electromagnetic wave absorption capacity needs to be improved.
Xin Sun et al (J.Mater.chem.C.2013, 1,765-777) report a simple method for synthesizing layered magnetic graphene, and the prepared graphene has high dielectric loss, low density and good electromagnetic wave absorption capacity in an X wave band. The literature indicates that pure graphene is nonmagnetic, and the microwave loss mechanism of the pure graphene is mainly caused by dielectric loss, but the electromagnetic parameters of the pure graphene are unbalanced, so that the impedance matching characteristic is poor.
Chinese patent document CN105000889A discloses an iron-containing silicon-carbon-nitrogen precursor ceramic, which comprises the following raw material components in percentage by mass: 96-98 percent of polysilazane, 2-4 percent of dicumyl peroxide, 10-20 percent of alpha-methacrylic acid based on the total mass of polysilazane and dicumyl peroxide, 20-100 percent of nano ferric oxide based on the mass of polysilazane, and N2Crosslinking at 500-700 ℃ in the atmosphere, grinding, pressing and molding, and then carrying out heat treatment at 1000-1400 ℃ to prepare the iron-silicon-containing carbon nitrogen precursor ceramic.
The PDCs-SiCN ceramic has potential electromagnetic wave absorption characteristics, but has the problems of high preparation temperature, low reflection loss or narrow absorption band.
Graphene has strong dielectric loss, and graphene and PDCs-SiCN ceramic are compounded, so that the reflection loss of the graphene is improved, the wave-absorbing frequency band is widened, and the wave-absorbing effect of light weight, high strength and wide frequency band can be achieved.
So far, no relevant report of graphene composite silicon carbon nitrogen precursor ceramic is found.
Disclosure of the invention
Aiming at the defects of the prior art, the invention solves the technical problems of high reflection loss and narrow absorption band of PDCs-SiCN ceramic through process improvement, and provides a graphene composite silicon carbon nitrogen precursor ceramic and a preparation method thereof.
The technical scheme of the invention is as follows:
summary of the invention:
according to the preparation method, polysilazane is used as a matrix, and a proper amount of graphene is added to prepare a precursor; and preparing the graphene composite silicon-carbon-nitrogen precursor ceramic by isostatic pressing and pre-pressing molding and then performing a heat treatment process.
Detailed description of the invention:
a method for preparing graphene composite silicon carbon nitrogen precursor ceramic by a precursor method comprises the following steps:
(1) mixing materials: in N2Stirring Polysilazane (PSZ) and graphene uniformly under the atmosphere to obtain a mixed solution;
the polysilazane: the mass ratio of graphene is 60-95%: 40 to 5 percent of ingredients;
(2) and (3) crosslinking and curing: heating the mixed solution obtained in the step (1) from room temperature to 300-800 ℃ at a heating rate of 3-5 ℃/min, and curing for 1-8 h;
(3) crushing and ball-milling: crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving the material with a 100-200-mesh sieve;
(4) and (3) granulation and forming: pressing and forming the powder obtained in the step (3) under the pressure of 5-15 MPa, carrying out cold isostatic pressing at 150-250 MPa, and maintaining the pressure for 200-400 s to obtain a green body;
(5) and (3) heat treatment: putting the green body obtained in the step (4) in N2And carrying out heat treatment at the temperature of 1000-1300 ℃ under the protection of atmosphere, and keeping the temperature for 2-6 h to obtain the product.
According to the present invention, it is preferable that the polysilazane used in the step (1) is HTT 1800. Polysilazanes are commercially available or can be prepared according to the prior art.
According to the invention, preferably, in the step (1), 5-40% of graphene is doped into a mixture, and further preferably 5%, 15%, 25% and 35% of graphene is doped into the mixture.
According to the present invention, it is preferable that the temperature rise rate in the step (1) is 3 ℃/min, the curing temperature is 600 ℃, and the curing time is 3 hours. A lower temperature rise rate and a proper curing time to promote sufficient progress of the crosslinking curing behavior.
According to the invention, preferably, the cold isostatic pressing in step (4) is carried out at 180MPa and the pressure is maintained for 300 s.
According to the present invention, it is preferable that the heat treatment is carried out by raising the temperature from room temperature to 1000 ℃ to 1300 ℃ at a rate of 3 ℃/min in step (5); further preferably, the heat treatment temperature is 1100 ℃.
The principle of the invention is as follows:
graphene with different components is doped by taking polysilazane as a precursor source, and the graphene is mixed with the polysilazane to prepare the SiCN ceramic material with the help of a double-row gas distributor (vacuum/inert multi-manifold system, commonly known as Schlenk line).
Advantageous effects
1. According to the invention, the graphene material is introduced in the preparation process of the precursor, the real part and the imaginary part of the relative complex dielectric constant of the ceramic material obtained by final heat treatment are increased, the loss factor is increased, and the reflection loss of the material is improved;
2. the method adopts isostatic pressing prepressing molding and then carries out precursor conversion process to prepare the graphene composite silicon carbon nitrogen precursor ceramic, and solves the problem that the ceramic is easy to crack in the heat treatment process.
(IV) description of the drawings
Fig. 1 is an SEM photograph of a graphene composite silicon carbon nitrogen precursor ceramic sample prepared in example 1 of the present invention.
Fig. 2 is an SEM photograph of a ceramic sample prepared in comparative example 2 of the present invention.
Fig. 3 is an SEM photograph of a ceramic sample prepared in comparative example 3 of the present invention.
(V) detailed description of the preferred embodiments
The technical solution of the present invention is further described with reference to the following examples, but the scope of the present invention is not limited thereto.
The raw materials used in the examples are conventional raw materials, and the equipment used is conventional equipment, commercially available products.
Example 1:
a method for preparing graphene composite silicon carbon nitrogen precursor ceramic by a precursor method comprises the following steps:
(1) mixing materials: in N2Stirring Polysilazane (PSZ) and graphene uniformly under the atmosphere to obtain a mixed solution;
the polysilazane: the mass ratio of graphene is 95%: 5 percent of ingredients;
(2) and (3) crosslinking and curing: heating the mixed solution obtained in the step (1) from room temperature to 600 ℃ at the heating rate of 3 ℃/min, and curing for 2 h;
(3) crushing and ball-milling: crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving with a 200-mesh sieve;
(4) and (3) granulation and forming: pressing and molding the powder obtained in the step (3) under the pressure of 15MPa, carrying out cold isostatic pressing at 200MPa, and maintaining the pressure for 300s to obtain a green body;
(5) and (3) heat treatment: putting the green body obtained in the step (4) in N2And (3) carrying out heat treatment at the temperature of 1100 ℃ under the protection of atmosphere, and preserving heat for 2h to obtain the graphene composite silicon carbon nitrogen precursor ceramic.
An SEM photograph of the graphene composite silicon carbon nitrogen precursor ceramic sample prepared in this embodiment is shown in fig. 1, and as can be seen from fig. 1, the graphene is successfully doped into the silicon carbon nitrogen precursor ceramic and is uniformly distributed.
Example 2:
a method for preparing graphene composite silicon carbon nitrogen precursor ceramic by a precursor method comprises the following steps:
(1) mixing materials: in N2Stirring Polysilazane (PSZ) and graphene uniformly under the atmosphere to obtain a mixed solution;
the polysilazane: the mass ratio of graphene is 85%: 15% of ingredients;
(2) and (3) crosslinking and curing: heating the mixed solution obtained in the step (1) from room temperature to 400 ℃ at the heating rate of 5 ℃/min, and curing for 4 h;
(3) crushing and ball-milling: crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving with a 200-mesh sieve;
(4) and (3) granulation and forming: pressing and molding the powder obtained in the step (3) under the pressure of 15MPa, carrying out cold isostatic pressing at 150MPa, and keeping the pressure for 200s to obtain a green body;
(5) and (3) heat treatment: putting the green body obtained in the step (4) in N2And carrying out heat treatment at 1200 ℃ under the protection of atmosphere, and preserving heat for 4h to obtain the graphene composite silicon carbon nitrogen precursor ceramic.
Example 3:
a method for preparing graphene composite silicon carbon nitrogen precursor ceramic by a precursor method comprises the following steps:
(1) mixing materials: in N2Stirring Polysilazane (PSZ) and graphene uniformly under the atmosphere to obtain a mixed solution;
the polysilazane: the mass ratio of graphene is 75%: 25% of ingredients;
(2) and (3) crosslinking and curing: heating the mixed solution obtained in the step (1) from room temperature to 600 ℃ at the heating rate of 5 ℃/min, and curing for 2 h;
(3) crushing and ball-milling: crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving with a 200-mesh sieve;
(4) and (3) granulation and forming: pressing and molding the powder obtained in the step (3) under the pressure of 15MPa, carrying out cold isostatic pressing at 200MPa, and maintaining the pressure for 300s to obtain a green body;
(5) and (3) heat treatment: putting the green body obtained in the step (4) in N2And (4) carrying out heat treatment at 1300 ℃ under the protection of atmosphere, and preserving heat for 4h to obtain the graphene composite silicon carbon nitrogen precursor ceramic.
Example 4:
a method for preparing graphene composite silicon carbon nitrogen precursor ceramic by a precursor method comprises the following steps:
(1) mixing materials: in N2Stirring Polysilazane (PSZ) and graphene uniformly under the atmosphere to obtain a mixed solution;
the polysilazane: the mass ratio of the graphene is 65%: 35% of ingredients;
(2) and (3) crosslinking and curing: heating the mixed solution obtained in the step (1) from room temperature to 600 ℃ at the heating rate of 3 ℃/min, and curing for 2 h;
(3) crushing and ball-milling: crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving with a 200-mesh sieve;
(4) and (3) granulation and forming: pressing and molding the powder obtained in the step (3) under the pressure of 10MPa, carrying out cold isostatic pressing at 180MPa, and maintaining the pressure for 300s to obtain a green body;
(5) and (3) heat treatment: putting the green body obtained in the step (4) in N2And (3) carrying out heat treatment at the temperature of 1100 ℃ under the protection of atmosphere, and preserving heat for 6 hours to obtain the graphene composite silicon carbon nitrogen precursor ceramic.
Comparative example 1:
as described in example 1, except that no graphene was incorporated during the compounding in step (1).
Comparative example 2:
except that 5 wt% of carbon nanotubes were incorporated during the compounding in step (1), as described in example 1.
Comparative example 3:
as described in example 1, except that 5 wt% fullerene was incorporated during the compounding in step (1).
Experimental example:
the graphene composite silicon carbon nitrogen precursor ceramic prepared in the examples 1 to 4 and the ceramic prepared in the comparative examples 1 to 3 were tested for real part of relative complex dielectric constant, imaginary part of relative complex dielectric constant, dielectric loss factor and reflection loss, and the results are shown in table 1.
TABLE 1
Figure BDA0001534294400000071
As can be seen from Table 1, the composite ceramic obtained by doping graphene has excellent wave-absorbing performance. The introduction of graphene obviously increases the relative complex dielectric constant real part, and the dielectric loss is correspondingly increased; the minimum reflection loss is correspondingly improved.
The dielectric property of the ceramic material obtained by doping the carbon nano tube and the fullerene is obviously improved compared with that of silicon-carbon-nitrogen ceramic, but the dielectric property is far inferior to that of the ceramic material obtained by doping the graphene, and the lowest reflection loss is higher.
It should be noted that the above-mentioned embodiments are merely examples of the present invention, and it is obvious that the present invention is not limited to the above-mentioned embodiments, and other modifications are possible. All modifications directly or indirectly derivable by a person skilled in the art from the present disclosure are to be considered within the scope of the present invention.

Claims (6)

1. A method for preparing graphene composite silicon carbon nitrogen precursor ceramic by a precursor method comprises the following steps:
(1) mixing materials: in N2Stirring polysilazane and graphene uniformly under the atmosphere to obtain a mixed solution;
the polysilazane: the mass ratio of the graphene is 60-85%: 40 to 15 percent of ingredients;
(2) and (3) crosslinking and curing: heating the mixed solution obtained in the step (1) from room temperature to 300-600 ℃ at a heating rate of 3-5 ℃/min, and curing for 1-3 h;
(3) crushing and ball-milling: crushing and ball-milling the material obtained by curing in the step (2) in a vibration ball mill, and sieving the material with a 100-200-mesh sieve;
(4) and (3) granulation and forming: pressing and forming the powder obtained in the step (3) under the pressure of 5-15 MPa, carrying out cold isostatic pressing at 150-250 MPa, and maintaining the pressure for 200-400 s to obtain a green body;
(5) and (3) heat treatment: putting the green body obtained in the step (4) in N2And carrying out heat treatment at the temperature of 1000-1300 ℃ under the protection of atmosphere, and keeping the temperature for 2-6 h to obtain the product.
2. The method for preparing the graphene composite silicon carbon nitrogen precursor ceramic according to the precursor method of claim 1, wherein the polysilazane in the step (1) is HTT 1800.
3. The method for preparing the graphene composite silicon carbon nitrogen precursor ceramic according to the precursor method of claim 1, wherein the graphene is mixed into the ingredients according to the proportion of 15%, 25% and 35% in the step (1).
4. The method for preparing the graphene composite silicon carbon nitrogen precursor ceramic according to the precursor method of claim 1, wherein the cold isostatic pressing in the step (4) is performed at 180MPa, and the pressure is maintained for 300 s.
5. The method for preparing the graphene composite silicon carbon nitrogen precursor ceramic according to the precursor method of claim 1, wherein in the step (5), the temperature is raised from room temperature to 1000 ℃ to 1300 ℃ at a heating rate of 3 ℃/min for heat treatment.
6. The method for preparing the graphene composite silicon carbon nitrogen precursor ceramic according to the precursor method of claim 1, wherein the heat treatment temperature in the step (5) is 1100 ℃.
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