CN108164268A - A kind of preparation method of the compound silicon-carbon nitrogen precursor ceramic of graphene - Google Patents
A kind of preparation method of the compound silicon-carbon nitrogen precursor ceramic of graphene Download PDFInfo
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Abstract
It is as follows including step the present invention relates to a kind of preparation method of the compound silicon-carbon nitrogen precursor ceramic of graphene：(1) in N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；(2) heating rate of the mixed solution obtained by step (1) in 3~5 DEG C/min is cured into 1~8h from room temperature to 300~800 DEG C；(3) material of step (2) curing gained in vibrator is crushed into ball milling, crosses 100~200 mesh sieve；(4) by powder compression moulding under the pressure of 5MPa~15MPa obtained by step (3), isostatic cool pressing, 150~250MPa, 200~400s of pressurize obtain green compact；(5) by green compact obtained by step (4) in N2Temperature under atmosphere protection at 1000 DEG C~1300 DEG C is heat-treated, heat preservation 2h~6h to get.The present invention introduces grapheme material in forerunner's production procedure, and the ceramic material being thermally treated resulting in increases with respect to complex dielectric permittivity real and imaginary parts, fissipation factor increase, and improves the reflection loss of material.
Description
(1) technical field
The present invention relates to a kind of preparation methods of the compound silicon-carbon nitrogen precursor ceramic of graphene, belong to field of microwave absorption.
(2) background technology
Traditional electromagnetic wave absorbent material density is higher, and absorbability is relatively low, and impedance matching property is poor.Novel wave-absorbing material
The advantages of just developing towards composite wave-suction material direction, i.e., inhaling wave medium by compound while two classes of utilization adjusts the electricity of material
Magnetic parameter, and then improve impedance matching, widen absorption band, other composite light absorbing material such as precursor ceramics can be with
Density of material is effectively reduced, improves the absorbing property of material, meets the needs of novel wave-absorbing material " thin, wide, light, strong ".
Presoma conversion method preparation ceramic (PDCs) is ceramic system for the major technological breakthrough in history, its substitution conventional high-temperature
The method that sintering prepares ceramics prepares the novel processing step of ceramics at a lower temperature.Unique nanometer in precursor ceramic
The presence of structure causes ceramics to have many properties, such as semiconductive, piezoelectricity, dielectricity etc..Precursor ceramic has
Have and higher answer dielectric Changshu real and imaginary parts and dielectric loss angle tangent relatively so that its electro-magnetic wave absorption in high band
Potential ability cause a large amount of concerns.In recent years, the electromaganic wave absorbing property of precursor ceramic is gradually developed.Before silicon-carbon nitrogen
It is the light ceramics for having unique non crystalline structure to drive body ceramic (PDCs-SiCN), and structure is uniform, thermal stability is high, has
Good creep-resistant property, theoretical density only have 2gcm-3Left and right, PDCs-SiCN ceramics are gradually from non-in heat treatment process
Free carbon is precipitated in crystal structure, makes it have special dielectric properties, is considered that there are certain potentiality in terms of absorbing property.
And graphene is New Two Dimensional carbon material, unique electrical property makes it gradually substitute other traditional materials in numerous scientific research fields
Material.And also gradually cause extensive research interest as absorbing material about graphene.
About silicon-carbon nitrogen precursor ceramic, there are many documents and patent report.(the Ceramics such as Xue Guo
International 43 (2017) 16866-16871) the crosslinking curing behavior of polysilazane polymeric presoma is described, refer to
Go out：The variation of hot polymerization reactive chemistry key during polymer precursor crosslinking curing, polymer precursor by double bond addition,
Hydrosilylation reactions, dehydrogenation coupled reaction, transamination reaction etc. after crosslinking temperature is more than 600 DEG C, are formd with Si-C, Si-
N, the SiCN back bone network structures based on C-C, complete the transformation from organic matter to inorganic matter.
Quan Li et al. (Journal of the European Ceramic Society 34 (2014) 589-598) is explained
The rich carbon type PDCs-SiCN ceramics prepared in high temperature are stated, the ceramic thermal stability of preparation is high, and dielectric constant is small, and loss is high, tool
There is preferable absorbing property, but the skin depth of ceramics is big, electromagnet shield effect is relatively low, and reflection loss is higher, electromagnetism
Wave absorbability is poor.
(16 October of Journal of the European Ceramic Society, Accepted such as Xue Guo
2017) in the PDCs-SiCN ceramics of 1100 DEG C of low temperature preparation, there is also reflection loss it is higher the problem of, while under low temperature by
Relatively low in free carbon content, the dielectric loss for leading to preparation ceramics is poor, and electro-magnetic wave absorption ability has to be hoisted.
Xin Sun etc. (J.Mater.Chem.C, 2013,1,765-777) report a kind of synthesis stratiform magnetic graphene
Straightforward procedure, prepared graphene has higher dielectric loss, and low-density has good electro-magnetic wave absorption in X-band
Ability.It is pointed out in document, pure graphene is non-magnetic, and lossy microwave mechanism is mainly caused by dielectric loss, however pure stone
The electromagnetic parameter of black alkene is uneven, causes impedance matching property poor.
Chinese patent document CN105000889A discloses a kind of iron content silicon-carbon nitrogen precursor ceramic, the quality of raw material components
Percentage is：Polysilazane accounts for 96%~98%, and cumyl peroxide accounts for 2%~4%, and α-methacrylic acid accounts for polysilazane
With the 10%~20% of cumyl peroxide gross mass, nano-sized iron oxide be add as outside polysilazane quality 20%~
100%, in N2500~700 DEG C of crosslinkings under atmosphere, after grinding compression moulding, are heat-treated at a temperature of 1000 DEG C~1400 DEG C, make
Standby to obtain iron content silicon-carbon nitrogen precursor ceramics, the ceramics of preparation are by composite magnetic, and loss ability is higher, and wave-sucking performance obtains
To improvement.
PDCs-SiCN ceramics have potential electromaganic wave absorbing property, but there is preparation temperature height, and reflection loss is low
Or absorption band it is narrow the problem of.
Graphene has very strong dielectric loss in itself, and graphite is dilute compound with the progress of PDCs-SiCN ceramics, and it is anti-to improve it
Loss is penetrated, widens and inhales wave frequency section, can reach lightweight, high-strength, wideband wave-absorbing effect.
Up to the present, it there are no the relevant report of the compound silicon-carbon nitrogen precursor ceramic of graphene.
(3) invention content
The present invention in view of the deficiencies of the prior art, by process modification, solves PDCs-SiCN ceramic reflectings loss height, inhales
The technical issues of frequency band is narrow is received, compound silicon-carbon nitrogen precursor ceramic of a kind of graphene and preparation method thereof is provided.
Technical solution of the present invention is as follows：
Summary of the invention：
The present invention adds appropriate graphene as matrix using polysilazane and prepares presoma；Using isostatic pressed pre-molding, so
Heat treatment process is carried out afterwards prepares the compound silicon-carbon nitrogen precursor ceramic of graphene.
Detailed description of the invention：
A kind of method that precursor process prepares the compound silicon-carbon nitrogen precursor ceramic of graphene is as follows including step：
(1) batch mixing：In N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；
The polysilazane：Graphene in mass ratio 60~95%：40%~5% dispensing；
(2) crosslinking curing：By mixed solution obtained by step (1) 3~5 DEG C/min heating rate from room temperature to
300~800 DEG C of 1~8h of curing；
(3) ball milling is crushed：The material of step (2) curing gained in vibrator is crushed into ball milling, crosses 100~200
Mesh sieves；
(4) granulating and forming：By powder compression moulding under the pressure of 5MPa~15MPa obtained by step (3), isostatic cool pressing,
150~250MPa, 200~400s of pressurize obtain green compact；
(5) it is heat-treated：By green compact obtained by step (4) in N2Temperature under atmosphere protection at 1000 DEG C~1300 DEG C carries out heat
Processing, heat preservation 2h~6h to get.
, according to the invention it is preferred to, the polysilazane described in step (1) is HTT1800.Polysilazane can market purchase
, it can also be obtained by prior art preparation.
, according to the invention it is preferred to, graphene described in step (1) by 5~40% incorporation dispensings, further preferred 5%,
15%, 25%, 35% incorporation dispensing.
, according to the invention it is preferred to, in step (1) heating rate be 3 DEG C/min, 600 DEG C of solidification temperature, hardening time
3h.Relatively low heating rate and appropriate hardening time are to promote the abundant progress of crosslinking curing behavior.
, according to the invention it is preferred to, isostatic cool pressing carries out under 180MPa in step (4), pressurize 300s.
, according to the invention it is preferred to, in step (5) 1000 DEG C~1300 are warming up to from room temperature with 3 DEG C/min heating rates
It DEG C is heat-treated；It is further preferred that heat treatment temperature is 1100 DEG C.
The principle of the present invention：
The graphene of different component is mixed using polysilazane as presoma source, in double gas distributor (vacuum/inertia
Branch manifold system is commonly called as Schlenk line) assistance under be mixed prepare SiCN ceramic materials.
Advantageous effect
1st, the present invention introduces grapheme material in forerunner's production procedure, and the ceramic material that final heat treatment obtains is relatively multiple
Real part of permittivity and imaginary part increase, fissipation factor increase, and improve the reflection loss of material；
2nd, the present invention prepares the compound silicon-carbon nitrogen of graphene using isostatic pressed pre-molding and then progress presoma conversion process
Precursor ceramic solves the problems, such as easily to crack in ceramic heat treatment process.
(4) it illustrates
Fig. 1 is the SEM photograph of the compound silicon-carbon nitrogen precursor ceramic sample of graphene prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM photograph of the ceramics sample prepared by comparative example 2 of the present invention.
Fig. 3 is the SEM photograph of the ceramics sample prepared by comparative example 3 of the present invention.
(5) specific embodiment
Technical scheme of the present invention is described further with reference to embodiment, but institute's protection domain of the present invention is not limited to
This.
Raw materials used in embodiment is convenient source, and device therefor is conventional equipment, commercial products.
Embodiment 1：
A kind of method that precursor process prepares the compound silicon-carbon nitrogen precursor ceramic of graphene is as follows including step：
(1) batch mixing：In N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；
The polysilazane：Graphene in mass ratio 95%：5% dispensing；
(2) crosslinking curing：By mixed solution obtained by step (1) 3 DEG C/min heating rate from room temperature to 600 DEG C
Cure 2h；
(3) ball milling is crushed：The material of step (2) curing gained in vibrator is crushed into ball milling, crosses 200 mesh sieve；
(4) granulating and forming：By powder compression moulding under the pressure of 15MPa obtained by step (3), isostatic cool pressing, 200MPa,
Pressurize 300s obtains green compact；
(5) it is heat-treated：By green compact obtained by step (4) in N2Temperature under atmosphere protection at 1100 DEG C is heat-treated, and is protected
Warm 2h is to get the compound silicon-carbon nitrogen precursor ceramic of graphene.
The SEM photograph of the compound silicon-carbon nitrogen precursor ceramic sample of graphene prepared by the present embodiment is as shown in Figure 1, by scheming
1 it is found that graphene is successfully doped in silicon-carbon nitrogen precursor ceramic, and is evenly distributed.
Embodiment 2：
A kind of method that precursor process prepares the compound silicon-carbon nitrogen precursor ceramic of graphene is as follows including step：
(1) batch mixing：In N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；
The polysilazane：Graphene in mass ratio 85%：15% dispensing；
(2) crosslinking curing：By mixed solution obtained by step (1) 5 DEG C/min heating rate from room temperature to 400 DEG C
Cure 4h；
(3) ball milling is crushed：The material of step (2) curing gained in vibrator is crushed into ball milling, crosses 200 mesh sieve；
(4) granulating and forming：By powder compression moulding under the pressure of 15MPa obtained by step (3), isostatic cool pressing, 150MPa,
Pressurize 200s obtains green compact；
(5) it is heat-treated：By green compact obtained by step (4) in N2Temperature under atmosphere protection at 1200 DEG C is heat-treated, and is protected
Warm 4h is to get the compound silicon-carbon nitrogen precursor ceramic of graphene.
Embodiment 3：
A kind of method that precursor process prepares the compound silicon-carbon nitrogen precursor ceramic of graphene is as follows including step：
(1) batch mixing：In N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；
The polysilazane：Graphene in mass ratio 75%：25% dispensing；
(2) crosslinking curing：By mixed solution obtained by step (1) 5 DEG C/min heating rate from room temperature to 600 DEG C
Cure 2h；
(3) ball milling is crushed：The material of step (2) curing gained in vibrator is crushed into ball milling, crosses 200 mesh sieve；
(4) granulating and forming：By powder compression moulding under the pressure of 15MPa obtained by step (3), isostatic cool pressing, 200MPa,
Pressurize 300s obtains green compact；
(5) it is heat-treated：By green compact obtained by step (4) in N2Temperature under atmosphere protection at 1300 DEG C is heat-treated, and is protected
Warm 4h is to get the compound silicon-carbon nitrogen precursor ceramic of graphene.
Embodiment 4：
A kind of method that precursor process prepares the compound silicon-carbon nitrogen precursor ceramic of graphene is as follows including step：
(1) batch mixing：In N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；
The polysilazane：Graphene in mass ratio 65%：35% dispensing；
(2) crosslinking curing：By mixed solution obtained by step (1) 3 DEG C/min heating rate from room temperature to 600 DEG C
Cure 2h；
(3) ball milling is crushed：The material of step (2) curing gained in vibrator is crushed into ball milling, crosses 200 mesh sieve；
(4) granulating and forming：By powder compression moulding under the pressure of 10MPa obtained by step (3), isostatic cool pressing, 180Mpa,
Pressurize 300s obtains green compact；
(5) it is heat-treated：By green compact obtained by step (4) in N2Temperature under atmosphere protection at 1100 DEG C is heat-treated, and is protected
Warm 6h is to get the compound silicon-carbon nitrogen precursor ceramic of graphene.
Comparative example 1：
As described in Example 1, it is not both not graphene-doped in step (1) mixing process.
Comparative example 2：
As described in Example 1, incorporation 5wt% carbon nanotubes in step (1) mixing process it are not both.
Comparative example 3：
As described in Example 1, incorporation 5wt% fullerenes in step (1) mixing process it are not both.
Experimental example：
Will be ceramic made from the compound silicon-carbon nitrogen precursor ceramic of graphene made from Examples 1 to 4 and comparative example 1-3, it surveys
The opposite complex dielectric permittivity real part of examination, opposite complex dielectric permittivity imaginary part, dielectric loss factor, reflection loss, the results are shown in Table 1.
Table 1
As shown in Table 1, the absorbing property of composite ceramics obtained after the present invention is graphene-doped is excellent.Introducing graphene makes
Answering the normal real part of dielectric relatively significantly increases, and dielectric loss also accordingly increases；Its minimum reflection loss also accordingly improves.
Incorporation carbon nanotube is compared silicon carbonitride ceramic with ceramic dielectric performance obtained by fullerene and is significantly improved, but remote poor
In graphene-doped obtained ceramic microwave absorbent properties, minimum reflection loss higher.
It should be noted that listed above is only several specific embodiments of the invention, it is clear that the present invention is not only
It is limited to above example, there can also be other deformations.Those skilled in the art directly exported from the disclosure of invention or
All deformations of amplification are connect, are considered as protection scope of the present invention.
Claims (8)
1. a kind of method that precursor process prepares the compound silicon-carbon nitrogen precursor ceramic of graphene, as follows including step：
(1) batch mixing：In N2Under atmosphere, polysilazane (PSZ), graphene are stirred evenly, obtain mixed solution；
The polysilazane：Graphene in mass ratio 60~95%：40%~5% dispensing；
(2) crosslinking curing：By mixed solution obtained by step (1) 3~5 DEG C/min heating rate from room temperature to 300~
800 DEG C of 1~8h of curing；
(3) ball milling is crushed：The material of step (2) curing gained in vibrator is crushed into ball milling, crosses 100~200 mesh sieve；
(4) granulating and forming：By powder compression moulding under the pressure of 5MPa~15MPa obtained by step (3), isostatic cool pressing, 150~
250MPa, 200~400s of pressurize obtain green compact；
(5) it is heat-treated：By green compact obtained by step (4) in N2Temperature under atmosphere protection at 1000 DEG C~1300 DEG C is heat-treated,
Keep the temperature 2h~6h to get.
2. precursor process according to claim 1 prepares the method for the compound silicon-carbon nitrogen precursor ceramic of graphene, feature
It is, the polysilazane described in step (1) is HTT1800.
3. precursor process according to claim 1 prepares the method for the compound silicon-carbon nitrogen precursor ceramic of graphene, feature
It is, graphene described in step (1) is by 5~40% incorporation dispensings.
4. precursor process according to claim 3 prepares the method for the compound silicon-carbon nitrogen precursor ceramic of graphene, feature
It is, graphene described in step (1) presses 5%, 15%, 25%, 35% incorporation dispensing.
5. precursor process according to claim 1 prepares the method for the compound silicon-carbon nitrogen precursor ceramic of graphene, feature
Be, in step (1) heating rate be 3 DEG C/min, 600 DEG C of solidification temperature, hardening time 3h.
6. precursor process according to claim 1 prepares the method for the compound silicon-carbon nitrogen precursor ceramic of graphene, feature
It is, isostatic cool pressing carries out under 180MPa in step (4), pressurize 300s.
7. precursor process according to claim 1 prepares the method for the compound silicon-carbon nitrogen precursor ceramic of graphene, feature
It is, being warming up to 1000 DEG C~1300 DEG C from room temperature with 3 DEG C/min heating rates in step (5) is heat-treated.
8. preparing the method for the compound silicon-carbon nitrogen precursor ceramic of graphene according to precursor process described in claim 1, feature exists
In heat treatment temperature is 1100 DEG C in step (5).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851363A (en) * | 2021-01-22 | 2021-05-28 | 哈尔滨工业大学 | Graphene oxide reinforced silicon-boron-carbon-nitrogen ceramic composite material and preparation method thereof |
| CN113929464A (en) * | 2021-11-02 | 2022-01-14 | 航天特种材料及工艺技术研究所 | CNT/graphene covalent modified high-thermal-conductivity carbide ceramic and preparation method thereof |
| CN115385715A (en) * | 2022-09-15 | 2022-11-25 | 南京信息工程大学 | Porous carbon-rich silicon carbon nitrogen ceramic wave-absorbing heat-conducting material and preparation method thereof |
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2017
- 2017-12-29 CN CN201711483578.7A patent/CN108164268B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851363A (en) * | 2021-01-22 | 2021-05-28 | 哈尔滨工业大学 | Graphene oxide reinforced silicon-boron-carbon-nitrogen ceramic composite material and preparation method thereof |
| CN112851363B (en) * | 2021-01-22 | 2022-03-22 | 哈尔滨工业大学 | Graphene oxide reinforced silicon-boron-carbon-nitrogen ceramic composite material and preparation method thereof |
| CN113929464A (en) * | 2021-11-02 | 2022-01-14 | 航天特种材料及工艺技术研究所 | CNT/graphene covalent modified high-thermal-conductivity carbide ceramic and preparation method thereof |
| CN113929464B (en) * | 2021-11-02 | 2022-10-25 | 航天特种材料及工艺技术研究所 | CNT/graphene covalent modified high-thermal-conductivity carbide ceramic and preparation method thereof |
| CN115385715A (en) * | 2022-09-15 | 2022-11-25 | 南京信息工程大学 | Porous carbon-rich silicon carbon nitrogen ceramic wave-absorbing heat-conducting material and preparation method thereof |
| CN115385715B (en) * | 2022-09-15 | 2023-09-19 | 南京信息工程大学 | Porous carbon-rich silicon-carbon-nitrogen ceramic heat absorption waveguide material and preparation method thereof |
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