CN108147823A - A kind of preparation method of nickeliferous silicon-carbon nitrogen precursor ceramic - Google Patents
A kind of preparation method of nickeliferous silicon-carbon nitrogen precursor ceramic Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of nickeliferous silicon-carbon nitrogen precursor ceramic, including：By raw material polysilazane, nickel source mixing step；Pyrolysis step.The present invention prepares SiCN (Ni) precursor ceramic by presoma conversion method, and even structure, intensity is high, introduces nickel in SiCN precursor ceramics, increases the loss mechanisms of material, is conducive to the raising of microwave absorbing property.The present invention is using presoma conversion method, and simple for process, easy to operate, production cost is low, short preparation period, and resulting materials oxidation resistance is strong, and chemical stability, high-temperature behavior are good.
Description
Technical field
The present invention relates to a kind of preparation methods of nickeliferous silicon-carbon nitrogen microwave-absorbing ceramic, belong to field of inorganic nonmetallic material.
Background technology
In recent years, it with the fast development of the communication technology, local area network etc., brings and is also made while providing amenities for the people
Into a degree of electromagnetic pollution, influence people’s lives and work or even can also endanger the health of the mankind；And in army
In terms of thing, the development of the advanced Detection Techniques such as radar makes stealth technology become the important subject of national defense and military fields.Cause
This, electromagnetic-wave absorbent is widely paid attention to due to its important function.Electromagnetic-wave absorbent is to electromagnetic wave by itself
Absorption, attenuation, incident electromagnetic energy is converted into thermal energy and is dissipated.A kind of absorbing material haveing excellent performance, needs
Meet impedance matching and the requirement of energy loss, in addition to this, material is also light, thin.And traditional absorbing material such as iron
Oxysome, metal alloy etc. make its application by larger limitation due to density is larger, structure design is difficult etc..
Precursor ceramic (Polymer-Derived Ceramics (PDCs)) is that organic polymer presoma is directly warm
Ceramic material obtained from solution has many advantages, such as light, easily molded.And using polysilazane as raw material, pass through presoma conversion method
Silicon-carbon nitrogen (SiCN) precursor ceramic of preparation is a kind of dielectric loss type absorbing material, has excellent mechanical performance, heatproof
Performance, inoxidizability etc..And the spillage of material ability of single lossy is weaker, and is difficult to adjust dielectric constant and magnetic conductivity simultaneously
The two parameters reach impedance matching, it is therefore desirable to which preparing, there is dielectric loss and the composite wave-suction material of magnetic loss to come simultaneously
Improve absorbing property.In order to introduce magnetic loss, magnetic element M (Fe, Co, Ni, Mn etc.) can be added in SiCN precursor ceramics
SiCN (M) precursor ceramic is made.And nickel is good soft magnetic material, has higher saturation magnetization and magnetic conductivity,
In terms of being applied to microwave absorption, magnetic loss that can be directly as wave absorbing agent or for increasing dielectric type absorbing material.
Chinese patent literature CN 105000889A disclose the side that a kind of presoma conversion method prepares iron content silicon carbonitride ceramic
Method is as follows including step：(1) polysilazane, α-methacrylic acid, cumyl peroxide are uniformly mixed, obtain mixed solution；
(2) mixed solution is cured；(3) the crushing material ball milling of curing gained；(4) powder after ball milling is mixed with nano-sized iron oxide
Uniformly；(5) by gained powder pre-molding, green compact are obtained；(6) by temperature of the green compact obtained by step (5) at 1000 DEG C~1400 DEG C
Be pyrolyzed/be sintered, keep the temperature.Chinese patent literature CN 105602194A disclose a kind of nanometer particle-modified graphenes of Ni and
The preparation method of its absorbing material.Graphene oxide is obtained using sonic oscillation, then using the further reduction-oxidation of reducing agent
Graphene and Ni2+ so as to which Ni nano-particles be made to be attached to graphene surface, then with epoxy blend, obtain having both electric suction
Receive the absorbing material with magnetic absorbing ability.
Above method, which prepares obtained absorbing material, has certain absorbing property, but the process is more complicated, and inhales
Wave poor performance.
Invention content
In view of the deficiencies of the prior art, especially current preparation process is complicated and the defects of Absorbing Materials are not good enough,
The present invention provides a kind of method that presoma conversion method prepares nickeliferous silicon-carbon nitrogen (SiCN (Ni)) precursor ceramic.This method technique
Simply, production cost is low, short preparation period, and obtained product electromagnetic consumable is high, and absorbing property is good.
Technical scheme is as follows：
A kind of preparation method for adulterating nickeliferous silicon-carbon nitrogen precursor ceramic, including：
By raw material polysilazane, nickel source mixing step；
Pyrolysis step.
, according to the invention it is preferred to, it is carried out under an inert atmosphere in raw material mixing step；
Preferably, the polysilazane：Nickel element mass ratio is 65wt%-95wt%：5wt%-35wt%；It is further excellent
Select 70wt-93wt%：7wt-30wt%；
Preferably, the polysilazane is HTT1800；
Preferably, the nickel source is nano-nickel powder or nano-nickel oxide, most preferably nano-nickel powder.
, according to the invention it is preferred to, in pyrolysis step, carry out under an inert atmosphere；
Preferably, pyrolysis temperature be 900 DEG C -1400 DEG C, more preferable 1000-1200 DEG C, pyrolysis time 2-4h；
It is further preferred that heating rate is 3-4 DEG C/min, it is warming up to pyrolysis temperature and is pyrolyzed.
According to the present invention, the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic, a kind of preferred embodiment is as follows：
(1) batch mixing：Under an inert atmosphere, polysilazane and nickel source are stirred into 5-30min, obtains a homogeneous mixture；
The polysilazane：The mass ratio of nickel element is 65wt%-95wt%：5wt%-35wt%；
(2) pyrolysis/sintering：By mixture obtained by step (1) under inert gas shielding, in 900 DEG C -1400 DEG C of temperature
2-4h is sintered to get nickeliferous silicon-carbon nitrogen precursor ceramic.
In the present invention polysilazane can market buy, can also be obtained by prior art preparation.
The principle of the present invention：
SiCN precursor ceramics are a kind of dielectric loss type absorbing materials, difficult due to there was only single dielectric loss performance
To adjust dielectric constant and magnetic conductivity the two parameters arrival impedance matching simultaneously, and only dielectric loss leads to loss ability
It is weaker.Nickel has higher saturation magnetization and magnetic conductivity, can be introduced into SiCN precursor ceramics as a kind of soft magnetic materials
Optimize its absorbing property.Therefore nickeliferous SiCN precursor ceramics are prepared by introducing nickel source, makes loss mechanisms diversification, increase damage
Consumption, and electromagnetic parameter is adjusted, enhance impedance matching, finally obtain the material with excellent absorbing property.But the addition of nickel
Not the higher the better for amount, is not also more lower better.The present invention obtains optimal nickel doping range by lot of experiments, makes
Obtaining SiCN precursor ceramics has optimal absorbing property.
Beneficial effects of the present invention are as follows：
1st, the present invention prepares SiCN (Ni) precursor ceramic by presoma conversion method, and even structure, intensity is high, in SiCN
Nickel is introduced in precursor ceramic, increases the loss mechanisms of material, is conducive to the raising of microwave absorbing property.
2nd, the present invention is using presoma conversion method, and simple for process, easy to operate, production cost is low, short preparation period, gained
Material against oxidative ability is strong, and chemical stability, high-temperature behavior are good.
3rd, it is produced by the present invention that there is excellent absorbing property containing SiCN (Ni) precursor ceramic.Wherein using nano-nickel powder as
SiCN (Ni) precursor ceramic of nickel source has preferable absorbing property, minimum value -40.9dB is reached at 17.1GHz, effectively
Frequency bandwidth is 1.6GHz, and when nickel incorporation is 30wt%, effective frequency belt width is up to 2.7GHz, and absorbing property is most
It is good.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of SiCN (Ni) precursor ceramic obtained by the embodiment of the present invention 1.
Fig. 2 is the SEM photograph of SiCN (Ni) precursor ceramic obtained by the embodiment of the present invention 1.
Fig. 3 is the TEM figures of SiCN (Ni) precursor ceramic obtained by the embodiment of the present invention 1.
Fig. 4 is the magnetic property analysis of SiCN (Ni) precursor ceramic obtained by the embodiment of the present invention 1.
Fig. 5 is the frequency-reflection loss change curve of SiCN (Ni) precursor ceramic obtained by the embodiment of the present invention 1
Figure.
Fig. 6 is embodiment 1-2, frequency-reflection loss variation of SiCN (Ni) precursor ceramic obtained by comparative example 1 is bent
Line compares figure.
Fig. 7 is embodiment 3-4, frequency-reflection loss variation of SiCN (Ni) precursor ceramic obtained by comparative example 2 is bent
Line compares figure.
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.
Polysilazane used be HTT1800, commercial products, from Guangzhou Hong Hai Chemical Industry Science Co., Ltd.
Embodiment 1
A kind of method that presoma conversion method prepares SiCN (Ni) precursor ceramic is as follows including step：
(1) batch mixing：In a nitrogen atmosphere, 4.61g polysilazanes and 0.39g nano-nickel powders are weighed, 20min is mixed,
Obtain a homogeneous mixture；
The polysilazane：Nickel element mass ratio is 92.2wt%：7.8wt%；
(2) pyrolysis/sintering：Mixture obtained by step (1) is put into tube furnace, under nitrogen atmosphere protection, 1000
DEG C temperature in be pyrolyzed 2h, 3 DEG C/min of heating rate is to get SiCN (Ni) precursor ceramic.
SiCN (Ni) precursor ceramic test X ray diffracting spectrum, SEM photograph, the TEM that the present embodiment is prepared
Figure, hysteresis loop figure and frequency-reflection loss change curve collection of illustrative plates, as shown in Fig. 1,2,3,4,5.
As shown in Figure 1, nickel simple substance is mainly contained in obtained product, in addition the also presence of carbon.
As shown in Figure 2, the grey matrix of SiCN (Ni) precursor ceramic illustrates without regular crystal grain for amorphous state.Finally
Product structure is uniform.
From the figure 3, it may be seen that black spheric granules is nickel in figure, grain size is about 25-50nm, is distributed on grey matrix.According to
Diffraction pattern further proves that SiCN matrixes are amorphous state.
As shown in Figure 4, SiCN (Ni) precursor ceramic shows hysteresis, and the area of hysteresis loop and remanent magnetism are all
Very little is presented typical soft magnetic materials feature, is easy to magnetize and demagnetize, can be by constantly magnetizing and moving back in alternating magnetic field
Magnetic dissipates electromagnetic energy for thermal energy.
As shown in Figure 5, reflection loss changes with frequency, minimum value -40.9dB is reached at 17.1GHz, less than -10dB
Effective frequency belt width be 1.6GHz.
Embodiment 2
A kind of method that presoma conversion method prepares SiCN (Ni) precursor ceramic is as follows including step：
(1) batch mixing：In a nitrogen atmosphere, 4.51g polysilazanes and 0.49g nano-nickel oxides are weighed, is mixed
20min obtains a homogeneous mixture；
The polysilazane：Nickel element mass ratio is 92.2wt%：7.8wt%；
(2) pyrolysis/sintering：Mixture obtained by step (1) is put into tube furnace, under nitrogen atmosphere protection, 1000
DEG C temperature in be pyrolyzed 2h, 3 DEG C/min of heating rate is to get SiCN (Ni) precursor ceramic.
Comparative example 1
A kind of method that presoma conversion method prepares SiCN (Ni) precursor ceramic is as follows including step：
(1) batch mixing：In a nitrogen atmosphere, 3.5g polysilazanes and 1.5g nickel (II) compound [Ni (CH are weighed3CO2)2
(C2H7NO)2], 20min is mixed, obtains a homogeneous mixture；
The polysilazane：Nickel element mass ratio is 92.2wt%：7.8wt%；
(2) pyrolysis/sintering：Mixture obtained by step (1) is put into tube furnace, under nitrogen atmosphere protection, 1000
DEG C temperature in be pyrolyzed 2h, 3 DEG C/min of heating rate is to get SiCN (Ni) precursor ceramic.
Embodiment 3
A kind of method that presoma conversion method prepares SiCN (Ni) precursor ceramic is as follows including step：
(1) batch mixing：In a nitrogen atmosphere, 4.5g polysilazanes and 0.5g nano-nickel powders are weighed, 20min is mixed, obtains
One homogeneous mixture；
The polysilazane：Nickel element mass ratio is 90wt%：10wt%；
(2) pyrolysis/sintering：Mixture obtained by step (1) is put into tube furnace, under nitrogen atmosphere protection, 1000
DEG C temperature in be pyrolyzed 2h, 3 DEG C/min of heating rate is to get SiCN (Ni) precursor ceramic.
Embodiment 4
A kind of method that presoma conversion method prepares SiCN (Ni) precursor ceramic is as follows including step：
(1) batch mixing：In a nitrogen atmosphere, 3.5g polysilazanes and 1.5g nano-nickel powders are weighed, 20min is mixed, obtains
One homogeneous mixture；
The polysilazane：Nickel element mass ratio is 70wt%：30wt%；
(2) pyrolysis/sintering：Mixture obtained by step (1) is put into tube furnace, under nitrogen atmosphere protection, 1000
DEG C temperature in be pyrolyzed 2h, 3 DEG C/min of heating rate is to get SiCN (Ni) precursor ceramic.
Comparative example 2
A kind of method that presoma conversion method prepares SiCN (Ni) precursor ceramic is as follows including step：
(1) batch mixing：In a nitrogen atmosphere, 3g polysilazanes and 2g nano-nickel powders are weighed, 20min is mixed, obtains one
Even mixture；
The polysilazane：Nickel element powder mass ratio is 60wt%：40wt%；
(2) pyrolysis/sintering：Mixture obtained by step (1) is put into tube furnace, under nitrogen atmosphere protection, 1000
DEG C temperature in be pyrolyzed 2h, 3 DEG C/min of heating rate is to get SiCN (Ni) precursor ceramic.
Test example 1
SiCN (Ni) precursor ceramics that embodiment 1-2 and comparative example 1 are prepared are changed into line frequency-reflection loss
Curve Comparative map is tested, as shown in Figure 6.
SiCN (Ni) precursor ceramics that embodiment 3-4 and comparative example 2 are prepared are changed into line frequency-reflection loss
Curve Comparative map is tested, as shown in Figure 7.
It will be appreciated from fig. 6 that in the case of identical nickel element mass fraction, nickel source is nickel (II) compound [Ni
(CH3CO2)2(C2H7NO)2] when, minimum value -7.7dB is reached at 9.7GHz；Illustrate that the present invention has weight for the selection of nickel source
It acts on, nickel source is improper, will seriously affect the absorbing property of ceramics.
When nickel source is nickel oxide, reflection loss reaches minimum value -24.2dB, effective frequency belt width 0.8GHz in 13GHz,
When nickel source is nano-nickel powder, minimum value -40.9dB, effective frequency belt width 1.6GHz are reached at 17.1GHz.
As shown in Figure 7, when nickel source is nano-nickel powder, when mass fraction is 10wt%, reach minimum in 17.2GHz
Value -15.2dB, effective frequency belt width 1.6GHz；When mass fraction be 30wt% when, reach at 16GHz minimum value-
18.4dB, effective frequency belt width 2.7GHz；
When mass fraction is 40wt%, reflection loss reaches minimum value -6.9dB in 14.9GHz.It is found that nickel content mixes
Excessively, the absorbing property of ceramics equally can be seriously reduced, the doping of nickel equally has important shadow for the absorbing property of ceramics
It rings.Addition nickel amount is excessively high, then nickel is more easy to reunite in matrix, increases eddy-current loss, is unfavorable for impedance matching, drops reflection loss
It is low.
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-described embodiment, there can also be other deformations.Those skilled in the art directly exported from the disclosure of invention or
All deformations amplified indirectly, are considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method for adulterating nickeliferous silicon-carbon nitrogen precursor ceramic, including：
By raw material polysilazane, nickel source mixing step；
Pyrolysis step.
2. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 1, which is characterized in that raw material mixes
It closes and is carried out under an inert atmosphere in step.
3. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 1, which is characterized in that described poly-
Silazane：Nickel element mass ratio is 65wt%-95wt%：5wt%-35wt%.
4. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 3, which is characterized in that described poly-
Silazane：Nickel element mass ratio is 70wt-93wt%：7wt-30wt%.
5. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 1, which is characterized in that described
Polysilazane is HTT1800.
6. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 1, which is characterized in that described
Nickel source is nano-nickel powder or nano-nickel oxide.
7. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 1, which is characterized in that pyrolysis step
In rapid, carry out under an inert atmosphere.
8. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 1, which is characterized in that pyrolysis temperature
It is 900 DEG C -1400 DEG C to spend, pyrolysis time 2-4h.
9. the preparation method of the nickeliferous silicon-carbon nitrogen precursor ceramic of doping according to claim 8, which is characterized in that heating speed
Rate is 3-4 DEG C/min, is warming up to pyrolysis temperature and is pyrolyzed.
10. a kind of preparation method of nickeliferous silicon-carbon nitrogen precursor ceramic, as follows including step：
(1) batch mixing：Under an inert atmosphere, polysilazane and nickel source are stirred into 5-30min, obtains a homogeneous mixture；
The polysilazane：The mass ratio of nickel element is 65wt%-95wt%：5wt%-35wt%；
(2) pyrolysis/sintering：By mixture obtained by step (1) under inert gas shielding, it is sintered in 900 DEG C -1400 DEG C of temperature
2-4h is to get nickeliferous silicon-carbon nitrogen precursor ceramic.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646813A (en) * | 2020-06-11 | 2020-09-11 | 西北工业大学 | Low-temperature preparation method for converting wave-absorbing polymer into silicon-carbon-nitrogen ceramic |
| CN113149656A (en) * | 2021-04-22 | 2021-07-23 | 西北工业大学 | Rich in Si3N4SiHfBCN ceramic of nanowire and preparation method |
| CN116409999A (en) * | 2023-03-22 | 2023-07-11 | 南京信息工程大学 | S-band silicon-carbon-nitrogen ceramic wave-absorbing material and preparation method thereof |
| CN116409999B (en) * | 2023-03-22 | 2024-05-28 | 南京信息工程大学 | S-band silicon-carbon-nitrogen ceramic wave-absorbing material and preparation method thereof |
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| CN111646813A (en) * | 2020-06-11 | 2020-09-11 | 西北工业大学 | Low-temperature preparation method for converting wave-absorbing polymer into silicon-carbon-nitrogen ceramic |
| CN111646813B (en) * | 2020-06-11 | 2022-03-15 | 西北工业大学 | Low-temperature preparation method for converting wave-absorbing polymer into silicon-carbon-nitrogen ceramic |
| CN113149656A (en) * | 2021-04-22 | 2021-07-23 | 西北工业大学 | Rich in Si3N4SiHfBCN ceramic of nanowire and preparation method |
| CN116409999A (en) * | 2023-03-22 | 2023-07-11 | 南京信息工程大学 | S-band silicon-carbon-nitrogen ceramic wave-absorbing material and preparation method thereof |
| CN116409999B (en) * | 2023-03-22 | 2024-05-28 | 南京信息工程大学 | S-band silicon-carbon-nitrogen ceramic wave-absorbing material and preparation method thereof |
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