CN109251038A - Polymer cracking containing phenyl ring converts SiBCN metal-free ceramic absorbing material and preparation method - Google Patents

Polymer cracking containing phenyl ring converts SiBCN metal-free ceramic absorbing material and preparation method Download PDF

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CN109251038A
CN109251038A CN201811195572.4A CN201811195572A CN109251038A CN 109251038 A CN109251038 A CN 109251038A CN 201811195572 A CN201811195572 A CN 201811195572A CN 109251038 A CN109251038 A CN 109251038A
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phenyl ring
sibcn
absorbing material
metal
hollow fiber
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孔杰
骆春佳
赫丽华
刘平桂
唐玉生
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Northwestern Polytechnical University
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    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/486—Boron containing organic compounds, e.g. borazine, borane or boranyl
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Abstract

The invention discloses a kind of conversion SiBCN metal-free ceramic absorbing material of polymer cracking containing phenyl ring and preparation methods, the preparation of synthesis and SiBCN ceramics absorbing material including the hyperbranched PVDF hollow fiber membrane containing phenyl ring, the present invention utilizes methyl dichloro diphenyl silane, two sila azane synthesis of super branched PVDF hollow fiber membrane of dichlorosilane, boron chloride and hexamethyl, again by tabletting after the crosslinking of hyperbranched PVDF hollow fiber membrane at idiosome, idiosome is cracked into ceramic absorbing material.The present invention starts with from the design of ceramics polymer precursor construction, it carries out the synthesis of high ceramic yield PVDF hollow fiber membrane presoma and is crosslinked constructing for topological system, phenyl ring is introduced directly into PVDF hollow fiber membrane precursor construction, the direct in-situ in cracking conversion process of the sp2 hydbridized carbon atoms in phenyl ring is set to form the structures such as graphitic carbon, carbon nanotube, the structure that high temperature wave absorbing agent is dispersed in amorphous low-loss carrier is realized, the good metal-free ceramic based composites of absorbing property are obtained.

Description

Polymer cracking containing phenyl ring converts SiBCN metal-free ceramic absorbing material and preparation Method
Technical field
The invention belongs to absorbing material technical fields, and in particular to SiBCN is without gold for one kind conversion of polymer cracking containing phenyl ring Belong to ceramic absorbing material and preparation method.
Background technique
PVDF hollow fiber membrane presoma is pyrolyzed available SiBCN complex phase ceramic, due to the introducing of boron, in ceramic conversion process Middle formation BN/B4C phase, BN/B4C phase itself has good high temperature resistance, can be from by oxygen barrier protective effect and synergistic effect The high temperature resistance for greatly improving ceramic matrix on the whole, according to Nature, SiBCN complex phase ceramic can reach 2000 DEG C or more Heatproof it is horizontal.Compared to single-phase SiC, Si3N4Matrix or complex phase SiCN ceramics, SiBCN complex phase ceramic matrix theoretically has higher High temperature resistant and better high temperature oxidation resistance, PVDF hollow fiber membrane presoma conversion ceramics be increasingly subject to the attention of researcher.
In terms of PDC-SiBCN complex phase ceramic absorbing material, Ye etc. has studied the dielectric properties of PDCs-SiBCN ceramics And microwave absorbing property, the dielectric constant in prepared SiBCN ceramics X-band is 11 hereinafter, loss tangent value is in 0.5- In the range of 0.7, reflectivity reaches minimum -15.78dB in 10GHz.CNTs is added in SiBCN ceramics by Zhang etc. to be changed The electromagnetic consumable ability of ceramics has been apt to it, ceramic loss tangent is more than 0.8, passes through the polymer-modified presoma of ferrocene Afterwards, transition metal element be introduced into can catalytic polymer presoma SiC, carbon nanometer are formed in Pintsch process conversion process The high temperature electromagnetic consumable phases such as line, onion and the isostructural crystalline carbon of graphene can obtain the better ceramic base of wave-absorbing effect and inhale Wave material.This is because agraphitic carbon can be using Fe, Co, Ni transition metal as atomic nucleus in ceramic matrix, the carbon atom of sp3 hydridization It is enriched with around it, is eventually converted into the carbon atom of sp2 hydridization, be finally converted to form the high dielectric such as graphitic carbon, carbon nanotube Phase is lost.
But existing polymer matrix conversion SiBCN ceramics need to add wave absorbing agent or transition metal to promote wave absorbtion Can, and the addition of transition metal has the following problems: (1) application environment of high temperature resistant absorbing material be mainly long-term high temperature item Part is equivalent to for PDC ceramics and is chronically at a high annealing environment, and the presence of transition metal element will be persistently right Amorphous state inside PDC ceramics carries out the catalysis of crystal habit, and the increase of the high dielectric loss phase of crystalline state may cause resistance Anti- matching is unbalance, is unfavorable for the stabilization of Absorbing Materials.(2) with the development of radar absorbing technology, structure function one Body is the emphasis of the following absorbing material research, and structural wave-absorbing material should have carrying and reduce the dual function of radar cross section Can, however the increase of crystalline phase will will cause the mechanical properties decrease of ceramic material, be unfavorable for ceramic material bearing capacity and Practical application.
Summary of the invention
The purpose of the present invention is intended to overcome the shortcomings of existing methods place, provides a kind of conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material and preparation method, this method is without the side such as the catalysis of transition metal or additional CNT Method realizes the structure that high temperature wave absorbing agent is dispersed in amorphous low-loss carrier, obtained SiBCN metal-free ceramic Absorbing material absorbing property is good.
In order to achieve the above object, the present invention provides a kind of polymer crackings containing phenyl ring to convert SiBCN metal-free ceramic The preparation method of absorbing material, specifically includes the following steps:
Step 1, the hyperbranched PVDF hollow fiber membrane containing phenyl ring is synthesized
Dichloro base silane, dimethyl dichlorosilane (DMCS) and boron chloride are uniformly mixed according to the molar ratio of 1:1:1, obtained Mixed reactant；Mixed reactant is placed in ice bath, then under agitation, is added dropwise into mixed reactant and is equivalent to first The two sila azane of hexamethyl of 3.5 times of base dichlorosilane mole, reacts 12h after being added dropwise, obtains reaction solution one；
Reaction solution one is warming up to 50 DEG C of reaction 1h, obtains reaction solution two；
Reaction solution two is warming up to 110 DEG C of reaction 2h, obtains reaction solution three；
Reaction solution three is warming up to 250 DEG C of reaction 4h, obtains reaction solution four；
Removal small molecule and oligomer is concentrated under reduced pressure in reaction solution four, obtains the hyperbranched PVDF hollow fiber membrane containing phenyl ring；
Step 2, SiBCN ceramics absorbing material is prepared
The hyperbranched PVDF hollow fiber membrane of phenyl ring will be contained and be crosslinked 2h at 380-400 DEG C, obtain cross-linking products, by cross-linking products ball Tabletting is put into high-temperature cracking furnace at idiosome, then by idiosome after grinds, is cracked into potsherd at 1200 DEG C to get described SiBCN metal-free ceramic absorbing material.
Preferably, mixing speed is 200-300r/min in the step 1.
Preferably, the structure of the hyperbranched PVDF hollow fiber membrane containing phenyl ring is as follows, and phenyl ring is indicated with Ph in figure:
The hyperbranched PVDF hollow fiber membrane of phenyl ring that contains is white clear crystalline solid.
Preferably, in the step 2 cross-linking products ball milling at 200 mesh powder.
Preferably, in the step 2 tabletting at idiosome having a size of 70mm*15mm*4mm.
The present invention also provides a kind of SiBCN metal-free ceramic absorbing materials prepared using the above method.
Compared with prior art, the beneficial effects of the present invention are:
The present invention starts with from the design of ceramics polymer precursor construction, carries out high ceramic yield PVDF hollow fiber membrane presoma Constructing for topological system is synthesized and be crosslinked, phenyl ring is introduced directly into the design of PVDF hollow fiber membrane precursor construction, makes in phenyl ring Sp2 hydbridized carbon atoms direct in-situ in cracking conversion process forms the structures such as graphitic carbon, carbon nanotube, without again by mistake Catalysis or the methods of the additional CNT for crossing metal, to realize that high temperature wave absorbing agent is dispersed in amorphous low-loss carrier Structure, obtain the good metal-free ceramic based composites of absorbing property.
Detailed description of the invention
Fig. 1 is the SiBCN metal-free ceramic absorbing property test chart of pyrolysis at different temperatures.
Specific embodiment
Methods of this invention will be better understood in order to enable art processes personnel, and scheme is practiced, below with reference to specific The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method and detection method described in following each embodiments are unless otherwise specified conventional method；The examination Agent and material can be commercially available on the market unless otherwise specified.
Embodiment 1
A kind of preparation method of polymer cracking containing phenyl ring conversion SiBCN metal-free ceramic absorbing material, specifically include with Lower step:
Step 1, the hyperbranched PVDF hollow fiber membrane containing phenyl ring is synthesized
4.1g dimethyl dichlorosilane (DMCS), 9.0g dichloro base silane and 35.5g boron chloride are added to the drying of 100ml In flask, it is uniformly mixed, obtains mixed reactant；Mixed reactant is placed in ice bath, then stirring in 200-300r/min It mixes under speed, two sila azane of 20g hexamethyl is added dropwise into mixed reactant, reacts 12h after being added dropwise, obtains reaction solution One；
Reaction solution one is warming up to 50 DEG C of reaction 1h, obtains reaction solution two；
Reaction solution two is warming up to 110 DEG C of reaction 2h, obtains reaction solution three；
Reaction solution three is warming up to 250 DEG C of reaction 4h, obtains reaction solution four；
Removal small molecule and micro- reaction dissolvent is concentrated under reduced pressure in reaction solution four, obtain white clear crystalline solid contains benzene The hyperbranched PVDF hollow fiber membrane of ring；
Step 2, SiBCN ceramics absorbing material is prepared
The hyperbranched PVDF hollow fiber membrane of phenyl ring will be contained and be crosslinked 2h at 380-400 DEG C, obtain cross-linking products, by cross-linking products ball The powder of 200 mesh is worn into, then tabletting is put into high-temperature cracking furnace at the idiosome having a size of 70mm*15mm*4mm, then by idiosome, Potsherd is cracked at 1200 DEG C to get SiBCN metal-free ceramic absorbing material.
It should be noted that the structure of the hyperbranched PVDF hollow fiber membrane containing phenyl ring is as follows, and phenyl ring is indicated with Ph in figure:
In the preparation process of present invention polymer cracking containing phenyl ring conversion SiBCN metal-free ceramic absorbing material, step 2 In cracking temperature the performance of the SiBCN metal-free ceramic absorbing material finally prepared is influenced it is significant, in order to furtherly Bright cracking temperature influences the performance of SiBCN metal-free ceramic absorbing material, and the present invention is provided with following comparative example, specifically such as Under.
Comparative example 1
Polymer cracking containing phenyl ring converts SiBCN metal-free ceramic absorbing material, and the preparation method is the same as that of Example 1, difference It is in the idiosome in step 2 and is cracked into SiBCN metal-free ceramic absorbing material at 1100 DEG C in high-temperature cracking furnace.
Comparative example 2
Polymer cracking containing phenyl ring converts SiBCN metal-free ceramic absorbing material, and the preparation method is the same as that of Example 1, difference It is in the idiosome in step 2 and is cracked into SiBCN metal-free ceramic absorbing material at 1250 DEG C in high-temperature cracking furnace.
Absorbing property test is carried out to the ceramic absorbing material that embodiment 1 and comparative example 1-2 are prepared, detailed process is such as Under:
The SiBCN metal-free ceramic absorbing material that embodiment 1 and comparative example 1-2 are prepared is polished into 22.86*10.16* The size of 2mm carries out absorbing property test, and test results are shown in figure 1.
It will be seen from figure 1 that the optimal SiBCN metal-free ceramic absorbing material of absorbing property is under conditions of 1200 DEG C It is prepared, the minimum -71.80dB of reflection coefficient, effectively inhaling wave range (RC < -10dB) is 3.65GHz (8.2- 11.85GHz)。
It should be noted that the present invention describes preferred embodiment, but method personnel in the art once know Basic creative concept, then additional changes and modifications may be made to these embodiments.So appended claims are intended to explain Being includes preferred embodiment and all change and modification for falling into the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by the method personnel of this field Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent processes Within be also intended to include these modifications and variations.

Claims (7)

1. a kind of preparation method of the conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material, which is characterized in that tool Body the following steps are included:
Step 1, the hyperbranched PVDF hollow fiber membrane containing phenyl ring is synthesized
Dichloro base silane, dimethyl dichlorosilane (DMCS) and boron chloride are uniformly mixed according to the molar ratio of 1:1:1, mixed Reactant；Mixed reactant is placed in ice bath, then under agitation, is added dropwise into mixed reactant and is equivalent to methyl two The two sila azane of hexamethyl that 3.5 times of chlorosilane mol, reacts 12h after being added dropwise, obtains reaction solution one；
Reaction solution one is warming up to 50 DEG C of reaction 1h, obtains reaction solution two；
Reaction solution two is warming up to 110 DEG C of reaction 2h, obtains reaction solution three；
Reaction solution three is warming up to 250 DEG C of reaction 4h, obtains reaction solution four；
Removal small molecule and oligomer is concentrated under reduced pressure in reaction solution four, obtains the hyperbranched PVDF hollow fiber membrane containing phenyl ring；
Step 2, SiBCN ceramics absorbing material is prepared
The hyperbranched PVDF hollow fiber membrane of phenyl ring will be contained and be crosslinked 2h at 380-400 DEG C, obtain cross-linking products, by cross-linking products ball milling at Tabletting is put into high-temperature cracking furnace at idiosome, then by idiosome after powder, is cracked into potsherd at 1200 DEG C to get the SiBCN Metal-free ceramic absorbing material.
2. the preparation side of the conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material according to claim 1 Method, which is characterized in that mixing speed is 200-300r/min in the step 1.
3. the preparation side of the conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material according to claim 1 Method, which is characterized in that the structure of the hyperbranched PVDF hollow fiber membrane containing phenyl ring is as follows, and phenyl ring is indicated with Ph in figure:
4. the preparation side of the conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material according to claim 3 Method, which is characterized in that the hyperbranched PVDF hollow fiber membrane of phenyl ring that contains is white clear crystalline solid.
5. the preparation side of the conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material according to claim 1 Method, which is characterized in that in the step 2 cross-linking products ball milling at 200 mesh powder.
6. the preparation side of the conversion of polymer cracking containing phenyl ring SiBCN metal-free ceramic absorbing material according to claim 1 Method, which is characterized in that in the step 2 tabletting at idiosome having a size of 70mm*15mm*4mm.
7. the SiBCN metal-free ceramic absorbing material that one kind is prepared method according to claim 1.
CN201811195572.4A 2018-10-15 2018-10-15 Polymer cracking containing phenyl ring converts SiBCN metal-free ceramic absorbing material and preparation method Withdrawn CN109251038A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN111393986A (en) * 2020-04-03 2020-07-10 朱生寿 Environment-friendly anticorrosive fireproof coating
CN113735597A (en) * 2021-08-23 2021-12-03 西北工业大学 Preparation method of polymer conversion ceramic-based wave-absorbing material loaded with nitrogen-doped graphene in situ
CN114560708A (en) * 2022-03-15 2022-05-31 深圳市基克纳科技有限公司 Method for converting porous ceramic by utilizing self-reaction pore-forming polymer
CN115340379A (en) * 2021-05-14 2022-11-15 中国科学院化学研究所 High-carbon-content silicon-boron-carbon-nitrogen ceramic fiber and preparation method and application thereof
CN115651202A (en) * 2022-09-28 2023-01-31 中国航空制造技术研究院 Preparation method of modified polycarbosilane containing pyridine ring and wave-absorbing silicon carbide ceramic powder
CN115959911A (en) * 2022-12-30 2023-04-14 长安大学 Divinylbenzene crosslinked polymer converted amorphous SiBCN wave-absorbing ceramic and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111393986A (en) * 2020-04-03 2020-07-10 朱生寿 Environment-friendly anticorrosive fireproof coating
CN115340379A (en) * 2021-05-14 2022-11-15 中国科学院化学研究所 High-carbon-content silicon-boron-carbon-nitrogen ceramic fiber and preparation method and application thereof
CN115340379B (en) * 2021-05-14 2023-09-01 中国科学院化学研究所 High-carbon-content silicon-boron-carbon-nitrogen ceramic fiber as well as preparation method and application thereof
CN113735597A (en) * 2021-08-23 2021-12-03 西北工业大学 Preparation method of polymer conversion ceramic-based wave-absorbing material loaded with nitrogen-doped graphene in situ
CN114560708A (en) * 2022-03-15 2022-05-31 深圳市基克纳科技有限公司 Method for converting porous ceramic by utilizing self-reaction pore-forming polymer
CN115651202A (en) * 2022-09-28 2023-01-31 中国航空制造技术研究院 Preparation method of modified polycarbosilane containing pyridine ring and wave-absorbing silicon carbide ceramic powder
CN115651202B (en) * 2022-09-28 2023-12-01 中国航空制造技术研究院 Preparation method of pyridine ring-containing modified polycarbosilane and wave-absorbing silicon carbide ceramic powder
CN115959911A (en) * 2022-12-30 2023-04-14 长安大学 Divinylbenzene crosslinked polymer converted amorphous SiBCN wave-absorbing ceramic and preparation method thereof
CN115959911B (en) * 2022-12-30 2023-10-31 长安大学 Divinylbenzene cross-linked polymer converted amorphous SiBCN wave-absorbing ceramic and preparation method thereof

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Application publication date: 20190122