CN103923601A - Preparation method of structure/microwave absorbing integrated composite material - Google Patents
Preparation method of structure/microwave absorbing integrated composite material Download PDFInfo
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- CN103923601A CN103923601A CN201410131798.3A CN201410131798A CN103923601A CN 103923601 A CN103923601 A CN 103923601A CN 201410131798 A CN201410131798 A CN 201410131798A CN 103923601 A CN103923601 A CN 103923601A
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Abstract
The invention discloses a preparation method of a structure/microwave absorbing integrated composite material and is used for solving the technical problem that a microwave absorbing material prepared by adopting the existing method has poor bearing capacity. According to the technical scheme, the preparation method of the structure/microwave absorbing integrated composite material comprises the following steps: firstly uniformly dispersing a microwave absorbent into a ceramic precursor and a solvent, and preparing a uniformly dispersed solution; then immersing the uniformly dispersed solution into a continuous fiber cloth deposited with a BN (boron nitride) interface by adopting a dipping or painting technology; finally, carrying out curing or high temperature heat treatment, so that a composite material is obtained, and the composite material is densified by dipping for multiple times or combining a chemical vapour deposition method; the long fiber cloth is adopted as reinforcement of the composite material, carrying capacity of the composite material is effectively improved, and bending property and toughness are 400MP and 20MP.m1/2; meanwhile, the composite material with excellent microwave absorbing property by regulating content of the microwave absorbent, and a large-scale complex structural component can be prepared.
Description
Technical field
The present invention relates to a kind of preparation method of absorbing material, particularly a kind of preparation method of structure/suction ripple integrated composite.
Background technology
Microwave absorbing material be a kind of can electromagnetic wave absorption and reflect, all very little functional materialss of scattering and transmission.Desirable absorbing material should have that absorption band is wide, quality is light, thin thickness, physical and mechanical properties are good, use and prepare the features such as easy.Wherein, there is microwave absorbing property and the structure that simultaneously can carry is inhaled ripple integrated material and had huge application potential in industrial production, environment protection and national defence field.
Microwave absorbing is mainly the matrix composition by the microwave absorption of high dielectric loss and low-k low-dielectric loss.The microwave absorption using comprises carbon nanotube, Graphene, carbon black, silicon carbide etc.; The matrix using is mainly oxide compound and the nitride ceramics with low dielectric constant and loss, as relative permittivity and dielectric loss are respectively 3.9 and 3 × 10
-4melt of si O
2, relative permittivity and dielectric loss are 5.2 and 1 × 10
-4bN, relative permittivity and dielectric loss are respectively 9.0 and 3 × 10
-3si
3n
4.
Document 1 " patent publication No. is the Chinese invention patent of CN10182388B " discloses a kind of preparation method of microwave absorbing material.The method adopts Graphene as microwave absorption, adopts wave transparent pottery (SiO
2, Si
3n
4deng) as matrix, use high-temperature sintering process to prepare microwave absorbing material.
Document 2 " Bo Wen; and ect; Temperature dependent microwave attenuation behavior for carbon-nanotube/silica composites, Carbon65 (2013) 124-139 " discloses a kind of CNT/SiO
2the preparation method of absorbing material.The method adopts CNT and SiO
2powder, as raw material, uses the method for sintering to prepare CNT/SiO
2absorbing material.Although, CNT/SiO
2have good absorbing property Deng material, still, because stupalith fragility is large, toughness is low, and material can not effectively be carried, and can not prepare structure/function integration absorbing material.And, adopt the method for sintering to be difficult to the large-scale and complicated structure of preparation, limit the application of absorbing material in engineering.
Summary of the invention
The poor deficiency of absorbing material supporting capacity of preparing in order to overcome existing method, the invention provides a kind of preparation method of structure/suction ripple integrated composite.First the method is distributed to microwave absorption in ceramic forerunner and solvent uniformly, prepares finely dispersed solution; Then adopt the technique of soaking stagnant or brushing solution to be immersed in the continuous fiber cloth at deposition BN interface; Finally, prepare matrix material through overcuring or high-temperature heat treatment, adopt repeatedly dipping or make matrix material densification in conjunction with chemical Vapor deposition process.Adopt the reinforcement of macrofiber cloth as matrix material, can effectively improve the supporting capacity of matrix material.Meanwhile, by regulating the content of microwave absorption can obtain the matrix material of absorbing property excellence, can prepare large complicated structural part.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of structure/suction ripple integrated composite, is characterized in comprising the following steps:
(a) be that 1:20 carries out proportioning to 1:1 ratio by ceramic forerunner and methylene dichloride according to weight ratio, the microwave absorption that is 2.5～60% by weight fraction joins in ceramic forerunner and solvent, use magnetic stirring apparatus to carry out mechanical stirring 0.5～5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 0.5～2h, thereby obtain the homodisperse solution of microwave absorption;
(b) adopt chemical Vapor deposition process at wave transparent cloth surface deposition BN interface, depositing temperature is 600～800 DEG C, and depositing time is 10～50h, and deposit thickness is 200～1500nm;
(c) cloth of preparing through step (b) is built up to precast body, then step up with graphite cake, adjust thickness, be then immersed in solution prepared by step (a), in vacuum impregnation tank, carry out vacuum impregnation 0.5～2h; Wherein the method for brushing is as follows: the cloth in one deck step (b) is laid on graphite cake, the solution of with brush being prepared by step (a) brushing is uniformly in cloth, then one deck cloth that tiles in the above, brushes with laying and hockets with this, prepares precast body;
(d) precast body step (c) being obtained is put in pyrolyzer and is cured and thermal treatment; In pyrolyzer, pass into mobile protective atmosphere, shield gas flow rate is 25～100ml/min; Pyrolyzer is warming up to 150～500 DEG C and be incubated 0.5～5h and be cured with 1～5 DEG C/min, is then warming up to 800～300 DEG C and be incubated 0.5～5h and heat-treat with 1～5 DEG C/min, obtains the matrix material that densification degree is not high;
(e) adopt CVI or PIP method densification matrix material; Wherein the method for CVI is as follows: the matrix material obtaining in step (d) is deposited to Si in CVI cvd furnace
3n
4, 700～1000 DEG C of depositing temperatures, depositing time 150～400h; Wherein the method for PIP is as follows: the matrix material obtaining in step (d), according to the pickling process dipping in step (b), is then solidified and thermal treatment according to the process of step (c), carry out 5～10 circulations with this.
Described microwave absorption is any of carbon nanotube, Graphene, nano SiC powder, nanometer SiCN or nano SiC fiber.
Described cloth is wave transparent SiC cloth, Si
3n
4cloth, Al
2o
3cloth, ZrO
2cloth or SiO
2any of cloth.
Described ceramic precursor is any of poly-silicon-carbon alkane, polysilazane, poly-silicon boron azane or the polysiloxane of ceramic yield more than 50%.
Described protective atmosphere is Ar or N
2any.
The invention has the beneficial effects as follows: first the method is distributed to microwave absorption in ceramic forerunner and solvent uniformly, prepare finely dispersed solution; Then adopt the technique of soaking stagnant or brushing solution to be immersed in the continuous fiber cloth at deposition BN interface; Finally, prepare matrix material through overcuring or high-temperature heat treatment, adopt repeatedly dipping or make matrix material densification in conjunction with chemical Vapor deposition process.Adopt the reinforcement of macrofiber cloth as matrix material, effectively improved the supporting capacity of matrix material, bending property and toughness have reached 400MP and 20MPm
1/2.Meanwhile, by regulating the content of microwave absorption to obtain the matrix material of absorbing property excellence, can prepare large complicated structural part.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo of carbon nanotube in the inventive method embodiment 1.
Fig. 2 is the stress-strain curve in the inventive method embodiment 1.
Fig. 3 is the reflectance test curve in embodiment 1 in the inventive method.
Embodiment
Describe the present invention in detail with reference to Fig. 1-3.
Embodiment 1:
(1) ratio that is 1:1 by polysiloxane and methylene dichloride according to weight ratio is carried out proportioning, by 2.5wt.% carbon nanotube dispersed in polysiloxane and methylene dichloride dispersion liquid, use magnetic stirring apparatus to carry out mechanical stirring 0.5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 0.5h, obtain the homodisperse solution of microwave absorption.
(2) adopt vacuum-impregnated method to prepare matrix material: by SiO
2cloth builds up and is of a size of 180 × 180 × 2.5mm
3precast body, then step up with graphite jig, adjust thickness, be immersed in microwave absorbing agent solution prepared by step (1), in vacuum impregnation tank, carry out vacuum impregnation 2h, obtain the composite preform that contains CNT.
(3) composite preform step (2) being obtained is put in pyrolyzer and is cured.In pyrolyzer, pass into mobile protective atmosphere Ar, shield gas flow rate is 25ml/min, and solidification value is 150 DEG C, and temperature rise rate is 1 DEG C/min, and insulation 0.5h, finally obtains Wave suction composite material.
Fig. 1 is the transmission electron microscope photo of the microwave absorption CNT of use in embodiment 1.As can see from Figure 2, the flexural strength of Wave suction composite material reaches 205MPa, illustrates that matrix material has higher mechanical property.As can see from Figure 3, the reflectivity of Wave suction composite material is minimum is-34dB to have excellent microwave absorbing.Known by above result, adopt this method can effectively prepare structure/suction ripple integrated composite.
Embodiment 2:
(1) ratio that is 1:10 by polysilazane and methylene dichloride according to weight ratio is carried out proportioning, the SiC particle that is 20nm by 60wt.% particle size is distributed in polysilazane and methylene dichloride dispersion liquid, use magnetic stirring apparatus to carry out mechanical stirring 5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 2h, thereby prepare the homodisperse solution of microwave absorption.
(2) adopt chemical Vapor deposition process at Si
3n
4cloth surface deposition BN interface, depositing temperature is 600 DEG C, and depositing time is 50h, and deposit thickness is 1500nm.
(3) adopt the method for brushing to prepare matrix material: by the Si of preparation in one deck step (2)
3n
4cloth is laid on graphite cake, and with brush, by the solution in step (1), brushing is in cloth uniformly, and one deck Si in the above then tiles
3n
4cloth, brushes with laying and hockets with this, and preparation has the composite preform of 3.5mm thickness.
(4) precast body step (3) being obtained is put in pyrolyzer and is cured and cracking.In pyrolyzer, pass into mobile protective atmosphere N
2, shield gas flow rate is 50ml/min, and solidification value is 500 DEG C, and temperature rise rate is 5 DEG C/min, and insulation 5h, is then warming up to 800 DEG C with 5 DEG C/min, is incubated 0.5h, obtains the matrix material of densification.
(5) matrix material of preparation in step (4) is put into and in cvd furnace, deposits Si
3n
4carry out densification, depositing time is 400h, and depositing temperature is 700 DEG C, and obtaining density is 2.5g/cm
3matrix material.
Embodiment 3:
(1) carry out proportioning by gathering the ratio that silicon boron azane and methylene dichloride are 1:20 according to weight ratio, 5wt.% Graphene is distributed in poly-silicon boron azane and methylene dichloride dispersion liquid, use magnetic stirring apparatus to carry out mechanical stirring 5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 2h, thereby prepare the finely dispersed solution of microwave absorption.
(2) adopt chemical Vapor deposition process at 180 × 180mm
2wave transparent SiC cloth surface deposition BN interface, depositing temperature is 800 DEG C, depositing time is 10h, deposit thickness is 200nm.
(3) adopt the method for brushing to prepare matrix material: the wave transparent SiC cloth of preparation in one deck step (2) is laid on graphite cake, with brush by uniformly brushing of the solution in step (1) in cloth, then one deck SiC cloth in the above tiles, brush with laying and hocket with this, preparation has the composite preform of 3.5mm thickness.
(4) precast body step (3) being obtained is put in pyrolyzer and is cured and cracking.In pyrolyzer, pass into mobile protective atmosphere Ar, shield gas flow rate is 75ml/min, and solidification value is 500 DEG C, and temperature rise rate is 5 DEG C/min, and insulation 5h, is then warming up to 1300 DEG C with 5 DEG C/min, is incubated 5h, obtains the matrix material of densification.
(5) matrix material of preparation in step (4) is put into and in cvd furnace, deposits Si
3n
4, depositing time is 150h, and depositing temperature is 1000 DEG C, and obtaining density is 2.3g/cm
3matrix material.
Embodiment 4:
(1) carry out proportioning by gathering the ratio that silicon-carbon alkane and methylene dichloride are 1:10 according to weight ratio, 5wt.% nanometer SiCN is distributed in poly-silicon-carbon alkane and methylene dichloride dispersion liquid, use magnetic stirring apparatus to carry out mechanical stirring 0.5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 0.5h, thereby prepare the finely dispersed solution of microwave absorption.
(2) adopt chemical Vapor deposition process at Al
2o
3cloth surface deposition BN interface, depositing temperature is 600 DEG C, and depositing time is 50h, and deposit thickness is 1500nm.
(3) adopt vacuum-impregnated method to prepare matrix material: by Al
2o
3cloth builds up and is of a size of 180 × 180 × 3.5mm
3precast body, then step up with graphite cake, adjust thickness, be immersed in the solution of step (1), in vacuum impregnation tank, carry out vacuum impregnation 2h, obtain the precast body that contains microwave absorption CNT.
(4) precast body step (3) being obtained is put in pyrolyzer and is cured and cracking.In pyrolyzer, pass into mobile protective atmosphere N
2, shield gas flow rate is 100ml/min, and solidification value is 500 DEG C, and temperature rise rate is 5 DEG C/min, and insulation 5h, is then warming up to 1000 DEG C with 5 DEG C/min, is incubated 5h, obtains the matrix material of densification.
(5) matrix material in step (4) is impregnated in the solution in step (1), is then cured and cracking according to step (4), circulate 10 times with this, obtaining density is 2.6g/cm
3matrix material.
Embodiment 5:
(1) ratio that is 1:10 by polysilazane and methylene dichloride according to weight ratio is carried out proportioning, by 5wt.% nano SiC fiber dispersion in polysilazane and methylene dichloride dispersion liquid, use magnetic stirring apparatus to carry out mechanical stirring 0.5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 0.5h, thereby prepare the finely dispersed solution of microwave absorption.
(2) adopt chemical Vapor deposition process at ZrO
2cloth surface deposition BN interface, depositing temperature is 600 DEG C, and depositing time is 50h, and deposit thickness is 1000nm.
(3) adopt vacuum-impregnated method to prepare matrix material: by ZrO
2cloth builds up and is of a size of 180 × 180 × 3.5mm
3precast body, then step up with graphite cake, adjust thickness, be immersed in the solution of step (1), in vacuum impregnation tank, carry out vacuum impregnation 2h.
(4) plank step (3) being obtained is put in pyrolyzer and is cured and cracking.In pyrolyzer, pass into mobile protective atmosphere Ar, shield gas flow rate is 75ml/min, and solidification value is 500 DEG C, and temperature rise rate is 5 DEG C/min, and insulation 5h, is then warming up to 800 DEG C with 5 DEG C/min, is incubated 5h, obtains the matrix material of densification.
(5) matrix material in step (4) is impregnated in the solution in step (1), is then cured and cracking according to step (4), circulate 5 times with this, obtaining density is 2.1g/cm
3matrix material.
Claims (5)
1. a preparation method for structure/suction ripple integrated composite, is characterized in that comprising the following steps:
(a) be that 1:20 carries out proportioning to 1:1 ratio by ceramic forerunner and methylene dichloride according to weight ratio, the microwave absorption that is 2.5～60% by weight fraction joins in ceramic forerunner and solvent, use magnetic stirring apparatus to carry out mechanical stirring 0.5～5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic dispersion 0.5～2h, thereby obtain the homodisperse solution of microwave absorption;
(b) adopt chemical Vapor deposition process at wave transparent cloth surface deposition BN interface, depositing temperature is 600～800 DEG C, and depositing time is 10～50h, and deposit thickness is 200～1500nm;
(c) cloth of preparing through step (b) is built up to precast body, then step up with graphite cake, adjust thickness, be then immersed in solution prepared by step (a), in vacuum impregnation tank, carry out vacuum impregnation 0.5～2h; Wherein the method for brushing is as follows: the cloth in one deck step (b) is laid on graphite cake, the solution of with brush being prepared by step (a) brushing is uniformly in cloth, then one deck cloth that tiles in the above, brushes with laying and hockets with this, prepares precast body;
(d) precast body step (c) being obtained is put in pyrolyzer and is cured and thermal treatment; In pyrolyzer, pass into mobile protective atmosphere, shield gas flow rate is 25～100ml/min; Pyrolyzer is warming up to 150～500 DEG C and be incubated 0.5～5h and be cured with 1～5 DEG C/min, is then warming up to 800～300 DEG C and be incubated 0.5～5h and heat-treat with 1～5 DEG C/min, obtains the matrix material that densification degree is not high;
(e) adopt CVI or PIP method densification matrix material; Wherein the method for CVI is as follows: the matrix material obtaining in step (d) is deposited to Si in CVI cvd furnace
3n
4, 700～1000 DEG C of depositing temperatures, depositing time 150～400h; Wherein the method for PIP is as follows: the matrix material obtaining in step (d), according to the pickling process dipping in step (b), is then solidified and thermal treatment according to the process of step (c), carry out 5～10 circulations with this.
2. the preparation method of structure/suction ripple integrated composite according to claim 1, is characterized in that: described microwave absorption is any of carbon nanotube, Graphene, nano SiC powder, nanometer SiCN or nano SiC fiber.
3. the preparation method of structure/suction ripple integrated composite according to claim 1, is characterized in that: described cloth is wave transparent SiC cloth, Si
3n
4cloth, Al
2o
3cloth, ZrO
2cloth or SiO
2any of cloth.
4. the preparation method of structure/suction ripple integrated composite according to claim 1, is characterized in that: described ceramic precursor is any of poly-silicon-carbon alkane, polysilazane, poly-silicon boron azane or the polysiloxane of ceramic yield more than 50%.
5. the preparation method of structure/suction ripple integrated composite according to claim 1, is characterized in that: described protective atmosphere is Ar or N
2any.
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| CN201410131798.3A CN103923601B (en) | 2013-12-20 | 2014-04-03 | The preparation method of structure/suction ripple integrated composite |
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| CN114573330A (en) * | 2022-02-24 | 2022-06-03 | 西北工业大学 | Defective graphene/wave-transparent ceramic composite wave-absorbing material, method and application |
| CN115637607A (en) * | 2022-09-07 | 2023-01-24 | 西安交通大学 | High-temperature-resistant fireproof electromagnetic shielding material and preparation method thereof |
| CN115637607B (en) * | 2022-09-07 | 2023-11-10 | 西安交通大学 | High-temperature-resistant fireproof electromagnetic shielding material and preparation method thereof |
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