CN103923601B - The preparation method of structure/suction ripple integrated composite - Google Patents
The preparation method of structure/suction ripple integrated composite Download PDFInfo
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- CN103923601B CN103923601B CN201410131798.3A CN201410131798A CN103923601B CN 103923601 B CN103923601 B CN 103923601B CN 201410131798 A CN201410131798 A CN 201410131798A CN 103923601 B CN103923601 B CN 103923601B
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Abstract
The invention discloses the preparation method of a kind of structure/suction ripple integrated composite, for solving the technical problem of absorbing material supporting capacity difference prepared by existing method.Technical scheme is first distributed to uniformly in ceramic forerunner and solvent by microwave absorption, prepares finely dispersed solution; Then leaching technique that is stagnant or brushing is adopted to be immersed in by solution in the continuous fiber cloth at deposition BN interface; Finally, prepare matrix material through overcuring or high-temperature heat treatment, adopt and repeatedly flood or make matrix material densification in conjunction with chemical Vapor deposition process.Adopt macrofiber cloth as the reinforcement of matrix material, effectively improve the supporting capacity of matrix material, bending property and toughness reach 400MP and 20MPm
1/2.Meanwhile, by the matrix material regulating the content of microwave absorption to obtain absorbing property excellence, large complicated structural part can be prepared.
Description
Technical field
The present invention relates to a kind of preparation method of absorbing material, the preparation method of particularly a kind of structure/suction ripple integrated composite.
Background technology
Microwave absorbing material be a kind of can electromagnetic wave absorption and reflect, scattering and all very little functional materials of transmission.Desirable absorbing material should have that absorption band is wide, quality is light, thickness is thin, physical and mechanical properties is good, uses 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.
Microwave absorbing is mainly made up of the microwave absorption of high dielectric loss and the matrix of low-k low-dielectric loss.The microwave absorption used comprises carbon nanotube, Graphene, carbon black, silicon carbide etc.; The matrix used mainly has oxide compound and the nitride ceramics of 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 " BoWen, andect, Temperaturedependentmicrowaveattenuationbehaviorforcarbo n-nanotube/silicacomposites, 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
2deng material, there is good absorbing property, but 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 structure of complexity of preparation, limit the application of absorbing material in engineering.
Summary of the invention
In order to overcome the deficiency of absorbing material supporting capacity difference prepared by existing method, the invention provides the preparation method of a kind of structure/suction ripple integrated composite.First microwave absorption is distributed in ceramic forerunner and solvent by the method uniformly, prepares finely dispersed solution; Then leaching technique that is stagnant or brushing is adopted to be immersed in by solution in the continuous fiber cloth at deposition BN interface; Finally, prepare matrix material through overcuring or high-temperature heat treatment, adopt and repeatedly flood or make matrix material densification in conjunction with chemical Vapor deposition process.Adopt macrofiber cloth as the reinforcement of matrix material, effectively can improve the supporting capacity of matrix material.Meanwhile, by the matrix material regulating the content of microwave absorption can obtain absorbing property excellence, large complicated structural part can be prepared.
The technical solution adopted for the present invention to solve the technical problems: the preparation method of a kind of structure/suction ripple integrated composite, is characterized in comprising the following steps:
A ceramic forerunner and methylene dichloride are that 1:20 to 1:1 ratio carries out proportioning according to weight ratio by (), by weight fraction be 2.5 ~ 60% microwave absorption join in ceramic forerunner and solvent, magnetic stirring apparatus is used to carry out mechanical stirring 0.5 ~ 5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 0.5 ~ 2h, thus obtain the homodisperse solution of microwave absorption;
B () adopts 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 the cloth prepared through step (b) is built up precast body by (), then step up with graphite cake, and adjustment thickness, is then immersed in solution prepared by step (a), in vacuum impregnation tank, carries out vacuum impregnation 0.5 ~ 2h; The method of wherein brushing is as follows: be laid on graphite cake by the cloth in one deck step (b), the brushing of dissolution homogeneity step (a) prepared with brush is in cloth, then tile above one deck cloth, brushes and hocket with laying, prepare precast body with this;
D precast body that step (c) obtains by () is put in pyrolyzer and is cured and thermal treatment; Pass into the protective atmosphere of flowing in pyrolyzer, shield gas flow rate is 25 ~ 100ml/min; Pyrolyzer is warming up to 150 ~ 500 DEG C with 1 ~ 5 DEG C/min and is incubated 0.5 ~ 5h and is cured, and is then warming up to 800 ~ 300 DEG C with 1 ~ 5 DEG C/min and is incubated 0.5 ~ 5h and heat-treat, obtain the matrix material that densification degree is not high;
E () adopts CVI or PIP method densification matrix material; Wherein the method for CVI is as follows: the matrix material obtained in step (d) is deposited Si in CVI cvd furnace
3n
4, depositing temperature 700 ~ 1000 DEG C, depositing time 150 ~ 400h; Wherein the method for PIP is as follows: by the matrix material that obtains in step (d) according to the impregnation in step (b), then according to process settings and the thermal treatment of step (c), carry out 5 ~ 10 circulations with this.
Described microwave absorption is any one 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 one of cloth.
Described ceramic precursor is any one of the poly-silicon-carbon alkane of ceramic yield more than 50%, polysilazane, poly-silicon boron azane or polysiloxane.
Described protective atmosphere is Ar or N
2any one.
The invention has the beneficial effects as follows: first microwave absorption is distributed in ceramic forerunner and solvent by the method uniformly, prepare finely dispersed solution; Then leaching technique that is stagnant or brushing is adopted to be immersed in by solution in the continuous fiber cloth at deposition BN interface; Finally, prepare matrix material through overcuring or high-temperature heat treatment, adopt and repeatedly flood or make matrix material densification in conjunction with chemical Vapor deposition process.Adopt macrofiber cloth as the reinforcement of matrix material, effectively improve the supporting capacity of matrix material, bending property and toughness reach 400MP and 20MPm
1/2.Meanwhile, by the matrix material regulating the content of microwave absorption to obtain absorbing property excellence, large complicated structural part can be prepared.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
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 the inventive method in embodiment 1.
Embodiment
The present invention is described in detail with reference to Fig. 1-3.
Embodiment 1:
(1) polysiloxane and methylene dichloride are carried out proportioning according to the ratio that weight ratio is 1:1, by 2.5wt.% carbon nanotube dispersed in polysiloxane and methylene dichloride dispersion liquid, magnetic stirring apparatus is used to carry out mechanical stirring 0.5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 0.5h, obtain the homodisperse solution of microwave absorption.
(2) vacuum-impregnated method is adopted 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, adjustment thickness, is immersed in microwave absorbing agent solution prepared by step (1), carries out vacuum impregnation 2h, obtain the composite preform containing CNT in vacuum impregnation tank.
(3) composite preform that step (2) obtains is put in pyrolyzer is cured.Pass into the protective atmosphere Ar of flowing in pyrolyzer, 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 used 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, has the microwave-absorbing of excellence.Known by above result, adopt this method effectively can prepare structure/suction ripple integrated composite.
Embodiment 2:
(1) polysilazane and methylene dichloride are carried out proportioning according to the ratio that weight ratio is 1:10, be that the SiC Granular composite of 20nm is in polysilazane and methylene dichloride dispersion liquid by 60wt.% particle size, magnetic stirring apparatus is used to carry out mechanical stirring 5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 2h, thus 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) method of brushing is adopted to prepare matrix material: by the Si of preparation in one deck step (2)
3n
4cloth is laid on graphite cake, with brush by the brushing of the dissolution homogeneity in step (1) in cloth, then tile above one deck Si
3n
4cloth, brushes with this and hockets with laying, and preparation has the composite preform of 3.5mm thickness.
(4) precast body that step (3) obtains is put in pyrolyzer is cured and cracking.The protective atmosphere N of flowing is passed in pyrolyzer
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, and insulation 0.5h, obtains the matrix material of densification.
(5) matrix material of preparation in step (4) is put 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) poly-silicon boron azane and methylene dichloride are carried out proportioning according to the ratio that weight ratio is 1:20, by 5wt.% graphene dispersion in poly-silicon boron azane and methylene dichloride dispersion liquid, magnetic stirring apparatus is used to carry out mechanical stirring 5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 2h, thus 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, and depositing time is 10h, and deposit thickness is 200nm.
(3) method of brushing is adopted to prepare matrix material: to be laid on graphite cake by the wave transparent SiC cloth of preparation in one deck step (2), with brush by the brushing of the dissolution homogeneity in step (1) in cloth, then tile above one deck SiC cloth, brush with this and hocket with laying, preparation has the composite preform of 3.5mm thickness.
(4) precast body that step (3) obtains is put in pyrolyzer is cured and cracking.Pass into the protective atmosphere Ar of flowing in pyrolyzer, 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, and insulation 5h, obtains the matrix material of densification.
(5) matrix material of preparation in step (4) is put 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) poly-silicon-carbon alkane and methylene dichloride are carried out proportioning according to the ratio that weight ratio is 1:10,5wt.% nanometer SiCN is distributed in poly-silicon-carbon alkane and methylene dichloride dispersion liquid, magnetic stirring apparatus is used to carry out mechanical stirring 0.5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 0.5h, thus 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) vacuum-impregnated method is adopted 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, adjustment thickness, be immersed in the solution of step (1), in vacuum impregnation tank, carry out vacuum impregnation 2h, obtain the precast body containing microwave absorption CNT.
(4) precast body that step (3) obtains is put in pyrolyzer is cured and cracking.The protective atmosphere N of flowing is passed in pyrolyzer
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, and insulation 5h, obtains the matrix material of densification.
(5) be impregnated in the solution in step (1) by the matrix material in step (4), be then cured and cracking according to step (4), circulate 10 times with this, obtaining density is 2.6g/cm
3matrix material.
Embodiment 5:
(1) polysilazane and methylene dichloride are carried out proportioning according to the ratio that weight ratio is 1:10, by 5wt.% nano SiC fiber dispersion in polysilazane and methylene dichloride dispersion liquid, magnetic stirring apparatus is used to carry out mechanical stirring 0.5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 0.5h, thus 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) vacuum-impregnated method is adopted 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, adjustment thickness, be immersed in the solution of step (1), in vacuum impregnation tank, carry out vacuum impregnation 2h.
(4) plank that step (3) obtains is put in pyrolyzer is cured and cracking.Pass into the protective atmosphere Ar of flowing in pyrolyzer, 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, and insulation 5h, obtains the matrix material of densification.
(5) be impregnated in the solution in step (1) by the matrix material in step (4), be then cured and cracking according to step (4), circulate 5 times with this, obtaining density is 2.1g/cm
3matrix material.
Claims (4)
1. a preparation method for structure/suction ripple integrated composite, is characterized in that comprising the following steps:
A ceramic forerunner and methylene dichloride are that 1:20 to 1:1 ratio carries out proportioning according to weight ratio by (), by weight fraction be 2.5 ~ 60% microwave absorption join in ceramic forerunner and methylene dichloride, magnetic stirring apparatus is used to carry out mechanical stirring 0.5 ~ 5h, then use ultrasonic emulsification dispersion machine to carry out ultrasonic disperse 0.5 ~ 2h, thus obtain the homodisperse solution of microwave absorption; Described microwave absorption is any one of carbon nanotube, Graphene, nano SiC powder, nanometer SiCN or nano SiC fiber.
B () adopts 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 () adopts the method for vacuum impregnation or brushing to prepare matrix material; Wherein vacuum-impregnated method is as follows: the cloth prepared through step (b) is built up precast body, then step up with graphite cake, adjustment thickness, is then immersed in solution prepared by step (a), in vacuum impregnation tank, carries out vacuum impregnation 0.5 ~ 2h; The method of wherein brushing is as follows: be laid on graphite cake by the cloth in one deck step (b), the brushing of dissolution homogeneity step (a) prepared with brush is in cloth, then tile above one deck cloth, brush with this and hocket with laying, prepare precast body;
D precast body that step (c) obtains by () is put in pyrolyzer and is cured and thermal treatment; Pass into the protective atmosphere of flowing in pyrolyzer, shield gas flow rate is 25 ~ 100ml/min; Pyrolyzer is warming up to 150 ~ 500 DEG C with 1 ~ 5 DEG C/min and is incubated 0.5 ~ 5h and is cured, and is then warming up to 800 ~ 1300 DEG C with 1 ~ 5 DEG C/min and is incubated 0.5 ~ 5h and heat-treat, obtain the matrix material that densification degree is not high;
E () adopts CVI or PIP method densification matrix material; Wherein the method for CVI is as follows: the matrix material obtained in step (d) is deposited Si in CVI cvd furnace
3n
4, depositing temperature 700 ~ 1000 DEG C, depositing time 150 ~ 400h; Wherein the method for PIP is as follows: by the matrix material that obtains in step (d) according to the impregnation in step (b), then according to process settings and the thermal treatment of step (c), carry out 5 ~ 10 circulations with this.
2. the preparation method of structure according to claim 1/suction ripple integrated composite, is characterized in that: described cloth is wave transparent SiC cloth, Si
3n
4cloth, Al
2o
3cloth, ZrO
2cloth or SiO
2any one of cloth.
3. the preparation method of structure according to claim 1/suction ripple integrated composite, is characterized in that: described ceramic precursor is any one of the poly-silicon-carbon alkane of ceramic yield more than 50%, polysilazane, poly-silicon boron azane or polysiloxane.
4. the preparation method of structure according to claim 1/suction ripple integrated composite, is characterized in that: described protective atmosphere is Ar or N
2any one.
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| CN109439281B (en) * | 2018-11-28 | 2020-08-25 | 北京航空航天大学 | Composite nano material with microwave absorption characteristic and preparation method thereof |
| CN113185299A (en) * | 2021-04-06 | 2021-07-30 | 中国航空制造技术研究院 | Preparation method of multilayer wave-absorbing ceramic matrix composite |
| CN113979766B (en) * | 2021-10-20 | 2022-07-15 | 哈尔滨工业大学（威海） | BCN/FexOy@CfPreparation process of/C composite structure wave-absorbing material |
| CN114573330B (en) * | 2022-02-24 | 2023-03-31 | 西北工业大学 | Defective graphene/wave-transparent ceramic composite wave-absorbing material, method and application |
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