CN104788130B - C/（SiC/BN）nCompound interface phase coating, coated fiber and preparation method thereof - Google Patents
C/（SiC/BN）nCompound interface phase coating, coated fiber and preparation method thereof Download PDFInfo
- Publication number
- CN104788130B CN104788130B CN201510190624.9A CN201510190624A CN104788130B CN 104788130 B CN104788130 B CN 104788130B CN 201510190624 A CN201510190624 A CN 201510190624A CN 104788130 B CN104788130 B CN 104788130B
- Authority
- CN
- China
- Prior art keywords
- layers
- sic
- layer
- fiber
- interface phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
A kind of C/ (SiC/BN)nCompound interface phase coating, including C layers and periodic stack, periodic stack refer to SiC layer, BN layers of alternating cyclical superposition.A kind of coated fiber, including fibrous matrix and the C/ (SiC/BN) of matrix surface coatingnCompound interface phase coating, fibrous matrix is mullite fiber, one kind in carbon fiber, silicon carbide fibre, quartz fibre.The preparation method of coated fiber of the present invention includes：Prepare fiber-based material, one layer C layers are first deposited on the surface of fibrous matrix using chemical vapor deposition method；Again using chemical vapor deposition method in C layer surface alternating deposit SiC layers and BN layer, repeatedly the number of alternating deposit 3~5 times, obtain coated fiber.The product of the present invention has the advantages that good physical chemistry compatibility, high temperature resistant, anti-oxidant, toughening effect is good.
Description
Technical field
It is multiple more particularly to one kind the invention belongs to the interface phase coating and its preparing technical field of ceramic matric composite
Close interface phase coating and preparation method thereof.
Background technology
Polycrystalline ceramic fiber has the characteristics that high specific strength, high ratio modulus, high temperature resistant, anti-oxidant, resistant to chemical etching, can use
Make polymer matrix, the high-performance compound phase of Metal Matrix and Ceramic Matrix Composites.It is compound by fibre-reinforced high performance ceramic base
Material can be used for the leading-edge fields such as space shuttle, high-performance enginer, be referred to as 21 century Aeronautics and Astronautics and new and high technology neck
The new material of domain application.The performance of ceramic matric composite performance depends not only on the property of ceramic fibre and ceramic matrix in itself
Can, it is often more important that interface phase therebetween.Interface plays decisive role with respect to the performance of ceramic matric composite, such as
Siwei L, Litong Z etc. impregnates the preparation of (CVI) technique using original Niccalon-SiC fibers through chemical gaseous phase
SiCf/ SiC ceramic matrix composite material bending strength only has 85.0MPa, and fiber surface is after carbon coating deposits, SiCf/ SiC ceramic matrix composite material
Interface be improved significantly, bending strength can bring up to 420.0MPa.Suitable interface mutually can protect fiber, make fiber multiple
Being damaged in condensation material preparation process reduces；Importantly, during interface mutually can also protect the fibers from technique and use
Corrosion, oxidation, interfacial chemical reaction and mechanical damage, significantly improve the mechanical property of composite material.
Mainly there are pyrolytic carbon (PyC) coating, boron nitride (BN) to apply applied to the interface phase coating in ceramic matric composite
Layer, carborundum (SiC) coating etc..PyC coatings can mutually significantly improve the mechanical property of composite material as interface, it earliest should
For being used as interface phase in SiC ceramic based composites.PyC coatings have the layered crystal structure being distributed along fiber, and have
There are suitable interlaminar shear strength and bond strength, but the inoxidizability of PyC is poor so that contain answering for PyC coating interface phases
Condensation material high temperature oxidation stability environment hydraulic performance decline it is serious.BN has and layered crystal structure as graphite-like, and BN
Antioxygenic property is better than PyC, and the common interface phase coating of ceramic matric composite；But the BN when temperature is higher than 850 DEG C
Generation B can be aoxidized2O3, cause material property to decline serious, therefore the temperature in use of the composite material containing BN coating interface phases is still
It is so limited.The inoxidizability of SiC coatings is preferable, can be used between 800 DEG C~900 DEG C, but shape between SiC and mullite fiber
Into strong―binding interface, cause easily to extend in fiber during the crack growth of matrix, be unfavorable for the hair of fiber reinforcement effect
Wave.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided one
Plant good physical chemistry compatibility, high temperature resistant, anti-oxidant, toughening effect the is good fiber and matrix that can be used as ceramic matric composite
Between C/ (SiC/BN)nCompound interface phase coating, it is low to correspondingly provide a kind of simple technical process, good product performance, cost
Foregoing C/ (SiC/BN)nThe preparation method of compound interface phase coating.
In order to solve the above technical problems, technical solution proposed by the present invention is a kind of fibre that can be used as ceramic matric composite
C/ (SiC/BN) between peacekeeping matrixnCompound interface phase coating, the compound interface phase coating have periodic stack structure, institute
State the alternating cyclical superposition that periodic stack structure specifically refers to SiC layer, BN layers；And in the periodic stack directly and C
Layer contact is SiC layer, and outermost layer is then preferably BN layers.
The above-mentioned technical proposal of the present invention is based primarily upon following thinking：Compound interface phase coating is as between fiber and matrix
Connecting material, interface bond strength is too strong, ceramic matric composite be broken when produce brittle fracture, be unfavorable for ceramic fibre increasing
The hair of tough performance, and interface bond strength is excessively weak, matrix bears load and can not effectively pass on, and is unfavorable for ceramic fibre enhancement
The hair of energy.And C coatings and fibrous physics chemical compatibility are good, there is the layer structure being distributed along machine direction, interface cohesion
Intensity and interlaminar shear strength are preferable first floor material, are conducive to crackle deviation, steering, bifurcated in layer, consumption fracture
Energy.In the structure design of the above-mentioned compound interface phase of the present invention, we creatively select preferable BN layer of toughening effect with
The preferable SiC layer of high-temperature oxidation resistance, constitutes the C/ (SiC/BN) in compound interface phase coatingnPeriodic stack.This is multiple
Closing anisotropic C, BN in the phase coating of interface has the layer structure of stacking, is conducive to matrix cracking in internal steering and divides
Fork, can meet the requirement of low modulus and low shear strength at the same time, moreover it is possible to effectively make up the fault of construction of fiber surface, make fiber
Strengthened, but aerial C oxidations, by 450 DEG C or so, the oxidation of BN is by 800 DEG C or so, and SiC is generally at 800 DEG C
Passive oxidation occurs in~1000 DEG C of oxidation environment, CVD SiC can play prevention and reflect " stopping for matrix cracking diffusion
Layer " effect.The oxide of BN is liquid at relatively high temperatures, can be with the SiO of SiC layer oxidation generation2Reaction generates a kind of borosilicate
Silicate glass, has certain barrier and Healing to interface oxidation.Therefore, (SiC/BN)nPeriodic structure possesses one in itself
Fixed oxidation resistance.As it can be seen that the preferable BN of toughening effect and high-temperature oxidation resistant are selected in the structure design of interface phase of the present invention
Property preferable SiC, form compound interface phase coating in periodic stack, its fibre be especially suitable for ceramic matric composite
Interface phase coating between peacekeeping matrix.In addition, our research is it is also shown that because of the weak interface cohesion of C, BN layers of formation, C, SiC layer
Strong interface cohesion is formed, therefore, the combination of C-BN is unfavorable for the performance of fiber reinforcement effect, and the knot of C-SiC and BN-SiC
Conjunction mode, then can significantly improve interface bond strength.As it can be seen that the present invention whole coating structure has been made it is accurate design and
Creative adjustment.
Above-mentioned C/ (SiC/BN)nIn compound interface phase coating, it is preferred that the lamination cycle cycle of the periodic stack
Number is 3~5 times；BN layers in the compound interface phase coating have the Turbostratic of anisotropic.C/(SiC/BN)nIt is compound
Interface phase coating preferably comprises multilayer BN Turbostratics, just because of Turbostratic possessed by anisotropy BN, does not refer to own
Stacking lamella it is all parallel with fibrous matrix surface, the deviation of crackle wherein and turn to and just become easy, crackle is along BN heaps
The direction change of pile lamella and ideally realize steering, crackle is at C/ (SiC/BN)nInside the sub-layer of compound interface phase, sub-layer it
Between, between interface and fibrous matrix there occurs deviation, bifurcated and steering, consume a large amount of energies to failure, lead crack is divided into more
Weight micro-crack, this can increase toughness of material, improve its damage tolerance.Under normal circumstances, BN layers of thickness is not in same period
The thickness of SiC layer is should be less than, preferably greater than the thickness of SiC layer.
Above-mentioned C/ (SiC/BN)nIn compound interface phase coating, it is preferred that thickness C layers described for 15.0nm~
20.0nm, thickness in monolayer BN layers described are 20.0nm~50.0nm, and the thickness in monolayer of the SiC layer is 8.0nm~25.0nm.
The technical concept total as one, the present invention also provides a kind of coated fiber, including fibrous matrix and fibrous matrix
The coating of surface coating, the coating is above-mentioned C/ (SiC/BN)nCompound interface phase coating, the fibrous matrix are mullite
One kind in fiber, carbon fiber, silicon carbide fibre, quartz fibre.In the coated fiber of the present invention, coating and fibrous matrix,
It is to be connected in a manner of mechanical bond and chemical bonding between each sub-layer.
The technical concept total as one, the present invention also provides a kind of preparation method of above-mentioned coated fiber, including with
Lower step：
(1) prepare fiber-based material, one is first deposited on the surface of fiber-based material using chemical vapor deposition method
C layers of layer；
(2) chemical vapor deposition method is used in the C layer surface alternating deposit SiC layers and BN of above-mentioned fiber-based material
Layer, the number of repetition alternating deposit 3~5 times；Obtain coated fiber.
In above-mentioned preparation method, chemical vapor deposition C layers first, then again with liquid precursor (preferably borazine, poly-
Carbon silane) it is raw material, using chemical vapor deposition (CVD) technique, prepared by way of alternately replacing source of the gas on C sub-layers surface
(SiC/BN)nPeriodicity coating.Preparing the device of BN, SiC sub-layer in the present invention for CVD includes：CVD chamber (pipe
Formula stove), temperature control system, pressure control system, flow control system, vacuum pump, gas imports and discharge system etc..
Above-mentioned preparation method, it is preferred that in the step (1), C layers of chemical vapor deposition conditions include：With propylene
For presoma, precursor gas source flux is 30.0sccm~70.0sccm, and reaction pressure is 50Pa~400Pa, and argon gas is carrier gas,
Argon gas is carrier gas, and depositing temperature is 900 DEG C~1000 DEG C, and sedimentation time is 30.0min~40.0min.
Above-mentioned preparation method, it is preferred that in the step (2), the chemical vapor deposition conditions of SiC layer include：With liquid
Body Polycarbosilane is presoma, and precursor gas source flux is 25.0sccm~60.0sccm, and reaction pressure is 100Pa~400Pa,
Carrier gas and carrier gas are argon gas, and depositing temperature is 1000 DEG C~1100 DEG C, and sedimentation time is 20.0min~50.0min.
Above-mentioned preparation method, it is preferred that in the step (2), BN layers of chemical vapor deposition conditions include：With ring boron
Azane is presoma, and precursor gas source flux is 40.0sccm~80.0sccm, and reaction pressure is 60Pa~300Pa, carrier gas and
Carrier gas is hydrogen, and depositing temperature is 800 DEG C~1000 DEG C, sedimentation time 20.0min~40.0min.
The above-mentioned technical proposal of the present invention is based primarily upon following thinking：C, BN, SiC are formed multi-layer composite coatings by the present invention
Interface phase, can further improve the oxidation-protective effect of interface phase coating, widen the use temperature range of composite material.BN exists
Less than 900 DEG C have excellent antioxygenic property, and SiC could only be aoxidized more than 900 DEG C and be formed continuous SiO2Film
And good oxidation-protective effect is shown, and the oxidation product B of BN, SiC2O3、SiO2Mutually it can melt to form continuous film, from
And effectively slow down the further oxidation of material.In addition, the first floor uses C coatings, be conducive to the combination between fiber and matrix, at the same time
BN, SiC sub-layer are introduced in the phase coating of interface, crackle can deflect between each sub-layer, can be right there is multistage toughening mechanisms
Composite material plays significant toughening effect.
Compared with prior art, the advantage of the invention is that：
1. the C/ (SiC/BN) of the present inventionnCompound interface phase coating uses multi-layer structure design, make use of combined type coating
Function is superimposed and mutual supplement with each other's advantages principle, the flexible C layers for mutually selecting chemical vapor deposition and BN layer, the two all has unrest layer stacking spy
Sign, is conducive to crackle at C/ (SiC/BN)nDeviation, bifurcated occur inside sub-layer, between sub-layer, between interface and fiber and turns
To consumption energy to failure, can make lead crack be divided into multiple micro-crack, increase toughness of material, improve its damage tolerance；In addition,
C/(SiC/BN)nPassive oxidation, the glass of generation can occur in 800 DEG C~1000 DEG C oxidation environments for the SiC in periodic structure
State SiO2Matrix cracking can be made up, suppress the oxidation of its internal structure and material.Therefore, C/ (SiC/BN)nPeriodic structure has in itself
Standby certain oxidation resistance, relative to simple BN coatings temperature in use higher, relative to simple SiC coatings toughening effect more
It is good.
2. the present invention by CVD method prepares BN coatings apply most precursors be boron halide BX3(such as BF3、BCl3、
BBr3) and NH3, the most commonly used precursor of SiC coatings is trichloromethyl silane (MTS), but there are itself and reaction for such system
Accessory substance corrosivity is strong, and to serious corrosion of equipment, and accessory substance ammonium salt settling chamber easy to pollute blocks pipeline, reactant and product pair
The deficiencies of fiber seriously corroded.The pioneer that the present invention is prepared using borazine as BN sub-layers, Polycarbosilane as SiC sub-layers
Body, both of which such as are halogen-free at the corrosive elements, will not generate corrosive byproducts, and ceramic conversion rate is high.
3. the present invention, in the case where not shifting fibrous matrix, continues to sink by way of alternately replacing precursor source of the gas
The follow-up sub-layer of product, simplifies coating deposition process, improves the uniformity of each sub-layer sedimentary condition.
On the whole, the present invention is finally obtained one by the design of the optimization to technological parameter, coating and sub-layer thickness
Kind physical chemistry compatibility is good, high temperature resistant, the nanostructured C/ (SiC/BN) that anti-oxidant, toughening effect is goodnCompound interface mutually applies
Layer, to improving fiber reinforced ceramic matrix composites performance (especially mullite fiber or carbon fiber ceramic based composites) tool
It is significant.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are the present invention
Some embodiments, for those of ordinary skill in the art, without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is C/ (SiC/BN) in the embodiment of the present invention 1nThe transmission electron microscope picture (low resolution) of compound interface phase coating.
Fig. 2 is C/ (SiC/BN) in the embodiment of the present invention 1nThe transmission electron microscope picture of compound interface phase coating SiC and BN sub-layer
(high-resolution).
Fig. 3 is C/ (SiC/BN) in the embodiment of the present invention 1nThe distribution diagram of element of compound interface phase coating.
Embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood implication of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
As shown in Figure 1, Figure 2, Figure 3 shows, a kind of of the invention silicon carbide fibre and matrix that can be used as ceramic matric composite
Between C/ (SiC/BN)nCompound interface phase coating, the compound interface phase coating have periodic stack structure, the periodic stack
The alternating cyclical that structure specifically refers to SiC layer, BN layers is superimposed, the lamination cycle cycle times of periodic stack in the present embodiment
For 3 times.Specifically, C layers of thickness is 20.0nm from the inside to the outside, the thickness of the first sub-layers of SiC is 25.0nm, the first sub-layers of BN
Thickness is 25.0nm, and the thickness of the second sub-layers of SiC is 8.0nm, and the thickness of the second sub-layers of BN is 20.0nm, the 3rd sub-layers of SiC
Thickness is 20.0nm, and the thickness of the 3rd sub-layers of BN is 50.0nm.
A kind of coated fiber of the invention, including fibrous matrix and the coating of fibrous matrix surface coating, the coating are upper
State the C/ (SiC/BN) of the present embodimentnCompound interface phase coating, fibrous matrix are silicon carbide fibre.In the coated fiber of the present invention
In, it is to be connected in a manner of mechanical bond and chemical bonding between coating and fibrous matrix, each sub-layer.
The preparation method of the coated fiber of the present embodiment, comprises the following steps：
(1) one layer C layers are deposited on the surface of silicon carbide fibre matrix using the method for chemical vapor deposition；C layers of deposition
Condition is as follows：Propylene is presoma, and precursor gas source flux is 70.0sccm, reaction pressure 400Pa, and dilution is used as using argon gas
Gas and carrier gas, depositing temperature are 1000 DEG C, sedimentation time 40.0min；
(2) one layer of SiC layer is deposited in the C layer surfaces of fibrous matrix using the method for chemical vapor deposition；The deposition of SiC layer
Condition is as follows：Using liquid Polycarbosilane as presoma, precursor gas source flux is 60.0sccm, reaction pressure 400Pa, with argon
Gas is carrier gas and carrier gas, and depositing temperature is 1100 DEG C, sedimentation time 50.0min；
(3) one layer BN layers are deposited on the SiC layer surface of fibrous matrix using the method for chemical vapor deposition；BN layers of deposition
Condition is as follows：Using borazine as presoma, precursor gas source flux is 40.0sccm, reaction pressure 60Pa, using hydrogen as
Carrier gas and carrier gas, depositing temperature are 800 DEG C, sedimentation time 25.0min；
(4) continue the primary operational of (2) of repeating the above steps in BN layer surfaces, be only that sedimentation time is changed to 20.0min；
(5) repeat the above steps (3), is only that sedimentation time is changed to 20.0min；
(6) repeat the above steps (4), is only that sedimentation time is changed to 40.0min；
(7) repeat the above steps (3), is only that sedimentation time is changed to 40.0min；
Preparing the device of BN, SiC sub-layer in the present embodiment for CVD includes：CVD chamber (tube furnace), temperature
Control system, pressure control system, flow control system, vacuum pump, gas importing and discharge system etc., obtain after the completion of deposition
Coated fiber.
By transmission electron microscope observing, C/ (SiC/BN) manufactured in the present embodimentnCompound interface phase coating is as shown in Figure 1, thoroughly
Radio mirror shows that the coating uniform is intactly covered in SiC fiber surfaces, and coating is tightly combined with fiber surface, and no hole etc. lacks
Fall into.Each sub-layer thickness is uniform in coating, each sub-layer uniform ingredients, the transmission electron microscope picture of compound interface phase coating SiC and BN sub-layer
As shown in Fig. 2, as seen from Figure 2, occurring a small amount of microstructure in SiC sub-layers, BN sub-layers are non-micro-structure.Fig. 3 is this hair
C/ (SiC/BN) in bright embodiment 1nThe distribution diagram of element of compound interface phase coating, in Fig. 3 it can be seen from face coat
Si Elemental redistributions are mainly in SiC sub-layers, and the distribution of first floor C element is more concentrated, and N element is distributed mainly among BN sub-layers, is said
Light fibers face coat sandwich is more apparent.
Embodiment 2：
A kind of C/ (SiC/BN) that can be used as between the silicon carbide fibre of ceramic matric composite and matrix of the inventionnIt is compound
Interface phase coating, the compound interface phase coating have a periodic stack structure, the periodic stack structure specifically refer to SiC layer,
BN layers of alternating cyclical is superimposed, and the lamination cycle cycle times of periodic stack are 5 times in the present embodiment.Specifically, by interior
It is 15.0nm to thickness C layers outer, the thickness of the first sub-layers of SiC is 8.0nm, and the thickness of the first sub-layers of BN is 20.0nm, SiC
The thickness of two sub-layers is 18.0nm, and the thickness of the second sub-layers of BN is 25.0nm, and the thickness of the 3rd sub-layers of SiC is 25.0nm, BN
The thickness of three sub-layers is 50.0nm, and the thickness of the 4th sub-layers of SiC is 25.0nm, and the thickness of the 4th sub-layers of BN is 50.0nm, SiC
The thickness of five sub-layers is 25.0nm, and the thickness of the 5th sub-layers of BN is 50.0nm.
A kind of coated fiber of the invention, including fibrous matrix and the coating of fibrous matrix surface coating, the coating are upper
State the C/ (SiC/BN) of the present embodimentnCompound interface phase coating, fibrous matrix are carbon fiber.In the coated fiber of the present invention,
It is to be connected in a manner of mechanical bond and chemical bonding between coating and fibrous matrix, each sub-layer.
The preparation method of the coated fiber of the present embodiment, comprises the following steps：
(1) one layer C layers are deposited on the surface of carbon fiber substrate using the method for chemical vapor deposition；C layers of sedimentary condition
It is as follows：Propylene is presoma, and precursor gas source flux is 30.0sccm, reaction pressure 50Pa, using argon gas as carrier gas and
Carrier gas, depositing temperature are 900 DEG C, sedimentation time 30.0min；
(2) one layer of SiC layer is deposited in the C layer surfaces of fibrous matrix using the method for chemical vapor deposition；The deposition of SiC layer
Condition is as follows：Using liquid Polycarbosilane as presoma, precursor gas source flux is 25.0sccm, reaction pressure 100Pa, with argon
Gas is carrier gas and carrier gas, and depositing temperature is 1100 DEG C, sedimentation time 20.0min；
(3) one layer BN layers are deposited on the SiC layer surface of fibrous matrix using the method for chemical vapor deposition；BN layers of deposition
Condition is as follows：Using borazine as presoma, precursor gas source flux is 80.0sccm, reaction pressure 60Pa, using hydrogen as
Carrier gas and carrier gas, depositing temperature are 1000 DEG C, sedimentation time 20.0min；
(4) continue the primary operational of (2) of repeating the above steps in BN layer surfaces, be only that sedimentation time is changed to 35.0min；
(5) repeat the above steps (3), is only that sedimentation time is changed to 25.0min；
(6) repeat the above steps (4), is only that sedimentation time is changed to 50.0min；
(7) repeat the above steps (3), is only that sedimentation time is changed to 40.0min；
(8) repeat the above steps (4), is only that sedimentation time is changed to 50.0min；
(9) repeat the above steps (3), is only that sedimentation time is changed to 40.0min；
(10) repeat the above steps (4), is only that sedimentation time is changed to 50.0min；
(11) repeat the above steps (3), is only that sedimentation time is changed to 40.0min；
Preparing the device of BN, SiC sub-layer in the present embodiment for CVD includes：CVD chamber (tube furnace), temperature
Control system, pressure control system, flow control system, vacuum pump, gas importing and discharge system etc., obtain after the completion of deposition
Coated fiber.
By transmission electron microscope observing, C/ (SiC/BN) manufactured in the present embodimentnIn compound interface phase coating, the coating uniform
Fiber C surface is intactly covered in, the defects of coating is tightly combined with fiber surface, no hole.Each sub-layer thickness is equal in coating
Even, there is a small amount of microstructure in the SiC sub-layers of compound interface phase coating, BN sub-layers are non-micro-structure in each sub-layer uniform ingredients.
Claims (3)
1. a kind of preparation method of coated fiber, the painting that the coated fiber includes fibrous matrix and fibrous matrix surface coats
Layer, the fibrous matrix is mullite fiber, one kind in carbon fiber, silicon carbide fibre, quartz fibre, and the coating is C/
（SiC/BN）nCompound interface phase coating, the compound interface phase coating include C layers and coated on the periodic stack on C layers, institutes
State the alternating cyclical superposition that periodic stack specifically refers to SiC layer, BN layers；And directly connect in the periodic stack with C layers
Tactile is SiC layer；The lamination cycle cycle times of the periodic stack are 3~5 times；It is same in the compound interface phase coating
BN layers of thickness is not less than the thickness of SiC layer in cycle；BN layers in the compound interface phase coating have the unrest of anisotropic
Rotating fields；The preparation method comprises the following steps：
（1）Prepare fiber-based material, one layer of C is first deposited on the surface of fiber-based material using chemical vapor deposition method
Layer；（2）Using chemical vapor deposition method in the C layer surface alternating deposit SiC layers of above-mentioned fiber-based material and BN layers, repetition
The number of alternating deposit 3~5 times；Coated fiber is obtained, the SiC layer depositing temperature is 1000 DEG C~1100 DEG C, the BN
Layer depositing temperature is 800 DEG C~1000 DEG C；
The step（2）In, the chemical vapor deposition conditions of SiC layer include：Using liquid Polycarbosilane as presoma, precursor gas
Source flux is the sccm of 25.0 sccm~60.0, and reaction pressure is the Pa of 100 Pa~400, and carrier gas and carrier gas are argon gas, are sunk
The product time is the min of 20.0 min~50.0；The step（2）In, BN layers of chemical vapor deposition conditions include：With ring boron nitrogen
Alkane is presoma, and precursor gas source flux is the sccm of 40.0 sccm~80.0, and reaction pressure is the Pa of 60 Pa~300, carrier gas
It is hydrogen with carrier gas, the min of 20.0 min of sedimentation time~40.0.
2. preparation method according to claim 1, it is characterised in that thickness C layers described is 15.0 nm~20.0
Nm, thickness in monolayer BN layers described are the nm of 20.0 nm~50.0, and the thickness in monolayer of the SiC layer is the nm of 8.0 nm~25.0.
3. preparation method according to claim 1, it is characterised in that the step（1）In, C layers of chemical vapor deposition
Condition includes：Using propylene as presoma, precursor gas source flux is the sccm of 30.0 sccm~70.0, and reaction pressure is 50 Pa
~400 Pa, argon gas are carrier gas, and argon gas is carrier gas, and depositing temperature is 900 DEG C~1000 DEG C, and sedimentation time is 30.0 min
~40.0 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510190624.9A CN104788130B (en) | 2015-04-21 | 2015-04-21 | C/（SiC/BN）nCompound interface phase coating, coated fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510190624.9A CN104788130B (en) | 2015-04-21 | 2015-04-21 | C/（SiC/BN）nCompound interface phase coating, coated fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104788130A CN104788130A (en) | 2015-07-22 |
| CN104788130B true CN104788130B (en) | 2018-04-17 |
Family
ID=53553380
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510190624.9A Active CN104788130B (en) | 2015-04-21 | 2015-04-21 | C/（SiC/BN）nCompound interface phase coating, coated fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104788130B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237020B (en) * | 2015-08-31 | 2018-08-24 | 中国人民解放军国防科学技术大学 | A kind of fibre reinforced ZrB2- ZrN multiphase ceramic matrix composites and preparation method thereof |
| CN106747671B (en) * | 2016-06-03 | 2017-12-12 | 北京航空航天大学 | The preparation method of superhigh temperature thermostructural composite boundary layer |
| CN106966742B (en) * | 2016-06-03 | 2020-07-28 | 北京航空航天大学 | Alumina fiber reinforced mullite ceramic containing interface phase and preparation method thereof |
| CN106431448A (en) * | 2016-10-20 | 2017-02-22 | 中南大学 | Boron nitride/silicon carbide composite coating layer and preparation method thereof |
| CN108396279B (en) * | 2018-03-12 | 2020-04-14 | 北京矿冶科技集团有限公司 | Ultrahigh-temperature sealing coating material, coating and preparation method thereof |
| CN109437975B (en) * | 2018-09-29 | 2021-06-29 | 中国人民解放军第五七一九工厂 | High-temperature-resistant and high-toughness SiCf/SiC composite material preform composite interface layer and preparation method thereof |
| CN109608208B (en) * | 2018-12-17 | 2021-12-31 | 中国科学院上海硅酸盐研究所 | Multilayer interface coating and preparation method and application thereof |
| CN112321331A (en) * | 2020-11-18 | 2021-02-05 | 江西信达航科新材料科技有限公司 | High-temperature-resistant antioxidant composite coating and preparation process thereof |
| CN113354435A (en) * | 2021-07-08 | 2021-09-07 | 西北工业大学 | SiC fibre reinforcement and toughening (SiC-BN)mMulti-element multi-layer self-healing ceramic matrix composite and preparation method thereof |
| CN114804895A (en) * | 2022-06-02 | 2022-07-29 | 中国航发北京航空材料研究院 | High-temperature self-healing BN/SiC fiber interface coating and preparation method thereof |
| CN116199519B (en) * | 2023-01-17 | 2023-12-29 | 中国科学院上海硅酸盐研究所 | Double BN interface layer fiber reinforced ceramic matrix composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030715A (en) * | 2014-06-25 | 2014-09-10 | 中国人民解放军国防科学技术大学 | Preparation method of Cf/BN-SiC composite material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167612B (en) * | 2011-01-14 | 2012-09-26 | 中国人民解放军国防科学技术大学 | Preparation method of boron nitride coating on fiber surface |
-
2015
- 2015-04-21 CN CN201510190624.9A patent/CN104788130B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030715A (en) * | 2014-06-25 | 2014-09-10 | 中国人民解放军国防科学技术大学 | Preparation method of Cf/BN-SiC composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104788130A (en) | 2015-07-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104788130B (en) | C/（SiC/BN）nCompound interface phase coating, coated fiber and preparation method thereof | |
| CN104817336B (en) | (BN/SiC) n compound interfaces phase coating, coated fiber and preparation method thereof | |
| CN101503305B (en) | Process for preparing self-sealing silicon carbide ceramic based composite material | |
| CN101445392B (en) | Graphite matrix flawless TaC coating and manufacturing method thereof | |
| CN107540400A (en) | A kind of SiC with compound interfacef/ SiC ceramic based composites | |
| CN102167612B (en) | Preparation method of boron nitride coating on fiber surface | |
| CN105152671B (en) | SiCfThe interface modification method of/SiC ceramic matrix composite material | |
| US8986845B2 (en) | Ceramic composite article having laminar ceramic matrix | |
| CN103058697B (en) | Method for modifying boron nitride interface phase of ceramic matrix composite material | |
| CN102470630B (en) | Composite material part having a ceramic matrix, and method for manufacturing same | |
| CN104609863B (en) | Silicon carbide fiber of appearance deposition SiBCN coating and preparation method thereof | |
| CN106342035B (en) | The resistance to ablation of FRCMC, anti-thermal shock high-temperature oxidation resistant coating and preparation method thereof | |
| CN109400168A (en) | It is a kind of comprising the SiC fiber and its preparation method and application of the SiBCN coating and SiC coating that are alternatively formed | |
| CN101913894A (en) | Dual self-healing modification method for silicon carbide ceramic matrix composite material | |
| US20220055957A1 (en) | Method of making a ceramic matrix composite that exhibits chemical resistance | |
| IE913637A1 (en) | Carbon-containing composite material part protected against oxidation and its production process | |
| CN107540399A (en) | CNT toughness reinforcing SiBCN (O) metal matrix ceramic composite coatings and its preparation method | |
| CN104611916B (en) | Carbon fiber of appearance deposition SiBCN coating and preparation method thereof | |
| CN105525273A (en) | Silicon carbide hydrogen permeation barrier coating for stainless steel and preparation method for silicon carbide hydrogen permeation barrier coating | |
| Qiang et al. | Oxidation resistance of SiC nanowires reinforced SiC coating prepared by a CVD process on SiC‐coated C/C composites | |
| JPH03232978A (en) | Multilayer coating for reinfoecing material in high temperature composite material | |
| CN102619081B (en) | Preparation technology for preparing interface layer of boron nitride fabric through CVD (Chemical Vapor Deposition) | |
| CN114163263B (en) | Novel environmental barrier coating and structure for SiC ceramic matrix composite | |
| CN108752012B (en) | Preparation method of boron nitride/silicon nitride composite interface layer on fiber surface | |
| CN104195522B (en) | Preparation method of glass fiber cotton felt with high thermal conductivity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |