CN110304931A - A kind of high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite and preparation method thereof - Google Patents
A kind of high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of high-volume fractional silicon-carbide nano wire enhancing ceramic matric composites and preparation method thereof, and the preparation method includes: that (1) disperses silicon carbide nanometer line and dispersing agent in solvent, obtains silicon carbide nanometer line suspension；(2) gained silicon carbide nanometer line suspension is obtained into silicon carbide nanometer line precast body after filtering；(3) modifying interface is carried out to gained silicon carbide nanometer line precast body using chemical vapor deposition process or chemical vapor infiltration technique；(4) densification is carried out to gained silicon carbide nanometer line precast body using at least one of chemical vapor infiltration technique and organic precursor impregnating cracking technology, obtains the high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite.
Description
Technical field
It is special the present invention relates to a kind of high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite and preparation method thereof
It is not related to the densification of high-volume fractional one dimension SiC nano material, belongs to field of nanometer material technology.
Background technique
Since 1991 after the discovery of carbon nanotube, monodimension nanometer material is concerned due to its excellent performance.It is one-dimensional
Nano material electricity, calorifics and in terms of the performance that can not reach with traditional material, be expected to as composite material
Novel enhanced material realizes structural material functionalization.Wherein, silicon carbide nanometer line attracts attention, intensity, modulus and calorifics
Silicon carbide whisker and block materials can be superior to, be expected to improve composite materials property as reinforced phase and enhance thermal conductance
Energy.
Silicon carbide nanometer line to be limited to volume fraction using obstacle relatively low, interface difficulty regulation, matrix is difficult to densify.Mesh
Before, there are two types of the applications of silicon carbide nanometer line；One is silicon carbide nanometer line is grown in material internal, this method has its own
Limitation, nano wire can not reach a uniform dispersion effect in material internal, and the Nanowire Quality of growth is irregular,
Impurity remains in the performance of matrix effect material property；Secondly, for the chemiluminescence of fiber and nano wire, the system at interface
It is standby to cannot concurrently reach optimization；In addition, the nano wire of this method preparation enhances composite material, nanowires body fraction is difficult
With control, when nanowires body fraction deficiency, can not play preferable reinforcing effect.Second is to select the nano wire of purifying former
Material carries out the preparation of matrix to it.The method avoids growth nano wire bring impurity, nano wire is uniformly dispersed, volume point
There are certain Modulatory characters for number.Traditional nano wire enhancing composite process directly mixes nano wire with ceramic powder,
The dispersibility of nano wire is bad.Powder sintering is also easily destroyed nanowire structure and performance is caused to decline.
Summary of the invention
For SiC nanowire application obstacle, the purpose of the invention is to propose a kind of high-volume fractional silicon-carbide nanometer
Line enhances ceramic matric composite and preparation method thereof.
On the one hand, the present invention provides a kind of preparations of high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite
Method, comprising:
(1) it disperses silicon carbide nanometer line and dispersing agent in solvent, obtains silicon carbide nanometer line suspension；
(2) gained silicon carbide nanometer line suspension is obtained into silicon carbide nanometer line precast body after filtering；
(3) interface is carried out to gained silicon carbide nanometer line precast body using chemical vapor deposition process or chemical vapor infiltration technique
Modification；
(4) using at least one of chemical vapor infiltration technique and organic precursor impregnating cracking technology to gained nanometer silicon carbide
Line precast body carries out densification, obtains the high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite.
In the present invention, the silicon carbide nanometer line precast body obtained using suction filtration ensure that the high volume of silicon carbide nanometer line
Score, CVI or preparation interface make nano wire preferably play reinforcing effect in the composite.Simple CVI technique easily makes
Surface pores blocking and inside there are still a large amount of holes, simple PIP process requirement thin slice has certain consistency, mechanical strength
And the porosity.The hybrid technique of CVI combination PIP the characteristics of two kinds of technique and will combine and perform to ultimate attainment, make silicon carbide nanometer line
Precast body reaches higher consistency.
Preferably, the diameter of the silicon carbide nanometer line is 0.02~0.6 μm in step (1), length is 10~200 μm,
Draw ratio is greater than 100, and the dispersing agent is in dodecyl sodium sulfate, isopropanol, polyvinylpyrrolidone, butyl glycol ether
At least one；Preferably, the mass ratio of the dispersing agent and silicon carbide nanometer line is 1:(0.1~30).
Preferably, the solvent is at least one of dehydrated alcohol, deionized water, acetone and formaldehyde in step (1).
Preferably, the mode of the dispersion is ultrasonic treatment in step (1)；The power of the ultrasonic treatment be 10~
1000W, time are 0.1~2 hour.
Preferably, in step (2), in step (2), being carried out using the machine of suction filtration, the running parameter of the suction filtration machine is 20~
60L/min, power are 160~500W；Preferably, it is preferable that after suction filtration, compressed under the pressure of 0.1~10MPa
Processing (the silicon carbide nanometer line precast body preliminary to gained after suction filtration carries out compression processing).Preferably, the nanometer silicon carbide
Line precast body with a thickness of 0.5mm~10mm.
Preferably, boundary layer obtained by the modifying interface is pyrolysis carbon boundary layer, silicon carbide interface layer, nitrogen in step (3)
Change at least one of boron boundary layer, silicon nitride interface layer；5~100nm of thickness of the boundary layer.
Preferably, the parameter of the chemical vapor infiltration technique includes: to be made using methyl trichlorosilane MTS in step (4)
For 100~400sccm of organic precursor, hydrogen is carrier gas and diluent gas rate is 10~90sccm；Temperature be 1000~
1100 DEG C, pressure is 1.5~6KPa, and the time is 300~1000 minutes.
Preferably, the parameter of the organic precursor impregnating cracking technology includes: organic precursor type in step (4)
Selected from least one of Polycarbosilane, polysiloxanes, polysilazane；Cracking temperature is 700~1100 DEG C.
On the other hand, the present invention provides a kind of according to the above-mentioned high-volume fractional silicon-carbide nanometer for obtaining preparation method preparation
Line enhances ceramic matric composite, nanometer silicon carbide in the high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite
The volume fraction of line is 10~37vol%.
The utility model has the advantages that
There is dispersibility, volume fraction, interface regulation, the problems such as nano pore densification, the present invention for the application of SiC nanowire
The netted SiC nanowire thin slice of high-volume fractional is obtained using filtering, using chemical vapor infiltration or other methods to SiC nanowire
The preparation for carrying out boundary layer has gained silicon carbide nanometer line enhancing ceramic matric composite using the method for CVI combination PIP and reaches
To higher consistency, density reaches 2.74g/cm3, three-point bending strength reaches 273 ± 32MPa, and nano impress shows modulus
494 ± 14GPa, to realize actual effect application of the silicon carbide nanometer line in ceramic matric composite.The present invention is to be with silicon carbide
Matrix, silicon carbide nanometer line do reinforced phase and prepare silicon carbide nanometer line ceramics of silicon carbide toughened based composites.The present invention is protecting
While demonstrate,proving silicon carbide nanometer line high-volume fractional, avoid traditional handicraft when preparing matrix to the damage of its performance, and only CVI
It is difficult to reach higher-density, the situation that only PIP can not directly to nano wire thin slice densification makes silicon carbide nanometer line in composite wood
Performance gives full play in material.
Detailed description of the invention
Fig. 1 be in embodiment 1 SiC nanowire by filtering dry (1), interface prepares (2), CVI matrix prepare (3) and
The outside drawing of composite material after PIP matrix (4) preparation；
Fig. 2 is the variation that sample quality under different duration CVI and PIP is passed through in the preparation of SiC nanowire sheet base in embodiment 1,
Wherein under (a) difference CVI duration quality variation, (b), (c), (d) and (e) respectively correspond in (a) figure 20 hours, 40 hours,
50 hours and 60 hours CVI；It (f) is 50 hours CVI in conjunction with sample section electron microscope after 3 PIP；
Fig. 3 is the SEM photograph of the netted silicon carbide nanometer line prepared after filtering in embodiment 1；
Fig. 4 is the SEM photograph of the section of composite material after CVI and PIP combination densification in embodiment 1.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention makes full use of silicon carbide nanometer line performance, is conducive to the high body that preparation has excellent mechanical, thermal property
Fraction silicon carbide nanometer line enhances ceramic matric composite, and Modulatory character is strong, application prospect is big.
The preparation of silicon carbide nanometer line suspension.The ratio for regulating and controlling silicon carbide nanometer line and dispersing agent, is scattered in solvent,
Obtain evenly dispersed silicon carbide nanometer line suspension.The diameter of silicon carbide nanometer line can be 0.02~0.6 μm, length be 10~
200 μm, draw ratio is greater than 100.Preferably, the nanometer silicon carbide linear diameter is 0.02~0.1 μm, length is 10~100 μ
M, draw ratio are greater than 100.The solvent is at least one of dehydrated alcohol, deionized water, acetone, formaldehyde.The dispersion
Agent includes at least one of dodecyl sodium sulfate, isopropanol, polyvinylpyrrolidone, butyl glycol ether.Dispersing agent and carbon
The mass ratio of SiClx nano wire can be 1:0.1~1:30.As an example, regulate and control the ratio of silicon carbide nanometer line and dispersing agent
Example, is dispersed silicon carbide nanometer line in solvent using techniques such as mechanical stirring or/and ultrasonic treatments, obtains evenly dispersed carbon
The nanowire suspended liquid of SiClx.The power of ultrasonic treatment is 10~1000W, and the time is 0.1h~2h.
The preparation of silicon carbide nanometer line precast body.It is pre- that high-volume fractional silicon-carbide nano wire is prepared using devices such as suction filtration machines
Body processed.Specific the step of filtering or parameter include: to mix silicon carbide nanometer line and aqueous solvent, polyethylene of dispersing agent pyrrolidones
It closes, the even line solution obtained after ultrasound pours into bottle,suction, and bottleneck places the filter paper of the duct 0.5um size.It filters
To the silicon carbide nanometer line thin slice of 0.5mm thickness.The running parameter of suction filtration machine can be 20~60L/min, power can for 160~
500W.It is dried to obtain anhydrous netted silicon carbide nanometer line thin slice.The present invention obtains pure silicon carbide nanometer line by filtering
Thin slice ensure that the high-volume fractional of SiC nanowire.It is preferred that while certain thickness is slightly compressed to it, thus it is possible to vary nanometer
Pore size between line further regulates and controls the volume fraction of silicon carbide nanometer line.The pressure size of the compression can be 0.1~10MPa.
The preparation of boundary layer.With the techniques such as chemical vapor infiltration (CVI) or chemical vapor deposition (CVD) to nanometer silicon carbide
Line precast body carries out modifying interface, obtains boundary layer.Wherein boundary layer includes but is not limited to pyrolytic carbon, silicon carbide, boron nitride, nitrogen
The interfaces such as SiClx.The thickness of boundary layer is best between 5~100nm.
Densification process.Silicon carbide is received using the single or hybrid technique such as CVI and organic precursor infiltration pyrolysis (PIP)
Rice noodles precast body carries out densification, obtains the modified ceramic matric composite of high-volume fractional silicon-carbide nano wire, realizes
Silicon carbide nanometer line macroscopic view is applied and gives full play to its excellent performance.Preferably in combination with CVI and PIP process advantage, to nanometer material
The advantages of material carries out densification, plays the two to greatest extent, makes composite material reach higher consistency.Wherein, PIP selects forerunner
Body PCS introduces silicon carbide nanometer line precast body, and presoma type includes but is not limited to Polycarbosilane, polysiloxanes, polysilazane
It is 700~1100 DEG C Deng, cracking temperature, cracking gained matrix material constituents are SiC.Wherein, the ginseng of chemical vapor infiltration technique
Number includes: using methyl trichlorosilane MTS as 100~400sccm of organic precursor, hydrogen be carrier gas and diluent gas 10~
90sccm；Temperature is 1000~1100 DEG C, and pressure is 1.5~6KPa, and the time is 300~1000 minutes, obtains preliminary dense carbon
The carbon/silicon carbide ceramic matrix composite of SiClx nano wire enhancing.Matrix material constituents obtained by chemical vapor infiltration technique are SiC.
In the present invention, high-volume fractional silicon-carbide nano wire enhances the body of silicon carbide nanometer line in ceramic matric composite
Fraction is 10~37vol%, and consistency is 73% or more, and density reaches 2.74g/cm3, three-point bending strength reaches
316MPa, nano impress show that modulus is up to 514GPa.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1:
(1) silicon carbide nanometer line and dodecyl sodium sulfate matter are controlled as dispersing agent (0.1g) using dodecyl sodium sulfate
Silicon carbide nanometer line is dispersed in deionized water using ultrasonic technique than being 5:1, obtains unordered silicon carbide nanometer line by amount
Suspension, ultrasonic power 300W, ultrasonic time 1h；
(2) silicon carbide nanometer line is prepared into reticulated film using the method for vacuum filtration, filters machine running parameter 20L/min,
Power 160W, the compression processing under the pressure of 0.15MPa, so that the thickness control of film is in 0.5mm~1.2mm.Through dry
To netted silicon carbide nanometer line thin slice；
(3) film obtained in (2) is placed in CVI furnace to the preparation for carrying out pyrolytic carbon or boron nitride interface, is pyrolyzed carbon boundary layer
(with a thickness of 5nm) preparation process: CH4Flow velocity is 50sccm, 1100 DEG C of temperature, pressure 3KPa, reaction time 60min.Boron nitride
Interfacial process parameter: BCl3Flow velocity 10sccm, NH3Flow velocity 30sccm, H2Flow velocity 60sccm, 800 DEG C of temperature, pressure 0.5KPa, instead
45min between seasonable；
(4) film obtained in (3) is continued into CVI depositing silicon silicon substrate, technological parameter MTS carrier gas H2Mixed gas rate
208sccm adjusts MTS air pressure tank outlet and cuts down, keeps pressure to maintain 0 scale or so, i.e. air inlet is identical with the rate of outlet.It is dilute
Release H2Flow velocity 62sccm, 1100 DEG C of temperature, pressure 3KPa, 300~1000min of reaction time；
(5) (4) are obtained into block and continues 3~7 silicon carbide precursor PCS infiltration pyrolysis circulations, until silicon carbide nanometer line enhances
Carbon/silicon carbide ceramic matrix composite mass change is within 1%.
Embodiment 2:
Part same as Example 1 no longer describes, except that cutting after step (4) to sample in embodiment 1
It cuts, polishes its surface, duct is exposed in section cutting, continues the carbonization that process (5) realize silicon carbide nanometer line enhancing
The densification of silicon ceramic matric composite, multiple infiltration pyrolysis realize that silicon carbide nanometer line enhances ceramic matric composite mass change
Within 1%.
Embodiment 3:
Part in the same manner as in Example 1 is no longer stated, is selected the method for infiltration to handle its siliconising in step (5), is reached it
To higher consistency.
Embodiment 4:
Part in the same manner as in Example 1 is no longer stated, PMMA (0.3g) is added afterwards in solution in step (1), heating stirring obtains
To half-dried colloid, mold is carried out to it, solidification obtains certain shapes blocks.Obtained blocks is placed in vacuum or inertia
Demoulding obtains the mesh nano line thin slice of certain shapes in gas stove.Step (3), (4), (5) are to netted in continuation embodiment 1
SiC nanowire densified, until silicon carbide nanometer line enhancing ceramic matric composite mass change is within 1%.
Table 1 is the performance parameter that high-volume fractional silicon-carbide nano wire prepared by the present invention enhances ceramic matric composite:
Fig. 1 be in embodiment 1 SiC nanowire by filtering dry (1), interface prepares (2), CVI matrix prepare (3) and
The outside drawing of composite material after PIP matrix (4) preparation, sample has higher nanometer by filtered thin slice as we know from the figure
Wire body fraction, appearance becomes black after the preparation of pyrolytic carbon interface, prepares by CVI matrix, and sample has comparatively dense ceramics
Feature finally passes through PIP technique, and sample consistency further increases, and has a small amount of silicon carbide dross to generate on its surface.CVI carbon
SiClx is uniform adsorption on nano wire, and PIP silicon carbide is based on blocky filling pore；
Fig. 2 is the variation that sample quality under different duration CVI and PIP is passed through in the preparation of SiC nanowire sheet base in embodiment 1,
Wherein the variation (b) of quality, (c), (d) and (e) respectively correspond 20 hours, 40 hours, 50 in (a) figure under (a) difference CVI duration
Hour and 60 hours CVI；(f) sample section electron microscope after 3 PIP is combined for 50 hours CVI, as we know from the figure the quality of thin slice
Increase with the increase of CVI time, from (b), (c), (d) and (e) it can be seen that the consistency of thin slice and nano wire it is straight
Diameter gradually increases, and shows that CVI has certain densification effects to it, figure (f) shows thin slice after 3 PIP, and sample reaches higher
Densification effects, be hardly visible hole；
Fig. 3 is the SEM photograph of the netted silicon carbide nanometer line prepared after filtering in embodiment 1, and nano wire interlocks as we know from the figure
Arrangement forms uniform duct；
Fig. 4 is the SEM photograph of the section of composite material after CVI and PIP combination densification in embodiment 1, and section is deposited as we know from the figure
In seldom hole, CVI combination PIP technique has preferable densification effects to netted silicon carbide nanometer line thin slice.
Claims (10)
1. a kind of preparation method of high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite characterized by comprising
(1) it disperses silicon carbide nanometer line and dispersing agent in solvent, obtains silicon carbide nanometer line suspension；
(2) gained silicon carbide nanometer line suspension is obtained into silicon carbide nanometer line precast body after filtering；
(3) interface is carried out to gained silicon carbide nanometer line precast body using chemical vapor deposition process or chemical vapor infiltration technique
Modification；
(4) using at least one of chemical vapor infiltration technique and organic precursor impregnating cracking technology to gained nanometer silicon carbide
Line precast body carries out densification, obtains the high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite.
2. preparation method according to claim 1, which is characterized in that in step (1), the diameter of the silicon carbide nanometer line
It is 0.02~0.6 μm, length is 10~200 μm, and draw ratio is greater than 100, and the dispersing agent is selected from dodecyl sodium sulfate, isopropyl
At least one of alcohol, polyvinylpyrrolidone, butyl glycol ether；Preferably, the matter of the dispersing agent and silicon carbide nanometer line
Amount is than being 1:(0.1~30).
3. preparation method according to claim 1 or 2, which is characterized in that in step (1), the solvent be dehydrated alcohol,
At least one of deionized water, acetone and formaldehyde.
4. preparation method according to any one of claim 1-3, which is characterized in that in step (1), the side of the dispersion
Formula is ultrasonic treatment；The power of the ultrasonic treatment is 10~1000W, and the time is 0.1~2 hour.
5. preparation method described in any one of -4 according to claim 1, which is characterized in that in step (2), using filter machine into
Row, the running parameter of the suction filtration machine are 20~60L/min, and power is 160~500W；Preferably, after suction filtration, 0.1
Compression processing is carried out under the pressure of~10MPa.
6. preparation method according to any one of claims 1-5, which is characterized in that in step (2), the silicon carbide is received
Rice noodles precast body with a thickness of the mm of 0.5 mm~10.
7. preparation method according to claim 1 to 6, which is characterized in that in step (3), the modifying interface
Gained boundary layer is at least one of pyrolysis carbon boundary layer, silicon carbide interface layer, boron nitride boundary layer, silicon nitride interface layer；
5~100 nm of thickness of the boundary layer.
8. preparation method described in any one of -7 according to claim 1, which is characterized in that in step (4), the chemical gaseous phase
The parameter of osmosis process includes: using methyl trichlorosilane MTS as 100~400sccm of presoma, and hydrogen is carrier gas and dilution
Gas velocity is 10~90 sccm；Temperature is 1000~1100 DEG C, and pressure is 1.5~6KPa, and the time is 300~1000 minutes.
9. preparation method according to claim 1 to 8, which is characterized in that in step (4), the presoma leaching
The parameter of stain cracking technology includes: that organic precursor type is selected from least one of Polycarbosilane, polysiloxanes, polysilazane；
Cracking temperature is 700~1100 DEG C.
10. a kind of high-volume fractional silicon-carbide nano wire of preparation method preparation according to claim 1 to 9
Enhance ceramic matric composite, which is characterized in that in the high-volume fractional silicon-carbide nano wire enhancing ceramic matric composite
The volume fraction of silicon carbide nanometer line is 10~37vol%.
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| CN111205100A (en) * | 2020-03-02 | 2020-05-29 | 西北工业大学 | Method for in-situ growth of silicon carbide nanowire by non-catalytic precursor impregnation pyrolysis method |
| CN111662091A (en) * | 2020-06-15 | 2020-09-15 | 中国科学院上海硅酸盐研究所 | Short carbon fiber reinforced Csf/SiC ceramic matrix composite material and preparation method thereof |
| CN118185525A (en) * | 2024-05-16 | 2024-06-14 | 江苏斯瑞达材料技术股份有限公司 | High-shear-strength thermosetting pressure-sensitive adhesive and preparation method thereof |
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