CN109881362A - A kind of silicon carbide fiber needle felt and preparation method thereof - Google Patents
A kind of silicon carbide fiber needle felt and preparation method thereof Download PDFInfo
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- CN109881362A CN109881362A CN201711264849.XA CN201711264849A CN109881362A CN 109881362 A CN109881362 A CN 109881362A CN 201711264849 A CN201711264849 A CN 201711264849A CN 109881362 A CN109881362 A CN 109881362A
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- silicon carbide
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Abstract
The present invention relates to a kind of silicon carbide fiber needle felt and preparation method thereof, which is prescinded shredding, air-flow combing by Polycarbosilane fusion-free fibre, is made at tire, needle thorn, high temperature inorganic.The silicon carbide fiber needle felt that the present invention prepares is on the basis of former silicon carbide entirety felt, single layer needle thorn and lamination needle thorn are carried out along Z-direction, while greatly improving Z-direction mechanical property, X/Y to mechanical property and thermophysical property also more non-Nomex increases significantly, expand its application range significantly, especially high temperature filtration, high-temperature catalytic, prepare the fields such as SiC/SiC composite material wide application prospect.
Description
Technical field
The present invention relates to a kind of anti-oxidant, lightweights, the silicon carbide fiber needle felt of good mechanical performance, more particularly to one kind
Silicon carbide fiber needle felt and preparation method thereof.
Background technique
Silicon carbide felt has many advantages, such as that low-density, wear-resisting, porosity is high, large specific surface area, corrosion-resistant, high temperature resistant, is boat
The important support material of the fields lightweight development trend such as empty space flight, precision instrument, communications and transportation, environmental protection, and its easy processing
Molding characteristic has important role to preparation SiCf/SiC composite material.
According to being consulted reference materials, Yu Yuxi, Chen Yong have invented " a kind of preparation method of flexibility polycrystal carborundum micrometer fibers felt "
(CN103320966A), Yu Yuxi, Chen Yong, Lai Delin, Yang Lu have invented a kind of " system of hydrophobic oil suction silicon carbide ceramic fiber felt
Preparation Method " (CN102877218A).But since silicon carbide fibre brittleness is big, while functional application, it is also desirable to the greatest extent may be used
Its mechanical property can be improved, therefore, it is fine to seek the high silicon carbide of a kind of thermophysical property stabilization, good mechanical performance, cost performance
Dimension Nomex and preparation method thereof is that expansion SiCf/SiC composite material, environmentally friendly high-temperature-resistant filtering material and emergency braking are heat-resisting wear-resistant
The important bottleneck of material application.
Summary of the invention
For the needs for meeting functional composite material, high temperature filter material and the heat-resisting wear-resistant application of emergency braking, mesh of the invention
The preparation method for being intended to provide a kind of silicon carbide fiber needle felt, wear-resistant using silicon carbide fibre, anti-oxidant, resistivity can
The features such as tune, large specific surface area, realizes the rapid of SiCf/SiC composite material (such as various high performance brake disks) preparation, thus
Cost is reduced, the production cycle is shortened.
In order to solve the above technical problem, a kind of preparation method of silicon carbide fiber needle felt of the invention,
(1) it prescinds shredding: Polycarbosilane fusion-free fibre is uniformly cut into the staple fiber of 5~8cm of length, cutter rotating velocity
120r/min~300r/min；
(2) air-flow combs, at tire: the fusion-free fibre prescinded reaches licker-in by feeding roller, in the high speed machine of licker-in
Be thrown under effect in the high-speed flow of blower generation, moved together with air-flow, air-flow eventually by lace curtaining, and fiber at
At tire on lace curtaining, net spee 10m/min~30m/min, main cylinder diameter 1020mm, revolving speed 150rpm~200rpm out；
(3) needle pierces: single layer mold being laid on input and output material panel, shakeouts, be aligned, starts needing machine, opens pre-needling master
Axis drives discharge velocity into after waiting it to stablize, reciprocal needle pierces 1 back and forth, then spreads a mold, declines bottom plate heights 2mm, repeats
Above step obtains 2 layers of silicon carbide Nomex, and so on, the multilayer silicon carbide Nomex of design thickness can be obtained；
(4) high temperature inorganic: the non-fusible felt of polycarbosilane fiber that needle has pierced is put into atmosphere protection cabinet-type electric furnace, and
It is sintered in inert gas shielding atmosphere or in a vacuum, 1h~5h is kept the temperature after being preheating to 550 DEG C, then be warming up to 900 DEG C
~1300 DEG C of heat preservation 0.5h~10h, then Temperature fall, can be obtained silicon carbide fiber needle felt；The Polycarbosilane is poly-
One of carbon silane, polyaluminocarbosilane, poly- titanium carbon silane, polyborazine, poly- yttrium carbon silane, poly- carborane and Polyferrocarbosilane
Or it is several.
The infusible Si -- H bond extent of reaction 65%~80% of Polycarbosilane used in preferred steps (1).
Preferred steps (2) go out net spee 10m/min~30m/min, and main cylinder diameter 1020mm, revolving speed 150rpm~
200rpm。
Pre-needling spindle frequency 10Hz~20Hz in preferred steps (3), input and output material rate frequency 10Hz,.
It is preferred that 1300 DEG C of sintering final temperature of the sintering step (4), sintering time 1h, inert gas (including nitrogen, argon
Gas etc.) protection, inert gas flow is 5L/min~20L/min, 1h~5h is kept the temperature after being preheating to 550 DEG C, then be warming up to 900 DEG C
~1300 DEG C of heat preservation 0.5h~10h, then Temperature fall, can be obtained silicon carbide fiber needle felt；The Polycarbosilane is poly-
One of carbon silane, polyaluminocarbosilane, poly- titanium carbon silane, polyborazine, poly- yttrium carbon silane, poly- carborane and Polyferrocarbosilane
Or it is several.
Silicon carbide fibre felt made from method is stated as above-mentioned, density 0.15g/cm3~0.30g/cm3,8 μm of fibre diameter~
15 μm, grammes per square metre 50g/m2~150g/m2, thickness 1mm~30mm, fiber volume fraction 10%~20%, tensile strength >=0.3N/
50mm, 5~10MPa of interlaminar shear strength.
From the point of view of the structure feature of silicon carbide fibre felt of the present invention, the felt early period using the Si -- H bond extent of reaction 65%~
80% Polycarbosilane fusion-free fibre, felt body fibre diameter is uniform, is combed, with air-flow at tire by prescinding, so that felt surface density
Uniformly, then through needle it pierces, increases felt body bed shear intensity and X-Y biaxial mechanical capability.
In order to obtain the uniform and stable silicon carbide fiber needle felt body of performance, wherein there is certain parameter to each technique
Limit, to realize high performance handicraft product, specifically: 1. the infusible Si -- H bond extent of reaction of Polycarbosilane 65%~
80%；2. opener goes out net spee 10m/min~30m/min, main cylinder diameter 1020mm, revolving speed 150rpm~200rpm；③
Pre-needling spindle frequency 10Hz~20Hz, input and output material rate frequency 10Hz；4. 1300 DEG C of final temperature, sintering time 1h of sintering, lazy
Property gas (including nitrogen, argon gas etc.) protect, inert gas flow be 5L/min~20L/min.
The present invention is for preparing with the beneficial effect for the SiCf/SiC composite material that grain catcher (DPF) is representative, letter
Singly it is described below:
(1) raw material uses Polycarbosilane fusion-free fibre, and flexibility is stronger, makes felt body obtained more evenly, it is easier to add
Work at various complicated shapes SiCf/SiC composite material；
(2) it is pierced by needle, the planar structure of felt can be switched to three-dimensional structure, overall porosity is high, and micropore increases, is distributed
It is even, aperture is small and deploys troops on garrison duty layer by layer, the effect of the filtration mechanisms such as screening, inertia, retention, diffusion can be given full play to, therefore trap high, resistance
Power is small, permeability is good, can achieve the effect that energy-saving and emission-reduction.
(3) it is pierced by needle, makes felt body that there is some strength in Z-direction, anti-shear ability is strengthened.
Compared with existing disclosed patent, advantage is the present invention:
(1) present invention is non-fusible as a raw material for production using Polycarbosilane, on the one hand can be by adjusting Polycarbosilane point
Minor structure produces different cultivars continuous carbofrax fibre fusion-free fibre, obtains the SiC fibrofelt for adulterating different element, expands
On the other hand the kind of felt also provides a kind of novel silicon carbide products for being applicable in different application to the processing of composite material,
Application field is expanded；
(2) present invention is non-fusible as a raw material for production using Polycarbosilane, and volatility is molten during avoiding electrostatic spinning
Pollution of the agent to environment, does not generate harm to human health；
(3) present invention has carried out needle thorn to felt body, so that felt body is had three-dimensional structure, and have certain shear resistant in Z-direction
Can, meanwhile, overall porosity improves, and trapping is high, resistance is small, good permeability, and filter effect is good.
Detailed description of the invention
Fig. 1 is the implementation process diagram of present invention preparation process by taking embodiment 1 as an example；
Fig. 2 is silicon carbide Nomex main ingredient XRD curve graph of the present invention by taking embodiment 1 as an example；
Fig. 3 is silicon carbide Nomex institutional framework schematic diagram of the present invention by taking embodiment 1 as an example；
Fig. 4 is silicon carbide Nomex sterogram obtained in the embodiment of the present invention 1.
Specific embodiment
Embodiment 1:
A kind of preparation method of silicon carbide fiber needle felt, Step 1: prescinding shredding: choosing the Si -- H bond extent of reaction 65%
~70% fusion-free fibre is uniformly cut into the staple fiber of 5~8cm of length, cutter rotating velocity 150r/min；Step 2: air-flow is combed
Manage, at tire: the fusion-free fibre prescinded reaches licker-in by feeding roller, is thrown into blower under the high speed machine effect of licker-in and produces
In raw high-speed flow, moved together with air-flow, air-flow eventually by lace curtaining, and fiber at lace curtaining at tire, network speed out
Spend 10m/min, main cylinder diameter 1020mm, revolving speed 160rpm；Step 3: needle pierces: single layer mold is laid in input and output material panel
On, it shakeouing, is aligned, start needing machine, open pre-needling main shaft, drive discharge velocity after waiting it to stablize into, reciprocal needle pierces 1 back and forth,
Then a mold is spread, bottom plate heights 2mm is declined, above step is repeated, obtains 2 layers of silicon carbide Nomex, pierce spindle frequency in advance
15Hz, loading frequency 10Hz；Step 3: high temperature inorganic: the non-fusible felt of polycarbosilane fiber that needle has pierced being put into atmosphere and is protected
It protects in cabinet-type electric furnace, and is sintered in nitrogen protection atmosphere, nitrogen flow rate 10L/min is kept the temperature after being first preheating to 550 DEG C
1h, then 1100 DEG C are risen to 1 DEG C/min, 2h is kept the temperature, then Temperature fall, can be obtained silicon carbide fiber needle felt.
Embodiment 2:
The present embodiment is with embodiment 1 the difference lies in that the Si -- H bond of Polycarbosilane fusion-free fibre reacts in step 1
Degree is 75%~80%, and piercing spindle frequency in step 3 in advance is 10Hz, and silicon carbide carpet veneer number is 3.
Embodiment 3:
The present embodiment and embodiment 1 the difference lies in that in step 4 550 DEG C~1100 DEG C of heating rate be 0.5 DEG C/
Min, keeps the temperature 1h, then Temperature fall by 1300 DEG C of final temperature.
Comparative example 1: the silicon carbide fiber needle felt that four step rule of the present invention is prepared, with other publication performances
Comparison is shown in Table 1.
Specific comparison result is referring to table 1.
It is characteristic of the invention that the innovation achievement of technical solution.Compared with existing silicon carbide felt Preparation Method, present invention wound
The three-dimension process that needing machine carries out felt is introduced to the property made, makes SiC Nomex obtained that there is some strength in Z-direction, in the direction X-Y
Upper have certain anti-shear performance, meanwhile, also substantially increase the overall porosity of felt, micropore increases, is evenly distributed, aperture is small and
It deploys troops on garrison duty layer by layer, the effect of the filtration mechanisms such as screening, inertia, retention, diffusion, therefore the high, resistance as filter material trapping can be given full play to
It is small, permeability is good, can achieve the effect that energy-saving and emission-reduction.The present invention is for preparing having the beneficial effect that for high-temperature-resistant filtering material:
(1) use Polycarbosilane pre-oxidized fibers for raw material, flexibility is good, easy to process；(2) using prescind, shredding, air-flow are combed into
The technology of tire can further improve the uniformity in felt face；(3) needling treatment is used, makes silicon carbide felt that there is centainly anti-shearing
Property, while felt overall porosity is improved, cycle-index can be effectively reduced, compounding period is reduced；(4) in high temperature filtration field,
Needled carbon SiClx felt micropore increases, is evenly distributed, aperture is small and deploys troops on garrison duty layer by layer, can give full play to screening, inertia, retention, diffusion
Equal filtration mechanisms effect, therefore trapping is high, resistance is small, permeability is good, can achieve the effect that energy-saving and emission-reduction.
The result of the present invention of table 1 and comparing result
Above-mentioned multiple embodiments are relatively intended to be easy to understand preparation method of the present invention properties of product on technical arrangement plan
Trend.So that those skilled in the art can understand the innovation essence for grasping technical solution of the present invention, not only in function or production
Moral character can go up the embodiment for proposing to limit.So in addition to the implementation, the present invention can also have other polynary embodiments.
All technical solutions formed using equivalent substitution or equivalent transformation, are fallen within the scope of protection required by the present invention.
Claims (2)
1. a kind of preparation method of silicon carbide fiber needle felt, it is characterised in that:
(1) it prescinds shredding: Polycarbosilane fusion-free fibre is uniformly cut into the staple fiber of 5~8cm of length, cutter rotating velocity 120-
300r/min；(2) air-flow combs, at tire: the fusion-free fibre prescinded reaches licker-in by feeding roller, in the high speed machine of licker-in
Be thrown under effect in the high-speed flow of blower generation, moved together with air-flow, air-flow eventually by lace curtaining, and fiber at
At tire on lace curtaining, net spee 10-30m/min, main cylinder diameter 1020mm, revolving speed 150-200rpm out；(3) needle pierces: by single layer
Mold is laid on input and output material panel, is shakeout, is aligned, and is started needing machine, is opened pre-needling main shaft, drives discharging speed into after it is stablized
Rate, reciprocal needle pierce 1 back and forth, then spread a mold, decline bottom plate heights 2mm, repeat above step, obtain 2 layers of silicon carbide
Nomex, and so on, obtain the multilayer silicon carbide Nomex of design thickness；(4) high temperature inorganic: the poly- carbon silicon that needle has been pierced
The non-fusible felt of alkane fiber is put into atmosphere protection cabinet-type electric furnace, and is sintered in inert gas shielding atmosphere, inert gas
Flow be 5-20L/min, 1-5h is kept the temperature after being preheating to 550 DEG C, then be warming up to 1300 DEG C of heat preservation 1h, then Temperature fall, i.e.,
Obtain silicon carbide fiber needle felt；
The density 0.15-0.30g/cm3 of the silicon carbide fiber needle felt is 8-15 μm of fibre diameter, grammes per square metre 50-150g/m2, thick
Spend 1-30mm, fiber volume fraction 10%-20%, tensile strength >=0.3N/50mm, interlaminar shear strength 5-10MPa；Step
(3) the pre-needling spindle frequency 10-20Hz in, input and output material rate frequency 10Hz.
2. the method as described in claim 1, it is characterised in that: the infusible Si -- H bond of Polycarbosilane used in step (1)
The extent of reaction is 50%-95%.
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| CN201711264849.XA CN109881362A (en) | 2017-12-05 | 2017-12-05 | A kind of silicon carbide fiber needle felt and preparation method thereof |
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| CN201711264849.XA CN109881362A (en) | 2017-12-05 | 2017-12-05 | A kind of silicon carbide fiber needle felt and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114836898A (en) * | 2022-06-02 | 2022-08-02 | 江苏天鸟高新技术股份有限公司 | Needled carbon fiber net felt and preparation method and application thereof |
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2017
- 2017-12-05 CN CN201711264849.XA patent/CN109881362A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114836898A (en) * | 2022-06-02 | 2022-08-02 | 江苏天鸟高新技术股份有限公司 | Needled carbon fiber net felt and preparation method and application thereof |
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Application publication date: 20190614 |