CN107620208A - Nitride fiber impregnating compound and coating method thereof - Google Patents
Nitride fiber impregnating compound and coating method thereof Download PDFInfo
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- CN107620208A CN107620208A CN201710887481.6A CN201710887481A CN107620208A CN 107620208 A CN107620208 A CN 107620208A CN 201710887481 A CN201710887481 A CN 201710887481A CN 107620208 A CN107620208 A CN 107620208A
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Abstract
The invention discloses an impregnating compound for continuous nitride ceramic fibers and a coating method thereof. By the two-step method, firstly, silica sol is coated and then polyurethane is coated, on one hand, the problem of large adsorption capacity in fiber sizing is solved by filling the defects and the nano pores on the fiber surface through the silica sol with the nano size, on the other hand, the surface chemical structure of the fiber is changed by forming a film on the fiber surface through the silica sol, the discreteness of the bundle fiber strength can be reduced, the subsequent weaving is facilitated, and the appearance, the flexibility and the fuzz phenomenon of the continuous fiber can be effectively improved.
Description
Technical field
The present invention relates to the size of continuous ceramic fiber and its painting method, more particularly, to a kind of nitride fiber
Size and its painting method.
Background technology
Pyroceram fibre material have high temperature resistant, high intensity, high-modulus, creep resistant, anti-yaw damper, anti-oxidant, wave transparent,
Inhaling performance, the high temperature resistant nitride ceramic fibres such as ripple has high temperature resistant wave-permeable performance, and it is in Near Space Flying Vehicles, space travel
Play an important roll in terms of the Aero-Space such as device, strategic arms.
Nitride ceramic fibre is mainly made by preceramic organosilicon polymer body conversion method, and its principle is that synthesis contains target
Ceramic element forms, and with the high precursor polymer of good spinnability, ceramic yield, is then prepared into by spinning
Organic fiber, then thermosetting fibre of its crosslinking as space network, final high temperature cracking, high temperature are made by chemical reaction
Ceramic treatment obtains ceramic fibre.
At present, nitride ceramic fibre subject matter present in mass production and practical application has：(1) prepared
Synnema is more open in journey, and has more lousiness and fracture of wire, has had a strong impact on the continuous production of fiber；(2) synnema intensity
It is relatively low, and as the increase of synnema length, intensity are decreased obviously；(3) fiber surface defect is more, compound working out, being molded
Serious fibre damage is easily caused in the actual applications such as material.
These problems largely limit the application of nitride fiber, and size is prepared and woven in continuous fiber should
Had a very important role in, also referred to as sizing agent, cementing agent etc..Handled by suitable starching, can be effectively
Synnema is collapsed, fiber surface defect is made up, so as to improve the synnema intensity of fiber and practical performance.Particularly increase in continuous fiber
Strong polymer matrix composites field, both at home and abroad carbon fiber, glass fibre, basalt fibre size in terms of carried out it is wide
Important technical foundation has been established in general research, performance boost and extensive use to above-mentioned fiber.
Such as in terms of the size of carbon fiber, formula, cross-linking reagent, painting method and method of testing of size etc.
Substantial amounts of, fruitful work has been carried out, may refer to following document：The role of sizing resins,
coupling agents and their blends on the formation of the interphase in glass
Fiber composites.Polymer, 1998 (39), 2607-2613；Surface and wettability property
analysis of CCF300 carbon fibers with different sizing or without
sizing.Materials and Design 2011(32):941–946；The research of carbon fiber cementing agent, fiber composite material
Material, 2001 (3)：3-4；The research glass fibres of carbon fiber size content assay method, 2014 (3):17-21.Relevant carbon is fine
Dimension quetsch is also disclosed patent, such as application number CN201621290872.7, CN201520973857.1 patent.
Such as in terms of glass fibre, both at home and abroad from size preparing process, drawing process and formula to stitchability,
Composite material aspect of performance has carried out system research, and bibliography is as follows：Sizing agent is to glass fiber yarn stitchability
Influence research, Donghua University's journal (natural science edition), 2004 (32):96-99；Size technology and glass fibre and glass
Relations I/II between steel part, glass fibre, 2003 (3-4)：21-24；Environmental resistance and
mechanical performance of alkali-resistant glass fibers with surface sizings,
Journal of Non-Crystalline Solids, 2003 (325):230–241.Particularly develop and be adapted to different bases
The size of body or purposes, refer to Patents (application number CN201710165873.1, CN201611115209.8,
CN201610963045.8 etc.).American wheat the research and development of door company and can manufacture the glass fiber infiltration agents of multi items, Dutch Supreme Being Si
Graceful group starts to produce glass fiber infiltration agent in Shanghai.
Effect of the size to continuous ceramic fiber mainly has two aspects：When reduce finished fiber packaging, transport,
The abrasion of the processes such as braiding, second, improving the woven performance of continuous fiber, it is adapted to various weaving manners.Therefore, ceramics are fine
Dimension has its special requirement to size, is totally different from the sizes such as carbon fiber, glass fibre, basalt fibre.
There is enriched carbon layer in silicon carbide fibre surface, in general solid resin can be used as the component of size, and nitrogenize
There is more nitride and oxide, and nano level hole in the top layer of silica fibre, then cause to collect using usual size
Beam tension, poor, the easy brittle failure of synnema flexibility.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, the surface characteristic of foundation nitride fiber,
The bi-component size and its substep painting method of a kind of nitride fiber are provided.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of size of nitride fiber, includes Ludox collecting agent and polyurethane sizing agent；
The Ludox collecting agent is to strengthen synthetic fibers convergence, improving its fiber number and intensity, and in spinning oil
In added surfactant, it is preferred that made of size is dispersed in absolute ethyl alcohol in below 50nm silica sol particle, silicon
Concentration range of the colloidal sol in absolute ethyl alcohol is 0.1~1wt%；
Preferably, dispersing mode of the Ludox in absolute ethyl alcohol is ultrasonic disperse；
The Ludox is selected as collecting agent, is due to the dispersiveness and good penetrability of Ludox, easily penetrates synnema
Inside, while Ludox water white transparency, dielectric constant is low, is not significantly affected by the outward appearance and dielectric properties of nitride fiber；
The polyurethane sizing agent, is the polymer substance of one or more kinds of energy film forming, and its effect is just formed into arranging
Slurry is padded on fabric, is allowed to be attached to fabric face, and forming epithelium after drying wraps up fabric face, is put down so as to assign fabric
Sliding, abundant, plentiful, stiffening feel；
It is preferred that aqueous polyurethane, is dispersed in water by soluble polyurethane and is made, concentration range of the polyurethane in water
For 0.5~2wt%；
It is because the covering property of polyurethane is good, cured, and avoids " heat as sizing agent to select aqueous polyurethane
It is viscous cold short " the shortcomings that, fiber folding is wear-resisting after coating, is adaptive to complicated braiding and machine braiding；
Preferably, dispersing mode of the soluble polyurethane in water is ultrasonic disperse；
Preferably, soluble polyurethane is scattered in deionized water.
Above-mentioned selected each material is chemical pure, purity>95%, tenor is less than 100ppm, is purchased by market
Buy approach acquisition.
The present invention also provides a kind of painting method of nitride fiber size, comprises the following steps：
S1, Ludox is configured, load storage tank；Aqueous polyurethane is configured, loads stock tank；
In below 50nm, the silica sol particle that concentration range is 0.1~1wt% divides the Ludox collecting agent preferred size
It is dispersed in absolute ethyl alcohol；
Preferably, dispersing mode of the Ludox in absolute ethyl alcohol is ultrasonic disperse；
The aqueous polyurethane, is dispersed in water by soluble polyurethane and is made, preferably concentration of the polyurethane in water
Scope is 0.5~2wt%；
Preferably, dispersing mode of the soluble polyurethane in water is ultrasonic disperse；
Preferably, soluble polyurethane is scattered in deionized water；
S2, using Ludox as collecting agent, nitride fiber synnema is passed through into impregnation hole, then dried by drying tunnel I, ensured
The uniformity of continuous coating procedure, drying tunnel I temperature range is 80~120 DEG C；
Further, to make fresh size constantly flow into impregnation hole, change in concentration is avoided to coating the influence of effect,
Two impregnation hole positions are symmetrically distributed in front and rear sides with 120 degree of angles, are in fiber wire straight line in cylindrical shape stainless steel outer wall
On；
Preferably, a diameter of 4-7mm in impregnation hole, preferably 5mm；
The nitride fiber synnema that S3 obtains through step S2, using aqueous polyurethane as sizing agent, using steeping vat impregnation,
After wire drawing impregnation, dried by drying tunnel II, that is, complete sizing agent coating, the temperature range of drying tunnel II is 150~250 DEG C；
Further, time efficiency and tensile strength of fiber factor are considered, it is preferred that in step S2 and step S3,
The drawing speed scope of silicon nitride fiber is 0.5~2m/min.
The present invention first applies Ludox by two-step method and applies polyurethane again, on the one hand fills up fine by the Ludox of nano-scale
Dimension table planar defect and nanoaperture, solve the problems, such as that adsorbance is big during fiber starching, on the other hand by Ludox in fiber
Surface filming, fiber surface chemical constitution is changed, the problem of boundling tension is really up to the mark when avoiding directly using aqueous phase size.
Present invention could apply to the infiltration of nitride fiber and coating, as silicon nitride fiber, boron nitride fiber, SiBN are fine
Dimension etc., the size and two component substep coating methods prepared using the present invention, has advantages below：
(1) the problem of avoiding fiber surface defect and excessive nanoaperture absorption size, has exempted from aqueous polyurethane
The problem of boundling tension is really up to the mark when directly coating；
(2) Ludox is first applied using this method and applies polyurethane again, the former is that ethanol solution the latter is the aqueous solution, and coating is equal
Even, fibre bundle is neatly clear after coating, improves lousiness phenomenon, is effectively improved outward appearance, the pliability of continuous fiber, also reduces
The discreteness of synnema intensity, advantageously reduce fiber accumulating, weave the damage of process.
Brief description of the drawings
Fig. 1 is that silicon nitride fiber synnema coats photo before size；
Fig. 2 is that silicon nitride fiber synnema coats (a step dip-coating) photo after Ludox；
Fig. 3 is that silicon nitride fiber synnema coats (two step dip-coatings) photo after Ludox and polyurethane；
Fig. 4 is two-step coating unit schematic diagram；
Fig. 5 is impregnation pore structure schematic diagram；
Fig. 6 is silica sol particle transmission electron microscope photo.
Embodiment
Below in conjunction with Figure of description and embodiment, the invention will be further described.The present invention is not restricted to following
Embodiment.
Fig. 4 is two-step coating unit schematic diagram, and nitride fiber beam is pulled out by spinning-drawing machine, and Ludox is coated through impregnation hole
Collecting agent, then dried by drying tunnel I, using aqueous polyurethane as sizing agent, after stock tank (steeping vat) impregnation, wire drawing impregnation,
Dried by drying tunnel II, that is, complete sizing agent coating.
Fig. 5 is impregnation pore structure schematic diagram, and as can be seen from the figure two impregnation hole positions are in cylindrical shape stainless steel outer wall, with
120 degree of angles are symmetrically distributed in front and rear sides, are on fiber wire straight line；Therefore fresh size constantly flows into impregnation hole,
Avoid influence of the change in concentration to coating effect, a diameter of 5mm in impregnation hole.
Embodiment 1
1st, sol particles of the size in below 50nm is stirred in absolute ethyl alcohol, it is 1wt% Ludox to be configured to concentration
Collecting agent；
2nd, soluble polyurethane is stirred in water and aqueous polyurethane is made, be configured to the polyurethane that concentration is 2wt%
The aqueous solution；
3rd, the coating processes step condition of above-mentioned size：
(1) Ludox and aqueous polyurethane configured step 1 and step 2 is respectively charged into storage tank and stock tank；
(2) using Ludox as collecting agent, silicon nitride fiber synnema is passed through into impregnation hole, dried by drying tunnel I, ensured continuous
The uniformity of coating procedure, drying tunnel I temperature are：120℃；
(3) the nitride fiber synnema obtained through step (2), using aqueous polyurethane as sizing agent, using impregnation drill traverse
Glue, after wire drawing impregnation, dried by drying tunnel II, that is, complete sizing agent coating, the temperature of drying tunnel II is：250℃；
(4) in step (2) and step (3), the drawing speed of silicon nitride fiber is 2m/min.
Embodiment 2
1st, by size below 50nm sol particles by ultrasonic disperse in absolute ethyl alcohol, being configured to concentration is
0.7wt% Ludox collecting agents.
2nd, aqueous polyurethane is made in soluble polyurethane ultrasonic disperse in deionized water, being configured to concentration is
1.2wt% aqueous polyurethane.
3rd, the coating processes step condition of above-mentioned size is with embodiment 1, and wherein nitride fiber is with 1.5m/min speed
Spend wire drawing.
Embodiment 3
1st, by size below 50nm sol particles by ultrasonic disperse in absolute ethyl alcohol, being configured to concentration is
0.1wt% Ludox collecting agents.
2nd, aqueous polyurethane is made in soluble polyurethane ultrasonic disperse in deionized water, being configured to concentration is
0.5wt% aqueous polyurethane.
3rd, the coating processes step condition of above-mentioned size：
(1) Ludox and aqueous polyurethane configured step 1 and step 2 is respectively charged into storage tank and stock tank；
(2) using Ludox as collecting agent, silicon nitride fiber synnema is passed through into impregnation hole, dried by drying tunnel I, ensured continuous
The uniformity of coating procedure, drying tunnel I temperature are：80℃；
(3) the nitride fiber synnema obtained through step (2), using aqueous polyurethane as sizing agent, using impregnation drill traverse
Glue, after wire drawing impregnation, dried by drying tunnel II, that is, complete sizing agent coating, the temperature of drying tunnel II is：150℃；
(4) in step (2) and step (3), the drawing speed of silicon nitride fiber is 0.5m/min.
The channel that above-mentioned raw material are bought by market obtains.
Embodiment 4
1st, by size below 50nm sol particles by ultrasonic disperse in absolute ethyl alcohol, being configured to concentration is
0.3wt% Ludox collecting agents.
2nd, aqueous polyurethane is made in soluble polyurethane ultrasonic disperse in deionized water, being configured to concentration is
1wt% aqueous polyurethane.
3rd, the coating processes step condition of above-mentioned size：
(1) Ludox and aqueous polyurethane configured step 1 and step 2 is respectively charged into storage tank and stock tank；
(2) using Ludox as collecting agent, boron nitride fiber synnema is passed through into impregnation hole, dried by drying tunnel I, ensured continuous
The uniformity of coating procedure, drying tunnel I temperature are：100℃；
(3) the boron nitride fiber synnema obtained through step (2), using aqueous polyurethane as sizing agent, using impregnation drill traverse
Glue, after wire drawing impregnation, dried by drying tunnel II, that is, complete sizing agent coating, the temperature of drying tunnel II is：200℃；
(4) in step (2) and step (3), the drawing speed of boron nitride fiber is 1m/min.
Filament tow intensity and its coefficient of dispersion are as shown in the table before and after embodiment 1,2,3,4 coats, and test foundation：GBT
3362-2005 carbon fiber tensile property of multi-filament test methods.
By, it is apparent that after implementing the present invention, synnema intensity has lifting, and coefficient of dispersion has obvious drop in table
Low, Figure of description 1~3 is it will be obvious that coat front and rear Contrast on effect.
Claims (7)
1. the size of nitride fiber, it is characterised in that：Comprising Ludox collecting agent and polyurethane sizing agent, the Ludox
Collecting agent is that size is dispersed in absolute ethyl alcohol in below 50nm silica sol particle and is made, and Ludox is dense in absolute ethyl alcohol
Degree scope is 0.1~1wt%；The polyurethane sizing agent, is aqueous polyurethane, and system is dispersed in water by soluble polyurethane
Into concentration range of the polyurethane in water is 0.5~2wt%.
2. the size of nitride fiber according to claim 1, it is characterised in that point of the Ludox in absolute ethyl alcohol
The mode of dissipating is ultrasonic disperse；Soluble polyurethane ultrasonic disperse is in deionized water.
3. a kind of size painting method of nitride fiber as claimed in claim 1 or 2, comprises the following steps：
(1) Ludox is configured, loads storage tank；Aqueous polyurethane is configured, loads stock tank；
The Ludox collecting agent is that size is dispersed in absolute ethyl alcohol in below 50nm silica sol particle and is made, and Ludox exists
Concentration range in absolute ethyl alcohol is 0.1~1wt%；The polyurethane sizing agent, is aqueous polyurethane, by water-soluble poly ammonia
Ester, which is dispersed in water, to be made, and concentration range of the polyurethane in water is 0.5~2wt%
(2) using Ludox as collecting agent, nitride fiber synnema is passed through into impregnation hole, dried by drying tunnel I, drying tunnel I temperature
Scope is：80~120 DEG C；
(3) the nitride fiber synnema obtained through step (2), using aqueous polyurethane as sizing agent, using steeping vat impregnation, draw
After silk impregnation, dried by drying tunnel II, that is, complete sizing agent coating, the temperature range of drying tunnel II is：150~250 DEG C.
4. the size painting method of nitride fiber according to claim 3, it is characterised in that the drawing of silicon nitride fiber
Silk velocity interval is 0.5~2m/min.
5. the size painting method of nitride fiber according to claim 3, it is characterised in that in the step (2),
Two impregnation holes are set, and the two is located at cylindrical shape stainless steel outer wall, is symmetrically distributed in front and rear sides with 120 degree of angles, is in fibre
Tie up on wire straight line.
6. the size painting method of the nitride fiber described in claim 5, it is characterised in that a diameter of 4- in impregnation hole
7mm。
7. the size painting method of the nitride fiber described in claim 6, it is characterised in that a diameter of 5mm in impregnation hole.
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| CN109234833A (en) * | 2018-08-17 | 2019-01-18 | 东华大学 | With the Porous hollow polyurethane fiber of fine and close clad structure and its preparation and application |
| CN109853225A (en) * | 2018-12-24 | 2019-06-07 | 吉祥三宝高科纺织有限公司 | A kind of postfinishing process of noctilucence water repellent polyester fabric |
| CN109853238A (en) * | 2019-03-06 | 2019-06-07 | 福建立亚新材有限公司 | A kind of silicon carbide or silicon nitride fiber sizing agent and its preparation method and application |
| CN110305464A (en) * | 2019-07-05 | 2019-10-08 | 天津工业大学 | A kind of continuous nitride silica fibre reinforced resin base composite wire and preparation method thereof |
| CN113957578A (en) * | 2020-07-21 | 2022-01-21 | 上海赛立特安全用品股份有限公司 | Inorganic non-metal fiber reinforced monofilament, coating wire, preparation method and application thereof |
| CN115321824A (en) * | 2022-09-09 | 2022-11-11 | 清远忠信世纪电子材料有限公司 | Low-dielectric glass fiber capable of being formed at low temperature |
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| CN109234833A (en) * | 2018-08-17 | 2019-01-18 | 东华大学 | With the Porous hollow polyurethane fiber of fine and close clad structure and its preparation and application |
| CN109234833B (en) * | 2018-08-17 | 2021-07-20 | 东华大学 | Porous hollow polyurethane fiber with compact coating structure and preparation and application thereof |
| CN109853225A (en) * | 2018-12-24 | 2019-06-07 | 吉祥三宝高科纺织有限公司 | A kind of postfinishing process of noctilucence water repellent polyester fabric |
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| CN110305464A (en) * | 2019-07-05 | 2019-10-08 | 天津工业大学 | A kind of continuous nitride silica fibre reinforced resin base composite wire and preparation method thereof |
| CN113957578A (en) * | 2020-07-21 | 2022-01-21 | 上海赛立特安全用品股份有限公司 | Inorganic non-metal fiber reinforced monofilament, coating wire, preparation method and application thereof |
| CN115321824A (en) * | 2022-09-09 | 2022-11-11 | 清远忠信世纪电子材料有限公司 | Low-dielectric glass fiber capable of being formed at low temperature |
| CN115321824B (en) * | 2022-09-09 | 2023-11-17 | 清远忠信世纪电子材料有限公司 | Low-dielectric glass fiber capable of being molded at low temperature |
| CN115807341A (en) * | 2022-12-20 | 2023-03-17 | 武汉纺织大学 | Preparation method and application of UV (ultraviolet) photocuring environment-friendly nitride fiber sizing agent |
| CN115807341B (en) * | 2022-12-20 | 2024-06-07 | 武汉纺织大学 | Preparation method and application of UV (ultraviolet) light-cured environment-friendly nitride fiber sizing agent |
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