CN101660225B - SiC fiber and fabric and preparation method thereof - Google Patents
SiC fiber and fabric and preparation method thereof Download PDFInfo
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- CN101660225B CN101660225B CN 200910093089 CN200910093089A CN101660225B CN 101660225 B CN101660225 B CN 101660225B CN 200910093089 CN200910093089 CN 200910093089 CN 200910093089 A CN200910093089 A CN 200910093089A CN 101660225 B CN101660225 B CN 101660225B
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Abstract
The invention relates to an SiC fiber or fabric and a preparation method thereof and belongs to the technical field of composite materials. By taking natural vegetable fiber or the fabric thereof as the template, the SiC fiber or fabric is obtained through impregnation in silica sol and high-temperature calcination. The preparation method includes the following steps: impregnating silica sol in natural vegetable fiber or fabric thereof carbonized or pretreated by organic expanding agent by adopting a vacuum or vacuum pressure way or the vacuum or vacuum pressure way simultaneously combined with a concentration gradient diffusion way to achieve 75-166 percent of weight gain rate, and then under protective gas, calcining the obtained material at the temperature of 1400-1600 DEG C for 1.5-4h, and converting the obtained material into complete SiC fiber or fabric. The SiC fiber or fabric not only completely maintains the structure of natural vegetable fiber, but also is characterized by high strength, high-temperature thermostability and resistance to acid and alkali corrosion of SiC material. Meanwhile, the SiC fiber or fabric is also characterized by vertical and horizontal performance uniformity of fabrics and very suitably used as the enhanced phase of in-plane equidirectional composite material of high performance.
Description
Technical field
The present invention relates to a kind of SiC fiber or fabric and preparation method thereof, belong to technical field of composite materials, being specifically related to a kind of is the SiC fiber of template or fabric and preparation method thereof with natural plant fibre or its fabric.
Background technology
The SiC fiber has good mechanical performance, characteristic such as high temperature resistant, corrosion-resistant, anti-oxidant and ageing-resistant, be widely used in high-tech sectors such as atomic energy, weapons, Aero-Space, be the good reinforcing material of preparation high performance polymer base, Metal Substrate and ceramic matric composite, have important effect for the development of China's advanced composite material industry.
The SiC fibre composites is raw material or precursor with artificial organic compound or artificial fibre mainly at present, and its preparation method has chemical vapour deposition technique, carbon fiber conversion method, presoma conversion method and micropowders method.Wherein, research is chemical vapour deposition technique the most widely at present.U.S. Pat 2004013876 has been reported a kind of precursor conversion method of the SiC of manufacturing fiber.Japan Patent JP5321037 has reported that with artificial charcoal fiber be presoma, under the pressure and high temperature of 10-500mmHg, makes itself and Si or SiO
2Reaction generates the method for SiC fiber.Said method has all used the raw material or the precursor of artificial organic compound or artificial fibre, at aspects such as preparation method, properties of product and environmental protection weak point is arranged.For example, preparation method's complexity of presoma conversion method, properties of product are not easy control, and cost is higher.Mercury vapor causes operator's mercurial poisoning at work easily in the chemical vapour deposition technique, and causes environmental pollution.Therefore seek a kind of new, stable performance, good SiC fiber and cost is low, very necessary to environment facies to close friend's SiC fiber preparation method.
Natural plant fibre is a kind of complete eco-friendly biological material, its fabric has complete structure of natural vegetable fiber and the fabric characteristics of performance homogeneous in length and breadth, if can with the SiC fiber composite with characteristics such as high strength, high high-temp stability and acid-alkali-corrosive-resistings, will be suitable as very much in the high-performance face wild phase of composite in the same way.
Based on above-mentioned consideration, the present invention has proposed a kind of SiC fiber or fabric and preparation method thereof according to the characteristics and the performance of natural plant fibre and SiC fiber.The present invention for improve added value of product, enlarge its range of application, aspects such as protection environment have important and practical meanings.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have high strength, high high-temp stability, acid-alkali-corrosive-resisting, and fabric the SiC fiber of the characteristics of performance homogeneous or fabric and to the preparation method of environment facies to the close friend in length and breadth.
SiC fiber of the present invention or fabric are to be template with natural plant fibre or its fabric, impregnate with high-temperature calcination by silicon dioxide gel to obtain.
Described natural plant fibre is selected from the flax fibre that comprises ramee and in the natural bamboo fibres one or more, preferred homogeneous fiber.
Described natural plant fibre fabric is to be made into by being selected from the flax fibre that comprises ramee and in the natural bamboo fibres one or more, preferably is made into the homogeneous fiber.This natural plant fibre fabric can be made certain breadth as required.
This SiC fiber or fabric are template with natural plant fibre or its fabric; adopt vacuum or vacuum pressed mode, when preferably adopting vacuum or vacuum pressed mode also in conjunction with the concentration gradient diffusion way; silicon dioxide gel is impregnated in pretreated natural plant fibre or its fabric; reach the rate of body weight gain of 75%-166%, then under protective gas between 1400-1600 ℃ calcining obtained in 1.5-4 hour.
Described preliminary treatment is that natural plant fibre or its fabric are carried out the charing processing under protective gas, promptly under protective gas, the charing under 700 ℃ of-1100 ℃ of high temperature with natural plant fibre or its fabric preferably 900 ℃ of charings, is made natural plants charcoal fiber or fabric; Perhaps with organic expander to natural plant fibre or its fabric immersion treatment 2-8 hour, to the abundant swollen of its cell membrane, so that next step impregnates.Wherein said organic expander includes but not limited to ethylene glycol, dimethyl sulfoxide (DMSO) and/or formamide.
Silicon dioxide gel of the present invention can adopt commercially available product or own product.During self-control, can adopt that to contain the silanol oxide be that presoma prepares silicon dioxide gel, wherein contain the silanol oxide and can select the various silanol oxides that contain for use, comprise that ethyl orthosilicate, MTES and other contain the silanol oxide.Preferable methyl triethoxysilane, more preferably ethyl orthosilicate.
Described silicon dioxide gel is formed by containing silanol oxide, alcohol organic solvent and water, and wherein alcohol organic solvent includes but not limited to ethanol and/or isopropyl alcohol.When adopting vacuum or vacuum pressed mode to impregnate, the mol ratio that adopts silanol oxide, alcohol organic solvent and water is 1: 4: 4 to 1: 4: 8 a silicon dioxide gel, and preferred mol ratio is 1: 4: 4, and preferred mol ratio is 1: 4: 8; As also in conjunction with the concentration gradient diffusion way, then concentration silicon dioxide gel is from small to large impregnated successively, the mol ratio of its each component can be 1: 4: 1 to 1: 4: 32, and the silicon dioxide gel that makes as silanol oxide, alcohol organic solvent and the water that can adopt mol ratio to be respectively 1: 4: 32,1: 4: 16,1: 4: 8,1: 4: 4 and 1: 4: 2 successively impregnates.Described concentration gradient diffusion way is by concentration order from small to large silicon dioxide gel to be impregnated in pretreated natural plant fibre or its fabric successively.The rate of body weight gain that impregnates back fiber or fabric should be between 75%-166%.Rate of body weight gain is high more, and the content of SiC is high more in SiC fiber that obtains or the fabric, but cost increases.
Described high-temperature calcination is that fiber or the fabric after will impregnating under protective gas calcined 1.5-4 hour between 1400-1600 ℃.
Protective gas includes but not limited to nitrogen and inert gas, preferred helium, more preferably nitrogen.
The present invention also provides described SiC fiber or process for making such fabric.
SiC fiber of the present invention or process for making such fabric; be to be template with natural plant fibre or its fabric; adopt vacuum or vacuum pressed mode, when preferably adopting vacuum or vacuum pressed mode also in conjunction with the concentration gradient diffusion way; silicon dioxide gel is impregnated in pretreated natural plant fibre or its fabric; high-temperature calcination under protective gas makes it change into complete SiC fiber or fabric.
Described natural plant fibre is selected from the flax fibre that comprises ramee and in the natural bamboo fibres one or more, preferred homogeneous fiber.
Described natural plant fibre fabric is to be made into by being selected from the flax fibre that comprises ramee and in the natural bamboo fibres one or more, preferably is made into the homogeneous fiber.This natural plant fibre fabric can be made certain breadth as required.
Described preliminary treatment is that natural plant fibre or its fabric are carried out the charing processing under protective gas, promptly under protective gas, the charing under 700 ℃ of-1100 ℃ of high temperature with natural plant fibre or its fabric preferably 900 ℃ of charings, is made natural plants charcoal fiber or fabric; Perhaps with organic expander to natural plant fibre or its fabric immersion treatment 2-8 hour, to the abundant swollen of its cell membrane, so that next step impregnates.Wherein said organic expander includes but not limited to ethylene glycol, dimethyl sulfoxide (DMSO) and/or formamide.
Silicon dioxide gel of the present invention can adopt commercially available product or own product.During self-control, can adopt that to contain the silanol oxide be that presoma prepares silicon dioxide gel, wherein contain the silanol oxide and can select the various silanol oxides that contain for use, comprise that ethyl orthosilicate, MTES and other contain the silanol oxide.Preferable methyl triethoxysilane, more preferably ethyl orthosilicate.
Described silicon dioxide gel is formed by containing silanol oxide, alcohol organic solvent and water, and wherein alcohol organic solvent includes but not limited to ethanol and/or isopropyl alcohol.When adopting vacuum or vacuum pressed mode to impregnate, the mol ratio that adopts silanol oxide, alcohol organic solvent and water is 1: 4: 4 to 1: 4: 8 a silicon dioxide gel, and preferred mol ratio is 1: 4: 4, and preferred mol ratio is 1: 4: 8; As also in conjunction with the concentration gradient diffusion way, then concentration silicon dioxide gel is from small to large impregnated successively, the mol ratio of its each component can be 1: 4: 1 to 1: 4: 32, and the silicon dioxide gel that makes as silanol oxide, alcohol organic solvent and the water that can adopt mol ratio to be respectively 1: 4: 32,1: 4: 16,1: 4: 8,1: 4: 4 and 1: 4: 2 successively impregnates.Described concentration gradient diffusion way is by concentration order from small to large silicon dioxide gel to be impregnated in pretreated natural plant fibre or its fabric successively.The rate of body weight gain that impregnates back fiber or fabric should be between 75%-166%.Rate of body weight gain is high more, and the content of SiC is high more in SiC fiber that obtains or the fabric, but cost increases.
Described high-temperature calcination is that fiber or the fabric after will impregnating under protective gas calcined 1.5-4 hour between 1400-1600 ℃.
Protective gas includes but not limited to nitrogen and inert gas, preferred helium, more preferably nitrogen.
Key problem in technology of the present invention is: (1) is template with natural plant fibre or its fabric; (2) natural plant fibre or its fabric are carried out the charing preliminary treatment, perhaps adopt the mode of organic expander swollen that natural plant fibre or its fabric are carried out preliminary treatment, to improve the load capacity of silicon dioxide gel; Also silicon dioxide gel is impregnated in pretreated natural plant fibre or its fabric when (3) preferably adopting vacuum or vacuum pressed mode, guaranteed that the q.s silicon dioxide gel is evenly distributed in the cell membrane of string or fabric in conjunction with the concentration gradient from small to large mode of impregnating.
SiC fiber of the present invention or fabric have not only intactly kept the structure of natural plant fibre or its fabric, the characteristics that also have SiC material high strength, high high-temp stability and acid-alkali-corrosive-resisting, this SiC fabric also has the fabric characteristics of performance homogeneous in length and breadth simultaneously, be a kind of low-density high-strength biomimesis SiC fiber or textile article, be suitable as very much in the high-performance face wild phase of composite in the same way; Its preparation method is simple and convenient, compares low, the environmental friendliness of cost with existing SiC fiber or process for making such fabric.
The specific embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment 1 SiC fiber and preparation method thereof
1. SiC fiber that should example: with the ramee is template.
2. SiC fiber preparation method that should example:
(1) under nitrogen protection with above-mentioned ramee 900 ℃ of charings 2 hours, make ramie charcoal fiber.Heating schedule is: being 1 ℃/min between 0 to 350 ℃, is 5 ℃/min between 350 ℃ to 900 ℃.
(2) preparation is the silicon dioxide gel of presoma with the ethyl orthosilicate, and ethyl orthosilicate: ethanol: the mol ratio of water was respectively 1: 4: 32,1: 4: 16,1: 4: 8,1: 4: 4 and 1: 4: 2.The hydrochloric acid that with concentration is 1mol/L is adjusted to 2.5 with the pH value of colloidal sol, stirs the water white transparency silicon dioxide gel of promptly making variable concentrations behind the 30min.
(3) adopt the vacuum pressed mode silicon dioxide gel to be impregnated in the ramie charcoal fiber successively by concentration order from small to large.Promptly at first ramie charcoal fiber is put into reactor, use vavuum pump to be evacuated to vacuum state in the reactor, keep vacuum state after 1 hour, in the silicon dioxide gel sucting reaction still that concentration is minimum, immediately inflated with nitrogen in the reactor (industrial nitrogen) is forced into the reactor internal gas pressure and reaches 0.6MPa, keep release after 1.5 hours, the ramie charcoal fiber after will impregnating takes out oven dry, and (60 ℃ of bakings are after 1 hour, 120 ℃ were dried by the fire 3 hours) be placed in the drier and cool off, claim that its over dry is heavy and calculate rate of body weight gain.Other concentration colloidal sols are repeated said process, and the rate of body weight gain of the ramie charcoal fiber after impregnating at last is 125%.
(4) the ramie charcoal fiber after will impregnating places the programme-control high temperature furnace, speed with 3 ℃/min is warming up to 500 ℃ of insulation 30min, speed with 8 ℃/min is warming up to 1450 ℃ of insulations 2.5 hours, speed with 5 ℃/min is cooled to 200 ℃ then, and obtaining with the ramee is the SiC fiber of template.
Embodiment 2 SiC fabrics and preparation method thereof
1. SiC fabric that should example: with the natural bamboo fibres fabric is template.Preparing breadth as required is the natural bamboo fibres fabric of 20mm * 150mm.
2. the preparation method of SiC fabric that should example:
(1) preparation is the silicon dioxide gel of presoma with the MTES, and MTES: isopropyl alcohol: the mol ratio of water was respectively 1: 4: 32,1: 4: 16,1: 4: 8,1: 4: 4 and 1: 4: 2.The hydrochloric acid that with concentration is 1mol/L is adjusted to 2 with the pH value of colloidal sol, stirs the water white transparency silicon dioxide gel of promptly making variable concentrations behind the 60min.
(2) the natural bamboo fibres fabric was soaked in ethylene glycol 6 hours.Adopt the vacuum pressed mode silicon dioxide gel to be impregnated in the natural bamboo fibres fabric successively by concentration order from small to large.Promptly at first the natural bamboo fibres fabric is put into reactor, use vavuum pump to be evacuated to vacuum state in the reactor, keep vacuum state after 1 hour, in the silicon dioxide gel sucting reaction still that concentration is minimum, immediately inflated with nitrogen in the reactor (industrial nitrogen) is forced into the reactor internal gas pressure and reaches 0.6MPa, keep high pressure conditions release after 1.5 hours, natural bamboo fibres fabric after will impregnating takes out oven dry, and (60 ℃ of bakings are after 1 hour, 120 ℃ were dried by the fire 3 hours) be placed in the drier and cool off, claim that its over dry is heavy and calculate rate of body weight gain.Other concentration colloidal sols are repeated said process, and the rate of body weight gain of the natural bamboo fibres fabric after impregnating at last is 135%.
(3) the natural bamboo fibres fabric after will impregnating places the programme-control high temperature furnace, speed with 1 ℃/min is warming up to 350 ℃ of insulation 30min, speed with 5 ℃/min is warming up to 1500 ℃ of insulations 2 hours, speed with 5 ℃/min is cooled to 200 ℃ then, and obtaining with the natural bamboo fibres fabric is the SiC fabric of template.
Claims (9)
1. SiC fiber or fabric, it is characterized in that, with natural plant fibre or its fabric is template, by adopting vacuum or vacuum pressed mode silicon dioxide gel is impregnated in pretreated natural plant fibre or its fabric, reach the rate of body weight gain of 75%-166%, then under protective gas between 1400-1600 ℃ calcining obtained in 1.5-4 hour; Described silicon dioxide gel is the presoma preparation to contain the silanol oxide.
2. SiC fiber as claimed in claim 1 or fabric is characterized in that, described natural plant fibre is selected from the flax fibre that comprises ramee and in the natural bamboo fibres one or more.
3. SiC fiber as claimed in claim 2 or fabric is characterized in that, described natural plant fibre is the homogeneous fiber.
4. SiC fiber as claimed in claim 1 or fabric; it is characterized in that; described preliminary treatment is that the charing under protective gas of described natural plant fibre or its fabric is handled, perhaps with organic expander to described natural plant fibre or its fabric immersion treatment 2-8 hour.
5. SiC fiber as claimed in claim 4 or fabric is characterized in that described organic expander comprises ethylene glycol, dimethyl sulfoxide (DMSO) and formamide.
6. SiC fiber as claimed in claim 1 or fabric is characterized in that, the described silanol oxide that contains is ethyl orthosilicate or MTES.
7. SiC fiber as claimed in claim 1 or fabric, it is characterized in that, when adopting vacuum or vacuum pressed mode also in conjunction with the concentration gradient diffusion way, described silicon dioxide gel is impregnated in described pretreated natural plant fibre or its fabric, and wherein said concentration gradient diffusion way is by concentration order from small to large described silicon dioxide gel to be impregnated successively.
8. a claim 1-7 each described SiC fiber or process for making such fabric, it is characterized in that, may further comprise the steps: (1) adopts vacuum or vacuum pressed mode that silicon dioxide gel is impregnated in pretreated natural plant fibre or its fabric, reaches the rate of body weight gain of 75%-166%; (2) under protective gas, between 1400-1600 ℃, calcined 1.5-4 hour, make it change into complete SiC fiber or fabric.
9. SiC fiber as claimed in claim 8 or process for making such fabric, it is characterized in that, when described step (1) adopts vacuum or vacuum pressed mode also in conjunction with the concentration gradient diffusion way, described silicon dioxide gel is impregnated in described pretreated natural plant fibre or its fabric by concentration order from small to large, reach the rate of body weight gain of 75%-166%.
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