CN106810287A - A kind of method for improving big thickness fiber reinforcement quartz composite density - Google Patents
A kind of method for improving big thickness fiber reinforcement quartz composite density Download PDFInfo
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- CN106810287A CN106810287A CN201510856952.8A CN201510856952A CN106810287A CN 106810287 A CN106810287 A CN 106810287A CN 201510856952 A CN201510856952 A CN 201510856952A CN 106810287 A CN106810287 A CN 106810287A
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- fiber reinforcement
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- reinforcement quartz
- density
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Abstract
The present invention proposes a kind of method for improving big thickness fiber reinforcement quartz composite density, it is primary substrate using the early stage experience fiber reinforcement quartz composite that repeatedly prepared by dipping-sintering process, with the freshly prepared multiple impregnation drying of orthosilicic acid solution, finally it is sintered.Present invention process is simple, to synthesis device low, the low cost of requirement, is conducive to being lifted the performance of fiber reinforcement quartz composite, it is adaptable to the preparation of the quartzy composite of large-size fiber enhancing.
Description
Technical field
The present invention relates to a kind of method for improving big thickness fiber reinforcement quartz composite density, belong to fiber increasing
Strong technical field of composite materials.
Background technology
Traditional quartz-ceramics breaking strain is relatively low, and when being acted on by external force, material damage often shows as fragility
Fracture, it is difficult to the use requirement of structural member under competent harsh conditions.In order to overcome its inherent limitation, state in recent years
Inside and outside researcher is prepared for the quartzy composite of multiple fiber enhancing using the toughening effect of fiber, extensively should
For high temperature wave transparent and the field such as heat-insulated.
The main preparation methods of current fiber reinforcement quartz composite are：Repeatedly impregnated using silicon dioxide gel
Fiber preform, is subsequently dried and sinters.The fiber preform of (more than 40mm) larger for thickness is more
After secondary dipping, silicon dioxide gel is difficult to enter the hole of composite inner, and the density refractory of composite is carrying
It is high.Fiber reinforcement quartz composite materials property can not meet the requirement to high-strength performance for increasingly improving.
The content of the invention
It is an object of the invention to overcome prior art not enough, there is provided a kind of process is simple, short preparation period,
The big thickness fiber reinforcement quartz composite density of raising of low cost, the side so as to significantly improve its mechanical property
Method.
Technical solution of the invention：A kind of side for improving big thickness fiber reinforcement quartz composite density
Method, is realized by following steps：
The first step, prepares fresh orthosilicic acid solution
A1.1, by industrial-grade sodium silicate solution distilled water diluting to 5wt%~8wt%；Water glass after such as diluting
Glass solution concentration is too high, and the orthosilicic acid solution of preparation has viscosity to become big phenomenon at room temperature in 6 hours, after being unfavorable for
Continuous dipping；If concentration is relatively low, gaining effect is reached, it is necessary to more dipping times, extension production week
Phase.Water glass solution control is optimal in the range of 5wt%~8wt% after dilution, within the range, by multiple
After dipping, the influence of the concentration of water glass solution to final densities is smaller.
Water glass solution after A1.2, dilution, by strong-acid type cation exchange column ion, by pH test paper
The pH value of efflux is tracked, efflux of the pH value less than 4 is collected, fresh orthosilicic acid solution is obtained；
Strong-acid type cation exchange column uses benzene sulfonic acid type cationic ion-exchange resin, molten using preceding use 1M hydrochloric acid
It is 5 or so with distilled water flushing to efflux pH after liquid activation.
Fresh orthosilicic acid solution is carried out at ambient temperature, and orthosilicic acid solution now-making-now-using, strong-acid type are wanted in preparation
Cation exchange column is cleaned after being finished with clear water.
Second step, fiber reinforcement quartz composite is placed in the orthosilicic acid solution of first step preparation and is impregnated
8~12h；
This step dipping makes the small-molecule substance in orthosilicic acid solution enter into fiber reinforcement quartz composite,
Due to the present invention use orthosilicic acid solution solid content it is low, viscosity is small, the size of small molecule in below 5nm,
In being easier to enter into and being difficult to carry highdensity fiber reinforcement quartz composite.The former silicon that the present invention is used
Acid solution solid content is very low, and 8~12h of dipping is that can reach preferable dipping effect.
This step use composite, for experience repeatedly dipping-sintering after, due to silicon dioxide gel be difficult into
Enter the hole of composite inner so that fiber reinforcement quartz composite of the density refractory to improve.The present invention for
The performance improvement effect of the fiber reinforcement quartz composite of thickness larger (fiber preform is more than 40mm) is most
For notable.
3rd step, by through the fiber reinforcement quartz composite high temperature drying of second step dipping orthosilicic acid solution；
Drying temperature is 300 ± 5 DEG C, and drying time is not less than 1h, by drying steps, immerses composite
In silicic acid experience dehydration so that it will not the dissolution from composite in follow-up impregnation steps.
4th step, repeats the first step to the 3rd step several times, high temperature sintering.
The number of times of repeated impregnations is generally 3~4 times, and number of times is more again, to the improvement effect of density and performance
Fruit influences little.
High-sintering process is consistent with the quartzy composite of fibrillation enhancing, is known in the art technology.
The present invention by use the orthosilicic acid solution containing small molecule to through multiple impregnation sintering, density refractory to increase
Fiber reinforcement quartz composite impregnated, the small molecule in orthosilicic acid solution enter into fiber reinforcement quartz
In composite, then through drying and sintering, although the fiber reinforcement quartz composite after processed by the invention is total
Volume density increase only 1.5~2%, but the performance of composite has and is obviously improved, compressive strength lifting
More than 50%, shear strength lifting more than 15%.The compression performance of composite is closely bound up with its matrix density.
Although total body density only lifts 1.5~2% after density, after fiber is subtracted out to the contribution of total body density, matrix
Density lifts more than 6% compared with the density of matrix before non-density.Therefore the defect of matrix can be preferable after density
Reparation, so as to lift the compression performance of material.From the point of view of the fracture port of material, fibre bundle inside is fine before density
Dimension is combined loosely with matrix, and fibre bundle internal fiber is combined more closely with matrix after density, therefore uses silicic acid
After small molecule density, fiber is strengthened with the interface interaction of matrix, and the cutting performance of material is lifted.
Present invention beneficial effect compared with prior art：
(1) present invention experiences multiple silicon dioxide gel dipping-burning using special orthosilicic acid solution impregnation early stage
The fiber reinforcement quartz composite of knot, sintered rear composite density lifting 1.5~2%, composite
Compressive strength lifting more than 50%, shear strength lifting more than 15%；
(2) present invention process is simple, to synthesis device low, the low cost of requirement, is conducive to lifting fiber reinforcement
The performance of quartzy composite, it is adaptable to the preparation of the quartzy composite of large-size fiber enhancing.
(3) raw material of the present invention are industrial-grade sodium silicate, and ion exchange resin can be reused, valency
Lattice are cheap, are suitable to commercial Application.
Figure of description
Fig. 1 is preparation flow figure of the present invention.
Specific embodiment
The method of the present invention using the early stage experience fiber that repeatedly prepared by dipping-sintering process as shown in figure 1, increased
Strong quartz composite is primary substrate, with the freshly prepared multiple impregnation drying of orthosilicic acid solution, is finally carried out
Sintering.
Below in conjunction with accompanying drawing and instantiation, the present invention is described in detail.
Embodiment 1
The needling structure quartz fibre enhancing quartz for experiencing multiple silicon dioxide gel dipping-sintering using early stage is multiple
Used as primary substrate, density is 1.50g/cm to condensation material (80mm is thick)3, compressive strength 44MPa, shearing is by force
Degree 5.0MPa.
Prepare as shown in figure 1, being realized by following steps：
1st, benzene sulfonic acid type strong-acid cation-exchange resin is activated with 8 times of 1M hydrochloric acid solutions of resin volume, and
With 8 times of resin volume clear water drip washing exchange columns.
2nd, after industrial-grade sodium silicate solution being diluted into 5wt% concentration, ion exchange is carried out by ion exchange column,
Collect efflux of the pH value less than 4.
3rd, will be positioned over as the composite of primary substrate in the orthosilicic acid solution of collection and impregnated 10 hours.
4th, composite is taken out, is drained after drying 1h at 300 DEG C.
5th, repeat step 1~4 four time.
6. will be sintered at 800 DEG C of composite.
The density for using the quartzy composite of needling structure quartz fibre enhancing after the inventive method is 1.53
g/cm3, increasing by 2%, compressive strength 81MPa increases by 84%, shear strength 6.0MPa, increases by 20%.
Embodiment 2
The three-dimensional orthohormbic structure quartz fibre for experiencing multiple silicon dioxide gel dipping-sintering using early stage strengthens stone
Used as primary substrate, density is 1.60g/cm to English composite (83mm is thick)3, compressive strength 100MPa,
Shear strength 11.0MPa.
Using with the step process of embodiment 1, using after the inventive method three-dimensional orthohormbic structure quartz fibre enhancing stone
The density of English composite is 1.63g/cm3, increase by 1.7%, compressive strength 160MPa, increase by 60%,
Shear strength 13.5MPa, increases by 22%.
Embodiment 3
The 2.5D structures quartz fibre for experiencing multiple silicon dioxide gel dipping-sintering using early stage strengthens quartz
Composite (70mm is thick) is used as primary substrate, density 1.61g/cm3, compressive strength 90MPa, shearing
Intensity 12MPa.
Using with the step process of embodiment 1, using after the inventive method 2.5D structures quartz fibre enhancing quartz
The density of composite is 1.64g/cm3, increase by 2%, compressive strength 140MPa, increase by 55%.Shearing is strong
Degree 15MPa, increases by 25%.
Embodiment 4
The three-dimensional orthohormbic structure mullite fiber for experiencing multiple silicon dioxide gel dipping-sintering using early stage strengthens
Quartzy composite (75mm is thick) is used as primary substrate, density 2.1g/cm3, compressive strength 150MPa cuts
Shearing stress 15MPa.
Using with the step process of embodiment 1, strengthened using three-dimensional orthohormbic structure mullite fiber after the inventive method
The 2.13g/cm of quartzy composite3, increase by 1.5%, compressive strength 230MPa, increase by 53%.Shearing is strong
Degree 17.8MPa, increases by 18.6%.
Unspecified part of the present invention is known to the skilled person technology.
Claims (4)
1. a kind of method for improving big thickness fiber reinforcement quartz composite density, it is characterised in that including with
Lower step：
The first step, prepares fresh orthosilicic acid solution,
A1.1, industrial-grade sodium silicate solution is diluted to 5wt%~8wt%；
Water glass solution after A1.2, dilution, by after strong-acid type cation exchange column ion exchange, collecting
Efflux of the pH value less than 4, is obtained fresh orthosilicic acid solution；
Second step, fiber reinforcement quartz composite is placed in the orthosilicic acid solution of first step preparation and is impregnated
8~12h；
3rd step, by through the fiber reinforcement quartz composite high temperature drying of second step dipping orthosilicic acid solution；
4th step, repeats the first step to the 3rd step several times, high temperature sintering.
2. a kind of side for improving big thickness fiber reinforcement quartz composite density according to claim 1
Method, it is characterised in that：Drying temperature is 300 ± 5 DEG C in the second step, and drying time is no less than 1h.
3. a kind of side for improving big thickness fiber reinforcement quartz composite density according to claim 1
Method, it is characterised in that：The number of times repeated in 4th step is 3~4 times.
4. a kind of side for improving big thickness fiber reinforcement quartz composite density according to claim 1
Method, it is characterised in that：After fiber reinforcement quartz composite is through repeatedly dipping-sintering in the second step,
Composite of the density refractory to improve.
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| CN201510856952.8A CN106810287B (en) | 2015-11-30 | 2015-11-30 | Method for improving density of large-thickness fiber reinforced quartz composite material |
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| CN201510856952.8A CN106810287B (en) | 2015-11-30 | 2015-11-30 | Method for improving density of large-thickness fiber reinforced quartz composite material |
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| CN106810287A true CN106810287A (en) | 2017-06-09 |
| CN106810287B CN106810287B (en) | 2020-06-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735110A (en) * | 2019-01-15 | 2019-05-10 | 哈尔滨工业大学 | A kind of modified phenolic-organic siliconresin composite material and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591192A (en) * | 2008-11-21 | 2009-12-02 | 中材高新材料股份有限公司 | The Enhancement Method of fibre-quartz ceramic-base composite material |
| CN102311122A (en) * | 2011-08-03 | 2012-01-11 | 南通海迅天恒纳米科技有限公司 | Silicic acid purification method |
| CN104446580A (en) * | 2014-12-16 | 2015-03-25 | 中国人民解放军国防科学技术大学 | Method for preparing continuous fiber cloth reinforced silica ceramic-based composite material |
| CN104909791A (en) * | 2015-05-27 | 2015-09-16 | 山东工业陶瓷研究设计院有限公司 | Quartz fiber reinforced silica ceramic composite material densification method |
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2015
- 2015-11-30 CN CN201510856952.8A patent/CN106810287B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591192A (en) * | 2008-11-21 | 2009-12-02 | 中材高新材料股份有限公司 | The Enhancement Method of fibre-quartz ceramic-base composite material |
| CN102311122A (en) * | 2011-08-03 | 2012-01-11 | 南通海迅天恒纳米科技有限公司 | Silicic acid purification method |
| CN104446580A (en) * | 2014-12-16 | 2015-03-25 | 中国人民解放军国防科学技术大学 | Method for preparing continuous fiber cloth reinforced silica ceramic-based composite material |
| CN104909791A (en) * | 2015-05-27 | 2015-09-16 | 山东工业陶瓷研究设计院有限公司 | Quartz fiber reinforced silica ceramic composite material densification method |
Non-Patent Citations (1)
| Title |
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| YONG LIU等: "Mechanical behavior of 2.5D (shallow bend-joint) and 3D orthogonal quartzf/silica composites by silicasol-infiltration-sintering", 《MATERIALS SCIENCE AND ENGINEERING A》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735110A (en) * | 2019-01-15 | 2019-05-10 | 哈尔滨工业大学 | A kind of modified phenolic-organic siliconresin composite material and preparation method |
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