CN106810287B - Method for improving density of large-thickness fiber reinforced quartz composite material - Google Patents
Method for improving density of large-thickness fiber reinforced quartz composite material Download PDFInfo
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Abstract
The invention provides a method for improving the density of a large-thickness fiber reinforced quartz composite material, which is characterized in that the fiber reinforced quartz composite material prepared by a plurality of dipping-sintering processes in the early stage is used as an original base material, a freshly prepared orthosilicic acid solution is used for dipping and drying for a plurality of times, and finally sintering is carried out. The method has the advantages of simple process, low requirement on synthesis equipment and low cost, is favorable for improving the performance of the fiber reinforced quartz composite material, and is suitable for preparing large-size fiber reinforced quartz composite materials.
Description
Technical Field
The invention relates to a method for improving the density of a large-thickness fiber-reinforced quartz composite material, and belongs to the technical field of fiber-reinforced composite materials.
Background
The traditional quartz ceramic has low fracture strain, and when the traditional quartz ceramic is acted by external force, the material damage is often expressed as brittle fracture and is difficult to meet the use requirement of a structural part under severe conditions. In order to overcome the inherent limitation, researchers at home and abroad in recent years use the toughening effect of the fiber to prepare various fiber reinforced quartz composite materials which are widely applied to the fields of high-temperature wave transmission, heat insulation and the like.
The main preparation method of the fiber reinforced quartz composite material at present comprises the following steps: the fiber preform is impregnated with the silica sol a plurality of times, followed by drying and sintering. For a fiber preform having a large thickness (more than 40mm), after many times of impregnation, the silica sol hardly enters pores inside the composite material, and the density of the composite material hardly increases. The mechanical properties of the fiber reinforced quartz composite material cannot meet the increasingly improved requirements for high strength properties.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for improving the density of a large-thickness fiber reinforced quartz composite material and obviously improving the mechanical property of the large-thickness fiber reinforced quartz composite material, which has the advantages of simple process, short preparation period and low cost.
The technical solution of the invention is as follows: a method for improving the density of a large-thickness fiber reinforced quartz composite material is realized by the following steps:
in a first step, a fresh orthosilicic acid solution is prepared
A1.1, diluting industrial water glass solution to 5 wt% -8 wt% by using distilled water; if the concentration of the diluted water glass solution is too high, the viscosity of the prepared orthosilicic acid solution is increased within 6 hours at room temperature, which is not beneficial to subsequent impregnation; if the concentration is lower, more times of impregnation are needed to achieve the weight increasing effect, and the production period is prolonged. The diluted water glass solution is optimally controlled within the range of 5 wt% -8 wt%, and the concentration of the water glass solution has small influence on the final density after multiple times of dipping.
A1.2, passing the diluted water glass solution through strong acid type cation exchange column ions, tracking the pH value of the effluent through a pH test paper, and collecting the effluent with the pH value less than 4 to prepare a fresh orthosilicic acid solution;
the strong acid cation exchange column adopts benzenesulfonic acid type cation exchange resin, and is activated by 1M hydrochloric acid solution before use, and then is washed by distilled water until the pH of effluent is about 5.
Fresh orthosilicic acid solution is carried out at room temperature, the prepared orthosilicic acid solution is used for preparing, and the strong acid type cation exchange column is cleaned by clear water after being used up.
Secondly, placing the fiber reinforced quartz composite material in the orthosilicic acid solution prepared in the first step for dipping for 8-12 hours;
the impregnation in the step enables small molecular substances in the orthosilicic acid solution to enter the fiber reinforced quartz composite material, and the orthosilicic acid solution adopted by the invention has low solid content and small viscosity, and the size of small molecules is below 5nm, so that the small molecular substances can easily enter the fiber reinforced quartz composite material with the density difficult to improve. The solid content of the orthosilicic acid solution adopted by the invention is very low, and a good impregnation effect can be achieved by impregnating for 8-12 hours.
The composite material adopted in the step is a fiber reinforced quartz composite material which is difficult to improve in density due to the fact that silica sol is difficult to enter pores in the composite material after multiple times of dipping and sintering. The invention has the most remarkable performance improvement effect on the fiber reinforced quartz composite material with larger thickness (the fiber preform exceeds 40 mm).
Thirdly, drying the fiber reinforced quartz composite material dipped with the orthosilicic acid solution in the second step at high temperature;
the drying temperature is 300 +/-5 ℃, the drying time is not less than 1h, and the silicic acid immersed in the composite material is subjected to a dehydration step through the drying step so that the silicic acid is not dissolved out of the composite material in the subsequent immersion step.
And fourthly, repeating the first step to the third step for a plurality of times, and sintering at high temperature.
The repeated dipping times are generally 3-4 times, and the times are more, so that the improvement effect on the density and the performance is not greatly influenced.
The high temperature sintering process is consistent with fibril reinforced quartz composites and is well known in the art.
According to the invention, the fiber reinforced quartz composite material which is subjected to multiple dipping and sintering and has difficultly increased density is dipped by adopting the orthosilicic acid solution containing small molecules, the small molecules in the orthosilicic acid solution enter the fiber reinforced quartz composite material, and then the fiber reinforced quartz composite material is dried and sintered, although the overall density of the fiber reinforced quartz composite material treated by the method is increased by only 1.5-2%, the performance of the composite material is remarkably improved, the compression strength is improved by more than 50%, and the shear strength is improved by more than 15%. The compression properties of a composite material are closely related to its matrix density. Although the total density after densification is only improved by 1.5-2%, after deducting the contribution of the fibers to the total density, the density of the matrix is improved by more than 6% compared with the density of the matrix before densification. Therefore, the defects of the densified matrix can be better repaired, and the compression performance of the material is improved. From the fracture opening of the material, the fibers in the fiber bundle before densification are loosely combined with the matrix, and the fibers in the fiber bundle after densification are tightly combined with the matrix, so that after the densification by adopting the silicic acid micromolecules, the interface action of the fibers and the matrix is enhanced, and the shearing performance of the material is improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, a fiber reinforced quartz composite material which is subjected to multiple times of silica sol impregnation-sintering in the early stage of impregnation by using a special orthosilicic acid solution is adopted, the density of the sintered composite material is improved by 1.5-2%, the compression strength of the composite material is improved by more than 50%, and the shear strength is improved by more than 15%;
(2) the method has the advantages of simple process, low requirement on synthesis equipment and low cost, is favorable for improving the performance of the fiber reinforced quartz composite material, and is suitable for preparing large-size fiber reinforced quartz composite materials.
(3) The raw material of the invention is industrial water glass, the ion exchange resin can be reused, the price is low, and the invention is suitable for industrial application.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The method of the invention is shown in figure 1, and uses the fiber reinforced quartz composite material which is prepared by a plurality of dipping-sintering processes in the early stage as an original base material, uses a freshly prepared orthosilicic acid solution for a plurality of dipping drying, and finally carries out sintering.
The invention is described in detail below with reference to the figures and specific examples.
Example 1
Adopting a needle-punched structure quartz fiber reinforced quartz composite material (80mm thick) which is subjected to silica sol impregnation-sintering for multiple times at the early stage as an original base material, wherein the density is 1.50g/cm3Compressive strength 44MPa, shear strength 5.0 MPa.
The preparation is as shown in figure 1 and is realized by the following steps:
1. the benzenesulfonic acid type strong acid cation exchange resin was activated with 1M hydrochloric acid solution 8 times the volume of the resin, and the column was rinsed with clear water 8 times the volume of the resin.
2. Diluting the industrial-grade water glass solution to 5 wt% concentration, ion exchange with ion exchange column, and collecting effluent liquid with pH value less than 4.
3. The composite material as the original substrate was immersed in the collected orthosilicic acid solution for 10 hours.
4. Taking out the composite material, draining, and drying at 300 ℃ for 1 h.
5. Repeating the step 1-4 times.
6. Sintering the composite material at 800 ℃.
The density of the quartz fiber reinforced quartz composite material with the needle-punched structure after the method is adopted is 1.53g/cm3The compressive strength is increased by 2 percent, the compressive strength is increased by 84 percent, the shear strength is increased by 6.0MPa and 20 percent.
Example 2
The quartz fiber reinforced quartz composite material (83mm thick) with three-dimensional orthogonal structure subjected to multiple silica sol impregnation-sintering at the early stage is used as an original base material, and the density is 1.60g/cm3The compressive strength is 100MPa, and the shear strength is 11.0 MPa.
The density of the quartz fiber reinforced quartz composite material with the three-dimensional orthogonal structure treated by the method of the invention and processed by the steps of the embodiment 1 is 1.63g/cm3The compressive strength is increased by 1.7 percent, the compressive strength is 160MPa and is increased by 60 percent, and the shear strength is 13.5MPa and is increased by 22 percent.
Example 3
The 2.5D structure quartz fiber reinforced quartz composite material (70mm thick) subjected to silica sol impregnation-sintering for multiple times at the early stage is used as an original substrate, and the density is 1.61g/cm3The compressive strength is 90MPa, and the shear strength is 12 MPa.
The density of the 2.5D structure quartz fiber reinforced quartz composite material treated by the method of the invention and processed by the steps of the embodiment 1 is 1.64g/cm3The compressive strength is increased by 2 percent, 140MPa and 55 percent. The shear strength is 15MPa, and is increased by 25 percent.
Example 4
The three-dimensional orthorhombic mullite fiber reinforced quartz composite material (75mm thick) subjected to multiple times of silica sol impregnation-sintering at the early stage is used as an original base material, and the density is 2.1g/cm3The compressive strength is 150MPa, and the shear strength is 15 MPa.
The procedure of example 1 is adopted, and the 2.13g/cm of the mullite fiber reinforced quartz composite material with the three-dimensional orthogonal structure is treated by the method3The compressive strength is increased by 1.5 percent, 230MPa and 53 percent. The shear strength is 17.8MPa, and the increase is 18.6 percent.
The invention has not been described in detail and is in part known to those of skill in the art.
Claims (4)
1. A method for improving the density of a large-thickness fiber reinforced quartz composite material is characterized by comprising the following steps:
in the first step, a fresh orthosilicic acid solution is prepared,
a1.1, diluting an industrial-grade water glass solution to 5-8 wt%;
a1.2, carrying out ion exchange on the diluted water glass solution through a strong acid type cation exchange column, and collecting an effluent liquid with the pH value less than 4 to prepare a fresh orthosilicic acid solution;
secondly, placing the fiber reinforced quartz composite material in the orthosilicic acid solution prepared in the first step for dipping for 8-12 hours;
thirdly, drying the fiber reinforced quartz composite material dipped with the orthosilicic acid solution in the second step at high temperature;
and fourthly, repeating the first step to the third step for a plurality of times, and sintering at high temperature.
2. The method for increasing the density of a high-thickness fiber reinforced quartz composite material according to claim 1, wherein: in the third step, the drying temperature is 300 +/-5 ℃, and the drying time is not less than 1 h.
3. The method for increasing the density of a high-thickness fiber reinforced quartz composite material according to claim 1, wherein: and repeating the fourth step for 3-4 times.
4. The method for increasing the density of a high-thickness fiber reinforced quartz composite material according to claim 1, wherein: the fiber reinforced quartz composite material in the second step is a composite material which is difficult to improve in density after multiple dipping and sintering.
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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 |
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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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| Mechanical behavior of 2.5D (shallow bend-joint) and 3D orthogonal quartzf/silica composites by silicasol-infiltration-sintering;Yong Liu等;《Materials Science and Engineering A》;20111025;第532卷;第230-235页 * |
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