CN105541197A - Preparation method for chopped silicon carbide fiber reinforced aluminosilicate polymer composite material - Google Patents
Preparation method for chopped silicon carbide fiber reinforced aluminosilicate polymer composite material Download PDFInfo
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- CN105541197A CN105541197A CN201510968238.8A CN201510968238A CN105541197A CN 105541197 A CN105541197 A CN 105541197A CN 201510968238 A CN201510968238 A CN 201510968238A CN 105541197 A CN105541197 A CN 105541197A
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- silicon carbide
- carbide fiber
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mineral polymers, e.g. geopolymers of the Davidovits type
Abstract
The invention provides a preparation method for a chopped silicon carbide fiber reinforced aluminosilicate polymer composite material, and relates to the preparation method for composite materials. The preparation method provided by the invention is to solve the problem of severe limitation of a conventional aluminosilicate polymer material extensively applied in the field of high-tech materials demanding a certain loading capacity and high reliability due to inherent brittleness and low mechanical strength and toughness of the conventional aluminosilicate polymer material. The preparation method for the chopped silicon carbide fiber reinforced aluminosilicate polymer composite material is realized through the following steps: 1, preparation of a raw material, i.e., active aluminosilicate; 2, preparation of a ball-milled mixture; 3, preparation of an alkali-activation solution; 4, preparation of an aluminosilicate polymer material slurry; and 5, curing. The preparation method provided by the invention is used for preparation of the chopped silicon carbide fiber reinforced aluminosilicate polymer composite material.
Description
Technical field
The present invention relates to the preparation method of matrix material.
Background technology
Aluminosilicate polymer material is owing to having the advantages that low density, low cost, fire-retardant and can prepare but can at high temperature use at low ambient temperatures, obtain application in fields such as building and refractory materialss, and be considered to be hopeful most replace macromolecular material and be applied to one of material of spacecraft, boats and ships and vehicle interior compartment body.But its intrinsic fragility, low mechanical strength and toughness, seriously limit it in the widespread use in High-tech Material field needing certain supporting capacity, require reliability high.In recent years, scholars greatly increases its toughness by the mode introducing reinforcement in aluminosilicate polymer one after another, has expanded its Application Areas.
Summary of the invention
The present invention will solve existing aluminosilicate polymer material intrinsic fragility, low mechanical strength and toughness, seriously limit it in the problem of widespread use in High-tech Material field needing certain supporting capacity, require reliability high, and provide short and cut the preparation method that silicon carbide fiber strengthens aluminosilicate polymer composite material.
The short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material, specifically carries out according to the following steps:
One, be under the condition of 600 DEG C ~ 900 DEG C in temperature, by aluminosilicate starting material calcining 1h ~ 5h, obtain activated aluminosilicate starting material;
Two, at ambient temperature, activated aluminosilicate starting material are cut silicon carbide fiber ball milling mixing 24h ~ 48h with short, obtains ball-milled mixtures;
Described short length of cutting silicon carbide fiber is 2mm ~ 10mm, and the short-and-medium percent by volume of cutting silicon carbide fiber of described ball-milled mixtures is 0.5% ~ 5%;
Three, alkali metal hydroxide is joined in silicon sol, magnetic agitation 48h, namely obtain alkali-activated carbonatite solution;
In described alkali metal hydroxide and silicon sol, the mol ratio of silicon-dioxide is 1:1;
Four, ball-milled mixtures to be mixed with alkali-activated carbonatite solution, and at ambient temperature, mechanical stirring ultrasonic vibration 0.5h ~ 2h, obtain aluminosilicate polymer slip;
In described ball-milled mixtures, in activated aluminosilicate starting material and alkali-activated carbonatite solution, the mol ratio of silicon-dioxide is 1:1;
Five, aluminosilicate polymer slip is injected mould, bagging seals, and then solidifies 3 days ~ 7 days at temperature is 60 DEG C ~ 80 DEG C, obtains shortly cutting silicon carbide fibre/aluminosilicate polymer composite material.
The present invention constructs short fiber reinforced aluminosilicate polymer based composites, adopt short advantage of cutting the aluminosilicate polymer composite material that silicon carbide fiber strengthens to be: one, it has obvious anisotropy unlike unidirectional continuous fiber reinforced composite materials; They are two years old, relative to carbon fiber reinforced aluminosilicate polymer composite material, not only there is higher strength and toughness, also there is excellent antioxidant property simultaneously, can to be on active service under aerobic environment condition at high temperature, while keeping aluminosilicate polymer materials thermophysics character, to improve ability and the reliability of material carry load.The present invention, to the development and the practical engineering application that promote novel aluminum silicate polymer and matrix material thereof, expands the range of application of aluminosilicate polymer material, improves its using value significant.Therefore, there is huge potential Social and economic benef@.
The invention has the beneficial effects as follows:
The short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material provided by the invention, the short silicon carbide fiber of cutting prepared strengthens the mechanical property that aluminosilicate polymer composite material has excellence, its fracture mode plastic fracture, the percent by volume of cutting silicon carbide fiber when described ball-milled mixtures is short-and-medium is 2%, and length is 5mm, its bending strength and work of rupture reach maximum value, are respectively 49MPa and 1888.1Jm
-2, be 5.6 times of matrix bending strength and 63 times of work of rupture.
Accompanying drawing explanation
Fig. 1 is be the short Fracture scan electromicroscopic photograph cutting silicon carbide fibre/aluminosilicate polymer composite material prepared by embodiment one;
Fig. 2 is be the short Fracture scan electromicroscopic photograph cutting silicon carbide fibre/aluminosilicate polymer composite material prepared by embodiment two;
Fig. 3 is be the short Fracture scan electromicroscopic photograph cutting silicon carbide fibre/aluminosilicate polymer composite material prepared by embodiment three;
Fig. 4 is the load-displacement curves of polymer composites prepared by different lengths silicon carbide fiber, a is aluminosilicate polymer composite material prepared by contrast experiment, b is that prepared by embodiment one short cuts silicon carbide fibre/aluminosilicate polymer composite material, c is that prepared by embodiment two short cuts silicon carbide fibre/aluminosilicate polymer composite material, and d is that prepared by embodiment three short cuts silicon carbide fibre/aluminosilicate polymer composite material;
Fig. 5 is the mechanical property comparison diagram of polymer composites prepared by different lengths silicon carbide fiber, and 1 is bending strength, and 2 is work of rupture.
Embodiment
Embodiment one: the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material described in present embodiment completes according to the following steps:
One, be under the condition of 600 DEG C ~ 900 DEG C in temperature, by aluminosilicate starting material calcining 1h ~ 5h, obtain activated aluminosilicate starting material;
Two, at ambient temperature, activated aluminosilicate starting material are cut silicon carbide fiber ball milling mixing 24h ~ 48h with short, obtains ball-milled mixtures;
Described short length of cutting silicon carbide fiber is 2mm ~ 10mm, and the short-and-medium percent by volume of cutting silicon carbide fiber of described ball-milled mixtures is 0.5% ~ 5%;
Three, alkali metal hydroxide is joined in silicon sol, magnetic agitation 48h, namely obtain alkali-activated carbonatite solution;
In described alkali metal hydroxide and silicon sol, the mol ratio of silicon-dioxide is 1:1;
Four, ball-milled mixtures to be mixed with alkali-activated carbonatite solution, and at ambient temperature, mechanical stirring ultrasonic vibration 0.5h ~ 2h, obtain aluminosilicate polymer slip;
In described ball-milled mixtures, in activated aluminosilicate starting material and alkali-activated carbonatite solution, the mol ratio of silicon-dioxide is 1:1;
Five, aluminosilicate polymer slip is injected mould, bagging seals, and then solidifies 3 days ~ 7 days at temperature is 60 DEG C ~ 80 DEG C, obtains shortly cutting silicon carbide fibre/aluminosilicate polymer composite material.
In present embodiment step 2 with activated aluminosilicate starting material and short silicon carbide fiber of cutting for expecting, carry out ball milling mixing, wherein ratio of grinding media to material is 5:1.
The beneficial effect of present embodiment is: the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material that present embodiment provides, the short silicon carbide fiber of cutting prepared strengthens the mechanical property that aluminosilicate polymer composite material has excellence, its fracture mode plastic fracture, the percent by volume of cutting silicon carbide fiber when described ball-milled mixtures is short-and-medium is 2%, and length is 5mm, its bending strength and work of rupture reach maximum value, are respectively 49MPa and 1888.1Jm
-2, be 5.6 times of matrix bending strength and 63 times of work of rupture.
Embodiment two: present embodiment and embodiment one unlike: the aluminosilicate starting material described in step one are kaolin, clay, flyash or blast-furnace slag.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two unlike: the alkali metal hydroxide described in step 3 is sodium hydroxide, potassium hydroxide or cesium hydroxide.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the short length of cutting silicon carbide fiber described in step 2 is 2mm.Other is identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: the short length of cutting silicon carbide fiber described in step 2 is 5mm.Other is identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: the short length of cutting silicon carbide fiber described in step 2 is 8mm.Other is identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: the short-and-medium percent by volume of cutting silicon carbide fiber of the ball-milled mixtures described in step 2 is 0.5%.Other is identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the short-and-medium percent by volume of cutting silicon carbide fiber of the ball-milled mixtures described in step 2 is 1.0%.Other is identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the short-and-medium percent by volume of cutting silicon carbide fiber of the ball-milled mixtures described in step 2 is 2.0%.Other is identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: the short-and-medium percent by volume of cutting silicon carbide fiber of the ball-milled mixtures described in step 2 is 3.0%.Other is identical with embodiment one to nine.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material described in the present embodiment completes according to the following steps:
One, be under the condition of 800 DEG C in temperature, by aluminosilicate starting material calcining 2h, obtain activated aluminosilicate starting material;
Two, at ambient temperature, activated aluminosilicate starting material are cut silicon carbide fiber ball milling mixing 36h with short, obtains ball-milled mixtures;
Described short length of cutting silicon carbide fiber is 2mm, and the short-and-medium percent by volume of cutting silicon carbide fiber of described ball-milled mixtures is 2%;
Three, alkali metal hydroxide is joined in silicon sol, magnetic agitation 48h, namely obtain alkali-activated carbonatite solution;
In described alkali metal hydroxide and silicon sol, the mol ratio of silicon-dioxide is 1:1;
Four, ball-milled mixtures to be mixed with alkali-activated carbonatite solution, and at ambient temperature, mechanical stirring ultrasonic vibration 1h, obtain aluminosilicate polymer slip;
In described ball-milled mixtures, in activated aluminosilicate starting material and alkali-activated carbonatite solution, the mol ratio of silicon-dioxide is 1:1;
Five, aluminosilicate polymer slip is injected mould, bagging seals, and then solidifies 4 days at temperature is 70 DEG C, obtains shortly cutting silicon carbide fibre/aluminosilicate polymer composite material;
In the present embodiment step 2 with activated aluminosilicate starting material and short silicon carbide fiber of cutting for expecting, carry out ball milling mixing, wherein ratio of grinding media to material is 5:1;
Aluminosilicate starting material described in step one are kaolin;
Alkali metal hydroxide described in step 3 is potassium hydroxide.
Embodiment two: the present embodiment and embodiment one unlike: the short length of cutting silicon carbide fiber described in step 2 is 5mm.Other is identical with embodiment one.
Embodiment three: the present embodiment and embodiment one unlike: the short length of cutting silicon carbide fiber described in step 2 is 8mm.Other is identical with embodiment one.
Contrast experiment: be one, under the condition of 800 DEG C in temperature, by aluminosilicate starting material calcining 2h, obtains activated aluminosilicate starting material;
Two, alkali metal hydroxide is joined in silicon sol, magnetic agitation 48h, namely obtain alkali-activated carbonatite solution;
In described alkali metal hydroxide and silicon sol, the mol ratio of silicon-dioxide is 1:1;
Three, activated aluminosilicate starting material to be mixed with alkali-activated carbonatite solution, and at ambient temperature, mechanical stirring ultrasonic vibration 1h, obtain polymkeric substance slip;
In described activated aluminosilicate starting material and alkali-activated carbonatite solution, the mol ratio of silicon-dioxide is 1:1;
Four, polymkeric substance slip is injected mould, bagging seals, and then solidifies 4 days at temperature is 70 DEG C, obtains aluminosilicate polymer composite material;
Aluminosilicate starting material described in step one are kaolin;
Alkali metal hydroxide described in step 2 is potassium hydroxide.
Fig. 1 is be the short Fracture scan electromicroscopic photograph cutting silicon carbide fibre/aluminosilicate polymer composite material prepared by embodiment one;
Fig. 2 is be the short Fracture scan electromicroscopic photograph cutting silicon carbide fibre/aluminosilicate polymer composite material prepared by embodiment two;
Fig. 3 is be the short Fracture scan electromicroscopic photograph cutting silicon carbide fibre/aluminosilicate polymer composite material prepared by embodiment three;
As seen from the figure, when staple length is 5mm, can ensure to have good distribution effect, the bend fracture of fiber can also be avoided simultaneously.
That prepares embodiment one to three shortly cuts aluminosilicate polymer composite material prepared by silicon carbide fibre/aluminosilicate polymer composite material and contrast experiment and carries out load-displacement and measuring mechanical property:
Fig. 4 is the load-displacement curves of polymer composites prepared by different lengths silicon carbide fiber, a is aluminosilicate polymer composite material prepared by contrast experiment, b is that prepared by embodiment one short cuts silicon carbide fibre/aluminosilicate polymer composite material, c is that prepared by embodiment two short cuts silicon carbide fibre/aluminosilicate polymer composite material, d is that prepared by embodiment three short cuts silicon carbide fibre/aluminosilicate polymer composite material, as seen from the figure, adopt and shortly cut after silicon carbide fiber strengthens, fracture mode is turned by brittle rupture Wei plastic fracture.
Fig. 5 is the mechanical property comparison diagram of polymer composites prepared by different lengths silicon carbide fiber, and 1 is bending strength, and 2 is work of rupture; Wherein 0mm is aluminosilicate polymer composite material prepared by contrast experiment, 2mm is that prepared by embodiment one short cuts silicon carbide fibre/aluminosilicate polymer composite material, 5mm is that prepared by embodiment two short cuts silicon carbide fibre/aluminosilicate polymer composite material, and 8mm is that prepared by embodiment three short cuts silicon carbide fibre/aluminosilicate polymer composite material; As seen from the figure, when staple length is 5mm, bending strength and work of rupture all reach maximum value, and the percent by volume of cutting silicon carbide fiber when described ball-milled mixtures is short-and-medium is 2%, and length is 5mm, its bending strength and work of rupture reach maximum value, are respectively 49MPa and 1888.1Jm
-2, be 5.6 times of matrix bending strength and 63 times of work of rupture.
Claims (10)
1. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material, is characterized in that the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material completes according to the following steps:
One, be under the condition of 600 DEG C ~ 900 DEG C in temperature, by aluminosilicate starting material calcining 1h ~ 5h, obtain activated aluminosilicate starting material;
Two, at ambient temperature, activated aluminosilicate starting material are cut silicon carbide fiber ball milling mixing 24h ~ 48h with short, obtains ball-milled mixtures;
Described short length of cutting silicon carbide fiber is 2mm ~ 10mm, and the short-and-medium percent by volume of cutting silicon carbide fiber of described ball-milled mixtures is 0.5% ~ 5%;
Three, alkali metal hydroxide is joined in silicon sol, magnetic agitation 48h, namely obtain alkali-activated carbonatite solution;
In described alkali metal hydroxide and silicon sol, the mol ratio of silicon-dioxide is 1:1;
Four, ball-milled mixtures to be mixed with alkali-activated carbonatite solution, and at ambient temperature, mechanical stirring ultrasonic vibration 0.5h ~ 2h, obtain aluminosilicate polymer slip;
In described ball-milled mixtures, in activated aluminosilicate starting material and alkali-activated carbonatite solution, the mol ratio of silicon-dioxide is 1:1;
Five, aluminosilicate polymer slip is injected mould, bagging seals, and then solidifies 3 days ~ 7 days at temperature is 60 DEG C ~ 80 DEG C, obtains shortly cutting silicon carbide fibre/aluminosilicate polymer composite material.
2. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the aluminosilicate starting material described in step one are kaolin, clay, flyash or blast-furnace slag.
3. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the alkali metal hydroxide described in step 3 is sodium hydroxide, potassium hydroxide or cesium hydroxide.
4. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short length of cutting silicon carbide fiber described in step 2 is 2mm.
5. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short length of cutting silicon carbide fiber described in step 2 is 5mm.
6. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short length of cutting silicon carbide fiber described in step 2 is 8mm.
7. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short-and-medium percent by volume of cutting silicon carbide fiber of ball-milled mixtures described in step 2 is 0.5%.
8. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short-and-medium percent by volume of cutting silicon carbide fiber of ball-milled mixtures described in step 2 is 1.0%.
9. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short-and-medium percent by volume of cutting silicon carbide fiber of ball-milled mixtures described in step 2 is 2.0%.
10. the short preparation method cutting silicon carbide fiber enhancing aluminosilicate polymer composite material according to claim 1, is characterized in that the short-and-medium percent by volume of cutting silicon carbide fiber of ball-milled mixtures described in step 2 is 3.0%.
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| CN106281218A (en) * | 2016-08-02 | 2017-01-04 | 哈尔滨工业大学 | Carbon back absorbing material prepared by a kind of aluminosilicate polymer and preparation method thereof |
| CN106587780A (en) * | 2016-12-20 | 2017-04-26 | 哈尔滨工业大学 | Method for preparing and printing aluminosilicate polymer composite material for 3D (three-dimensional) printing |
| CN108250985A (en) * | 2018-01-29 | 2018-07-06 | 黑龙江省科学院石油化学研究院 | A kind of room temperature fast-curing high-temperature Resistance Adhesives and preparation method thereof |
| CN111718180A (en) * | 2020-07-01 | 2020-09-29 | 北京玻钢院复合材料有限公司 | Chopped carbon fiber reinforced aluminum silicate ceramic matrix composite and preparation method thereof |
| CN114933480A (en) * | 2022-06-06 | 2022-08-23 | 哈尔滨工业大学 | Preparation method of Csf/SiBCN composite material with pseudo-plastic fracture |
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| CN111718180A (en) * | 2020-07-01 | 2020-09-29 | 北京玻钢院复合材料有限公司 | Chopped carbon fiber reinforced aluminum silicate ceramic matrix composite and preparation method thereof |
| CN114933480A (en) * | 2022-06-06 | 2022-08-23 | 哈尔滨工业大学 | Preparation method of Csf/SiBCN composite material with pseudo-plastic fracture |
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