CN113999032A - Silicon-boron-nitrogen fiber reinforced quartz ceramic material and preparation method thereof - Google Patents
Silicon-boron-nitrogen fiber reinforced quartz ceramic material and preparation method thereof Download PDFInfo
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- CN113999032A CN113999032A CN202111483455.XA CN202111483455A CN113999032A CN 113999032 A CN113999032 A CN 113999032A CN 202111483455 A CN202111483455 A CN 202111483455A CN 113999032 A CN113999032 A CN 113999032A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000000835 fiber Substances 0.000 title claims abstract description 68
- VGRSPALDTNRXMC-UHFFFAOYSA-N [B].[N].[Si] Chemical compound [B].[N].[Si] VGRSPALDTNRXMC-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000010453 quartz Substances 0.000 title claims abstract description 45
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000005350 fused silica glass Substances 0.000 claims abstract description 34
- 239000000919 ceramic Substances 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims description 38
- 239000011521 glass Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052602 gypsum Inorganic materials 0.000 claims description 5
- 239000010440 gypsum Substances 0.000 claims description 5
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 238000007569 slipcasting Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000011268 mixed slurry Substances 0.000 description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- B28—WORKING CEMENT, CLAY, OR STONE
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- B28B1/00—Producing shaped prefabricated articles from the material
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Abstract
The invention provides a silicon-boron-nitrogen fiber reinforced quartz ceramic material and a preparation method thereof. The silicon boron nitrogen fiber reinforced quartz ceramic material comprises a fused quartz ceramic matrix and silicon boron nitrogen fibers distributed in the fused quartz ceramic matrix. The method comprises the steps of adding short-cut silicon boron nitrogen fibers into quartz ceramic slurry, forming a wet blank by adopting a grouting process, and drying and sintering to prepare the silicon boron nitrogen fiber reinforced quartz ceramic material and product. The composite material is prepared based on the high-temperature resistance of the silicon-boron-nitrogen fiber and the quartz ceramic, so that the strength and the reliability of the quartz ceramic are improved; meanwhile, the preparation process is simple, convenient and quick, the cost is low, and the mass production and the application are convenient.
Description
Technical Field
The invention relates to a silicon boron nitrogen (SiBN) fiber reinforced quartz ceramic material and a preparation method thereof, belonging to the technical field of preparation of functional and structural ceramic matrix composite materials.
Background
The quartz ceramic has the characteristics of excellent thermal shock resistance, ablation resistance, oxidation resistance and the like, can bear sudden temperature change without being damaged, has the use temperature as high as 1500 ℃, and is widely applied to the preparation of various high-temperature resistant structural components; meanwhile, the quartz ceramic has low dielectric constant, low loss, excellent electrical property and little influence of temperature change, and is an ideal material for a wave-transparent window of a high-speed aircraft. However, the mechanical property of the quartz ceramic is poor, the quartz ceramic can meet the requirement of general structural strength, but is very sensitive to stress concentration and microcrack, and the fracture toughness does not exceed 0.5 MPa.m1/2The reliability of the performance is affected, and the application field is limited.
In order to improve the brittleness of the quartz ceramic, researchers adopt quartz fibers, mullite fibers, carbon fibers and the like to reinforce and toughen the quartz ceramic. Although the carbon fiber reinforced quartz ceramic composite material has higher mechanical property, the carbon fiber is a conductor, so that the requirement of wave transmission cannot be met; the preparation technology of the quartz fiber reinforced quartz ceramic composite material is mature, the requirement of a wave-transparent window below 1000 ℃ can be met, but when the temperature is further increased, the fiber becomes brittle, the material performance is rapidly reduced, and the wave-transparent requirement for long-term use above 1000 ℃ cannot be met; the mullite fiber reinforced quartz ceramic improves the use temperature of the quartz ceramic in the wave-transmitting field to about 1200 ℃, but the wave-transmitting performance of the mullite fiber reinforced quartz ceramic is obviously reduced, and the requirement of high-precision guidance cannot be met.
The silicon-boron-nitrogen fiber is a high-temperature resistant fiber which is widely concerned in recent years, and a composite material can be prepared by adopting an impregnation-composite process, but the process needs to be cracked in the atmosphere of nitrogen or ammonia, so that the silicon-boron-nitrogen fiber is prevented from being oxidized and damaged at high temperature; in addition, the current impregnation-compounding process for preparing fiber reinforced quartz ceramic requires the use of acidThe silicon-boron-nitrogen fiber is easy to corrode in the dipping process of the alkaline or alkaline silica sol, so that the strength of the silicon-boron-nitrogen fiber is greatly reduced, and the fracture toughness obtained by preparing the silicon-boron-nitrogen fiber reinforced quartz ceramic by using the silica sol is lower than 1.0 MPa.m1/2And the use requirements cannot be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a wave-transparent ceramic material which is resistant to high temperature of 1400 ℃, low in cost and convenient to popularize and a preparation method thereof.
The technical solution of the invention is as follows:
in a first aspect, the present invention provides a silicon boron nitrogen fiber reinforced quartz ceramic material, which includes a fused quartz ceramic matrix and silicon boron nitrogen fibers distributed in the fused quartz ceramic matrix.
Furthermore, the silicon-boron-nitrogen fiber is a chopped silicon-boron-nitrogen fiber, and the length of the chopped silicon-boron-nitrogen fiber is 0.5 mm-2 mm.
Further, the mass ratio of the chopped silicon-boron-nitrogen fibers in the silicon-boron-nitrogen fiber reinforced quartz ceramic material is 2-15%.
Further, the fused silica ceramic matrix is amorphous silicon dioxide, and the purity is not lower than 99.95%.
In a second aspect, the invention provides a preparation method of a silicon boron nitrogen fiber reinforced quartz ceramic material, which comprises the following steps:
crushing the fused quartz glass, mixing the crushed fused quartz glass with deionized water, and grinding the mixture in a ball mill to obtain fused quartz slurry;
transferring the ground fused quartz slurry into a homogenizing barrel, and slowly stirring to homogenize the slurry;
adding the silicon-boron-nitrogen fibers into the fused quartz slurry, and quickly and uniformly stirring;
and injecting the fused quartz slurry into a mold, and forming a wet blank with a certain thickness after the mold absorbs moisture in the slurry.
And (4) demoulding the wet blank, drying and sintering to obtain the silicon-boron-nitrogen fiber reinforced quartz ceramic material.
Further, the stirring is carried out slowly, the rotating speed of a homogenizing barrel does not exceed 10rpm, and the homogenizing time is 3 days to 10 days.
Further, the rapid stirring is carried out, the rotating speed of the homogenizing barrel is 500 rpm-2000 rpm, and the stirring time is 15 min-40 min.
Further, the mould is a gypsum or porous resin mould, and non-pressure grouting or pressure grouting is adopted.
Further, the molding pressure of the pressure grouting is 0.2 MPa-3 MPa, the pressure holding time is related to the thickness of the product and is determined by the following empirical formula:
H2＝k·t
in the formula, H is the thickness of the blank, t is the pressure maintaining time, k is a constant related to the properties of the die and the slurry, and a specific value is obtained through experiments.
Further, after demoulding of the wet blank, naturally drying the wet blank for 3-5 days, placing the wet blank into a muffle furnace, sintering the wet blank for 1-4 hours at 1190-1250 ℃, and cooling the wet blank to room temperature along with the furnace to obtain the silicon-boron-nitrogen fiber reinforced quartz ceramic material.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the silicon boron nitrogen fiber reinforced quartz ceramic matrix which can resist high temperature of more than 1400 ℃ is adopted, so that the use temperature of the fiber reinforced quartz ceramic material in the wave-transparent field is increased to more than 1400 ℃;
(2) the silicon-boron-nitrogen fiber adopted by the invention has higher toughening effect, and effectively improves the toughness and reliability of the fiber reinforced quartz ceramic material;
(3) according to the invention, the fused quartz slurry is introduced into the composite material matrix, and the pH value of the slurry is 6-7, so that the corrosion and damage of the matrix precursor to fibers are avoided;
(4) the composite material after grouting compounding and forming is sintered in an air environment, and as the solid content of the slurry is higher and the slurry is fully contacted with the fibers, liquid phase precipitation begins to occur on fused quartz particles at the temperature of above 1050 ℃, the fused quartz particles are attached to the surfaces of the fibers, and the fibers are prevented from being oxidized in a high-temperature environment, so that nitrogen or ammonia protection is not needed, and the applicability of the process is improved;
(5) the invention is based on the slip casting method, has low cost and good universality, and is convenient to popularize and apply.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
Weighing 0.1kg of chopped silicon-boron-nitrogen fiber with the length of 2.0mm and the diameter of 0.8 mm; weighing 4.9kg of fused quartz glass with the purity of 99.97 percent and the granularity of 30 meshes; 1.02kg of deionized water was weighed. The fused quartz glass and the deionized water are filled into a ball mill, the ball mill is used for 8 hours, and then the fused quartz glass and the deionized water are transferred into a homogenizing barrel and homogenized for 5 days at the rotating speed of 6 rpm. The weighed chopped silicon boron nitrogen fibers are added into a homogenizing barrel and mixed for 20min at the rotating speed of 500 rpm. And injecting the mixed slurry into a gypsum mold, standing and sucking the slurry for 2 hours, pouring out the redundant slurry, demolding the wet blank, naturally drying for 3 days, putting the wet blank into a muffle furnace, sintering for 2 hours at 1200 ℃, and cooling to room temperature along with the furnace to obtain the silicon-boron-nitrogen fiber reinforced quartz ceramic material.
For the materials prepared in this example, the fracture toughness was measured according to ASTM standard E1820-05a, and the dielectric constant and the loss tangent were measured according to ASTM standard D2520-95, the data being shown in Table 1.
Example 2
Weighing 0.9kg of chopped silicon-boron-nitrogen fibers with the length of 1.5mm and the diameter of 0.8 mm; weighing 5.1kg of fused quartz glass with the purity of 99.97 percent and the granularity of 30 meshes; 1.23kg of deionized water was weighed. The fused quartz glass and the deionized water are filled into a ball mill, the ball mill is used for 8 hours, and then the fused quartz glass and the deionized water are transferred into a homogenizing barrel and homogenized for 5 days at the rotating speed of 6 rpm. The weighed chopped silicon boron nitrogen fibers are added into a homogenizing barrel and mixed for 20min at the rotating speed of 500 rpm. And injecting the mixed slurry into a gypsum mold, applying pressure of 0.5MPa, keeping for 1h, pouring out the redundant slurry, demolding the wet blank, naturally drying for 3 days, putting into a muffle furnace, sintering at 1230 ℃ for 2h, and cooling to room temperature along with the furnace to obtain the silicon boron nitrogen fiber reinforced quartz ceramic material.
For the materials prepared in this example, the fracture toughness was measured according to ASTM standard E1820-05a, and the dielectric constant and the loss tangent were measured according to ASTM standard D2520-95, the data being shown in Table 1.
Example 3
Weighing 0.5kg of chopped silicon-boron-nitrogen fibers with the length of 1.5mm and the diameter of 0.8 mm; weighing 9.5kg of fused quartz glass with the purity of 99.97 percent and the granularity of 30 meshes; 2.05kg of deionized water were weighed. The fused quartz glass and the deionized water are filled into a ball mill, the ball mill is used for 8 hours, and then the fused quartz glass and the deionized water are transferred into a homogenizing barrel and homogenized for 5 days at the rotating speed of 6 rpm. The weighed chopped silicon boron nitrogen fibers are added into a homogenizing barrel and mixed for 20min at the rotating speed of 500 rpm. And injecting the mixed slurry into a gypsum mold, applying a pressure of 0.5MPa, keeping for 1h, standing, sucking slurry for 2h, pouring out the redundant slurry, demolding a wet blank, naturally drying for 3 days, placing the wet blank into a muffle furnace, sintering at 1220 ℃ for 1h, and cooling to room temperature along with the furnace to obtain the silicon-boron-nitrogen fiber reinforced quartz ceramic material.
For the materials prepared in this example, the fracture toughness was measured according to ASTM standard E1820-05a, and the dielectric constant and the loss tangent were measured according to ASTM standard D2520-95, the data being shown in Table 1.
Example 4
Weaving a prefabricated body by adopting silicon-boron-nitrogen fibers with the diameter of 0.8 mm; weighing 9.5kg of fused quartz glass with the purity of 99.97 percent and the granularity of 30 meshes; 2.05kg of deionized water were weighed. The fused quartz glass and the deionized water are filled into a ball mill, the ball mill is used for 8 hours, and then the fused quartz glass and the deionized water are transferred into a homogenizing barrel and homogenized for 5 days at the rotating speed of 6 rpm. And (3) placing the prefabricated body in a pressure kettle, injecting the mixed slurry, applying the pressure of 3MPa, keeping for 1h, discharging the redundant slurry, demolding the wet blank, naturally drying for 3 days, placing the wet blank into a muffle furnace, sintering at 1220 ℃ for 2h, and cooling to room temperature along with the furnace to obtain the silicon-boron-nitrogen long fiber reinforced quartz ceramic composite material.
TABLE 1
| Test specimen | Fracture toughness (MPa. m)1/2) | Dielectric constant | tanδ(×10-3) |
| Example 1 | 2.35 | 3.35 | 3.17 |
| Example 2 | 2.69 | 3.36 | 2.85 |
| Example 3 | 2.41 | 3.35 | 3.26 |
The silicon-boron-nitrogen fiber adopted by the invention has higher toughening effect, and effectively improves the toughness and reliability of the fiber reinforced quartz ceramic material.
The invention has not been described in detail and is in part known to those of skill in the art.
The particular embodiments of the present invention disclosed above are illustrative only and are not intended to be limiting, since various alternatives, modifications, and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The invention should not be limited to the disclosure of the embodiments in the present specification, but the scope of the invention is defined by the appended claims.
Claims (10)
1. The silicon boron nitrogen fiber reinforced quartz ceramic material is characterized by comprising a fused quartz ceramic matrix and silicon boron nitrogen fibers distributed in the fused quartz ceramic matrix.
2. A silicon boron nitrogen fiber reinforced quartz ceramic material according to claim 1, characterized in that: the silicon-boron-nitrogen fiber is a chopped silicon-boron-nitrogen fiber, and the length of the fiber is 0.5 mm-2 mm.
3. A silicon boron nitrogen fiber reinforced quartz ceramic material according to claim 2, characterized in that: the mass proportion of the chopped silicon-boron-nitrogen fibers in the silicon-boron-nitrogen fiber reinforced quartz ceramic material is 2-15%.
4. A silicon boron nitrogen fiber reinforced quartz ceramic material according to claim 1, characterized in that: the fused quartz ceramic matrix is amorphous silicon dioxide, and the purity is not lower than 99.95%.
5. A preparation method of a silicon-boron-nitrogen fiber reinforced quartz ceramic material is characterized in that the material is molded by adopting a slip casting process, and comprises the following steps:
crushing the fused quartz glass, mixing the crushed fused quartz glass with deionized water, and grinding the mixture in a ball mill to obtain fused quartz slurry;
transferring the ground fused quartz slurry into a homogenizing barrel, and slowly stirring to homogenize the slurry;
adding the silicon-boron-nitrogen fibers into the fused quartz slurry, and quickly and uniformly stirring;
injecting the uniformly stirred slurry into a mold, and absorbing moisture in the slurry by the mold to form a wet blank;
and (4) demolding the wet blank, drying and sintering to obtain the silicon-boron-nitrogen fiber reinforced quartz ceramic material.
6. The method of claim 5, wherein: the stirring is carried out at a slow speed, the rotating speed of a homogenizing barrel does not exceed 10rpm, and the homogenizing time is 3 days to 10 days.
7. The method of claim 5, wherein: the rapid stirring is carried out, the rotating speed of the homogenizing barrel is 500 rpm-2000 rpm, and the stirring time is 15 min-40 min.
8. The method of claim 5, wherein: the mould is a gypsum or porous resin mould and adopts non-pressure grouting or pressure grouting.
9. The method of claim 8, wherein: the molding pressure of the pressure grouting is 0.2 MPa-3 MPa, the pressure maintaining time is related to the thickness of a product and is determined by the following empirical formula:
H2＝k·t
wherein H is the thickness of the blank, t is the pressure maintaining time, and k is a constant related to the properties of the die and the slurry, and a specific value is obtained through experiments.
10. The method of claim 5, wherein: and (3) demoulding the wet blank, naturally drying for 3-5 days, putting the wet blank into a muffle furnace, sintering for 1-4 hours at 1190-1250 ℃, and cooling to room temperature along with the furnace to obtain the silicon-boron-nitrogen fiber reinforced quartz ceramic material.
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