CN113307633B - Preparation method of rapidly sintered porous ceramic - Google Patents
Preparation method of rapidly sintered porous ceramic Download PDFInfo
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- CN113307633B CN113307633B CN202110766610.2A CN202110766610A CN113307633B CN 113307633 B CN113307633 B CN 113307633B CN 202110766610 A CN202110766610 A CN 202110766610A CN 113307633 B CN113307633 B CN 113307633B
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- 238000010304 firing Methods 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 33
- 229910052580 B4C Inorganic materials 0.000 claims description 15
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 7
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 241000241413 Propolis Species 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229940069949 propolis Drugs 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
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- 239000000843 powder Substances 0.000 abstract description 12
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- 238000005467 ceramic manufacturing process Methods 0.000 abstract 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 13
- 229910010271 silicon carbide Inorganic materials 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000001514 detection method Methods 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 7
- 239000010431 corundum Substances 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
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- 239000004576 sand Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
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- 238000000926 separation method Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920005552 sodium lignosulfonate Polymers 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of rapidly sintered porous ceramic, which comprises the following steps: weighing ceramic main materials, adhesives and other additives, and uniformly mixing to form a mixture; step two: treating the mixture obtained in the first step to form a solid mixture or slurry; step three: filling the solid mixture or slurry obtained in the step two into a mold cavity, and forming a blank body by dry powder pressing or casting molding; step four: firing the green body obtained in the third step, and setting the firing air pressure to be 10 ‑3 ～10 5 Pa, the temperature is lower than 1000 ℃, and the porous ceramic is prepared. Setting of atmospheric pressure conditions by firing process in porous ceramic manufacturing process 10 ‑3 ～10 5 Pa, the firing process is finished within 4 hours at the temperature lower than 1000 ℃, so that the bending strength of the porous ceramic is ensured and even improved, and the oxidation of the main material is inhibited while the firing period is shortened.
Description
Technical Field
The invention belongs to the technical field of porous ceramics, and particularly relates to a preparation method of rapidly sintered porous ceramics.
Background
The porous ceramic material is prepared by taking corundum sand, silicon carbide and other raw materials as main materials through molding and a special high-temperature sintering process. The porous ceramic material has the advantages of high temperature and high pressure resistance, acid-base and organic medium corrosion resistance, good biological inertia, controllable pore structure and porosity, long service life, renewable products and the like. The composite material is prepared by methods such as an extrusion forming method, a foaming method, a dipping method, a sol-gel method, 3D additive printing and the like, and is widely applied to the fields of metal smelting filter residue nets, environment-friendly treatment filter carriers, composite materials, refractory materials and the like.
The firing process in the porous ceramic preparation process has the mechanism of promoting solid-liquid phase sintering to meet the necessary mechanical strength, generally needs to adopt high temperature not lower than 1200 ℃, and is fired under the condition of normal pressure or positive pressure, and the firing period is longer (for example, patent CN112778020A, patent CN 111763097A). Under the conditions of high temperature and high pressure, the separation processes of sublimation, evaporation, cracking, gasification and the like of additives such as adhesives and the like for forming porous ceramics are hindered, the degreasing and glue discharging processes are influenced, and the blank body is cracked in a severe condition. According to the invention, by optimizing process conditions and optimizing additives, the firing period is effectively shortened and the open porosity and the bending strength of the product are ensured.
Disclosure of Invention
The invention aims to provide a preparation method of rapidly sintered porous ceramic, which adopts negative pressure firing and selects a binder mixed by a high-temperature binder and a low-temperature binder, thereby ensuring and even improving the mechanical strength of the porous ceramic while shortening the firing period.
The purpose of the invention is realized by the following technical scheme: a preparation method of rapid sintering porous ceramic comprises the following steps:
the method comprises the following steps: weighing ceramic main materials and additives, and uniformly mixing to form a mixture;
step two: processing the mixture obtained in the step one to prepare a solid mixture or slurry;
step three: filling the solid mixture or slurry obtained in the step two into a mold cavity, and forming a blank body by dry powder pressing or casting molding;
step four: firing the green body obtained in the third step, and setting the air pressure value to be 10 -3 ～10 5 Pa, and the firing temperature is lower than 1000 ℃, thus obtaining the porous ceramic.
Preferably, the step one comprises the ceramic main material of one or more of silicon carbide, corundum sand, zirconia, boron carbide, alumina, silicon nitride and diamond; the additive comprises a low-temperature adhesive and a high-temperature adhesive, wherein the low-temperature adhesive is one or more of paraffin, polyvinyl alcohol, emulsified paraffin, propolis, silica gel and sodium lignosulfonate; the high-temperature adhesive is one or more of silicone resin 249, silica glass powder, aluminum dihydrogen phosphate, cryolite and low-temperature molten salt.
Preferably, the solid mixture in the second step is granulated by a sample separation sieve or spray drying, and the third step is carried out after the moisture content is controlled to be less than or equal to 2.0 wt%.
Preferably, the slurry in the third step is poured and molded, then is demoulded and taken out, and the blank body is dried for 5 to 7 hours at the temperature of between 60 and 90 ℃.
Preferably, in the fourth step, the firing temperature is 100-350 ℃ for degreasing, 150-650 ℃ for degumming, and 700-980 ℃ for sintering and forming; the firing process time is less than 4h.
Preferably, the air pressure in the fourth step is 2X 10 -3 ～4×10 4 Pa degreasing, 4X 10 -3 ～7×10 4 Pa removing glue, 1X 10 -3 ～9×10 4 And Pa sintering and forming.
Preferably, the air pressure in the fourth step is 1 × 10 -2 ～9×10 3 Pa degreasing, 3X 10 -2 About 6X 10Pa for glue removal, 2X 10 -3 Sintering and forming at 6X 10 Pa.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention sets the firing process air pressure condition in the porous ceramic preparation process as negative pressure 10 -3 ～10 5 Pa, promoting the separation process of sublimation, evaporation, cracking, gasification and the like of additives such as adhesive and the like, promoting the degreasing and glue-removing process, and completing the firing process at the temperature of less than 1000 DEG CAnd the firing time is not more than 4h.
2) The invention promotes the binding action between the main materials of the porous ceramics by preferably selecting the mixture of the low-temperature binder and the high-temperature binder as the binder, reduces the requirement of the firing process condition and leads the porous ceramics to be under the negative pressure of 10 -3 ～10 5 Pa is lower than 1000 ℃, and the firing time is not more than 4h.
3) The porous ceramic product obtained by negative pressure firing can keep the bending strength higher than 2MPa, even improve the bending strength, which is 1.2-2 times of that of a normal pressure pressed product; and can inhibit the oxidation process of the easily oxidized ceramic main material (such as boron carbide and silicon carbide) so that the oxidation product is from about 50% to about 0.01%.
Drawings
FIG. 1 is a graph of the firing process temperature and pressure at step four of example 1;
FIG. 2 is a graph of the firing process temperature and pressure in step four of example 3;
FIG. 3 is a graph of the firing process temperature and pressure in step four of example 4.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings and examples.
Example 1
The method comprises the following steps: weighing 1000g of particle diameter D 50 5 μm silicon carbide and 85g of fully refined paraffin, 50g of aluminium dihydrogen phosphate were added to form a mixture;
step two: heating the mixture obtained in the step one to paraffin to form a liquid state, fully and uniformly mixing the mixture with silicon carbide particles and aluminum dihydrogen phosphate, and cooling the mixture to paraffin to form a solid state to form a blocky solid mixture; granulating the massive solid mixture through a 60-mesh sample sieve to obtain granulated powder;
step three: filling the granulation powder obtained in the second step into a die cavity, and pressing the dry powder with the pressure of 55kgf/cm 2 The size of the blank is 100mm multiplied by 20mm;
step four: and (3) firing the green body obtained in the third step, wherein the temperature curve of the firing process is shown in figure 1: heating from room temperature at a heating rate of 4.5 deg.C/min for 50min to 240 deg.C, and maintaining at constant temperature for 20min; heating at a speed of 11 deg.C/min for 30 min-460 deg.C, and maintaining at constant temperature for 20min; heating at a speed of 12 deg.C/min for 40 min-940 deg.C, and maintaining at constant temperature for 20min; finally, cooling to room temperature along with the furnace;
the kiln inlet and outlet are provided with air pressure control valves for regulating air pressure via regulating air (air, oxygen, argon, nitrogen or carbon dioxide), and the negative pressure curve (one standard atmospheric pressure is 1.013 × 10) 5 Pa) (as shown in fig. 1): the pressure in the furnace is 2X 10 from 0min 4 Keeping the constant pressure Pa for 50min; the firing time is 50min to 70min, and the air pressure is stably and synchronously adjusted to 4 x 10 4 Pa, keeping constant pressure for 30min; the firing time is 100min to 120min, and the air pressure is stably and synchronously adjusted to 7 x 10 4 Pa, keeping constant pressure for 40min; the firing time is 160min to 180min, the air pressure is stably regulated to 9 x 10 4 Pa; maintaining the air pressure until the temperature is reduced to below 200 ℃; and preparing the silicon carbide porous ceramic.
The detection result of the performance of the negative pressure sintered silicon carbide porous ceramic is as follows:
| name(s) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 1 | 54.3 | 2.9 | 95.4 |
| |
54.6 | 2.8 | 95.6 |
| Sample 3 | 54.4 | 3.0 | 95.3 |
Comparative example 1
The difference from example 1 is that:
the method comprises the following steps: weighing 1000g of particle diameter D 50 5 μm of silicon carbide, and 100g of polyvinyl alcohol (10% of effective solid content), 30g of sodium citrate, 10g of lubricant (Luoyangyeli YF-125, 40% of effective solid content) were added to form a mixture;
step two: adding a proper amount of deionized water into the mixture obtained in the step one, stirring the mixture by a stirrer until the mixture is fully and uniformly mixed, preparing silicon carbide micro powder by adopting a spray granulation mode, sieving the silicon carbide micro powder by a 20-mesh sample sieve, and controlling the water content to be between 0.3 and 1.0 percent to prepare granulated powder;
the detection result of the performance of the negative pressure sintered silicon carbide porous ceramic is as follows:
| name (R) | Volume fraction (%) | Bending Strength (MPa) | Open porosity (%) |
| Sample 1' | 53.9 | 2.4 | 94.3 |
| Sample 2' | 53.1 | 2.4 | 95.1 |
| Sample 3' | 53.5 | 2.3 | 94.8 |
Comparative example 2
The difference from comparative example 1 is:
step four: and (3) firing the green body obtained in the step three, wherein the firing process is normal pressure, and the temperature curve is as follows: heating from room temperature at a heating rate of 2 deg.C/min to 165-350 deg.C for 100min, and defatting; heating at a heating rate of 3 deg.C/min for 100min to 650 deg.C, maintaining at constant temperature for 30min, and removing gel; heating at a heating rate of 4 deg.C/min for 150-1250 deg.C, and maintaining at constant temperature for 120min; and then heating at the heating rate of 2 ℃/min to 1780 ℃ for 180min, keeping the constant temperature for 180min, cooling at the temperature of 6 ℃/min for 100min to 1200 ℃ for 20min, cooling with the furnace for about 720min to 100 ℃, and sintering and molding to obtain the silicon carbide fine-particle recrystallized porous ceramic.
The performance detection result of the silicon carbide porous ceramic sintered under normal pressure is as follows:
| name (R) | Volume fraction (%) | High bending resistanceDegree (MPa) | Open porosity (%) |
| Sample 4' | 51.2 | 1.8 | 83.2 |
| Sample 5' | 51.4 | 2.0 | 82.8 |
| Sample 6' | 51.0 | 1.5 | 82.6 |
Example 2
The method comprises the following steps: weighing 1000g of particle diameter D 50 The method comprises the following steps of (1) adding 350g of polyvinyl alcohol (PVA) 1788 aqueous solution (the effective solid content is 10%), 65g of boron glass powder (the particle size is 20 mu m), 50g of polyethylene glycol (the effective solid content is 20%), 10g of lubricant (Luoyangyeqi YF-125, the effective solid content is 40%) into 120 mu m corundum ceramic raw material to form a mixture;
step two: adding a proper amount of deionized water into the mixture obtained in the step one, and stirring the mixture by using a stirrer until the mixture is fully and uniformly formed into slurry; then placing the mixture in a resistance wire drying box with the set temperature of 70 ℃ and drying for 4 hours to form a solid mixture; granulating the solid mixture by using a 50-mesh sample separation sieve, and placing the solid mixture into a closed container for moisture homogenization treatment, wherein the moisture range is controlled to be 0.3-2.0%;
step three: filling the granulated powder obtained in the step two into a mold cavity, and pressing the dry powder with the pressure of 55kgf/cm 2 The size of the blank is 100mm multiplied by 20mm;
step four: and (5) firing the green body obtained in the step four, wherein the temperature curve of the firing process is as follows: heating from room temperature at a rate of 5.5 deg.C/min for 40min to 240 deg.C, and maintaining at constant temperature for 20min; then heating at a speed of 8.8 ℃/min for 25min to 460 ℃, and keeping the constant temperature for 20min; heating at a speed of 10.5 deg.C/min for 40min to 880 deg.C, and maintaining at constant temperature for 20min; finally, cooling to room temperature along with the furnace;
kiln air inlet, gas outlet set up the air pressure control valve, adjust atmospheric pressure through adjusting gas (air, oxygen, argon gas, nitrogen gas or carbon dioxide), atmospheric pressure curve: the pressure in the furnace is 2X 10 from 0min 3 Keeping the constant pressure of Pa for 40min; the firing time is from 40min to 60min, and the air pressure is stably regulated to 4 × 10 3 Pa, keeping constant pressure for 25min; the firing time is from 85min to 105min, and the air pressure is stably regulated to 7 × 10 3 Pa, keeping constant pressure for 40min; the firing time is 145min to 165min, and the air pressure is stably and synchronously adjusted to 1 x 10 4 Pa; maintaining the air pressure until the temperature is reduced to below 150 ℃, and returning to the normal pressure; and obtaining the corundum sand porous ceramic.
The detection result of the performance of the corundum sand porous ceramic fired under negative pressure is as follows:
| name (R) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 4 | 51.3 | 2.6 | 98.0 |
| Sample No. 5 | 51.2 | 2.4 | 98.2 |
| Sample 6 | 51.2 | 2.6 | 98.0 |
Comparative example 3
The difference from example 2 is that the step four: and (4) firing the green body obtained in the step three, wherein the temperature curve of the firing process is as follows: heating from room temperature at a heating rate of 2 deg.C/min for 110min to 240 deg.C, and maintaining at constant temperature for 80min; then heating at the speed of 4 ℃/min for 55min to 460 ℃, and keeping the constant temperature for 40min; then heating at a heating speed of 3 ℃/min for 140min to 880 ℃, and keeping the constant temperature for 60min; and finally, cooling to room temperature along with the furnace to obtain the corundum sand porous ceramic.
The detection result of the performance of the corundum sand porous ceramic fired under normal pressure is as follows:
| name(s) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 7' | 49.6 | 1.9 | 95.3 |
| Sample 8' | 50.2 | 2.0 | 94.9 |
| Sample 9' | 50.1 | 2.0 | 95.0 |
Example 3
The method comprises the following steps: 150g of particle size D are weighed 50 100 μm boron carbide (boron carbide content: 90%), 50g particle diameter D 50 Boron carbide at 20 μm (boron carbide content 90%), and 31.58g of propolis (38% effective solids), 8g of aluminum dihydrogen phosphate (40% strength), 1.2g of sodium citrate were added to form a mixture;
step two: adding a proper amount of distilled water into the mixture obtained in the step one, stirring the mixture by using a stirrer until the mixture is fully and uniformly stirred, and vacuumizing the mixture for 60min at the room temperature under the vacuum degree of 10Pa to form slurry;
step three: guiding the slurry obtained in the step two into a gypsum mold cavity for casting molding, demolding and taking a blank, drying the blank at the temperature of 60-90 ℃ for 5-7 h, wherein the size of the blank is
Step four: and (3) firing the green body obtained in the third step by adopting a vacuum furnace, wherein the firing process temperature curve (shown in figure 2) is as follows: heating from room temperature at a heating rate of 10 deg.C/min for 36min to 350 deg.C, and maintaining at constant temperature for 30min; heating at a speed of 6 deg.C/min for 50min to 650 deg.C, and maintaining at constant temperature for 20min; then heating at a speed of 6 ℃/min for 45min to 920 ℃, and keeping the constant temperature for 30min; and finally, cooling to room temperature along with the furnace to obtain the boron carbide porous ceramic.
Air pressure curve (as shown in FIG. 2), vacuum degree of 10 -3 ～10 3 Pa, at a gas pressure of 2X 10 2 Degreasing at about 2X 10Pa, 10 -1 About 6X 10Pa for glue removal, 10 -2 ～6×10 -2 And Pa sintering and forming.
The detection result of the performance of the negative pressure fired boron carbide porous ceramic is as follows:
example 4
The difference from example 3 is that:
step four: and (3) firing the green body obtained in the third step by adopting a vacuum furnace, wherein the firing process temperature curve (shown in figure 3) is as follows: heating from room temperature at a heating rate of 6.5 deg.C/min for 50min to 350 deg.C, and maintaining at constant temperature for 20min; heating at a speed of 5 deg.C/min for 60-650 deg.C for 20min; then heating at a speed of 6 ℃/min for 45min to 920 ℃, and keeping the constant temperature for 30min; and finally, cooling to room temperature along with the furnace.
Air pressure curve (as shown in fig. 3): before raising the temperature, vacuumizing in the furnace to keep the air pressure below 5X 10 -3 Pa, 0min, filling argon gas to adjust the pressure to 1 × 10 3 Pa, constant pressure to 50min, firing time from 50min to 70min, regulating pressure to 10Pa, constant pressure to 130min, firing time from 130min to 150min, and regulating pressure to 3 × 10 -2 Pa, and keeping constant pressure until the firing is finished (the temperature is within 100 ℃), thus preparing the boron carbide porous ceramic.
The detection result of the performance of the negative pressure fired boron carbide porous ceramic is as follows:
comparative example 4
The difference from example 3 is that:
step four: and (4) firing the green body obtained in the step three, wherein the firing process is normal pressure.
The detection result of the performance of the boron carbide porous ceramic fired under normal pressure is as follows:
although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the true spirit and scope of the present invention, which is defined by the appended claims.
Claims (1)
1. The preparation method of the rapid sintering porous ceramic is characterized by comprising the following steps:
the method comprises the following steps: 150g of particle size D are weighed 50 Boron carbide of 100 μm, 50g particle diameter D 50 Boron carbide at 20 μm and added 31.58g of propolis, 8g of aluminum dihydrogen phosphate, 1.2g of sodium citrate to form a mixture; wherein the content of boron carbide is 90%, the effective solid content of the propolis is 38%, and the concentration of the aluminum dihydrogen phosphate is 40%;
step two: adding a proper amount of distilled water into the mixture obtained in the step one, stirring the mixture by using a stirrer until the mixture is fully and uniformly stirred, and vacuumizing the mixture for 60min at the room temperature and the vacuum degree of 10Pa to form slurry;
step three: introducing the slurry obtained in the second step into a gypsum mold cavity, casting and molding, demolding, taking a blank, drying the blank at 60 to 90 ℃ for 5 to 7 hours, wherein the size of the blank is phi 40 mm multiplied by 30 mm;
step four: firing the green body obtained in the step three by adopting a vacuum furnace, wherein the firing process temperature curve is as follows: heating from room temperature at a heating rate of 10 deg.C/min for 36min to 350 deg.C, and maintaining at constant temperature for 30min; heating at a speed of 6 deg.C/min for 50-650 deg.C, and maintaining at constant temperature for 20min; heating at 6 deg.C/min for 45min to 920 deg.C for 30min; finally, cooling to room temperature along with the furnace to prepare the boron carbide porous ceramic;
air pressure curve, vacuum degree of 10 -3 ~10 3 Pa, at a gas pressure of 2X 10 2 Degreasing at 2 × 10Pa, 10% -1 6 x 10Pa for glue removal, 10 -2 ~6×10 -2 And Pa sintering and forming.
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