CN103102160A - Microwave sintering method for preparing beta-Sialon powder by using coal ash - Google Patents
Microwave sintering method for preparing beta-Sialon powder by using coal ash Download PDFInfo
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Abstract
The invention discloses a microwave sintering method for preparing beta-Sialon powder by using coal ash. The microwave sintering method comprises the following steps of: adding 3-6 percent of Y2O3 sintering auxiliary agents to the beta-Sialon powder prepared from the coal ash, and ultrasonically mixing in an anhydrous alcohol medium for 1 hour to prepare slurry; then drying the slurry, and then adding 2-5 percent of polyvinyl alcohol, namely a PVA (Polyvinyl Alcohol) forming adhesive; granulating, screening, carrying out mould pressing, then carrying out isostatic pressing, and carrying out binder removal on a formed sample in a muffle furnace at 450-650 DEG C for 1-4 hours; and then heating to 1450-1600 DEG C under the condition of powder burying by utilizing microwaves, preserving heat for 15-40 minutes, and then naturally cooling to room temperature to prepare a sintered product which has good property. The microwave sintering method disclosed by the invention can be used for synthesizing the beta-Sialon powder by utilizing an industrial waste, namely the coal ash, can realize the flash sintering of the beta-Sialon powder at a low temperature within a short time in cooperation with a microwave sintering process and has the advantages of waste utilization realization, easiness in operation, low energy consumption and cost reduction.
Description
Technical field
The present invention relates to a kind of method of utilizing industrial solid castoff to prepare advanced ceramics material, particularly a kind of microwave sintering method with the standby beta-Sialon powder of coal ash for manufacturing.
Background technology
(general general formula is Si to beta-Sialon
6-zAl
zO
zN
8-z0＜Z≤4.2 wherein) be the most excellent a kind of of Sialon pottery family performance, have good erosion resistance, resistance to sudden heating, hot strength and chemical stability etc., and with molten metal, extraordinary blending is arranged, be difficult for being corroded, be widely used in fields such as fire-resistant, corrosion-resistant, machinofacture.
The industrial preparative method commonly used of beta-Sialon material is with high-purity Al
2O
3, Si
3N
4, AlN, SiO
2, Si powder etc. is synthetic for the raw material high temperature solid state reaction; Flyash is the main solid waste that firepower electrical plant is discharged, and the annual flyash total amount of discharging of China is greater than 100,000,000 tons, if reasonably do not develop, not only contaminate environment, also cause the wasting of resources.The main ingredient of flyash is also SiO
2And Al
2O
3, and close with the stoichiometric ratio of beta-Sialon, be one of desirable feedstock of preparation beta-Sialon.
At present, the common sintering method of beta-Sialon pottery is the technology such as hot pressing sintering method, conventional pressureless sintering method, plasma activated sintering, and the sintering temperature of its requirement is higher, thus the long sintering high cost that caused of soaking time; Microwave Sintering Techniques has developed into a kind of novel powder metallurgy Fast Sintering technology gradually since being introduced into the advanced ceramics field eighties; It is to be that it utilizes the dielectric loss of material internal to generate heat that microwave heating is different from the conventional heating part, it is a kind of " globality " heating, sample itself can be considered thermal source, conventional heating is to utilize thermal conduction inwardly to be heated by outer thermal source, microwave heating has advantages of that conventional heating can't realize, as rate of heating and sintering velocity energy-conservation, that be exceedingly fast; The microwave sintering research report of relevant beta-Sialon pottery is also few, especially utilizes the research of the microwave sintering process of the standby beta-Sialon powder of industrial solid castoff coal ash for manufacturing to there is not yet relevant report.
" utilizing the method for microwave technology sintering Sialon carborundum refractory material " is provided in the Chinese invention patent application of publication number for CN200510086915.X, the method uses raw material to be silicon nitride, silica flour, aluminum oxide powder, what utilize the microwave technology preparation is Sialon based on silicon carbide matrix material, is different from the present invention.
Characteristics of the present invention are: by utilizing Microwave Sintering Techniques, the beta-Sialon powder of the preparation take industrial solid castoff flyash as raw material is carried out sintering, obtain well behaved sintered article.
Summary of the invention
The purpose of this invention is to provide a kind of microwave sintering method for preparing the beta-Sialon powder take industrial solid castoff flyash as raw material.
The present invention is take flyash as main raw material, by the synthetic Si of carbothermal reduction-nitridation method
4Al
2O
2N
6(beta-Sialon, z=2) mass percentage content greater than 96% Sialon powder, utilizes this powder to carry out microwave sintering, and concrete steps are:
(1) flyash is mixed according to mass ratio 100:30 with the reductive agent gac after, be that 0.5 liter/min of clock, purity are under 99.9% flowing nitrogen atmosphere at flow, in 1450 ℃ of insulations obtained in 6 hours the z value be 2 and mass percentage content be Si greater than 96% beta-Sialon
4Al
2O
2N
6Powder.
(2) after the beta-Sialon powder that step (1) is made is crossed 0.074 mm sieve, mix quality and be the Y of the rear powder quality 3 ~ 6% of sieving
2O
3Sintering aid, then the ultrasonic mixing of normal temperature made slip in 1 hour in anhydrous ethanol medium.
(3) slip that step (2) is made is placed in common loft drier and dried 24 hours under 80 ℃, makes dried powder.
(4) add quality in the dried powder that step (3) makes and be polyvinyl alcohol (PVA) molding adhesive of powder quality 2 ~ 5% after dry, grind granulation in mortar, the powder that granulation is good is crossed 60 mesh sieves, use subsequently common tabletting machine normal temperature presuppression under the pressure of 10 ~ 25MPa to get the premolding base substrate, then gained premolding idiosome is made molding blank with iso-static pressure shaping machine normal temperature isostatic pressing under the forming pressure of 50 ~ 150MPa.
(5) molding blank that step (6) is made temperature rise rate with 1 ~ 2.5 ℃/minute in retort furnace rises to 450 ~ 650 ℃, is incubated 1 ~ 4 hour to get rid of the PVA molding adhesive, namely completes binder removal.
(6) molding blank after step (5) binder removal being placed in microwave agglomerating furnace, is 60%SiC+30%Si with mass percent
3N
4The powder mix of+10%BN carries out powder embedded sintering, the operating frequency of microwave agglomerating furnace is 2.45GHz, power input is continuous adjustable by 100 ~ 1500 watts, the temperature rise rate of controlling this step by the power input of regulating microwave agglomerating furnace is 25 ~ 40 ℃/minute, sintering temperature is 1450 ~ 1600 ℃, soaking time is 15 ~ 40 minutes, and then naturally cooling to and namely making the volume density size after room temperature is 2.80 ~ 2.95gcm
-3, vickers microhardness is 1466 ~ 1563 beta-Sialon powder sintering goods.
The present invention is by the application to industrial solid castoff, alleviate environmental pollution, improve the sintering process of beta-Sialon, reduce energy consumption, the beta-Sialon sintered article that processability is good overcome the problems such as traditional normal pressure-sintered and gas pressure sintering heating efficiency is low, sintering temperature is high, sintering time is long, and this technological operation is simple, production cost is low, is conducive to industrial mass manufacture.
Embodiment
The below will enumerate some embodiments of the invention, and in the following example, flyash used is from the power station, Guilin, and its main chemical constitution is (mass percent):
| Composition | SiO 2 | Al 2O 3 | Fe 2O 3 | TiO 2 | CaO | MgO | K 2O | Na 2O | Loss on ignition |
| Flyash | 55.95 | 25.71 | 1.31 | 2.77 | 3.73 | 1.48 | 2.84 | 1.16 | 4.61 |
Embodiment 1:
(1) flyash is mixed according to mass percent 100:30 with the reductive agent gac after, be that 0.5 liter/min of clock, purity are under 99.9% flowing nitrogen atmosphere at flow, in 1450 ℃ of insulations obtained in 6 hours the z value be 2 and mass percentage content be Si greater than 96% beta-Sialon
4Al
2O
2N
6Powder;
(2) after the beta-Sialon powder that step (1) is made is crossed 0.074 mm sieve, mix quality and be the Y of rear opaque amount 3% of sieving
2O
3Sintering aid, then the ultrasonic mixing of normal temperature made slip in 1 hour in anhydrous ethanol medium;
(3) slip that step (2) is made is placed in common loft drier and dried 24 hours under 80 ℃, makes dried powder;
(4) add quality in the dried powder that step (3) makes and be the PVA molding adhesive of powder quality 3% after dry, grind granulation in mortar, the powder that granulation is good is crossed 60 mesh sieves, get the premolding base substrate with common tabletting machine normal temperature presuppression under the pressure of 20MPa subsequently, then gained premolding idiosome is made molding blank with iso-static pressure shaping machine normal temperature isostatic pressing under the forming pressure of 100MPa;
(5) molding blank that step (6) is made temperature rise rate with 1.5 ℃/minute in retort furnace rises to 550 ℃, is incubated 4 hours to get rid of the PVA molding adhesive, namely completes binder removal;
(6) molding blank after step (5) binder removal being placed in microwave agglomerating furnace, is 60%SiC+30%Si with mass percent
3N
4The powder mix of+10%BN carries out powder embedded sintering, the operating frequency of microwave agglomerating furnace is 2.45GHz, the temperature rise rate of controlling this step by the power input of regulating microwave agglomerating furnace is 30 ℃/minute, sintering temperature is 1450 ℃, soaking time is 20 minutes, namely makes beta-Sialon powder sintering goods after then naturally cooling to room temperature.
The resulting product volume density is 2.80 gcm
-3, vickers microhardness (HV
0.5) be 1466.
Embodiment 2:
(1) flyash is mixed according to mass percent 100:30 with the reductive agent gac after, be that 0.5 liter/min of clock, purity are under 99.9% flowing nitrogen atmosphere at flow, in 1450 ℃ of insulations obtained in 6 hours the z value be 2 and mass percentage content be Si greater than 96% beta-Sialon
4Al
2O
2N
6Powder;
(2) after the beta-Sialon powder that step (1) is made is crossed 0.074 mm sieve, mix quality and be the Y of rear opaque amount 3% of sieving
2O
3Sintering aid, then the ultrasonic mixing of normal temperature made slip in 1 hour in anhydrous ethanol medium;
(3) slip that step (2) is made is placed in common loft drier and dried 24 hours under 80 ℃, makes dried powder;
(4) add quality in the dried powder that step (3) makes and be the PVA molding adhesive of powder quality 3% after dry, grind granulation in mortar, the powder that granulation is good is crossed 60 mesh sieves, get the premolding base substrate with common tabletting machine normal temperature presuppression under the pressure of 20MPa subsequently, then gained premolding idiosome is made molding blank with iso-static pressure shaping machine normal temperature isostatic pressing under the forming pressure of 100MPa;
(5) molding blank that step (6) is made temperature rise rate with 1.5 ℃/minute in retort furnace rises to 550 ℃, is incubated 4 hours to get rid of the PVA molding adhesive, namely completes binder removal;
(6) molding blank after step (5) binder removal being placed in microwave agglomerating furnace, is 60%SiC+30%Si with mass percent
3N
4The powder mix of+10%BN carries out powder embedded sintering, the operating frequency of microwave agglomerating furnace is 2.45GHz, the temperature rise rate of controlling this step by the power input of regulating microwave agglomerating furnace is 30 ℃/minute, sintering temperature is 1500 ℃, soaking time is 30 minutes, namely makes beta-Sialon powder sintering goods after then naturally cooling to room temperature.
Resulting product volume density size is 2.86 gcm
-3, vickers microhardness (HV
0.5) be 1528.
Embodiment 3:
(1) flyash is mixed according to mass percent 100:30 with the reductive agent gac after, be that 0.5 liter/min of clock, purity are under 99.9% flowing nitrogen atmosphere at flow, in 1450 ℃ of insulations obtained in 6 hours the z value be 2 and mass percentage content be Si greater than 96% beta-Sialon
4Al
2O
2N
6Powder;
(2) after the beta-Sialon powder that step (1) is made is crossed 0.074 mm sieve, mix quality and be the Y of rear opaque amount 6% of sieving
2O
3Sintering aid, then the ultrasonic mixing of normal temperature made slip in 1 hour in anhydrous ethanol medium;
(3) slip that step (2) is made is placed in common loft drier and dried 24 hours under 80 ℃, makes dried powder;
(4) add quality in the dried powder that step (3) makes and be the PVA molding adhesive of powder quality 5% after dry, grind granulation in mortar, the powder that granulation is good is crossed 60 mesh sieves, get the premolding base substrate with common tabletting machine normal temperature presuppression under the pressure of 20MPa subsequently, then gained premolding idiosome is made molding blank with iso-static pressure shaping machine normal temperature isostatic pressing under the forming pressure of 100MPa;
(5) molding blank that step (6) is made temperature rise rate with 1.5 ℃/minute in retort furnace rises to 550 ℃, is incubated 4 hours to get rid of the PVA molding adhesive, namely completes binder removal;
(6) molding blank after step (5) binder removal being placed in microwave agglomerating furnace, is 60%SiC+30%Si with mass percent
3N
4The powder mix of+10%BN carries out powder embedded sintering, the operating frequency of microwave agglomerating furnace is 2.45GHz, the temperature rise rate of controlling this step by the power input of regulating microwave agglomerating furnace is 35 ℃/minute, sintering temperature is 1550 ℃, soaking time is 30 minutes, namely makes beta-Sialon powder sintering goods after then naturally cooling to room temperature.
Resulting product volume density size is 2.91gcm
-3, vickers microhardness (HV
0.5) be 1543.
Embodiment 4:
(1) flyash is mixed according to mass percent 100:30 with the reductive agent gac after, be that 0.5 liter/min of clock, purity are under 99.9% flowing nitrogen atmosphere at flow, in 1450 ℃ of insulations obtained in 6 hours the z value be 2 and mass percentage content be Si greater than 96% beta-Sialon
4Al
2O
2N
6Powder;
(2) after the beta-Sialon powder that step (1) is made is crossed 0.074 mm sieve, mix quality and be the Y of rear opaque amount 3% of sieving
2O
3Sintering aid, then the ultrasonic mixing of normal temperature made slip in 1 hour in anhydrous ethanol medium;
(3) slip that step (2) is made is placed in common loft drier and dried 24 hours under 80 ℃, makes dried powder;
(4) add quality in the dried powder that step (3) makes and be the PVA molding adhesive of powder quality 3% after dry, grind granulation in mortar, the powder that granulation is good is crossed 60 mesh sieves, get the premolding base substrate with common tabletting machine normal temperature presuppression under the pressure of 20MPa subsequently, then gained premolding idiosome is made molding blank with iso-static pressure shaping machine normal temperature isostatic pressing under the forming pressure of 100MPa;
(5) molding blank that step (6) is made temperature rise rate with 1.5 ℃/minute in retort furnace rises to 550 ℃, is incubated 4 hours to get rid of the PVA molding adhesive, namely completes binder removal;
(6) molding blank after step (5) binder removal being placed in microwave agglomerating furnace, is 60%SiC+30%Si with mass percent
3N
4The powder mix of+10%BN carries out powder embedded sintering, the operating frequency of microwave agglomerating furnace is 2.45GHz, the temperature rise rate of controlling this step by the power input of regulating microwave agglomerating furnace is 40 ℃/minute, sintering temperature is 1550 ℃, soaking time is 40 minutes, namely makes beta-Sialon powder sintering goods after then naturally cooling to room temperature.
Resulting product volume density size is 2.95gcm
-3, vickers microhardness (HV
0.5) be 1563.
Claims (1)
1. microwave sintering method with the standby beta-Sialon powder of coal ash for manufacturing is characterized in that concrete steps are:
(1) flyash is mixed according to mass ratio 100:30 with the reductive agent gac after, be that 0.5 liter/min of clock, purity are under 99.9% flowing nitrogen atmosphere at flow, in 1450 ℃ of insulations obtained in 6 hours the z value be 2 and mass percentage content be Si greater than 96% beta-Sialon
4Al
2O
2N
6Powder;
(2) after the beta-Sialon powder that step (1) is made is crossed 0.074 mm sieve, mix quality and be the Y of the rear powder quality 3 ~ 6% of sieving
2O
3Sintering aid, then the ultrasonic mixing of normal temperature made slip in 1 hour in anhydrous ethanol medium;
(3) slip that step (2) is made is placed in common loft drier and dried 24 hours under 80 ℃, makes dried powder;
(4) adding quality in the dried powder that step (3) makes is that after drying, the polyvinyl alcohol of powder quality 2 ~ 5% is the PVA molding adhesive, grind granulation in mortar, the powder that granulation is good is crossed 60 mesh sieves, use subsequently common tabletting machine normal temperature presuppression under the pressure of 10 ~ 25MPa to get the premolding base substrate, then gained premolding idiosome is made molding blank with iso-static pressure shaping machine normal temperature isostatic pressing under the forming pressure of 50 ~ 150MPa;
(5) molding blank that step (6) is made temperature rise rate with 1 ~ 2.5 ℃/minute in retort furnace rises to 450 ~ 650 ℃, is incubated 1 ~ 4 hour to get rid of the PVA molding adhesive, namely completes binder removal;
(6) molding blank after step (5) binder removal being placed in microwave agglomerating furnace, is 60%SiC+30%Si with mass percent
3N
4The powder mix of+10%BN carries out powder embedded sintering, the operating frequency of microwave agglomerating furnace is 2.45GHz, power input is continuous adjustable by 100 ~ 1500 watts, the temperature rise rate of controlling this step by the power input of regulating microwave agglomerating furnace is 25 ~ 40 ℃/minute, sintering temperature is 1450 ~ 1600 ℃, soaking time is 15 ~ 40 minutes, and then naturally cooling to and namely making the volume density size after room temperature is 2.80 ~ 2.95gcm
-3, vickers microhardness is 1466 ~ 1563 beta-Sialon powder sintering goods.
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Cited By (7)
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|---|---|---|---|---|
| CN104402455A (en) * | 2014-10-30 | 2015-03-11 | 高坚珂 | Manufacturing method of sialon ceramic oil gas combustion tail gas treatment device |
| CN108147379A (en) * | 2018-01-04 | 2018-06-12 | 吉林大学 | A kind of flyash acid dissolution slag prepares the method for matching grand powder |
| CN111635236A (en) * | 2020-05-26 | 2020-09-08 | 南京理工大学 | Method for microwave sintering of sialon ceramic material |
| CN112661512A (en) * | 2020-12-23 | 2021-04-16 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature |
| CN113443920A (en) * | 2021-07-12 | 2021-09-28 | 长飞光纤光缆股份有限公司 | Powder granulation and tabletting method |
| CN114956838A (en) * | 2022-06-02 | 2022-08-30 | 山东工业陶瓷研究设计院有限公司 | Preparation method of anode support body for SOFC (solid oxide Fuel cell) |
| CN115849925A (en) * | 2022-12-30 | 2023-03-28 | 江苏材睿科技有限公司 | Preparation method of pressureless sintering refractory material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402455A (en) * | 2014-10-30 | 2015-03-11 | 高坚珂 | Manufacturing method of sialon ceramic oil gas combustion tail gas treatment device |
| CN108147379A (en) * | 2018-01-04 | 2018-06-12 | 吉林大学 | A kind of flyash acid dissolution slag prepares the method for matching grand powder |
| CN111635236A (en) * | 2020-05-26 | 2020-09-08 | 南京理工大学 | Method for microwave sintering of sialon ceramic material |
| CN112661512A (en) * | 2020-12-23 | 2021-04-16 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature |
| CN113443920A (en) * | 2021-07-12 | 2021-09-28 | 长飞光纤光缆股份有限公司 | Powder granulation and tabletting method |
| CN114956838A (en) * | 2022-06-02 | 2022-08-30 | 山东工业陶瓷研究设计院有限公司 | Preparation method of anode support body for SOFC (solid oxide Fuel cell) |
| CN114956838B (en) * | 2022-06-02 | 2023-10-27 | 山东工业陶瓷研究设计院有限公司 | Preparation method of anode support for SOFC |
| CN115849925A (en) * | 2022-12-30 | 2023-03-28 | 江苏材睿科技有限公司 | Preparation method of pressureless sintering refractory material |
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Application publication date: 20130515 |