CN103288436B - Method for synthetizing fused cast by combustion of MgAl2O4 ceramic - Google Patents

Method for synthetizing fused cast by combustion of MgAl2O4 ceramic Download PDF

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CN103288436B
CN103288436B CN201310213521.0A CN201310213521A CN103288436B CN 103288436 B CN103288436 B CN 103288436B CN 201310213521 A CN201310213521 A CN 201310213521A CN 103288436 B CN103288436 B CN 103288436B
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pottery
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mgal
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CN103288436A (en
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郑永挺
杨攀
赫晓东
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Harbin Institute of Technology
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Abstract

The invention discloses a method for synthetizing a fused cast by combustion of MgAl2O4 ceramic, relates to a method for synthetizing the fused cast by combustion of the MgAl2O4 ceramic, and aims at solving the technical problems of high cost, complicated process and environmental pollution of the traditional MgAl2O4 ceramic. Reactants in the method disclosed by the invention are Al and nitrate; diluents are Al2O3 and MgO; the materials are ignited to react through combustion and heat release of the Al and the nitrate; the experimental process is fast; the reaction time is less than 10 minutes. Thus, the method is short in preparation cycle, low in cost, high in purity of obtained product, simple in experimental process, and easy to control and operate. The temperature and the pressure of a system can be controlled by controlling the content of the diluents; each ingredient is controlled to meet the required ratio when the safety of the experiment is ensured; an external heat source is not needed; the system is heated by the heat release of reaction. Thus, the cost is low; no toxic gas is generated; the method can be applied to the field of preparation of the MgAl2O4 ceramic.

Description

A kind of MgAl 2o 4the method of the synthetic founding of burning of pottery
Technical field
The present invention relates to a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery.
Background technology
MgAl 2o 4as high-melting-point refractory oxide (Tm=2100 DEG C), at MgO-Al 2o 3in binary system, it is unique a kind of compound that can stable existence, and its good mechanical performance, chemical resistance of concrete excellence, good thermal shock (comparing with corundum with its composition phase periclasite), refractoriness under load is high, and slag resistance is good and creep-resistant property is good, thereby has a wide range of applications in high-temperature structural ceramics, refractory materials, electronic industry and optical device field.
MgAl 2o 4pottery can obtain by the step such as powder process and sintering, and in recent years, investigator has researched and developed several different methods and prepared MgAl 2o 4nano-powder, [Li J g, Ikegami T, Lee J H, the et al.A wet-chemical process yielding reactive magnesium aluminate spinel (MgAl such as Li 2o 4) powder.Ceram.Int., 2001,27 (4): 481-489.] prepare the MgAl that particle size is less than 100nm by coprecipitation method 2o 4powder.Coprecipitation method is simple, cheap preparation method, but prepared powder hard aggregation is seriously unfavorable for sintering.Shiono[Shiono T, Shiono K, Miyamoto K, et al.Synthesis and characterization of (MgAl2O4) spinel precursor from a heterogeneous alkoxide solution containing fine MgO powder.J.Am.Ceram.Soc., 2000,83 (1): 235-237.], Ye[Ye g, Oprea g, Troczynski T.Synthesis of MgAl 2o 4spinel powder by combination of Sol-gel and precipitation processes.J.Am.Ceram.Soc., 2005, 88 (11): 3241-3244.] and Saberi[Saberi A, golestani-Fard F, Willert-Porada M, et al.A novel approach to synthesis of nanosize MgAl2O4 spinel powder through S ol-gel citrate technique and subsequent heat treatment.Ceram.Int., 2009, 35 (3): 933-937.] etc. prepared superfine Mg Al by sol-gel method 2o 4powder, and realized sintering densification at 1400 DEG C.Nano-powder size prepared by sol-gel method is little, reunites light, but alkoxide price comparison costliness used, and the high and complicated process of preparation of cost.Investigator has also developed macromolecule network method, and Pechini method is prepared MgAl 2o 4nano-powder, prepared nano-powder particle is tiny, narrow size distribution, reunion are few, but can emit a large amount of SO in preparation process x, NO xtoxic gas, these gas serious environment pollutions, therefore aforesaid method can not be used for preparing in batches MgAl 2o 4nano-powder.Except wet chemistry method, Physical is also used to prepare MgAl 2o 4nano-powder.Common Physical is high-energy ball milling method, utilizes high energy ball mill in reactant system, to introduce high-energy, thereby reduces the needed temperature of solid state reaction.High-energy ball milling method is simple to operate, but the powder reuniting of preparation is serious, is unfavorable for sintering.
Existing one section of title and author who is published in APPLIED SURFACE SCIENCE for 2011 is (" Microstructure and mechanism of Al 2o 3– ZrO 2eutectic coating prepared by combustion-assisted thermal explosion spraying " author: Yongting Zheng, Hongbo Li, Tao Zhou) document, in the document, adopt detonation flame spraying to prepare Al 2o 3/ ZrO 2eutectic coating, separately having one section of title and author who is published in JOURNAL OF ALLOYS AND COMPOUNDS for 2012 is (" Microstructure and mechanical properties of Al 2o 3/ ZrO 2eutectic ceramic composites prepared by explosion synthesis " author: Yongting Zheng, Hongbo Li, Tao Zhou, Jing Zhao, Pan Yang) document, in the document, adopt the synthetic Al that prepared of blast 2o 3/ ZrO 2eutectic ceramic, but aforesaid method all has following shortcoming: and (1) reaction pressure is large, in 30～100MPa scope, has blast impulse effect simultaneously, and very large (2) the product size of preparation technology's danger is little, is Φ 20*40mm to the maximum 3.
Summary of the invention
The present invention is for solving existing MgAl 2o 4high, the complex process of cost of pottery and have the technical problem of environmental pollution, and a kind of MgAl is provided 2o 4the method of the synthetic founding of burning of pottery.
A kind of MgAl of the present invention 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, nitrate is placed on to independent drying treatment in loft drier, obtains nitrate reaction agent;
Two, Al powder is placed on to drying treatment in vacuum drying oven, obtains Al powder reagent;
Three, thinner is placed on to drying treatment in vacuum drying oven, obtains thinner; Wherein said thinner is by Al 2o 3with MgO composition, and the Al in system after reaction 2o 3with the mol ratio of MgO be 1:1;
Four, the thinner that nitrate reaction agent step 1 being obtained, the Al powder reagent that step 2 obtains and step 3 obtain, mix by ball milling, then pack in reaction unit, light raw material, the thermopositive reaction of burning, reaction times <10min, temperature of reaction <4300K, in reaction pressure <10MPa reaction process, get rid of the gas in reaction system, obtain MgAl 2o 4pottery; The mol ratio of the Al powder reagent that the nitrate reaction agent that wherein step 1 described in step 4 obtains and step 2 obtain is 3:(16～24), the ratio of the thinner that wherein in the step 1 described in step 4, in nitrate reaction agent and step 2, the quality sum of metal-powder reagent and step 3 obtain is 1:(0.536～1.008).
The reagent of the inventive method is Al and nitrate, and thinner is Al 2o 3and MgO, light raw material, burning heat release by Al and nitrate is reacted, method of the present invention has the following advantages: (1) rapid heating systems temperature of burning thermopositive reaction by metal-powder and nitrate is to more than the fusing point of all substances in system, by the percentage composition of strict control thinner, more than hierarchy of control temperature remains on the fusing point of all substances in system, this reaction is the controlled combustion reactions of speed; (2) under without centrifugal, high temperature, large-sized condition, can pass through the gas that the methods such as mechanical shock, ultrasonic vibration or induction stirring are got rid of systems, make ceramic dense; (3), under centrifugal condition, setting centrifugal force is 10g～500g, can obtain fully dense as-cast structure, through fast cooling, solidify getable large-sized MgAl 2o 4pottery, its crystalline ceramics is at infrared transmitance >80%, and at the transmitance >80% of shortwave, ceramic size is large; (4) add excessive Al powder reagent, in reaction, can neutralize nitrogen, reaction is carried out under normal pressure or very low pressure, reaction pressure is 0.1MPa～10MPa, and reaction pressure is low, can fully ensure the security of producing; (5) speed of synthesis process is controlled, but rapidly synthetic compared to traditional technology, efficiency is high, reaction times changes with the size of production product, the difference of synthesis technique, be generally 1min～10min, preparation cycle is short and cost is low, and products therefrom purity is high; (6) experimentation is simple, easy to control, by controlling the temperature and pressure that the content of thinner can the hierarchy of control, when ensureing the safety of experiment and control each composition and meet required ratio; (7) without external heat source, rely on reaction self heat release heating systems, cost is low, and does not produce toxic gas, can be applicable to MgAl 2o 4the preparation field of pottery.
Embodiment
Technical scheme of the present invention is not limited to following embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of MgAl of present embodiment 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, nitrate is placed on to independent drying treatment in loft drier, obtains nitrate reaction agent;
Two, Al powder is placed on to drying treatment in vacuum drying oven, obtains Al powder reagent;
Three, thinner is placed on to drying treatment in vacuum drying oven, obtains thinner; Wherein said thinner is by Al 2o 3with MgO composition, and the Al in system after reaction 2o 3with the mol ratio of MgO be 1:1;
Four, the thinner that nitrate reaction agent step 1 being obtained, the Al powder reagent that step 2 obtains and step 3 obtain, mix by ball milling, then pack in reaction unit, light raw material, the thermopositive reaction of burning, reaction times <10min, temperature of reaction <4300K, in reaction pressure <10MPa reaction process, get rid of the gas in reaction system, obtain MgAl 2o 4pottery; The mol ratio of the Al powder reagent that the nitrate reaction agent that wherein step 1 described in step 4 obtains and step 2 obtain is 3:(16～24), the ratio of the thinner that wherein in the step 1 described in step 4, in nitrate reaction agent and step 2, the quality sum of metal-powder reagent and step 3 obtain is 1:(0.536～1.008).
The reactional equation of present embodiment is as follows:
16Al+3Mg(NO 3) 2→5Al 2O 3+3MgO+6AlN (1)
8Al+Al(NO 3) 3→3AlN+3Al 2O 3(2)
Or (1) (2) mixing (Mg (NO between the two 3) 2and Al (NO 3) 3);
The reagent of the method for present embodiment is Al and nitrate, and thinner is Al 2o 3and MgO, light raw material, burning heat release by Al and nitrate is reacted, the method of present embodiment has the following advantages: (1) rapid heating systems temperature of burning thermopositive reaction by metal-powder and nitrate is to more than the fusing point of all substances in system, by the percentage composition of strict control thinner, more than hierarchy of control temperature remains on the fusing point of all substances in system, this reaction is the controlled combustion reactions of speed; (2) under without centrifugal, high temperature, large-sized condition, can pass through the gas that the methods such as mechanical shock, ultrasonic vibration or induction stirring are got rid of systems, make ceramic dense; (3), under centrifugal condition, setting centrifugal force is 10g～500g, can obtain fully dense as-cast structure, through fast cooling, solidify getable large-sized MgAl 2o 4pottery, its crystalline ceramics is at infrared transmitance >80%, and at the transmitance >80% of shortwave, ceramic size is large; (4) add excessive Al powder reagent, in reaction, can neutralize nitrogen, reaction is carried out under normal pressure or very low pressure, reaction pressure is 0.1MPa～10MPa, and reaction pressure is low, can fully ensure the security of producing; (5) speed of synthesis process is controlled, but rapidly synthetic compared to traditional technology, efficiency is high, reaction times changes with the size of production product, the difference of synthesis technique, be generally 1min～10min, preparation cycle is short and cost is low, and products therefrom purity is high; (6) experimentation is simple, easy to control, by controlling the temperature and pressure that the content of thinner can the hierarchy of control, when ensureing the safety of experiment and control each composition and meet required ratio; (7) without external heat source, rely on reaction self heat release heating systems, cost is low, and does not produce toxic gas, can be applicable to MgAl 2o 4the preparation field of pottery.
Embodiment two: present embodiment is different from embodiment one: the nitrate reaction agent described in step 1 is Mg (NO 3) 2and Al (NO 3) 3in one or both mixture.Other step and parameter are identical with embodiment one.
When nitrate reaction agent in present embodiment is mixture, both are with arbitrarily than mixing.
Embodiment three: present embodiment is different from embodiment one or two: the drying treatment described in step 1 is by being under the condition of 50～70 DEG C in temperature, and be that 8h～12h realizes time of drying.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: the drying treatment described in step 2 is by being under the condition of 70～90 DEG C in temperature, and be that 8h～12h realizes time of drying.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: the drying treatment described in step 3 is by being under the condition of 70～90 DEG C in temperature, and be that 8h～12h realizes time of drying.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: the ball milling described in step 4 is by under the condition that is 3:1 at ball material mass ratio, ball milling mixing 4h～6h realizes.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: in step 4, temperature of reaction is 2300K～4300K.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: in step 4, reaction pressure is 0.1MPa～10MPa.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight: the gas of getting rid of in the reaction process described in step 4 in reaction system is by under the condition without centrifugal, adopts mechanical shock, ultrasonic vibration or induction stirring to realize.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine: the gas of getting rid of in the reaction process described in step 4 in reaction system is by under centrifugal condition, reaction unit is arranged in centrifugation systems, and setting centrifugal force is that 10g～500g realizes; Described centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.Other step and parameter are identical with one of embodiment one to nine.
With following verification experimental verification beneficial effect of the present invention:
Embodiment 1, a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, by Mg (NO 3) 26H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and be 10h time of drying, obtains Mg (NO 3) 2;
Two, Al is placed in vacuum drying oven and is dried, drying temperature is 80 DEG C, and be 10h time of drying;
Three, by Al 2o 3be placed in vacuum drying oven and be dried with MgO, drying temperature is 80 DEG C, and be 10h time of drying;
Four, take the Mg (NO that 77.8g step 1 obtains 3) 2, 75.5g the step 2 Al, the Al that 95g step 3 obtains that obtain 2o 3the MgO obtaining with 51.7g step 3, by ball milling mixing 5h, ball material mass ratio is 3:1, then packs in reaction unit, reaction unit is arranged in centrifugation systems, setting centrifugal force is 50g, then lights raw material, the thermopositive reaction of burning, reaction times is 10min, temperature of reaction is 3200K, and reaction pressure is 2MPa, obtains being of a size of Φ 100mmMgAl 2o 4pottery; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
Embodiment 2, a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, by Mg (NO 3) 26H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and be 10h time of drying, obtains Mg (NO 3) 2;
Two, Al is placed in vacuum drying oven and is dried, drying temperature is 80 DEG C, and be 10h time of drying;
Three, by Al 2o 3be placed in vacuum drying oven and be dried with MgO, drying temperature is 80 DEG C, and be 10h time of drying;
Four, take the Mg (NO that 81.8g step 1 obtains 3) 2, 79.3g the step 2 Al, the Al that 88.9g step 3 obtains that obtain 2o 3the MgO obtaining with 50.0g step 3, by ball milling mixing 5h, ball material mass ratio is 3:1, then packs in reaction unit, reaction unit is arranged in centrifugation systems, setting centrifugal force is 50g, then lights raw material, the thermopositive reaction of burning, reaction times is 10min, temperature of reaction is 3400K, and reaction pressure is 3MPa, obtains being of a size of Φ 150mmMgAl 2o 4pottery; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
Embodiment 3, a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, by Mg (NO 3) 26H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and be 10h time of drying, obtains Mg (NO 3) 2;
Two, Al is placed in vacuum drying oven and is dried, drying temperature is 80 DEG C, and be 10h time of drying;
Three, by Al 2o 3be placed in vacuum drying oven and be dried with MgO, drying temperature is 80 DEG C, and be 10h time of drying;
Four, take the Mg (NO that 85.7g step 1 obtains 3) 2, 83.1g the step 2 Al, the Al that 82.9g step 3 obtains that obtain 2o 3the MgO obtaining with 48.3g step 3, by ball milling mixing 5h, ball material mass ratio is 3:1, then packs in reaction unit, reaction unit is arranged in centrifugation systems, setting centrifugal force is 50g, then lights raw material, the thermopositive reaction of burning, reaction times is 10min, temperature of reaction is 3600K, and reaction pressure is 3MPa, obtains being of a size of Φ 200mmMgAl 2o 4pottery; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
Embodiment 4, a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, by Mg (NO 3) 26H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and be 10h time of drying, obtains Mg (NO 3) 2;
Two, Al is placed in vacuum drying oven and is dried, drying temperature is 80 DEG C, and be 10h time of drying;
Three, by Al 2o 3be placed in vacuum drying oven and be dried with MgO, drying temperature is 80 DEG C, and be 10h time of drying;
Four, take the Mg (NO that 89.6g step 1 obtains 3) 2, 86.9g the step 2 Al, the Al that 76.9g step 3 obtains that obtain 2o 3the MgO obtaining with 46.6g step 3, by ball milling mixing 5h, ball material mass ratio is 3:1, then packs in reaction unit, reaction unit is arranged in centrifugation systems, setting centrifugal force is 200g, then lights raw material, the thermopositive reaction of burning, reaction times is 10min, temperature of reaction is 3800K, and reaction pressure is 3MPa, obtains being of a size of the transparent MgAl of Φ 200mm 2o 4pottery; Wherein said centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
Embodiment 5, a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, by Mg (NO 3) 26H 2o is placed in loft drier dry separately, and drying temperature is 60 DEG C, and be 10h time of drying, obtains Mg (NO 3) 2;
Two, Al is placed in vacuum drying oven and is dried, drying temperature is 80 DEG C, and be 10h time of drying;
Three, by Al 2o 3be placed in vacuum drying oven and be dried with MgO, drying temperature is 80 DEG C, and be 10h time of drying;
Four, take the Mg (NO that 85.7g step 1 obtains 3) 2, 83.1g the step 2 Al, the Al that 82.9g step 3 obtains that obtain 2o 3the MgO obtaining with 48.3g step 3, by ball milling mixing 5h, ball material mass ratio is 3:1, then packs in reaction unit, lights raw material, the thermopositive reaction of burning, reaction times is 10min, and temperature of reaction is 3600K, and reaction pressure is 5MPa, by the gas in mechanical vibration eliminating system, obtain being of a size of the MgAl of Φ 300mm 2o 4pottery.

Claims (9)

1. a MgAl 2o 4the method of the synthetic founding of burning of pottery, is characterized in that a kind of MgAl 2o 4the method of the synthetic founding of burning of pottery is carried out according to the following steps:
One, nitrate is placed on to independent drying treatment in loft drier, obtains nitrate reaction agent; Nitrate reaction agent described in step 1 is Mg (NO 3) 2and Al (NO 3) 3in one or both mixture;
Two, Al powder is placed on to drying treatment in vacuum drying oven, obtains Al powder reagent;
Three, thinner is placed on to drying treatment in vacuum drying oven, obtains thinner; Wherein said thinner is by Al 2o 3with MgO composition, and the Al in system after reaction 2o 3with the mol ratio of MgO be 1:1;
Four, the thinner that nitrate reaction agent step 1 being obtained, the Al powder reagent that step 2 obtains and step 3 obtain, mix by ball milling, then pack in reaction unit, light raw material, the thermopositive reaction of burning, reaction times <10min, temperature of reaction <4300K, in reaction pressure <10MPa reaction process, get rid of the gas in reaction system, obtain MgAl 2o 4pottery; The mol ratio of the Al powder reagent that the nitrate reaction agent that wherein step 1 described in step 4 obtains and step 2 obtain is 3:(16～24), the ratio of the thinner that wherein in the step 1 described in step 4, in nitrate reaction agent and step 2, the quality sum of metal-powder reagent and step 3 obtain is 1:(0.536～1.008).
2. a kind of MgAl according to claim 1 2o 4the method of the synthetic founding of burning of pottery, is characterized in that the drying treatment described in step 1 is by being that under the condition of 50～70 DEG C, be that 8h～12h realizes time of drying in temperature.
3. a kind of MgAl according to claim 1 and 2 2o 4the method of the synthetic founding of burning of pottery, is characterized in that the drying treatment described in step 2 is by being that under the condition of 70～90 DEG C, be that 8h～12h realizes time of drying in temperature.
4. a kind of MgAl according to claim 3 2o 4the method of the synthetic founding of burning of pottery, is characterized in that the drying treatment described in step 3 is by being that under the condition of 70～90 DEG C, be that 8h～12h realizes time of drying in temperature.
5. a kind of MgAl according to claim 3 2o 4the method of the synthetic founding of burning of pottery, is characterized in that the ball milling described in step 4 is by under the condition that is 3:1 at ball material mass ratio, and ball milling mixing 4h～6h realizes.
6. a kind of MgAl according to claim 3 2o 4the method of the synthetic founding of burning of pottery, is characterized in that in step 4 that temperature of reaction is for being more than or equal to 2300K and being less than 4300K.
7. a kind of MgAl according to claim 3 2o 4the method of the synthetic founding of burning of pottery, is characterized in that in step 4 that reaction pressure is for being more than or equal to 0.1MPa and being less than 10MPa.
8. a kind of MgAl according to claim 3 2o 4the method of the synthetic founding of burning of pottery, is characterized in that the gas of getting rid of in reaction system in the reaction process described in step 4 is by under the condition without centrifugal, adopts mechanical shock, ultrasonic vibration or induction stirring to realize.
9. a kind of MgAl according to claim 3 2o 4the method of the synthetic founding of burning of pottery, is characterized in that the gas of getting rid of in reaction system in the reaction process described in step 4 is by under centrifugal condition, and reaction unit is arranged in centrifugation systems, and setting centrifugal force is that 10g～500g realizes; Described centrifugation systems has circulating water cooling device, portfire, electric heater unit, temperature testing device and pressure test device.
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