CN102180679B - Preparation method of multiphase alpha-beta-Sialon ceramic material added with La2O3 - Google Patents
Preparation method of multiphase alpha-beta-Sialon ceramic material added with La2O3 Download PDFInfo
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- CN102180679B CN102180679B CN 201110030271 CN201110030271A CN102180679B CN 102180679 B CN102180679 B CN 102180679B CN 201110030271 CN201110030271 CN 201110030271 CN 201110030271 A CN201110030271 A CN 201110030271A CN 102180679 B CN102180679 B CN 102180679B
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Abstract
The invention provides a preparation method of a multiphase alpha-beta-Sialon ceramic material added with La2O3, and belongs to the technical field of metallurgic refractory materials. The invention prepares a multiphase alpha-beta-Sialon ceramic material with excellent performance by adding rare earth oxides La2O3 and Nd2O3. The preparation method mainly includes: well mixing the used materials Si powder, Al powder, Al2O3 powder, Y2O3, La2O3, Nd2O3 and performing compression molding to obtain a green body of the alpha-beta-Sialon ceramic material; sintering the green body in a graphite resistance furnace with a sintering temperature increased from room temperature to 1750 DEG C and a heating rate of 30 DEG C/min; when the sintering temperature reaches 400 DEG C, charging nitrogen into the graphite resistance furnace with a nitrogen flow rate of 3.0 L/min; when the sintering temperature reaches 1750 DEG C, performing heat insulation for 1 hour; cooling the graphite resistance furnace to room temperature to obtain the alpha-beta-Sialon ceramic material. The method of the invention has simple process, low cost, and high nitridation synthesis rate.
Description
Technical field:
The invention belongs to metallurgical technical field of refractory materials, be specifically related to a kind of interpolation La
2O
3The preparation method of multiphase alpha-beta-Sialon ceramic material.
Background technology:
Development along with the modern steel metallurgical technology, particularly blast furnace long service life, continuous casting and Secondary Refining Technology is universal, the duration of contact of high-temperature steel (iron) liquid and metallurgical tank refractory materials is more and more longer, and using single aluminium, silicon, magnesium is that the common anti-material of natural refractory production can not meet the needs of smelting technology and production process far away.Therefore, use the anti-material of high-performance of synthetic and to add the anti-material of high-performance in traditional refractory materials be to improve the refractory materials use properties and improve one of the important means in refractory materials work-ing life.At the Si3N4 base growth Sialon pottery that gets up, because having outstanding mechanical property, thermal property and chemical stability, be the first-selection of high-performance ceramic and high-temperature refractory.But single-phase Sialon pottery only has characteristics separately, and its over-all properties is difficult to adapt to the day by day harsh demand of hi-tech development.Complex phaseization has become the main direction of Sialon stupalith development.Complex phase Sialon introduces other mutually and two-phase or multiphase matrix material that consists of in the Sialon matrix.Utilize the different differences that form on structure and performance to carry out complementation and stack, thereby improve some performance of single-phase Sialon, to satisfy the special requirement of different field development.
The synthetic complex phase alpha-beta of nitrogenize at present-Sialon pottery adopts the single rare earth oxide compound to improve sintering character as sintering aid, cause α-Sialon in material, beta-Sialon phase growing amount is few, nitriding rate is low, affect the physicochemical properties such as its wear resisting property, thermal shock resistance, intensity and hardness, the not good situation of use properties that causes multiphase alpha-beta-Sialon ceramic material can not meet the needs of modern smelting technology and production process.
Summary of the invention:
The above-mentioned single rare earth oxide compound of pin of the present invention balances each other and crystal chemistry knowledge by ceramic system as the synthetic problem that the complex phase alpha-beta-Sialon ceramic nitriding synthetic ratio is low of sintering aid nitrogenize, selects reasonably to form and processing condition, adds rare earth oxide La
2O
3, Y
2O
3And Nd
2O
3Make the multiphase alpha-beta-Sialon ceramic material of excellent property.
A kind of interpolation La provided by the present invention
2O
3Preparation method's concrete steps of multiphase alpha-beta-Sialon ceramic material as follows:
(1) the chemical formula elemental composition according to multiphase alpha-beta-Sialon ceramic material requires to prepare burden, and raw materials used and mass percent is: the Si powder: 60%66%, Al powder: 14.5%-17%, Al
2O
3Powder: 5.6%-8.0%, Y
2O
3: 4%, La
2O
3: 5.7%-7.5%, Nd
2O
3: 4.5%-5.5% obtains the mixing material with raw materials used fully mixing in blender;
(2) the mixing material that step (1) is obtained is poured in agate mortar and is ground take raw spirit as medium, make the mixing material granularity less than 0.44 μ m, add the polyvinyl alcohol solution of mass concentration 7% to be mixed after mixing material drying, after being mixed under 25Mpa pressure compression molding obtain the green compact of alpha-beta-Sialon ceramic material;
The green compact of the alpha-beta-Sialon ceramic material that (3) step (2) is obtained carry out sintering in graphite resistor furnace, sintering temperature is from room temperature to 1750 ℃, temperature rise rate is 30 ℃/min, during sintering temperature to 400 ℃, pass into nitrogen in graphite resistor furnace, nitrogen flow is 3.0L/min, and sintering temperature is incubated when rising to 1750 ℃, be incubated and be cooled to room temperature with graphite resistor furnace after 1 hour, obtain alpha-beta-Sialon ceramic material.
The main chemical reactions of preparation process of the present invention is as follows:
Reaction formula (1):
Si+Al+Al
2O
3+M
2O
3+N
2(g)→MxSi
12-(m+n)Al
m+nO
nN
16-n (1)
Wherein M is Y and lanthanon
Reaction formula (2):
(6-z)Si+(4-0.5z)N
2(g)+z/3Al
2O
3+z/3Al＝Si
(6-z)Al
zO
zN
(8-z) (2)
Composite rare-earth oxide La
2O
3+ Y
2O
3+ Nd
2O
3Be not only the important composition of α-S i al on and generate agent, promote simultaneously α-Sialon transformation of beta-Sialon phase in opposite directions, formed simultaneously α-Sialon and beta-Sialon mutually in synthetic sintering.Compare with adding the single rare earth oxide compound, add the synthetic sintering temperature that composite rare-earth oxide can reduce α-Sialon, beta-Sialon phase significantly, accelerate the liquid phase of α-Sialon, beta-Sialon phase and synthesize and sintering.Composite rare-earth oxide is conducive to form α-Sialon, the beta-Sialon phase of more amount, improves the nitrogenize synthetic ratio of Sialon.
Advantage of the present invention is when preparation alpha-beta-Sialon, and the value that the composition by controlling raw material and proportioning are regulated α/β is added rare earth oxide La
2O
3+ Y
2O
3+ Nd
2O
3, can make the pottery with different densityes and performance.The hardness of alpha-beta-Sialon ceramic material increases along with the increase of α-Sialon phase content, what of beta-Sialon phase content, determining the height of intensity, be that α-Sialon provides high rigidity mutually, beta-Sialon provides high strength mutually, and both are in conjunction with the complex phase ceramic that can obtain having suitable strength and hardness.
This preparation method's technique is simple, cost is lower, the nitrogenize synthetic ratio is high, has larger economic and social benefits.
Embodiment:
Embodiment 1: composition is Si powder 62% (mass percent, lower same), Al powder 16.5%, Al
2O
3Powder 6.8%, Y
2O
3Powder 4%, La
2O
3Powder 6.2%, Nd
2O
34.5%, add the polyvinyl alcohol solution of mass concentration 7% to be mixed, rear compression molding is mixed, sintering in graphite resistor furnace, temperature rise rate is 30 ℃/min, passes into nitrogen when being warming up to 400 ℃, nitrogen flow is 3.0L/min, sintering temperature is incubated when rising to 1750 ℃, is incubated after 1 hour, cools to room temperature with the furnace and takes out the alpha-beta-Sialon ceramic material that makes.This stupalith is through scanning electron microscope and energy spectrum analysis, and the nitrogenize synthetic ratio of complex phase alpha-beta-Sialon reaches 93.2%.
Embodiment 2: the composition of sample is Si powder 63% (mass percent, lower same), Al powder 15.5%, Al
2O
3Powder 5.8%, Y
2O
3Powder 4%, La
2O
3Powder 6.7%, Nd
2O
35.0%, add the polyvinyl alcohol solution of mass concentration 7% to be mixed, rear compression molding is mixed, sintering in graphite resistor furnace, temperature rise rate is 30 ℃/min, passes into nitrogen when being warming up to 400 ℃, nitrogen flow is 3.0L/min, sintering temperature is incubated when rising to 1750 ℃, is incubated after 1 hour, cools to room temperature with the furnace and takes out the alpha-beta-Sialon ceramic material that makes.This stupalith is through scanning electron microscope and energy spectrum analysis, and the nitrogenize synthetic ratio of complex phase alpha-beta-Sialon reaches 94.7%.
Embodiment 3: composition is Si powder 61% (mass percent, lower same), Al powder 17.5%, Al
2O
3Powder 6.8%, Y
2O
3Powder 4%, La
2O
3Powder 5.7%, Nd
2O
35.0%, add the polyvinyl alcohol solution of mass concentration 7% to be mixed, rear compression molding is mixed, sintering in graphite resistor furnace, temperature rise rate is 30 ℃/min, passes into nitrogen when being warming up to 400 ℃, nitrogen flow is 3.0L/min, sintering temperature is incubated when rising to 1750 ℃, is incubated after 1 hour, cools to room temperature with the furnace and takes out the alpha-beta-Sialon ceramic material that makes.This stupalith is through scanning electron microscope and energy spectrum analysis, and the nitrogenize synthetic ratio of complex phase alpha-beta-Sialon reaches 94.1%.
Claims (1)
1. one kind is added La
2O
3The preparation method of multiphase alpha-beta-Sialon ceramic material, it is characterized in that these preparation method's concrete steps are as follows:
(1) the chemical formula elemental composition according to multiphase alpha-beta-Sialon ceramic material requires to prepare burden, and raw materials used and mass percent is: Si powder: 60%-66%, Al powder: 14.5%-17%, Al
2O
3Powder: 5.6%-8.0%, Y
2O
3: 4%, La
2O
3: 5.7%-7.5%, Nd
2O
3: 4.5%-5.5% obtains the mixing material with raw materials used fully mixing in blender;
(2) the mixing material that step (1) is obtained is poured in agate mortar and is ground take raw spirit as medium, make the mixing material granularity less than 0.44 μ m, add the polyvinyl alcohol solution of mass concentration 7% to be mixed after mixing material drying, after being mixed under 25Mpa pressure compression molding obtain the green compact of alpha-beta-Sialon ceramic material;
The green compact of the alpha-beta-Sialon ceramic material that (3) step (2) is obtained carry out sintering in graphite resistor furnace, sintering temperature is from room temperature to 1750 ℃, temperature rise rate is 30 ℃/min, during sintering temperature to 400 ℃, pass into nitrogen in graphite resistor furnace, nitrogen flow is 3.0L/min, and sintering temperature is incubated when rising to 1750 ℃, be incubated and be cooled to room temperature with graphite resistor furnace after 1 hour, obtain alpha-beta-Sialon ceramic material.
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| US6693054B1 (en) * | 2000-11-28 | 2004-02-17 | Kennametal Inc. | Method of making SiAlON containing ytterbium |
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