CN104030664A - Beta-sialon/Al2O3 composite powder and preparation method thereof - Google Patents

Beta-sialon/Al2O3 composite powder and preparation method thereof Download PDF

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CN104030664A
CN104030664A CN201410291499.6A CN201410291499A CN104030664A CN 104030664 A CN104030664 A CN 104030664A CN 201410291499 A CN201410291499 A CN 201410291499A CN 104030664 A CN104030664 A CN 104030664A
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sialon
beta
composite granule
preparation
powder
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CN104030664B (en
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李享成
邓兴
朱伯铨
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention relates to a beta-sialon/Al2O3 composite powder and a preparation method thereof. The technical scheme is as follows: the preparation method comprises the following steps: mixing 40-50 wt% of aluminum oxide powder, 35-45 wt% of silicon powder and 10-20 wt% of aluminum powder used as raw materials with transition group metal accounting for 0.1-3.5 wt% of the raw materials to obtain a mixture; and putting the mixture in a corundum ball milling tank, adding corundum balls and ethanol into the corundum ball milling tank according to the corundum ball:mixture:ethanol mass ratio of (2-3):1:(0.5-1.5), and carrying out ball milling for 2-4 hours; drying at 110 DEG C for 16-36 hours, and calcining at 1100-1300 DEG C in a nitrogen atmosphere for 2-6 hours to obtain the beta-sialon/Al2O3 composite powder. The method has the characteristics of low synthesis temperature, simple technique and high product purity.

Description

A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof
Technical field
The invention belongs to composite granule technical field.Relate in particular to a kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.
Background technology
Beta-Sialon is a kind of sosoloid of antioxidant property in Sialon series, resistance to elevated temperatures and thermostability the best, its linear expansivity [2 ~ 3 × 10 -6(1/ DEG C)] slightly lower than β-Si 3n 4, and thermal conductivity is than β-Si 3n 4much lower, and there is good heat-shock resistance; Beta-Sialon also has good anti-molten iron and slag corrosion, the good performance such as physical strength and hardness.Therefore, beta-Sialon material is widely used in industrial circle.
The industrial preparative method that beta-Sialon material is conventional is with high-purity Si 3n 4, A1 2o 3, A1N and SiO 2for raw material synthesizes by high temperature solid-state method, but cause too high production cost because the method Raw is expensive, and then limited being widely used of beta-Sialon material.Therefore forefathers have done a large amount of research work aspect beta-Sialon material synthetic, the purity that is intended to reduce the production cost of synthetic beta-Sialon material and improves product.
At present, disclosed technology has: " a kind of Sialon composite ceramic material and preparation method thereof " (CN200710052469.x) patented technology, this technical scheme is by aluminium ash, bauxitic clay grog fine powder, SiO 2fine powder, metallic aluminium fine powder and elemental silicon fine powder are mixed in proportion, through stirring aftershaping; Base substrate after moulding is first warmed to 1000-1100 DEG C under nitrogen atmosphere in Reaktionsofen; insulation 0.5-5h; be warmed to 1300-1350 DEG C with the heat-up rate of 2-5 DEG C/min again; insulation 1-6h; then be warmed to 1360-1500 DEG C with the heat-up rate of 2-5 DEG C/min; insulation 2-10h finally naturally cools to room temperature under nitrogen protection, obtains Sialon composite ceramic material.But to be synthetic temperature higher and product impurity is more for the technological deficiency of the method." a kind of method of preparing the beta-Sialon ceramic powder of different Z values with flyash and kaolin " (CN20120508421.6) patented technology, this technology is that 1.08 ~ 1.85 ︰s 1 mix with kaolin according to Si ︰ Al mol ratio in raw material by flyash; Again mixture is mixed according to mass ratio 100 ︰ 25 ~ 45 with gac; Raw material after ball milling, oven dry is under flowing nitrogen atmosphere, and 1400 ~ 1550 DEG C are incubated 2 ~ 8 hours; Then in retort furnace, be incubated 3 hours in 750 DEG C and remove remaining charcoal, make the beta-Sialon ceramic powder of different Z values.The technological deficiency of the method is that complex process and synthesis temperature are high." one is prepared Al with flyash and kyanite 2o 3the method of/beta-Sialon composite granule " (CN201210321568.4) patented technology; be to be less than the industrial waste flyash of 100um and commercially available kyanite mineral as raw material using particle diameter; taking coke as reductive agent; three kinds of raw materials are mixed by a certain percentage; be incubated 1 ~ 6h under the nitrogen atmosphere of 1350 ~ 1500 DEG C, react synthetic Al by carbothermal reduction-nitridation 2o 3/ beta-Sialon composite granule.The technological deficiency of this method is that synthesis temperature is high and product impurity is more.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide the low and simple beta-Sialon/Al of technique of a kind of synthesis temperature 2o 3the preparation method of composite granule.Beta-Sialon/the Al preparing by the method 2o 3composite granule purity is high.
For achieving the above object, the technical solution adopted in the present invention is: taking aluminum oxide powder, the silica flour of 35 ~ 45wt% and the aluminium powder of 10 ~ 20wt% of 40 ~ 50wt% as raw material, the additional magnesium-yttrium-transition metal that accounts for raw material 0.1 ~ 3.5wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1100 ~ 1300 DEG C and nitrogen atmosphere condition, calcine 2 ~ 6 hours, obtain beta-Sialon/Al 2o 3composite granule.
Described aluminum oxide powder is the one in analytical pure aluminum oxide powder, chemical pure aluminum oxide powder and commercial alumina powder, and the particle diameter of aluminum oxide powder is less than 0.149mm.
Described silica flour is the one in analytical pure silica flour, chemical pure silica flour and industrial silica fume, and the particle diameter of silica flour is less than 0.149mm.
Described aluminium powder is the one in analytical pure aluminium powder, chemical pure aluminium powder and industrial aluminium powder, and the particle diameter of aluminium powder is less than 0.149mm.
Described magnesium-yttrium-transition metal is the one in iron, nickel and cobalt; The granularity D of magnesium-yttrium-transition metal 90be 1 ~ 3um, purity>=99wt%.
Described nitrogen atmosphere is: nitrogen pressure 0.02 ~ 0.08Mpa, nitrogen gas purity >=99wt%.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
1, the synthetic preparation temperature of composite granule of the present invention is 1100 ~ 1300 DEG C, therefore synthesis temperature is low.
2, technique of the present invention is divided into following 3 steps: batching; Ball milling; Calcining, therefore technique is simple.
3, beta-Sialon/Al that prepared by the present invention 2o 3composite granule is the composite granule of beta-Sialon and aluminum oxide, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 96 ~ 99wt%; Wherein, the content of beta-Sialon powder is 53 ~ 66wt%.
Therefore, the present invention have that synthesis temperature is low, technique is simple and product purity is high feature.
Brief description of the drawings
Fig. 1 is a kind of beta-Sialon/Al prepared by the present invention 2o 3the XRD figure spectrum of composite granule.
Embodiment
below in conjunction with the drawings and specific embodiments, the present invention will be further described, not the restriction to its protection domain .
for avoiding repetition, first technical parameter unification related this embodiment is described below, in embodiment, repeat no more:
Described aluminum oxide powder is the one in analytical pure aluminum oxide powder, chemical pure aluminum oxide powder and commercial alumina powder, and the particle diameter of aluminum oxide powder is less than 0.149mm.
Described silica flour is the one in analytical pure silica flour, chemical pure silica flour and industrial silica fume, and the particle diameter of silica flour is less than 0.149mm.
Described aluminium powder is the one in analytical pure aluminium powder, chemical pure aluminium powder and industrial aluminium powder, and the particle diameter of aluminium powder is less than 0.149mm.
Granularity D in iron, nickel and cobalt 90be 1 ~ 3um, the purity>=99wt% of iron, nickel and cobalt.
Described nitrogen atmosphere is: nitrogen pressure 0.02 ~ 0.08Mpa, nitrogen gas purity >=99wt%.
embodiment 1
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 35 ~ 40wt% and the aluminium powder of 15 ~ 20wt% of 40 ~ 45wt% as raw material, the additional iron that accounts for raw material 0.1 ~ 1.0wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1200 ~ 1300 DEG C and nitrogen atmosphere condition, calcine 4 ~ 6 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 97 ~ 99wt%; Wherein, the content of beta-Sialon powder is 53 ~ 57wt%.
embodiment 2
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 35 ~ 40wt% and the aluminium powder of 15 ~ 20wt% of 40 ~ 45wt% as raw material, the additional cobalt that accounts for raw material 1.0 ~ 2.0wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1150 ~ 1250 DEG C and nitrogen atmosphere condition, calcine 3 ~ 5 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 98 ~ 99wt%; Wherein, the content of beta-Sialon powder is 56 ~ 59wt%.
embodiment 3
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 35 ~ 40wt% and the aluminium powder of 15 ~ 20wt% of 40 ~ 45wt% as raw material, the additional nickel that accounts for raw material 2.0 ~ 3.5wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1100 ~ 1200 DEG C and nitrogen atmosphere condition, calcine 2 ~ 4 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 98 ~ 99wt%; Wherein, the content of beta-Sialon powder is 60 ~ 64wt%.
embodiment 4
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 40 ~ 45wt% and the aluminium powder of 10 ~ 15wt% of 45 ~ 50wt% as raw material, the additional iron that accounts for raw material 1.0 ~ 2.0wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1100 ~ 1200 DEG C and nitrogen atmosphere condition, calcine 2 ~ 4 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 96 ~ 99wt%; Wherein, the content of beta-Sialon powder is 55 ~ 60wt%.
embodiment 5
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 40 ~ 45wt% and the aluminium powder of 10 ~ 15wt% of 45 ~ 50wt% as raw material, the additional cobalt that accounts for raw material 2.0 ~ 3.5wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1200 ~ 1300 DEG C and nitrogen atmosphere condition, calcine 4 ~ 6 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 96 ~ 99wt%; Wherein, the content of beta-Sialon powder is 57 ~ 62wt%.
embodiment 6
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 40 ~ 45wt% and the aluminium powder of 10 ~ 15wt% of 45 ~ 50wt% as raw material, the additional nickel that accounts for raw material 0.1 ~ 1.0wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1150 ~ 1250 DEG C and nitrogen atmosphere condition, calcine 3 ~ 5 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 96 ~ 99wt%; Wherein, the content of beta-Sialon powder is 62 ~ 66wt%.
embodiment 7
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 37 ~ 42wt% and the aluminium powder of 12 ~ 17wt% of 42 ~ 47wt% as raw material, the additional iron that accounts for raw material 2.0 ~ 3.5wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1200 ~ 1300 DEG C and nitrogen atmosphere condition, calcine 4 ~ 6 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 97 ~ 99wt%; Wherein, the content of beta-Sialon powder is 56 ~ 61wt%.
embodiment 8
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 37 ~ 42wt% and the aluminium powder of 12 ~ 17wt% of 42 ~ 47wt% as raw material, the additional cobalt that accounts for raw material 0.1 ~ 1.0wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1100 ~ 1200 DEG C and nitrogen atmosphere condition, calcine 2 ~ 4 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 97 ~ 99wt%; Wherein, the content of beta-Sialon powder is 58 ~ 61wt%.
embodiment 9
A kind of beta-Sialon/Al 2o 3composite granule and preparation method thereof.Taking aluminum oxide powder, the silica flour of 37 ~ 42wt% and the aluminium powder of 12 ~ 17wt% of 42 ~ 47wt% as raw material, the additional nickel that accounts for raw material 1.0 ~ 2.0wt%, obtains compound.
Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours.Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1150 ~ 1300 DEG C and nitrogen atmosphere condition, calcine 3 ~ 6 hours, obtain beta-Sialon/Al 2o 3composite granule.
Beta-Sialon/Al prepared by the present embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 97 ~ 99wt%; Wherein, the content of beta-Sialon powder is 62 ~ 66wt%.
This embodiment compared with prior art has following positively effect:
1, the synthetic preparation temperature of the composite granule described in this embodiment is 1100 ~ 1300 DEG C, therefore synthesis temperature is low.
2, the technique of this embodiment is divided into following 3 steps: batching; Ball milling; Calcining, therefore technique is simple.
3, beta-Sialon/Al that prepared by this embodiment 2o 3composite granule is the composite granule of beta-Sialon and aluminum oxide.Fig. 1 is a kind of beta-Sialon/Al of preparation in embodiment 9 2o 3the XRD figure spectrum of composite granule.The diffraction peak of (100), (110) by beta-Sialon in Fig. 1, (200), (101), (210) crystal face, calculate its lattice parameter a=b=0.76637nm, c=0.29552nm, and then can calculate its Z=2, can know that to burn after product be Z=2 beta-Sialon and the composite granule of aluminum oxide.
Beta-Sialon/Al prepared by this embodiment 2o 3composite granule, after testing: the total content of the composite granule of beta-Sialon and aluminum oxide is 96 ~ 99wt%; Wherein, the content of beta-Sialon powder is 53 ~ 66wt%.
Therefore, this embodiment have that synthesis temperature is low, technique is simple and product purity is high feature.

Claims (7)

1. a beta-Sialon/Al 2o 3the preparation method of composite granule, is characterized in that aluminum oxide powder, the silica flour of 35 ~ 45wt% and the aluminium powder of 10 ~ 20wt% taking 40 ~ 50wt% is as raw material, and the additional magnesium-yttrium-transition metal that accounts for raw material 0.1 ~ 3.5wt%, obtains compound; Described compound is placed in to corundum ball grinder, then by corundum Qiu ︰ compound: the mass ratio of ethanol is 2 ~ 3: 1: 0.5 ~ 1.5, in corundum ball grinder, add corundum ball and ethanol, ball milling 2 ~ 4 hours; Then under 110 DEG C of conditions dry 16 ~ 36 hours, under 1100 ~ 1300 DEG C and nitrogen atmosphere condition, calcine 2 ~ 6 hours, obtain beta-Sialon/Al 2o 3composite granule.
2. according to beta-Sialon/Al claimed in claim 1 2o 3the preparation method of composite granule, is characterized in that described aluminum oxide powder is the one in analytical pure aluminum oxide powder, chemical pure aluminum oxide powder and commercial alumina powder, and the particle diameter of aluminum oxide powder is less than 0.149mm.
3. according to beta-Sialon/Al claimed in claim 1 2o 3the preparation method of composite granule, is characterized in that described silica flour is the one in analytical pure silica flour, chemical pure silica flour and industrial silica fume, and the particle diameter of silica flour is less than 0.149mm.
4. according to beta-Sialon/Al claimed in claim 1 2o 3the preparation method of composite granule: it is characterized in that described aluminium powder is the one in analytical pure aluminium powder, chemical pure aluminium powder and industrial aluminium powder, the particle diameter of aluminium powder is less than 0.149mm.
5. according to beta-Sialon/Al claimed in claim 1 2o 3the preparation method of composite granule: it is characterized in that described magnesium-yttrium-transition metal is the one in iron, nickel and cobalt; The granularity D of magnesium-yttrium-transition metal 90be 1 ~ 3um, purity>=99wt%.
6. according to beta-Sialon/Al claimed in claim 1 2o 3the preparation method of composite granule: it is characterized in that described nitrogen atmosphere is: nitrogen pressure 0.02 ~ 0.08Mpa, nitrogen gas purity>=99wt%.
7. a beta-Sialon/Al 2o 3composite granule, is characterized in that described beta-Sialon/Al 2o 3composite granule is according to the beta-Sialon/Al described in any one in claim 1 ~ 6 2o 3prepared beta-Sialon/the Al of preparation method of composite granule 2o 3composite granule.
CN201410291499.6A 2014-06-26 2014-06-26 A kind of beta-Sialon/Al2O3Composite granule and its preparation method Expired - Fee Related CN104030664B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108727043A (en) * 2018-06-11 2018-11-02 武汉科技大学 A kind of low-carbon aluminum-carbon refractory material and preparation method thereof with multidimensional enhancing

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CN1686922A (en) * 2005-03-29 2005-10-26 郑州大学 Method for preparing composite material combined with corundum based on bauxite beta-Sialon
CN101748488A (en) * 2009-12-21 2010-06-23 中国地质大学（北京） Novel rare-earth Ln-Sialon mono-crystal and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1552669A (en) * 2003-06-02 2004-12-08 贵州工业大学 Cylon-corundum powdery material and its production
CN1562884A (en) * 2004-04-16 2005-01-12 清华大学 Fe-Sialon multiphase material of shock resistant and wearproof in high temperature and preparation method
CN1686922A (en) * 2005-03-29 2005-10-26 郑州大学 Method for preparing composite material combined with corundum based on bauxite beta-Sialon
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* Cited by examiner, † Cited by third party
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