CN103601500B - SiAlON ceramic containing crystalline phase Y4SiAlO8N, and preparation method and application thereof - Google Patents
SiAlON ceramic containing crystalline phase Y4SiAlO8N, and preparation method and application thereof Download PDFInfo
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- CN103601500B CN103601500B CN201310515280.5A CN201310515280A CN103601500B CN 103601500 B CN103601500 B CN 103601500B CN 201310515280 A CN201310515280 A CN 201310515280A CN 103601500 B CN103601500 B CN 103601500B
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- 229910003564 SiAlON Inorganic materials 0.000 title claims abstract description 124
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 title abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 41
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000011268 mixed slurry Substances 0.000 claims abstract description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 14
- 238000005238 degreasing Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 3
- 239000003960 organic solvent Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 29
- 238000002425 crystallisation Methods 0.000 claims description 27
- 230000008025 crystallization Effects 0.000 claims description 27
- 229910052727 yttrium Inorganic materials 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000012798 spherical particle Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 229910052581 Si3N4 Inorganic materials 0.000 abstract 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000000748 compression moulding Methods 0.000 abstract 1
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 73
- 230000003078 antioxidant effect Effects 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000011863 silicon-based powder Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910002795 Si–Al–O–N Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910018509 Al—N Inorganic materials 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical group [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a SiAlON ceramic containing crystalline phase Y4SiAlO8N. In the crystalline phase structure of the ceramic, main phase crystals mainly comprise alpha-SiAlON or an alpha-SiAlON and beta-SiAlON composite phase, Y4SiAlO8N exists in the crystal boundary of the main phase crystals, an alpha phase contains alpha-Si3N4, and a beta phase contains beta-Si3N4. A preparation method of the SiAlON ceramic comprises the following steps: uniformly mixing raw materials according to a ratio, adding an organic solvent and an adhesive, and ball-milling to obtain a mixed slurry; carrying out spray drying granulation of the mixed slurry, carrying out compression molding, and degreasing to form a green compact; and pre-burning the green compact in nitrogen atmosphere, carrying out furnace cooling, carrying out sintering heat-insulation of the obtained pre-burned body in the nitrogen atmosphere, and carrying out furnace cooling to obtain the SiAlON ceramic. The SiAlON ceramic has a good high-temperature stability and a good oxidation resistance.
Description
Technical field
The invention belongs to technical field of ceramic material, particularly relate to a kind of SiAlON containing crystallization phases pottery and its preparation method and application.
Background technology
SiAlON pottery is come out in early 1970s, is developed rapidly afterwards, becomes important high-temperature structural material gradually.It is with Si
3n
4for the general name of the class sosoloid in the Si-Al-O-N system of base and related system, basic structural unit is (Si, Al) (O, N) tetrahedron.
Si
3n
4be covalent linkage crystal, self-diffusion coefficient is very little, is not easy densified sintering product, needs to add MgO, CaO, Y
2o
3deng and some rare-earth oxides as sintering aid.In sintering process, these sintering aids under the high temperature conditions can with Si
3n
4contained SiO in powder
2liquid phase, acceleransstoff transmitting procedure, acceleration of sintering densification is formed Deng impurity.With Si
3n
4unlike, the phase can enter lattice formation SiAlON phase to the Transient liquid phase ion that SiAlON pottery is formed in sintering process after sintering, crystal boundary is purified, is conducive to the high-temperature behavior improving material.
SiAlON material can be divided into α-SiAlON, β-SiAlON, O-SiAlON etc. according to the difference of structure and component, and wherein the above two are the most important in Tool Industry.The general formula of α-SiAlON is generally M
x(Si, Al)
12(O, N)
16, 0<x<2, more Accurate Points can be written as M
xsi
12-m-nal
m+no
nn
16-n, wherein x≤2, have m Al-N key and n Al-O key to instead of (m+n) individual Si-N key in each unit cell.If the valence state of Mc is v, then according to electric neutrality, x=m/v, a chemical reaction that may produce this sosoloid is:
1/3(12-m-n)Si
3N
4+1/3(4m+n)AlN+(m/2v)Me
2O
v+1/6(2n-m)Al
2O
3 →α-Me
m/vSi
12-m-nAl
m+nO
nN
16-n
The general formula of β-SiAlON is Si
6-zal
zo
zn
8-z, 0<z<4.2, not containing other ion in its lattice, a kind of chemical reaction that may produce this sosoloid is: (2-z/3) α-Si
3n
4+ (z/3) AlN+ (z/3) Al
2o
3 →β-Si
6-zal
zo
zn
8-z.
α-SiAlON phase hardness is high, and toughness is poor, mostly is equi-axed crystal; β-SiAlON phase good toughness, difference of hardness, mostly is Elongated grain.And α/β-SiAlON composite ceramics can in conjunction with the features of α-SiAlON with β-SiAlON, over-all properties is better, and the advantage such as the cutting tool adopting this complex phase ceramic to prepare has that wear resistance is high, thermal-shock resistance good, easy densification, Application Areas are wide, at present for the processing of the materials such as cast iron, nickel-base alloy, cobalt base alloy, high-aluminium alloy, high mangaenese steel, it is a kind of ceramic cutting tool material had wide application prospects.
CN101133001A Chinese patent literature discloses a kind of by Si
3n
4for the SiAlON ceramic body that the mixture of main raw material is made, this SiAlON ceramic body comprises: the two-phase mixture containing α '-SiAlON and β '-SiAlON phase, and containing one or more selected rare earth elements in α '-SiAlON.Described SiAlON material can contain α principal phase (or α ' phase) and β principal phase (or β ' phase), and one or more other phases, such as glassy phase and/or crystallization phases.The chemical formula of α '-SiAlON phase can be M
xsi
12-(m+n)al
m+no
nn
16-n, wherein, M is Li, Ca, Y or other lanthanon, and the maximum theoretical of x is 2,0<n≤2.0,0.9≤m≤3.5.The chemical formula of β '-SiAlON can be Si
6-zal
zo
zn
8-z, wherein 0<z≤4.2.When M is yttrium, crystallization phases can comprise: YAG(yttrium aluminum garnet, and this is a kind of formula is Y
3al
5o
12emission in Cubic), YAM(this be a kind of formula be Y
4al
2o
9monocline crystalline phase), N-YAM(this be a kind of formula be Y
4si
2o
7n
2monocline crystalline phase), and Y-N-α-wollastonite (this is a kind of formula is YSiO
2the monocline crystalline phase of N).
Existing SiAlON sintex, be mainly used in superalloy high speed cutting, it has high requirement to mechanical behavior under high temperature, therefore, its high-temperature behavior of further raising (such as hot hardness, toughness, heat-shock resistance) is then the unremitting effort direction of association area expert.
Y
4siAlO
8n(J-Phase) be the sosoloid that YAM phase mixes by 1:1 with N-YAM two-phase, it has high fusing point and antioxidant property.Dirk Matusch Ph D dissertation " is mentioned in Phasenuntersuchungen im System Y-Si-Al-O-N: at Si
3n
4or SiAlON pottery intergranular place, when there being appropriate Y
4siAlO
8when N exists, then can improve high-temperature stability and the antioxidant property of this stupalith.But, along with crystallization phases Y
4siAlO
8the increase of N content, the toughness of SiAlON pottery can decline.Dirk Matusch Ph D dissertation does not mention how control Y
4siAlO
8the content of N, and the high-temperature stability and the antioxidant property that improve SiAlON sintex.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, provides a kind of high temperature stability performance and oxidation-resistance to contain crystallization phases Y
4siAlO
8n SiAlON pottery, also corresponding provide this contain crystallization phases Y
4siAlO
8the preparation method of the SiAlON pottery of N and embody rule.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of containing crystallization phases Y
4siAlO
8the SiAlON pottery of N, in the crystal phase structure of described SiAlON pottery, SiAlON is principal phase crystal, there is crystallization phases Y at the grain boundaries of principal phase crystal
4siAlO
8n, and principal phase crystal SiAlON is mainly α-SiAlON, or be α-SiAlON and β-SiAlON compound phase, include α-Si in described α-SiAlON
3n
4, in described β-SiAlON, include β-Si
3n
4.
Above-mentioned contains crystallization phases Y
4siAlO
8the SiAlON pottery of N, as further optimization, described SiAlON pottery after carrying out X-ray diffraction, α-SiAlON peak intensity near 2 θ=34.2 ° be X, β-SiAlON near 2 θ=33.5 ° peak intensity Y, Y
4siAlO
8the peak intensity Z of N near 2 θ=29.4 °, and Y/X=0 ~ 18(is particularly preferably 0.4 ~ 6), Z/X=0.05 ~ 2(is particularly preferably 0.1 ~ 1.0).
As a total technical conceive, the present invention also provides a kind of preparation method of above-mentioned SiAlON pottery, comprises the following steps:
(1) with Si, Si
3n
4, Al
2o
3, AlN and Y
2o
3powder as material powder, by proportioning, each material powder is mixed, adds organic solvent (such as ethanol) and tackiness agent (such as polyoxyethylene glycol), ball milling mixing after obtain mixed slurry;
(2) mixed slurry that step (1) obtains is carried out spray-drying process, obtain spherical particle powder, more repressed shaping, degreasing, obtains green compact;
(3) green compact that step (2) obtains are inserted in a container (described container is preferably the crystal vessel that scribbles BN), then pre-burning is carried out in a nitrogen atmosphere, it is 1250 DEG C ~ 1550 DEG C that calcined temperature controls, nitrogen partial pressure 1 ~ 3 normal atmosphere, burn-in time 2 ~ 10 hours, obtain nitride and account for overall weight more than 90%, then furnace cooling, obtain pre-burning body;
(4) the pre-burning body that step (3) obtains is inserted in a container (described container is preferably the crystal vessel that scribbles BN), then sinter in a nitrogen atmosphere, it is 1650 DEG C ~ 1950 DEG C that sintering temperature controls, soaking time is 1 ~ 8 hour, 1200 DEG C are cooled to subsequently by 1 ~ 12 DEG C/min speed, furnace cooling again, obtains SiAlON pottery.
Above-mentioned preparation method, in described material powder, the massfraction proportion optimization of each material is as follows:
Si and Si
3n
4total mass account for 50% ~ 90% of material powder total mass;
Al
2o
3account for 1% ~ 15% of material powder total mass;
AlN accounts for 5% ~ 30% of material powder total mass;
Y
2o
3account for 2% ~ 20% of material powder total mass;
Material powder quality summation is 100%.
Wherein, described Si and Si
3n
4mass ratio be preferably 70:30 ~ 90:10.
In above-mentioned preparation method of the present invention, mainly consider too high oxygen level and too fast rate of temperature fall to generating crystallization phases Y
4siAlO
8n is unfavorable, has therefore given prominence to the key points with Si powder for raw material and control oxide content in preparation technology, reduces the rate of cooling in technological process as far as possible simultaneously.
The invention has the advantages that: SiAlON stupalith of the present invention for principal crystalline phase, exists crystallization phases Y between its crystalline phase with SiAlON phase
4siAlO
8n, and crystallization phases Y
4siAlO
8the content of N controls at 0.5% ~ 1.2%(massfraction), due to crystallization phases Y
4siAlO
8n has high fusing point and antioxidant property, when it exists Si
3n
4or SiAlON pottery intergranular place, then can improve high-temperature stability and the antioxidant property of this stupalith, and not containing crystallization phases Y
4siAlO
8the SiAlON ceramic phase ratio that N, other composition are basically identical, the present invention, by the further improvement of formula adjustment and sintering process, makes crystallization phases Y
4siAlO
8the content of N is controlled, and makes the high-temperature stability of product and antioxidant property improve 15% ~ 35%, the cutting tool be prepared into by this material, and when cutting superalloy, work-ing life extends 30% ~ 40%, and material cost is reduced.
Accompanying drawing explanation
Fig. 1 is sample microcosmic electronic scanning structure back scattering figure.
Fig. 2 is the X-x ray diffration pattern x of the embodiment of the present invention 1 product.
Fig. 3 is the X-x ray diffration pattern x of the embodiment of the present invention 2 product.
Fig. 4 is the X-x ray diffration pattern x of the embodiment of the present invention 3 product.
Fig. 5 is the X-x ray diffration pattern x of the embodiment of the present invention 4 product.
Embodiment
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but protection domain not thereby limiting the invention.
embodiment 1:
A kind of of the present invention containing crystallization phases Y
4siAlO
8the SiAlON pottery of N, in the crystal phase structure of SiAlON pottery, SiAlON is principal phase crystal, there is crystallization phases Y at the grain boundaries of principal phase crystal
4siAlO
8n, and principal phase crystal SiAlON is mainly α-SiAlON and β-SiAlON compound phase, includes α-Si in α-SiAlON
3n
4, in β-SiAlON, include β-Si
3n
4(see figure 1).The present embodiment SiAlON pottery after carrying out X-ray diffraction, α-SiAlON peak intensity near 2 θ=34.2 ° be X, β-SiAlON near 2 θ=33.5 ° peak intensity Y, Y
4siAlO
8the peak intensity Z of N near 2 θ=29.4 °, and Y/X=4.79, Z/X=0.79.
The preparation method of the present embodiment SiAlON pottery, comprises the following steps:
(1) by Si powder 67wt%, α-Si
3n
4powder 12wt%, Al
2o
3powder 4wt%, AlN powder 8.5wt%, Y
2o
3powder 8.5wt% takes weight, above powder particle size D
50=1 μm, then each material powder is placed in ball grinder, add alcohol solvent and tackiness agent, through mixing of ball mill pulverizing and appropriate time, obtain the mixed slurry mixed;
(2) the mixed slurry spray granulating and drying device that step (1) obtains is carried out spray-drying process, obtain spherical particle powder, more repressed shaping, degreasing, obtains green compact;
(3) green compact that step (2) obtains are inserted scribble in the crystal vessel of BN, pre-burning in nitrogen atmosphere stove, calcined temperature 1550 DEG C, nitrogen partial pressure 1.5 normal atmosphere, burn-in time 4 hours, accounts for overall weight more than 90% be as the criterion to obtain nitrogenize object, then furnace cooling, obtains pre-burning body;
(4) inserted by the pre-burning body that step (3) obtains and scribble in the crystal vessel of BN, sinter in a nitrogen atmosphere, sintering temperature 1900 DEG C, soaking time is 1.5h, and be cooled to 1200 DEG C by 10 DEG C/min speed subsequently, furnace cooling obtains SiAlON ceramic product.
After tested, the diffracting spectrum of the present embodiment finished product as shown in Figure 2, wherein Y/X=4.79, Z/X=0.79.The present embodiment finished product Vickers' hardness (18.5kg load) is more than or equal to about 17.5Gpa, and fracture toughness property is more than or equal to about 6.8MpaM
1/2.Resistance toheat can improve 15% ~ 20%, and antioxidant property can improve 30% ~ 35%.
embodiment 2:
A kind of of the present invention containing crystallization phases Y
4siAlO
8the SiAlON pottery of N, in the crystal phase structure of SiAlON pottery, SiAlON is principal phase crystal, there is crystallization phases Y at the grain boundaries of principal phase crystal
4siAlO
8n, and principal phase crystal SiAlON is mainly α-SiAlON and β-SiAlON compound phase, includes α-Si in α-SiAlON
3n
4, in β-SiAlON, include β-Si
3n
4(can see Fig. 1).The present embodiment SiAlON pottery after carrying out X-ray diffraction, α-SiAlON peak intensity near 2 θ=34.2 ° be X, β-SiAlON near 2 θ=33.5 ° peak intensity Y, Y
4siAlO
8the peak intensity Z of N near 2 θ=29.4 °, and Y/X=0.84, Z/X=0.32.
The preparation method of the present embodiment SiAlON pottery, comprises the following steps:
(1) by Si powder 67wt%, α-Si
3n
4powder 12wt%, Al
2o
3powder 4wt%, AlN powder 8.5wt%, Y
2o
3powder 8.5wt% takes weight, above powder particle size D
50=1 μm, then each material powder is placed in ball grinder, add alcohol solvent and tackiness agent, through mixing of ball mill pulverizing and appropriate time, obtain the mixed slurry mixed;
(2) the mixed slurry spray granulating and drying device that step (1) obtains is carried out spray-drying process, obtain spherical particle powder, more repressed shaping, degreasing, obtains green compact;
(3) green compact that step (2) obtains are inserted scribble in the crystal vessel of BN, pre-burning in nitrogen atmosphere stove, calcined temperature 1550 DEG C, nitrogen partial pressure 1.5 normal atmosphere, burn-in time 4 hours, accounts for overall weight more than 90% be as the criterion to obtain nitrogenize object, then furnace cooling, obtains pre-burning body;
(4) inserted by the pre-burning body that step (3) obtains and scribble in the crystal vessel of BN, sinter in a nitrogen atmosphere, sintering temperature 1900 DEG C, soaking time is 1.5h, and be cooled to 1200 DEG C by 5 DEG C/min speed subsequently, furnace cooling obtains SiAlON ceramic product.
After tested, the diffracting spectrum of the present embodiment finished product as shown in Figure 3, wherein Y/X=0.84, Z/X=0.32.The present embodiment finished product Vickers' hardness (18.5kg load) is more than or equal to about 18.5Gpa, and fracture toughness property is more than or equal to about 6.6MpaM
1/2, resistance toheat can improve 20% ~ 30%, and antioxidant property can improve 15% ~ 25%.
embodiment 3:
A kind of of the present invention containing crystallization phases Y
4siAlO
8the SiAlON pottery of N, in the crystal phase structure of SiAlON pottery, SiAlON is principal phase crystal, there is crystallization phases Y at the grain boundaries of principal phase crystal
4siAlO
8n, and principal phase crystal SiAlON is mainly α-SiAlON and β-SiAlON compound phase, includes α-Si in α-SiAlON
3n
4, in β-SiAlON, include β-Si
3n
4(can see Fig. 1).The present embodiment SiAlON pottery after carrying out X-ray diffraction, α-SiAlON peak intensity near 2 θ=34.2 ° be X, β-SiAlON near 2 θ=33.5 ° peak intensity Y, Y
4siAlO
8the peak intensity Z of N near 2 θ=29.4 °, and Y/X=0, Z/X=0.32.
The preparation method of the present embodiment SiAlON pottery, comprises the following steps:
(1) by Si powder 54.4wt%, α-Si
3n
4powder 9.6wt%, Al
2o
3powder 4.5wt%, AlN powder 19.5wt%, Y
2o
3powder 12wt% takes weight, above powder particle size D
50=1 μm, then each material powder is placed in ball grinder, add alcohol solvent and tackiness agent, through mixing of ball mill pulverizing and appropriate time, obtain the mixed slurry mixed;
(2) the mixed slurry spray granulating and drying device that step (1) obtains is carried out spray-drying process, obtain spherical particle powder, more repressed shaping, degreasing, obtains green compact;
(3) green compact that step (2) obtains are inserted scribble in the crystal vessel of BN, pre-burning in nitrogen atmosphere stove, calcined temperature 1550 DEG C, nitrogen partial pressure 1.5 normal atmosphere, burn-in time 4 hours, accounts for overall weight more than 90% be as the criterion to obtain nitrogenize object, then furnace cooling, obtains pre-burning body;
(4) inserted by the pre-burning body that step (3) obtains and scribble in the crystal vessel of BN, sinter in a nitrogen atmosphere, sintering temperature 1900 DEG C, soaking time is 1.5h, and be cooled to 1200 DEG C by 10 DEG C/min speed subsequently, furnace cooling obtains SiAlON ceramic product.
After tested, the diffracting spectrum of the present embodiment finished product as shown in Figure 4, wherein Y/X=0, Z/X=0.18.The present embodiment finished product Vickers' hardness (18.5kg load) is more than or equal to about 19.5Gpa, and fracture toughness property is more than or equal to about 6.2MpaM
1/2, resistance toheat can improve 25% ~ 35%, and antioxidant property can improve 20% ~ 30%.
embodiment 4:
A kind of of the present invention containing crystallization phases Y
4siAlO
8the SiAlON pottery of N, in the crystal phase structure of SiAlON pottery, SiAlON is principal phase crystal, there is crystallization phases Y at the grain boundaries of principal phase crystal
4siAlO
8n, and principal phase crystal SiAlON is mainly α-SiAlON and β-SiAlON compound phase, includes α-Si in α-SiAlON
3n
4, in β-SiAlON, include β-Si
3n
4(can see Fig. 1).The present embodiment SiAlON pottery after carrying out X-ray diffraction, α-SiAlON peak intensity near 2 θ=34.2 ° be X, β-SiAlON near 2 θ=33.5 ° peak intensity Y, Y
4siAlO
8the peak intensity Z of N near 2 θ=29.4 °, and Y/X=0.84, Z/X=0.32.
The preparation method of the present embodiment SiAlON pottery, comprises the following steps:
(1) by Si powder 54.4wt%, α-Si
3n
4powder 9.6wt%, Al
2o
3powder 4.5wt%, AlN powder 19.5wt%, Y
2o
3powder 12wt% takes weight, above powder particle size D
50=1 μm, then each material powder is placed in ball grinder, add alcohol solvent and tackiness agent, through mixing of ball mill pulverizing and appropriate time, obtain the mixed slurry mixed;
(2) the mixed slurry spray granulating and drying device that step (1) obtains is carried out spray-drying process, obtain spherical particle powder, more repressed shaping, degreasing, obtains green compact;
(3) green compact that step (2) obtains are inserted scribble in the crystal vessel of BN, pre-burning in nitrogen atmosphere stove, calcined temperature 1550 DEG C, nitrogen partial pressure 1.5 normal atmosphere, burn-in time 4 hours, accounts for overall weight more than 90% be as the criterion to obtain nitrogenize object, then furnace cooling, obtains pre-burning body;
(4) inserted by the pre-burning body that step (3) obtains and scribble in the crystal vessel of BN, sinter in a nitrogen atmosphere, sintering temperature 1900 DEG C, soaking time is 1.5h, and be cooled to 1200 DEG C by 5 DEG C/min speed subsequently, furnace cooling obtains SiAlON ceramic product.
After tested, the diffracting spectrum of the present embodiment finished product as shown in Figure 5, wherein Y/X=0.1, Z/X=0.26.The present embodiment finished product Vickers' hardness (18.5kg load) is more than or equal to about 17Gpa, and fracture toughness property is more than or equal to about 6.9MpaM
1/2, resistance toheat can improve 22% ~ 32%, and antioxidant property can improve 30% ~ 35%.
Claims (5)
1. one kind contains crystallization phases Y
4siAlO
8the SiAlON pottery of N, in the crystal phase structure of described SiAlON pottery, SiAlON is principal phase crystal, it is characterized in that: there is crystallization phases Y at the grain boundaries of principal phase crystal
4siAlO
8n, and principal phase crystal SiAlON is mainly α-SiAlON, or be α-SiAlON and β-SiAlON compound phase, include α-Si in described α-SiAlON
3n
4, in described β-SiAlON, include β-Si
3n
4;
Described SiAlON pottery after carrying out X-ray diffraction, α-SiAlON peak intensity near 2 θ=34.2 ° be X, β-SiAlON near 2 θ=33.5 ° peak intensity Y, Y
4siAlO
8the peak intensity Z of N near 2 θ=29.4 °, and Y/X=0 ~ 18, Z/X=0.05 ~ 2.
2. according to claim 1 containing crystallization phases Y
4siAlO
8the SiAlON pottery of N, is characterized in that: described Y/X=0.4 ~ 6, Z/X=0.1 ~ 1.0.
3. a preparation method for SiAlON pottery as claimed in claim 1 or 2, comprises the following steps:
(1) with Si, Si
3n
4, Al
2o
3, AlN and Y
2o
3powder as material powder, by proportioning, each material powder is mixed, adds organic solvent and tackiness agent, ball milling mixing after obtain mixed slurry;
(2) mixed slurry that step (1) obtains is carried out spray-drying process, obtain spherical particle powder, more repressed shaping, degreasing, obtains green compact;
(3) insert in a container by the green compact that step (2) obtains, then carry out pre-burning in a nitrogen atmosphere, it is 1250 DEG C ~ 1550 DEG C that calcined temperature controls, nitrogen partial pressure 1 ~ 3 normal atmosphere, burn-in time 2 ~ 10 hours, and then furnace cooling, obtains pre-burning body;
(4) inserted in a container by the pre-burning body that step (3) obtains, then sinter in a nitrogen atmosphere, it is 1650 DEG C ~ 1950 DEG C that sintering temperature controls, soaking time is 1 ~ 8 hour, 1200 DEG C are cooled to subsequently by 1 ~ 12 DEG C/min speed, then furnace cooling, obtain SiAlON pottery;
In described material powder, the massfraction proportioning of each material is as follows:
Si and Si
3n
4total mass account for 50% ~ 90% of material powder total mass;
Al
2o
3account for 1% ~ 15% of material powder total mass;
AlN accounts for 5% ~ 30% of material powder total mass;
Y
2o
3account for 2% ~ 20% of material powder total mass;
Described Si and Si
3n
4mass ratio be 70:30 ~ 90:10.
4. preparation method according to claim 3, is characterized in that, described container is a crystal vessel scribbling BN.
5. the application of SiAlON pottery in cutting tool preparation as claimed in claim 1 or 2.
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| CN201310515280.5A CN103601500B (en) | 2013-10-28 | 2013-10-28 | SiAlON ceramic containing crystalline phase Y4SiAlO8N, and preparation method and application thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1521141A (en) * | 2003-02-14 | 2004-08-18 | 中国科学院上海硅酸盐研究所 | Self-propagating high-temperature synthesis preparation method of low-cost α-sialon powder |
| CN1569745A (en) * | 2004-01-19 | 2005-01-26 | 中国科学院上海硅酸盐研究所 | Process for self-propagating synthesis of alpha-sialon powder with stable rare earth ion |
-
2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1521141A (en) * | 2003-02-14 | 2004-08-18 | 中国科学院上海硅酸盐研究所 | Self-propagating high-temperature synthesis preparation method of low-cost α-sialon powder |
| CN1569745A (en) * | 2004-01-19 | 2005-01-26 | 中国科学院上海硅酸盐研究所 | Process for self-propagating synthesis of alpha-sialon powder with stable rare earth ion |
Non-Patent Citations (1)
| Title |
|---|
| Phasenuntersuchungen im System Y-Si-Al-O-N;Dirk Matusch;《》;20031231 * |
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