CN102041425B - (Ti, Nb) 3AlC2/Al2O3 solid solution composite material and preparation method thereof - Google Patents
(Ti, Nb) 3AlC2/Al2O3 solid solution composite material and preparation method thereof Download PDFInfo
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- CN102041425B CN102041425B CN 201010623889 CN201010623889A CN102041425B CN 102041425 B CN102041425 B CN 102041425B CN 201010623889 CN201010623889 CN 201010623889 CN 201010623889 A CN201010623889 A CN 201010623889A CN 102041425 B CN102041425 B CN 102041425B
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000006104 solid solution Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910052593 corundum Inorganic materials 0.000 title abstract 3
- 229910001845 yogo sapphire Inorganic materials 0.000 title abstract 3
- 239000000843 powder Substances 0.000 claims abstract description 91
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 229910044991 metal oxide Inorganic materials 0.000 claims description 8
- 150000004706 metal oxides Chemical class 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 abstract description 29
- 238000000034 method Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000010304 firing Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000005728 strengthening Methods 0.000 abstract description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 238000007731 hot pressing Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 9
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003832 thermite Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
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- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention discloses a (Ti, Nb) 3AlC2/Al2O3 solid solution composite material and a preparation method thereof. The preparation method comprises the following steps: hot pressing and sintering the following materials in percentage by weight: 45.87-72.95% of Ti powder, 14.02-19.10% of Al powder, 9.23-12.25% of C powder and 0.78-25.81% of Nb2O5 powder, wherein a particle wild phase grows in the matrix phase generating process via thermit reaction, a fine crystal composite material of Al2O3 dispersed phase strengthened matrix phase Ti3AlC2 is prepared, and Nb generated by the reaction is used for carrying out solid solution strengthening on the matrix. Because the material ingredients have big adjustability, low firing temperature, even and compact structure, lower cost and excellent mechanical property, the application range of the composite material is expanded. In addition, the method lowers the firing temperature and the hot-press pressure and realizes crystalline grain micritization in the quick firing process.
Description
Technical field
The invention belongs to matrix material and make field, particularly a kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material and preparation method thereof.
Background technology
_ 2 Ceramics material Ti
3AlC
2Attracted lot of domestic and foreign scholar's broad research with its excellent properties.Ti
3AlC
2Performance with metal as having at normal temperatures good thermal conductivity and electroconductibility, lower Vickers' hardness, higher Young's modulus and shearing modulus, can carrying out traditional mechanical workout, has plasticity under comparatively high temps; This material has again the performance of pottery, such as high-melting-point, high thermal stability and good antioxidant property.But this material also exists sintering temperature high, and temperature range is little, and the shortcoming such as hardness is low, intensity is smaller and limited its further application.
In recent years, for improving Ti
3AlC
2The performance of material, people utilize the means of solid solution highly malleablized and Composite that it has been carried out study on the modification, have obtained preferably effect.(Scripta Materialia 53 (2005) 1369-1372) utilize the simple substance V element to carry out the solid solution study on the modification such as bibliographical information, its mechanical property is greatly improved, same principle we can utilize the Nb element that it is melted modification admittedly, but the method raw materials cost is higher, synthesis temperature is higher simultaneously, is unfavorable for its industrialization production; Also there is document (Scripta Materialia 50 (2004) 897-901) report to utilize Al
2O
3Particle can be to Ti
3AlC
2Material property carries out modification.But currently used method is all more single, simultaneously, on the preparation method mainly with Al
2O
3And Ti
3AlC
2Sintering is carried out in two kinds of powders mixing, perhaps with Al, C, TiO
2For raw material high temperature generates Ti by reduction reaction
3AlC
2/ Al
2O
3Matrix material, but no matter the sort of technique all exists temperature of reaction high, and undercapacity, can't large-scale industrialized production.Document (AdvancedPowder Technology 03 (2010) 1-4) has been reported and has been utilized high-energy ball milling to synthesize Ti
3AlC
2/ Al
2O
3The novel method of matrix material, the material that the method is synthesized is greatly improved in performance, but high-energy ball milling is difficult to suitability for industrialized production, simultaneously, matrix phase is not carried out the solid solution modification.Therefore, how to take effective approach, utilize cheap material to synthesize Al
2O
3The solid-solution type Ti of particle highly malleablized
3AlC
2Matrix material is research emphasis from now on.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material and preparation method thereof utilizes Ti-Al-C-Nb
2O
5System is raw material, prepares Al by thermite reaction reaction in－situ technique low temperature
2O
3The Ti that strengthens
3AlC
2Solid solution composite material; The method is utilized cheap oxide compound Nb
2O
5Substitute expensive metal simple-substance, reduced raw materials cost; Utilize the reaction heat of thermite reaction self, reduced the synthesis temperature of material, simultaneously generated in-situ Al
2O
3The wild phase particle is tiny, even, and the performance of material is greatly improved; The material of preparation has high-strength, fine and close, high temperature resistant, machinable characteristics.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material, its initial feed be purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5Carry out proportioning by following reaction formula:
3(1-x)Ti+(1+5x)Al+2C+3x/2Nb
2O
5→(Ti
1-xNb
x)
3AlC
2+5x/2Al
2O
3 (1)(x＝0.0039～0.1685)，
The result is: a kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material, the raw material moiety is: the Ti powder accounts for 45.87～72.95% of gross weight, and the Al powder accounts for 14.02～19.10% of gross weight, and the C powder accounts for 9.23～12.25% and Nb of gross weight
2O
5Powder accounts for 0.78～25.81% of gross weight.
A kind of (Ti, Nb)
3AlC
2/ Al
2O
3The preparation technology of solid solution composite material the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5By following proportioning weighing, the Ti powder accounts for 45.87～72.95% of gross weight, and the Al powder accounts for 14.02～19.10%, C powder and accounts for 9.23～12.25% and Nb
2O
5Powder accounts for 0.78～25.81%;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 600～900 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 0.5～1.5 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 4～8 hours at 40～50 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1100 ℃～1400 ℃, the pressure hot pressed sintering of 5.0～30MPa 1～2 hour;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
(Ti, the Nb) that the present invention synthesized
3AlC
2/ Al
2O
3Solid solution composite material is characterized in that: it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for the 81.5-99.5% of matrix material gross weight, and wild phase accounts for the 0.5-18.5% of gross weight, and matrix phase is (Ti
1-x, Nb
x)
3AlC
2, wherein x gets 0.0039～0.1685, and wild phase is Al
2O
3If Al in the matrix material that generates
2O
3Growing amount does not have enhancing, toughness reinforcing Ti less than 0.5% of product quality
3AlC
2The effect of matrix, otherwise, if Al in the product
2O
3Phasor surpasses Ti
3AlC
2The content of matrix phase can not be referred to as Ti
3AlC
2Based composites, simultaneously, Al
2O
3Growing amount will be above 18.5%, excessive Al
2O
3Not only do not have and improve Ti
3AlC
2Effect, can worsen its performance on the contrary.Therefore determined above compositional range.
The present invention utilizes Ti powder, Al powder, C powder and Nb
2O
5Powder is raw material, by thermite reaction spontaneous particulates reinforcements Al in the process that matrix phase generates
2O
3The metal simple-substance Nb that restores simultaneously is to Ti
3AlC
2Carry out solution strengthening.Thereby prepared Al
2O
3The thin brilliant Ti of dispersion consolidatedization
3AlC
2Solid solution composite material.Because the material composition adjustability that this technique is synthesized is large, firing temperature is low, and even structure is fine and close, and cost is lower, and mechanical property is excellent, has widened the range of application of this matrix material.
Embodiment
Embodiment one
A kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material, its raw material weight moiety is: 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight
2O
5Powder accounts for 6.58% of gross weight.
The step of preparation process of present embodiment is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder and C powder and metal oxide Nb
2O
5By following proportioning weighing, 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight
2O
5Powder accounts for 6.58% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
(Ti, the Nb) that present embodiment synthesized
3AlC
2/ Al
2O
3Solid solution composite material is characterized in that: it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 96% of matrix material gross weight, and wild phase accounts for 4% of gross weight, and matrix phase is (Ti
0.9675, Nb
0.0325)
3AlC
2, wild phase is Al
2O
3
Embodiment two
A kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material, its raw material weight moiety is: 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.93% and Nb of gross weight
2O
5Powder accounts for 3.38% of gross weight.
The step of preparation process of present embodiment is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5By following proportioning weighing, 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 11.93%, Nb
2O
5Powder accounts for 3.38% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 47 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
(Ti, the Nb) that present embodiment synthesized
3AlC
2/ Al
2O
3Solid solution composite material is characterized in that: it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 98% of matrix material gross weight, and wild phase accounts for 2% of gross weight, and matrix phase is (Ti
0.9842, Nb
0.0158)
3AlC
2, wild phase is Al
2O
3
Embodiment three
A kind of (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material, its raw material weight moiety is: 59.92%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for 16.31%, 1200 purpose C powder and account for 10.77% and Nb
2O
5Powder accounts for 13.00%.
The step of preparation process of present embodiment is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5By following proportioning weighing, 16.31%, the 1200 purpose C powder that 59.92%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.77%, Nb
2O
5Powder accounts for 13.00% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
(Ti, the Nb) that present embodiment synthesized
3AlC
2/ Al
2O
3Solid solution composite material is characterized in that: it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 92% of matrix material gross weight, and wild phase accounts for 8% of gross weight, and matrix phase is (Ti
0.9304, Nb
0.0696)
3AlC
2, wild phase is Al
2O
3
Claims (3)
1. one kind (Ti, Nb)
3AlC
2/ Al
2O
3The preparation technology of solid solution composite material is characterized in that, the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5By following proportioning weighing, the Ti powder accounts for 45.87～72.95% of gross weight, and the Al powder accounts for 14.02～19.10% of gross weight, and the C powder accounts for 9.23～12.25% and Nb of gross weight
2O
5Powder accounts for 0.78～25.81% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 600～900 rpms, material: ball: the mass ratio=1:3:1 of ethanol, ball milling 0.5～1.5 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 4～8 hours at 40～50 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1100 ℃～1400 ℃, the pressure hot pressed sintering of 5.0～30MPa 1～2 hour;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
2. a kind of (Ti, Nb) according to claim 1
3AlC
2/ Al
2O
3The preparation technology of solid solution composite material is characterized in that, the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5By following proportioning weighing, 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight
2O
5Powder accounts for 6.58% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio=1:3:1 of ethanol, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
3. a kind of (Ti, Nb) according to claim 1
3AlC
2/ Al
2O
3The preparation technology of solid solution composite material is characterized in that, the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb
2O
5By following proportioning weighing, 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 11.93%, Nb
2O
5Powder accounts for 3.38% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio=1:3:1 of ethanol, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 47 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Nb)
3AlC
2/ Al
2O
3Solid solution composite material.
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| CN107042315A (en) * | 2017-05-03 | 2017-08-15 | 济南大学 | A kind of preparation method of titanium aluminum oxide cermet material |
| CN107805071B (en) * | 2017-10-26 | 2020-12-18 | 西南交通大学 | Preparation method of titanium-trialuminum-carbon-mullite composite ceramic with low glass wettability |
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| CN1804068A (en) * | 2006-01-18 | 2006-07-19 | 陕西科技大学 | Preparation method of highly dispersed AI2O3 particle reinforced Ti-Al based composite material |
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| CN101717252A (en) * | 2009-12-03 | 2010-06-02 | 陕西科技大学 | Ti3AlC2/Al2O3 compound material and preparation method thereof |
| CN101768686A (en) * | 2009-12-03 | 2010-07-07 | 陕西科技大学 | Al2O3/TiAl intermetallic compound composite material and preparation method thereof |
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2010
- 2010-12-31 CN CN 201010623889 patent/CN102041425B/en active Active
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| CN1804068A (en) * | 2006-01-18 | 2006-07-19 | 陕西科技大学 | Preparation method of highly dispersed AI2O3 particle reinforced Ti-Al based composite material |
| CN101100710A (en) * | 2007-07-31 | 2008-01-09 | 陕西科技大学 | Method for preparing high-niobium TiAl intermetallic compound composite material |
| CN101717252A (en) * | 2009-12-03 | 2010-06-02 | 陕西科技大学 | Ti3AlC2/Al2O3 compound material and preparation method thereof |
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| Title |
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| T.H.Scabarozi et al.Combinatorial investigation of (Ti1xNbx)2AlC.《Applied Physics Letters》.2009,第95卷(第10期),第101907-1至101907-3. * |
| 艾桃桃等.原位合成Al2O3颗粒增强双相TiAl基复合材料的组织与性能.《中国有色金属学报》.2007,第17卷(第11期),第1849页-第1854页. * |
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