CN112795816B - Preparation process of AlTi10 intermediate alloy - Google Patents
Preparation process of AlTi10 intermediate alloy Download PDFInfo
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- CN112795816B CN112795816B CN202011451253.2A CN202011451253A CN112795816B CN 112795816 B CN112795816 B CN 112795816B CN 202011451253 A CN202011451253 A CN 202011451253A CN 112795816 B CN112795816 B CN 112795816B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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Abstract
The invention discloses a preparation process of an AlTi10 intermediate alloy, belongs to the technical field of aluminum alloy, and is used for solving the problems that the preparation process of the AlTi10 intermediate alloy in the prior art is complex, pollutes the environment or has high production cost and the like. The preparation process of the invention adopts pure aluminum and Ti6Al4V alloy as raw materials, and comprises the following steps: step 1, weighing pure aluminum and Ti6Al4V alloy with corresponding weight; step 2, filling pure aluminum into an electric induction furnace, and electrifying the electric induction furnace to completely melt the pure aluminum; step 3, heating the molten pure aluminum to 950-1200 ℃; step 4, adding Ti6Al4V alloy, stirring and heating to melt to obtain alloy liquid; step 5, heating the alloy liquid to 950-1200 ℃, and then powering off the induction furnace; step 6, skimming the surface scum after the temperature of the alloy liquid is reduced to 750-800 ℃; and 7, casting the alloy liquid after the scum is removed into a cast ingot to prepare the AlTi10 intermediate alloy. The method is suitable for preparing the AlTi10 intermediate alloy.
Description
Technical Field
The invention belongs to the technical field of aluminum alloy, and particularly relates to a preparation process of an AlTi10 intermediate alloy.
Background
The AlTi10 intermediate alloy is used as an additive, has important effect in the Al alloy smelting field, is mainly used for preparing Al-Si series cast aluminum alloy, and in the Al-Si series cast aluminum alloy, Ti element can play a role in refining grains.
The AlTi10 intermediate alloy is generally sponge titanium or titanium dioxide (TiO)2) And (4) preparation.
However, the preparation of the AlTi10 intermediate alloy by using the titanium sponge has high cost and is not suitable for industrial production. The AlTi10 intermediate alloy prepared by using titanium dioxide is obtained by reducing potassium chlorate at high temperature by using an aluminothermic reaction principle, and is accompanied with the generation of irritant KCl smoke, so that the smelting process is complex, and the environment is polluted to a certain extent.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a preparation process of an AlTi10 intermediate alloy, so as to solve the problems in the prior art that the preparation process of the AlTi10 intermediate alloy is complex, causes environmental pollution or has high production cost, and the like.
The purpose of the invention is mainly realized by the following technical scheme:
the invention provides a preparation process of an AlTi10 intermediate alloy, which adopts pure aluminum and Ti6Al4V alloy as raw materials;
the method comprises the following steps:
step 1, weighing pure aluminum and Ti6Al4V alloy with corresponding weight;
step 2, filling pure aluminum into an electric induction furnace, and electrifying the electric induction furnace to completely melt the pure aluminum;
step 3, heating the molten pure aluminum to 950-1200 ℃;
step 4, adding Ti6Al4V alloy, stirring and heating to melt to obtain alloy liquid;
step 5, heating the alloy liquid to 950-1200 ℃, and then powering off the induction furnace;
step 6, skimming the surface scum after the temperature of the alloy liquid is reduced to 750-800 ℃;
and 7, casting the alloy liquid after the scum is removed into a cast ingot to prepare the AlTi10 intermediate alloy.
Further, in the step 1, the weight of the pure aluminum is calculated according to the mass of the Ti6Al4V alloy, and the calculation formula is as follows:
wherein M isTiM is the weight of Ti6Al4V alloyAlIs the weight of pure aluminum, cTiIs the mass fraction of Ti in the Ti6Al4V alloy.
Further, in step 1, the Ti6Al4V alloy was cut into 50 × 50mm size3The following small blocks.
Further, in the step 2:
after pure aluminum is loaded into an induction electric furnace, cryolite powder is scattered on the surface of the pure aluminum and in the induction electric furnace for covering, and then the pure aluminum is melted by electric heating;
and continuously scattering the cryolite powder in the melting process.
Further, before heating and melting, the weight of the cryolite powder scattered on the surface of the pure aluminum and in the furnace is 0.2-0.3% of that of the pure aluminum;
the total weight of the cryolite powder sprinkled in the melting process and the cryolite powder sprinkled before heating and melting is below 0.5 percent of the weight of the pure aluminum.
Further, in the step 4, the Ti6Al4V alloy is added in batches, and the amount of the Ti6Al4V alloy added in each batch is less than 1/5 of the total weight of the Ti6Al4V alloy.
Further, the amount of the Ti6Al4V alloy added in each batch is more than 1/10 of the total weight of the Ti6Al4V alloy.
Further, in the step 4, the Ti6Al4V alloy is preheated to 300-350 ℃, and then is added into an induction furnace.
Further, in the step 4, a stone mill rod is used for stirring.
Further, in the step 5, the alloy liquid is heated to 950-1200 ℃, stirred for 10-15 min, then the induction furnace is powered off, and then kept stand for 10-20 min,
further, in the step 7, the casting process is finished within 15-30 min.
Further, the preparation process further comprises the following steps:
and 8, measuring the components of the prepared AlTi10 intermediate alloy.
Compared with the prior art, the invention can at least realize one of the following technical effects:
1) the invention uses Ti6Al4V to prepare AlTi10 intermediate alloy. On one hand, the production process can be improved, and the environmental pollution can be reduced. On the other hand, the repeated utilization rate of Ti6Al4V alloy casting and riser or casting scrapped due to no component reasons can be improved, and the preparation cost of the AlTi10 intermediate alloy is reduced. The Ti6Al4V alloy is smelted in a vacuum consumable electrode water-cooled copper crucible in the casting process of aviation and aerospace products, has less alloy impurities, generates a pouring gate and a riser with thinner tissues, can be inherited into the AlTi10 intermediate alloy through remelting, thins the alloy tissue of the AlTi10 intermediate alloy, and has good alloy tissue of the AlTi10 intermediate alloy smelted by using the Ti6Al4V alloy. Compared with the AlTi10 intermediate alloy prepared by the traditional processes such as titanium dioxide and the like, the crystal grain of the AlTi10 intermediate alloy prepared by the method has better alloy structure, and Ti in the Ti6Al4V alloy has better refining effect on the AlTi10 intermediate alloy.
2) The Ti6Al4V alloy adopts Ti6Al4V casting gates and risers of the same heat, three test blocks at different positions are selected to measure the components of the Ti6Al4V alloy, and the average value is taken. The proportion of pure aluminum and the Ti6Al4V alloy is accurately controlled from the beginning of the process, so that the uniformity and the accuracy of the Ti content in the final AlTi10 intermediate alloy are improved.
3) Cutting Ti6Al4V alloy into pieces with size 50 x 50mm3The following small blocks are used for increasing the contact area of Ti6Al4V and aluminum liquid and accelerating the melting speed.
4) After pure aluminum is loaded into an induction electric furnace, cryolite powder is scattered on the surface of the pure aluminum and in the induction electric furnace for covering, and then the pure aluminum is melted by electric heating; and in the melting process, the cryolite powder is continuously scattered, so that the high-temperature aluminum liquid is prevented from contacting with air to generate aluminum oxide impurities.
Before heating and melting, the weight of the cryolite powder scattered on the surface of the pure aluminum and in the furnace is 0.2-0.3% of that of the pure aluminum; the total weight of the cryolite powder sprinkled in the melting process and the cryolite powder sprinkled before being melted by heating is less than 0.5 percent of the weight of the pure aluminum. Too much cryolite powder is added resulting in waste of cryolite powder.
5) In order to prevent the metal melting tool from melting into the alloy at high temperature, a stone grinding rod is used for stirring. The graphite rod with the flat head is used for manual stirring, and the graphite rod is required to be rolled up and down in a crucible during stirring, so that the alloy components are more uniform.
6) The Ti6Al4V alloy is added in batches, the amount of the Ti6Al4V alloy added in each batch is less than 1/5 of the total weight of the Ti6Al4V alloy, and the condition that the excessive addition at one time causes uneven stirring and segregation is prevented. Too little Ti6Al4V alloy is added per batch to result in poor efficiency, and to avoid too low efficiency, it is preferred that the Ti6Al4V alloy be added per batch in an amount greater than 1/10 of the total weight of the Ti6Al4V alloy.
7) The pouring process is finished within 15-30min, and segregation is prevented from occurring after the pouring time is too long.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description.
Detailed Description
The process for preparing an AlTi10 master alloy is described in further detail below with reference to specific examples, which are provided for purposes of comparison and explanation only and to which the present invention is not limited.
A process for preparing an AlTi10 intermediate alloy uses pure aluminum and Ti6Al4V alloy as raw materials.
The Ti6Al4V alloy is a common titanium alloy, is mainly used for casting aviation and aerospace products, a large number of gates and risers are generated in the casting process, and the gates and the risers which are cut from castings and are not scrapped due to component reasons can be remelted and used as primary scrap returns, but only degraded and used, and cannot be used for aviation and aerospace products again.
The Ti6Al4V is used for preparing the AlTi10 intermediate alloy, firstly, the main alloy elements of the Ti6Al4V are Ti and Al, and secondly, the casting gates and the risers generated in the casting process of aviation and aerospace products have fine structures, and the alloy can be inherited into the AlTi10 intermediate alloy through remelting, so that the alloy structure of the AlTi10 intermediate alloy is refined, and the method is beneficial to improving the metallurgical quality of the AlTi10 intermediate alloy. In addition, the low content of the element V in the Ti6Al4V alloy can be treated as an impurity, and the existence of the element V does not influence the metallurgical quality of the AlTi10 intermediate alloy.
Preferably, the raw material Ti6Al4V alloy in the invention is a pouring gate and/or a riser generated in the casting process. On one hand, the production process can be improved, and the environmental pollution can be reduced. On the other hand, the repeated utilization rate of Ti6Al4V alloy casting and riser or casting scrapped due to no component reasons can be improved, and the preparation cost of the AlTi10 intermediate alloy is reduced. The Ti6Al4V alloy is smelted by a vacuum consumable electrode water-cooled copper crucible, has less alloy impurities and good structure alloying effect, and the AlTi10 intermediate alloy smelted by the Ti6Al4V alloy has good alloy structure due to the inheritance of the alloy. Compared with the AlTi10 intermediate alloy prepared by the traditional processes such as titanium dioxide and the like, the crystal grain of the AlTi10 intermediate alloy prepared by the method has better alloy structure, and Ti in the Ti6Al4V alloy has better refining effect on the AlTi10 intermediate alloy.
The preparation process of the AlTi10 intermediate alloy comprises the following steps:
step 1, weighing pure aluminum and Ti6Al4V alloy with corresponding weight.
Calculating the weight of pure aluminum according to the mass of the Ti6Al4V alloy, wherein the calculation formula is as follows:
wherein M isTiM is the weight of Ti6Al4V alloyAlIs the weight of pure aluminum, cTiIs the mass fraction of Ti in the Ti6Al4V alloy.
Preferably, the Ti6Al4V alloy adopts a Ti6Al4V casting gate and a riser of the same heat, three test blocks at different positions are selected to measure the components of the Ti6Al4V alloy, and the average value is taken. The proportion of pure aluminum and the Ti6Al4V alloy is accurately controlled from the beginning of the process, so that the uniformity and the accuracy of the Ti content in the final AlTi10 intermediate alloy are improved.
Cutting Ti6Al4V alloy into pieces with size 50 x 50mm3The following small blocks are used for increasing the contact area of Ti6Al4V and aluminum liquid and accelerating the melting speed.
Preferably, the purity of the pure aluminum is 99.7-99.99%.
And 2, filling the pure aluminum into an electric induction furnace, and electrifying the electric induction furnace to completely melt the pure aluminum.
After pure aluminum is loaded into an induction electric furnace, cryolite powder is scattered on the surface of the pure aluminum and in the induction electric furnace for covering, and then the pure aluminum is melted by electric heating; and in the melting process, the cryolite powder is continuously scattered, so that the high-temperature aluminum liquid is prevented from contacting with air to generate aluminum oxide impurities.
Before heating and melting, the weight of the cryolite powder scattered on the surface of the pure aluminum and in the furnace is 0.2-0.3% of that of the pure aluminum; the total weight of the cryolite powder sprinkled in the melting process and the cryolite powder sprinkled before being melted by heating is less than 0.5 percent of the weight of the pure aluminum. Too much cryolite powder is added resulting in waste of cryolite powder.
And 3, heating the molten pure aluminum to 950-1200 ℃, wherein the Ti6Al4V alloy which is added subsequently is difficult to melt when the temperature is too low, and the aluminum is possibly oxidized when the temperature is too high. Preferably, the temperature is maintained between 950 ℃ and 1050 ℃.
In the pure aluminum melting and heating processes, the induction furnace is electrified to the maximum current until the aluminum liquid is completely melted and heated to 950-.
And step 4, adding Ti6Al4V alloy, stirring and heating to melt to obtain alloy liquid.
Preferably, in order to prevent the metal melting tool from melting into the alloy at high temperatures, stirring is performed using a graphite rod. The graphite rod with the flat head is used for manual stirring, and the graphite rod is required to be rolled up and down in a crucible during stirring, so that the alloy components are more uniform.
Preferably, the Ti6Al4V alloy is added in batches, and the amount of the Ti6Al4V alloy added in each batch is less than 1/5 of the total weight of the Ti6Al4V alloy, so that the phenomenon that the stirring is not uniform and segregation is formed due to excessive addition at one time is prevented. Too little Ti6Al4V alloy is added per batch to result in poor efficiency, and to avoid too low efficiency, it is preferred that the Ti6Al4V alloy be added per batch in an amount greater than 1/10 of the total weight of the Ti6Al4V alloy.
Preferably, the Ti6Al4V alloy is preheated to 300-350 ℃ before the Ti6Al4V alloy is added into the induction furnace, and then the alloy is added into the induction furnace.
And 5, heating the alloy liquid to 950-1200 ℃, and then powering off the induction furnace.
Specifically, after the alloy liquid is heated to 950-1200 ℃, stirring for 10-15 min, then powering off the induction furnace, and standing for 10-20 min to ensure that impurities float and sink for enough time.
And 6, after the temperature of the alloy liquid is reduced to 750-800 ℃, skimming the surface scum by using a scum-removing spoon.
And 7, casting the alloy liquid after the scum is removed into a cast ingot to prepare the AlTi10 intermediate alloy.
And when the scum is completely removed, the tilting crucible pours the alloy liquid into an ingot, and the pouring is finished within 15-30min according to the size of the melting amount in the pouring process, so that the segregation caused by overlong pouring time is prevented.
The preparation process of the AlTi10 intermediate alloy further comprises the following steps: and 8, measuring the components of the prepared AlTi10 intermediate alloy.
Specifically, a spindle cast in the middle stage of each furnace is taken as a sampling spindle after casting is finished, three points are drilled on the sampling spindle along the diagonal direction, one point is centered, through holes with the diameter of 5-10mm are drilled at the positions, one quarter of the length of the diagonal, of the other two points, and the components of the AlTi10 intermediate alloy are measured by the chemical method according to HB 5372.
When the element content Ti: 9-11%, and the AlTi10 intermediate alloy is qualified when the impurity content meets the requirements of GB/T27677-2017 on the components of the AlTi10 intermediate alloy.
And when the impurity content meets the requirements of GB/T27677-2017 on the components of the AlTi10 intermediate alloy and the mass content of the Ti alloy is not 9-11% (namely the AlTi10 intermediate alloy which is not scrapped due to excessive impurities), smelting the prepared AlTi10 intermediate alloy again according to the steps 1-7. However, the number of remelting should not exceed three times to prevent coarse grains after multiple melting.
The impurities are other elements except Al and Ti elements in the AlTi10 intermediate alloy, such as Fe, Si and other elements.
Example 1
(1) Selecting a pouring gate and a riser of a Ti6Al4V casting of the same heat as raw materials, selecting three test blocks at different positions to measure alloy components, averaging, and simultaneously recording the weights of the pouring gate and the riser.
(2) Pure aluminum with the purity of 99.95 percent is used, the weight of the pure aluminum is calculated according to the mass of the Ti6Al4V alloy, and the calculation formula is as follows:
wherein M isTiM is the weight of Ti6Al4V alloyAlIs the weight of pure aluminum, cTiThe content (%) of Ti in Ti6Al 4V.
(3) After pure aluminum is loaded into an induction electric furnace, cryolite powder with 0.2 percent of the weight of the pure aluminum is scattered on the surface of the pure aluminum and in the induction electric furnace for covering, and then the pure aluminum is electrified and heated for melting; in the melting process, the cryolite powder is continuously scattered, and the weight of the scattered cryolite powder is 0.4 percent of that of the pure aluminum.
In the pure aluminum melting and heating processes, the induction furnace is electrified to the maximum current until the aluminum liquid is completely melted and heated to 1000 ℃, and then the current is reduced to maintain the temperature at about 1000 ℃.
(4) The Ti6Al4V alloy preheated to 330 ℃ is averagely divided into 5 parts, added into the aluminum liquid in batches, and stirred by a stone grinding rod until the Ti6Al4V alloy is completely melted.
(5) Stirring the AlTi10 alloy liquid with a flat-head graphite rod at 1000 deg.C for 10min, turning the solution up and down while stirring, and standing for 15min after stirring.
(6) And casting into ingots when the temperature of the AlTi10 alloy liquid is reduced to 800 ℃.
(7) The composition of the AlTi10 master alloy was measured by chemical analysis as HB5372 and the results are as follows:
| serial number | Test items | Test data |
| 1 | Ti | 10.34％ |
| 2 | Fe | 0.03％ |
| 3 | Si | 0.02％ |
From the above table, the ratio of Ti in the AlTi10 master alloy prepared in this example: 9-11 percent of the alloy, less than or equal to 0.3 percent of impurities, meeting the requirements, and qualified AlTi10 intermediate alloy.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (9)
1. The preparation process of the AlTi10 intermediate alloy is characterized in that pure aluminum and Ti6Al4V alloy are used as raw materials, and the Ti6Al4V alloy is smelted in a vacuum consumable electrode water-cooled copper crucible;
the method comprises the following steps:
step 1, weighing pure aluminum and Ti6Al4V alloy according to the corresponding weight, wherein the weight of the pure aluminum is calculated according to the mass of the Ti6Al4V alloy, and the calculation formula is as follows:
wherein M isTiM is the weight of Ti6Al4V alloyAlIs the weight of pure aluminum, cTiIs the mass fraction of Ti in the Ti6Al4V alloy;
step 2, filling pure aluminum into an electric induction furnace, and electrifying the electric induction furnace to completely melt the pure aluminum;
step 3, heating the molten pure aluminum to 950-1200 ℃;
step 4, adding Ti6Al4V alloy, stirring and heating to melt to obtain alloy liquid;
step 5, heating the alloy liquid to 950-1200 ℃, and then powering off the induction furnace;
step 6, skimming surface scum after the temperature of the alloy liquid is reduced to 750-800 ℃;
and 7, casting the alloy liquid after the scum is removed into a cast ingot to prepare the AlTi10 intermediate alloy.
2. The process for preparing an AlTi10 master alloy as claimed in claim 1, wherein in step 1, the Ti6Al4V alloy is sliced to a size of 50 x 50mm3The following small blocks.
3. The process for preparing an AlTi10 master alloy according to claim 1, wherein, in step 2:
after pure aluminum is loaded into an induction electric furnace, cryolite powder is scattered on the surface of the pure aluminum and in the induction electric furnace for covering, and then the pure aluminum is melted by electric heating;
and continuously scattering the cryolite powder in the melting process.
4. The process for preparing the AlTi10 intermediate alloy according to claim 3, wherein the weight of the cryolite powder sprinkled on the surface of the pure aluminum and in the furnace is 0.2-0.3% of the weight of the pure aluminum before the pure aluminum is heated and melted;
the total weight of the cryolite powder sprinkled in the melting process and the cryolite powder sprinkled before heating and melting is below 0.5 percent of the weight of the pure aluminum.
5. The process for preparing the AlTi10 intermediate alloy according to the claim 1, wherein in the step 4, the Ti6Al4V alloy is added in batches, and the amount of the Ti6Al4V alloy added in each batch is less than 1/5 of the total weight of the Ti6Al4V alloy.
6. The process for preparing the AlTi10 intermediate alloy according to claim 1, wherein in the step 4, the Ti6Al4V alloy is preheated to 300-350 ℃, and then is added into an induction furnace.
7. The process for preparing an AlTi10 intermediate alloy according to claim 1, wherein in the step 4, graphite rods are used for stirring.
8. The process for preparing an AlTi10 intermediate alloy according to any one of claims 1 to 7, wherein in step 7, the casting process is completed within 15-30 min.
9. The process for preparing an AlTi10 master alloy according to any one of claims 1 to 7, wherein the process further comprises:
and 8, measuring the components of the prepared AlTi10 intermediate alloy.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002309333A (en) * | 2001-04-09 | 2002-10-23 | Toyota Motor Corp | Aluminum alloy, aluminum alloy for plain bearing and plain bearing |
| CN101054638A (en) * | 2007-05-26 | 2007-10-17 | 太原理工大学 | Aluminum-titanium-carbon-yttrium intermediate alloy and preparing method thereof |
| CN104762496A (en) * | 2015-04-22 | 2015-07-08 | 铜山县超特有色金属添加剂厂 | Production process of aluminum-titanium alloy AlTi10 |
| CN110747372A (en) * | 2019-09-04 | 2020-02-04 | 宝钛集团有限公司 | Low-cost high-strength titanium alloy plate prepared from 100% returned furnace burden and preparation method thereof |
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2020
- 2020-12-10 CN CN202011451253.2A patent/CN112795816B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002309333A (en) * | 2001-04-09 | 2002-10-23 | Toyota Motor Corp | Aluminum alloy, aluminum alloy for plain bearing and plain bearing |
| CN101054638A (en) * | 2007-05-26 | 2007-10-17 | 太原理工大学 | Aluminum-titanium-carbon-yttrium intermediate alloy and preparing method thereof |
| CN104762496A (en) * | 2015-04-22 | 2015-07-08 | 铜山县超特有色金属添加剂厂 | Production process of aluminum-titanium alloy AlTi10 |
| CN110747372A (en) * | 2019-09-04 | 2020-02-04 | 宝钛集团有限公司 | Low-cost high-strength titanium alloy plate prepared from 100% returned furnace burden and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 成分均匀的高纯AlTi10中间合金熔炼工艺;郑亚虹;《铸造》;20001031;第49卷(第10期);第800-802页 * |
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