CN1552544A - Preparation of oriented alloy material by original position deep supercooling process - Google Patents
Preparation of oriented alloy material by original position deep supercooling process Download PDFInfo
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- CN1552544A CN1552544A CNA2003101227353A CN200310122735A CN1552544A CN 1552544 A CN1552544 A CN 1552544A CN A2003101227353 A CNA2003101227353 A CN A2003101227353A CN 200310122735 A CN200310122735 A CN 200310122735A CN 1552544 A CN1552544 A CN 1552544A
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Abstract
A in-situ deep overcold process for preparing the oriented alloy material includes such steps as using HF induction heater and the combination of fused glass protection with cyclic overheat to make the Ni-Fe-Ga, Co-Ni-Ga, or Fe-Ga alloy in overcold state, heating the alloy to the soft point of quartz tube, and flowing the alloy from the first quartz tube to the second one whose bottom is in contact with molten Ga-In alloy.
Description
Technical field
What the present invention relates to is a kind of method for preparing the directionally solidified alloy material, and particularly a kind of original position high undercooling prepares the method for directionally solidified alloy material, belongs to the material technology field.
Background technology
The magneticsubstance anisotropy, its performance difference of the material of different orientation is very big, and in order to satisfy practical engineering application, the material scholar has proposed a series of directional material technologies of preparing in succession.Comprise that power reduces method (PD), rapid solidification method (HRS), liquid cooled method (LMC) etc., but utilize these methods to prepare directed immiscible alloy material, need to consider that alternate wetting situation, immiscible range height, liquidus line slope, growth velocity, freezing interface temp gradient at front edge etc. are all multifactor, cause the actual production complex process, be difficult to control, production cost is very high.Find by literature search, Chinese patent application number 03114937.5, publication number CN1431327A, patent name: high undercooling prepares the method for directed Ni-Pb immiscible alloy, this patent proposes to adopt the high undercooling technology to prepare the method for directed Ni-Pb alloy material, employing prepares directional material to the method for Ni-Pb triggering forming core in the literary composition in the condensate depression scope of 70～110K, but the big or small unmanageable shortcoming that has trigger position and trigger point in the actual mechanical process, it is not very desirable often causing directional effect, and scrap rate is high.Also find in the retrieval, people such as Fu Hengzhi are at " Science and Technology of Advanced Materials " (advanced material science and technology), Volume:2, Issue:1, March, 2001, " the Thesolidification characteristics of near rapid and supercooling directionalsolidification " that delivers on the pp.193-196 (the nearly coagulating property of a high undercooling directional freeze process fast) literary composition, this article proposes high undercooling and the directed technology of proceeding in two phases that triggers, effect increases, but owing to adopted for two steps, the alloy high undercooling that causes the first step to obtain was difficult to keep in second step, the orientation in second step triggers and also has the alloy melting non-uniform temperature, be prone to latch up phenomenon, the scrap rate height.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, on the basis that systematic study high undercooling Ni-Fe-Ga, Co-Ni-Ga, Fe-Ga magneticalloy solidified structure develop, provide a kind of original position high undercooling to prepare the method for directionally solidified alloy material, it is the method that the original position high undercooling prepares directed Ni-Fe-Ga, Co-Ni-Ga, Fe-Ga magneticalloy, directional effect is obvious, and scrap rate is low.
The present invention is achieved by the following technical solutions, original position high undercooling preparation process of the present invention is undertaken by high-frequency induction heating apparatus, the method that adopts molten glass purification and cyclical superheating to combine makes Ni-Fe-Ga, Co-Ni-Ga, the Fe-Ga alloy obtained cold, in condensate depression during more than or equal to 200K, alloy is heated to the silica tube softening temperature, (first silica tube is an end opening type to rely on alloy self gravitation and electromagnetic force to make the silica tube of winning, bottom thickness＜0.5mm, sidewall thickness 2mm) Nei alloy bleeds, and (second silica tube is the both ends open type to second silica tube, bottom diameter＜2mm, upper-end inner diameter 3～5mm, height 40～50mm), distance 10～15cm between two silica tubes, second silica tube bottom contact Ga-In alloy liquid is prepared directionally solidified alloy.
Below the inventive method is further specified, its step is specific as follows:
1. alloy material is put into first silica tube of vacuum chamber insulation shell, and added an amount of glass scavenging agent in the metal charge upper and lower surface;
Each component of glass scavenging agent and weight percent thereof are: 72%SiO
2, 8.4%B
2O
3, 1.1%Al
2O
3, 0.3%CaO, 18.2%Na
2O fires in 1473K fusion in the conventional ceramic crucible and to form in 36 hours.
2. be evacuated to 5 * 10
-3Behind the Pa, 99.99% argon gas that recoils is to 0.08MPa;
3. by radio-frequency induction coil induction heating alloy to 1273～1373K, make the scavenging agent fusion coated at alloy surface;
4. be warming up to 1650～1850K, be incubated degasification in 2 minutes;
5. be heated to 1850～1950K, be incubated 2 minutes, carry out " solidifying-remelting-overheated " circular treatment, the temperature optical signal of preparation process interalloy is measured by infrared probe, through after the signal processing unit processes, utilize registering instrument real-time continuous record temperature variation, the condensate depression of monitoring alloy is in the refrigerative process, after condensate depression is more than or equal to 200K, be warming up to 2100K, insulation is in alloy bleeds second silica tube.Second silica tube bottom contact Ga-In alloy liquid.Molten metal is grown from bottom to top, forms the alloy with directed tissue.
Compared with prior art; the present invention unites two into one high undercooling process and orientation process; process of setting is controlled easily; only need control alloy condensate depression scope can prepare directed Ni-Fe-Ga, Co-Ni-Ga, Fe-Ga magneticalloy fast; the alloy preparation needs vacuum argon shield environment; not oxidation of alloy and Ga element volatilization loss are few under the molten glass purification protection, and it is fine that glass is crossed cold effect, reaches more than the 200K easily.
Embodiment
The present invention only requires to control the alloy condensate depression, after condensate depression is more than or equal to 200K, be warming up to 2150K, insulation is until alloy second silica tube that bleeds, second silica tube bottom contacts Ga-In alloy liquid, can obtain Ni-Fe-Ga, Co-Ni-Ga, the Fe-Ga magneticalloy of oriented growth.Content below in conjunction with the inventive method further provides embodiment:
Embodiment one: high undercooling prepares directed Ni
2The FeGa alloy
1. with Ni
2The FeGa alloy material is put into first silica tube of insulation shell, and adds an amount of glass scavenging agent in the metal charge upper and lower surface; 2. be evacuated to 5 * 10
-3Behind the Pa, 99.99% argon gas that recoils is to 0.08MPa; 3. pass through radio-frequency induction coil induction heating alloy to 1273K, make the scavenging agent fusion coated at alloy surface; 4. be warming up to 1650K, be incubated 2 minutes; 5. be heated to 1850K, be incubated 2 minutes, solidify-remelting-overheated circular treatment, the temperature optical signal of experimentation interalloy is measured by infrared probe, through after the signal processing unit processes, utilize the desk-top registering instrument real-time continuous record of 3056 types temperature variation, the condensate depression of monitoring alloy.In the refrigerative process, when condensate depression reaches 200K, be warming up to 2100K, behind the insulation 1min, alloy second silica tube that bleeds, second silica tube bottom contact Ga-In alloy liquid, obtaining along the direction of growth is the directed Ni of columanar structure
2The FeGa alloy.
Embodiment two: high undercooling prepares directed Co
2The NiGa alloy
1. with Co
2The NiGa alloy material is put into first silica tube of insulation shell, and adds an amount of glass scavenging agent in the metal charge upper and lower surface; 2. be evacuated to 5 * 10
-3Behind the Pa, 99.99% argon gas that recoils is to 0.08MPa; 3. pass through radio-frequency induction coil induction heating alloy to 1323K, make the scavenging agent fusion coated at alloy surface; 4. be warming up to 1800K, be incubated 2 minutes; 5. be heated to 1900K, be incubated 2 minutes, solidify-remelting-overheated circular treatment, the temperature optical signal of experimentation interalloy is measured by infrared probe, through after the signal processing unit processes, utilize the desk-top registering instrument real-time continuous record of 3056 types temperature variation, the condensate depression of monitoring alloy.In the refrigerative process, when condensate depression reaches 240K, be warming up to 2100K, be incubated after 1.2 minutes, alloy second silica tube that bleeds, second silica tube bottom contact Ga-In alloy liquid, obtaining along the direction of growth is the directed Co of columanar structure
2The NiGa alloy.
Embodiment three: high undercooling prepares directed Fe
80Ga
20Alloy
1. with Fe
80Ga
20Alloy material is put into first silica tube of insulation shell, and adds an amount of glass scavenging agent in the metal charge upper and lower surface; 2. be evacuated to 5 * 10
-3Behind the Pa, 99.99% argon gas that recoils is to 0.08MPa; 3. pass through radio-frequency induction coil induction heating alloy to 1373K, make the scavenging agent fusion coated at alloy surface; 4. be warming up to 1850K, be incubated 2 minutes; 5. be heated to 1950K, be incubated 2 minutes, solidify-remelting-overheated circular treatment, the temperature optical signal of experimentation interalloy is measured by infrared probe, through after the signal processing unit processes, utilize the desk-top registering instrument real-time continuous record of 3056 types temperature variation, the condensate depression of monitoring alloy.In the refrigerative process, when condensate depression reaches 280K, be warming up to 2100K, be incubated after 1.5 minutes, alloy second silica tube that bleeds, second silica tube bottom contact Ga-In alloy liquid, obtaining along the direction of growth is the directed Fe of columanar structure
80Ga
20Alloy.
Claims (4)
1, a kind of original position high undercooling prepares the method for directionally solidified alloy material, it is characterized in that, original position high undercooling preparation process is undertaken by high-frequency induction heating apparatus, the method that adopts molten glass purification and cyclical superheating to combine, make Ni-Fe-Ga, Co-Ni-Ga, the Fe-Ga alloy obtained cold, in condensate depression during more than or equal to 200K, alloy is heated to the silica tube softening temperature, rely on alloy self gravitation and electromagnetic force to make alloy in the silica tube of winning second silica tube that bleeds, distance 10～15cm between two silica tubes, second silica tube bottom contact Ga-In alloy liquid is prepared directionally solidified alloy.
2, original position high undercooling according to claim 1 prepares the method for directionally solidified alloy material, it is characterized in that,
Concrete steps are as follows:
1. alloy material is put into first silica tube of vacuum chamber insulation shell, and added an amount of glass scavenging agent in the metal charge upper and lower surface;
2. be evacuated to 5 * 10
-3Behind the Pa, 99.99% argon gas that recoils is to 0.08MPa;
3. by radio-frequency induction coil induction heating alloy to 1273～1373K, make the fusion of glass scavenging agent coated at alloy surface;
4. be warming up to 1650～1850K, be incubated degasification in 2 minutes;
5. be heated to 1850～1950K, be incubated 2 minutes, carry out " solidifying-remelting-overheated " circular treatment, the temperature optical signal of preparation process interalloy is measured by infrared probe, through after the signal processing unit processes, utilize registering instrument real-time continuous record temperature variation, the condensate depression of monitoring alloy, in the refrigerative process, after condensate depression is more than or equal to 200K, be warming up to 2100K, insulation is in alloy bleeds second silica tube, second silica tube bottom contact Ga-In alloy liquid, molten metal is grown from bottom to top, forms the alloy with directed tissue.
3, original position high undercooling according to claim 2 prepares the method for directionally solidified alloy material, it is characterized in that, each component of glass scavenging agent and weight percent thereof are: 72%SiO
2, 8.4%B
2O
3, 1.1%Al
2O
3, 0.3%CaO, 18.2%Na
2O fires in 1473K fusion in the conventional ceramic crucible and to form in 36 hours.
4, original position high undercooling according to claim 1 and 2 prepares the method for directionally solidified alloy material, it is characterized in that, first silica tube is an end opening type, bottom thickness＜0.5mm, sidewall thickness 2mm, second silica tube are the both ends open type, bottom diameter＜2mm, upper-end inner diameter 3～5mm, height 40～50mm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608281B (en) * | 2009-07-16 | 2010-12-08 | 上海交通大学 | Giant magnetostrictive large volume Fe81Ga19 alloy material and preparation method thereof |
| CN101613811B (en) * | 2009-07-16 | 2010-12-08 | 上海交通大学 | Fe-Ga alloy deep undercooling cleaning agent and preparation method thereof |
| CN106903266A (en) * | 2017-04-27 | 2017-06-30 | 郑州大学 | A kind of glass fluxing technique suspension high undercooling Rapid Directional Solidification device and its clotting method |
| CN109628756A (en) * | 2019-01-04 | 2019-04-16 | 江苏理工学院 | A method of purification small size aluminium and aluminium alloy melt |
| CN111299553A (en) * | 2020-04-10 | 2020-06-19 | 西北工业大学 | Multi-mode excited deep supercooling directional solidification device and method |
| CN111872356A (en) * | 2020-08-06 | 2020-11-03 | 上海大学 | Preparation device and preparation method of carbon fiber-reinforced alloy composite material with magnetic refrigeration function |
| CN113667916A (en) * | 2021-08-27 | 2021-11-19 | 西北工业大学 | GH605 high-temperature alloy subjected to deep supercooling treatment and preparation method thereof |
| CN115418588A (en) * | 2022-09-15 | 2022-12-02 | 西北工业大学 | Magnetic field deep supercooling treatment method for improving toughness of cobalt-based high-temperature alloy |
-
2003
- 2003-12-19 CN CN 200310122735 patent/CN1244425C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608281B (en) * | 2009-07-16 | 2010-12-08 | 上海交通大学 | Giant magnetostrictive large volume Fe81Ga19 alloy material and preparation method thereof |
| CN101613811B (en) * | 2009-07-16 | 2010-12-08 | 上海交通大学 | Fe-Ga alloy deep undercooling cleaning agent and preparation method thereof |
| CN106903266A (en) * | 2017-04-27 | 2017-06-30 | 郑州大学 | A kind of glass fluxing technique suspension high undercooling Rapid Directional Solidification device and its clotting method |
| CN109628756A (en) * | 2019-01-04 | 2019-04-16 | 江苏理工学院 | A method of purification small size aluminium and aluminium alloy melt |
| CN111299553A (en) * | 2020-04-10 | 2020-06-19 | 西北工业大学 | Multi-mode excited deep supercooling directional solidification device and method |
| CN111299553B (en) * | 2020-04-10 | 2021-05-25 | 西北工业大学 | Multi-mode excited deep supercooling directional solidification device and method |
| CN111872356A (en) * | 2020-08-06 | 2020-11-03 | 上海大学 | Preparation device and preparation method of carbon fiber-reinforced alloy composite material with magnetic refrigeration function |
| CN113667916A (en) * | 2021-08-27 | 2021-11-19 | 西北工业大学 | GH605 high-temperature alloy subjected to deep supercooling treatment and preparation method thereof |
| CN115418588A (en) * | 2022-09-15 | 2022-12-02 | 西北工业大学 | Magnetic field deep supercooling treatment method for improving toughness of cobalt-based high-temperature alloy |
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| CN1244425C (en) | 2006-03-08 |
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