CN1431327A - Deep super-cooling method for preparing directional difficult mixed dissolve Ni-Pb alloy - Google Patents
Deep super-cooling method for preparing directional difficult mixed dissolve Ni-Pb alloy Download PDFInfo
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- CN1431327A CN1431327A CN 03114937 CN03114937A CN1431327A CN 1431327 A CN1431327 A CN 1431327A CN 03114937 CN03114937 CN 03114937 CN 03114937 A CN03114937 A CN 03114937A CN 1431327 A CN1431327 A CN 1431327A
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Abstract
A process for preparing orientated Ni-Pb alloy difficult to mix and dissolve mutural by deep over-cold features that the HF induction heater isused, and the fused glass cleaning and cyclic over-heat are combined to obtain the over-cold (77-110 deg.K). Its advantages are easy control, no need of vacuum environment, and less loss of Pb.
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 high undercooling prepares the method for directed Ni-Pb immiscible alloy, belongs to the material technology field.
Background technology
The distinguishing feature of immiscible alloy is that its phasor high-temperature area exists a liquid phase immiscibility district, when alloy melt is reduced to this district by high temperature, two liquid phases are separated automatically, because two density of liquid phase differences are very big, under the foundry engieering condition of the ground of routine, very easily cause serious segregation even form laminated tissue, without any the engineering practical value.If by appropriate means second-phase dispersion is distributed, such alloy then has many special physics and mechanical property.Along with people's deepening continuously and the develop rapidly of modern material technology of preparing and to immiscible alloy liquid-liquid phase separation mechanism understanding to the requirement of the miscible class alloy of difficulty property, the investigation of materials personnel have attempted studying the preparation method of multiple immiscible alloy, as powder metallurgic method, traditional directional solidification method, microgravity melt casting, rapid solidification/powder metallurgic method after the match, have only traditional directional solidification method can be used for preparing directed immiscible alloy material at present.Traditional directional solidification process comprises 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 also very high.Find by literature search, people such as Liu Yuan are at " Acta Metallurgica Sinica ", 2000,12, write articles " microstructure of rapid solidification Al-In monotectic alloy " on p1233～1236, this article has reported that employing single-roller method chilling fast solidification technology prepares homogeneous Al-In monotectic alloy, chilling flash set technology characteristics are exactly that setting rate is exceedingly fast, under the chilling condition, two-phase does not have time enough to separate to alloy because setting rate is exceedingly fast by the immiscible range time, can obtain the immiscible alloy of meticulous disperse structure equally, but this method is difficult to prepare directed difficult miscible class alloy.
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-Pb immiscible alloy solidified structure develops, provide a kind of high undercooling to prepare the method for directed Ni-Pb immiscible alloy, make it have the advantage of traditional directional solidification technique and flash set technology concurrently, technology is simple, and cost is lower.The present invention is achieved by the following technical solutions, high undercooling preparation process of the present invention is undertaken by high-frequency induction heating apparatus, it is cold that the method that adopts molten glass purification and cyclical superheating to combine makes that the Ni-Pb alloy obtained, at the condensate depression scope internal trigger forming core of 77～110K, prepare directionally solidified alloy.
Below the inventive method is further specified, its step is specific as follows:
1. Ni, Pb alloy material are put into the quartz crucible of 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: 39.5%SiO
2, 40.9%B
2O
3, 1.1%Al
2O
3, 0.3%CaO, 18.2%Na
2O fires in 1223K fusion in the conventional ceramic crucible and to form in 24 hours.
2. by radio-frequency induction coil induction heating alloy to 1173～1273K, make the scavenging agent fusion coated at alloy surface;
3. be warming up to 1650～1750K, be incubated degasification in 2 minutes;
4. 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, when condensate depression reaches 77～110K interval, adopt Ni artificially to trigger forming core, naturally cooling subsequently, Water Quenching when being cooled to 1073K at the sample top.
The present invention has substantive distinguishing features and marked improvement; process of setting of the present invention is controlled easily; only need control alloy condensate depression scope can prepare directed Ni-Pb alloy fast; alloy prepares the needing no vacuum environment; not oxidation of alloy and Pb element volatilization loss are few under the molten glass purification protection; the condensate depression that needs is less, reaches easily.
Embodiment
The present invention only requires to control the alloy condensate depression, when condensate depression between 77～110K scope internal trigger sample top, can obtain directionally solidified alloy.Content below in conjunction with the inventive method further provides embodiment:
Embodiment one: high undercooling prepares directed Ni-25wt%Pb immiscible alloy material
1. the Ni-25wt%Pb alloy material is put into the quartz crucible of insulation shell, and added an amount of glass scavenging agent in the metal charge upper and lower surface; 2. pass through radio-frequency induction coil induction heating alloy to 1173K, make the scavenging agent fusion coated at alloy surface; 3. be warming up to 1650K, be incubated 2 minutes; 4. 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 77K, adopt Ni artificially to trigger forming core at the sample top, naturally cooling solidifies subsequently, obtains the symbiotic directed Ni-25wt%Pb alloy graining tissue of two-phase.
Embodiment two: high undercooling prepares directed Ni-31.44wt%Pb immiscible alloy material
1. the Ni-31.44wt%Pb alloy material is put into the quartz crucible of insulation shell, and added an amount of glass scavenging agent in the metal charge upper and lower surface; 2. pass through radio-frequency induction coil induction heating alloy to 1223K, make the scavenging agent fusion coated at alloy surface; 3. be warming up to 1700K, be incubated 2 minutes; 4. 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 96K, adopt Ni artificially to trigger forming core at the sample top, naturally cooling solidifies subsequently, obtains the symbiotic directed Ni-31.44wt%Pb alloy graining tissue of two-phase.
Embodiment three: high undercooling prepares directed Ni-40wt%Pb immiscible alloy material
1. the Ni-40wt%Pb alloy material is put into the quartz crucible of insulation shell, and added an amount of glass scavenging agent in the metal charge upper and lower surface; 2. pass through radio-frequency induction coil induction heating alloy to 1273K, make the scavenging agent fusion coated at alloy surface; 3. be warming up to 1750K, be incubated 2 minutes; 4. 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 110K, adopt Ni artificially to trigger forming core at the sample top, naturally cooling solidifies subsequently, obtains the symbiotic directed Ni-40wt%Pb alloy graining tissue of two-phase.
Claims (3)
1, a kind of high undercooling prepares the method for directed Ni-Pb immiscible alloy, it is characterized in that: the high undercooling preparation process is undertaken by high-frequency induction heating apparatus, it is cold that the method that adopts molten glass purification and cyclical superheating to combine makes that the Ni-Pb alloy obtained, at the condensate depression scope internal trigger forming core of 77～110K, prepare directionally solidified alloy.
2, high undercooling according to claim 1 prepares the method for directed Ni-Pb immiscible alloy, it is characterized in that concrete steps are as follows:
1. Ni, Pb alloy material are put into the quartz crucible of insulation shell, and added the glass scavenging agent in the metal charge upper and lower surface;
2. by radio-frequency induction coil induction heating alloy to 1173～1273K, make the scavenging agent fusion coated at alloy surface;
3. be warming up to 1650～1750K, be incubated degasification in 2 minutes;
4. be heated to 1850～1950K, be incubated 2 minutes, solidify-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, when condensate depression reaches 77～110K interval, adopt Ni artificially to trigger forming core, naturally cooling subsequently, Water Quenching when being cooled to 1073K at the sample top.
3, high undercooling according to claim 2 prepares the method for directed Ni-Pb immiscible alloy, it is characterized in that each component of glass scavenging agent and weight percent thereof are: 39.5%SiO
2, 40.9%B
2O
3, 1.1%Al
2O
3, 0.3%CaO, 18.2%Na
2O fires in 1223K fusion in the conventional ceramic crucible and to form in 24 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03114937 CN1431327A (en) | 2003-01-16 | 2003-01-16 | Deep super-cooling method for preparing directional difficult mixed dissolve Ni-Pb alloy |
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| CN 03114937 CN1431327A (en) | 2003-01-16 | 2003-01-16 | Deep super-cooling method for preparing directional difficult mixed dissolve Ni-Pb alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304605C (en) * | 2003-09-17 | 2007-03-14 | 南京理工大学 | Process for preparing block nano crystal alloy by deep over cold melting body |
-
2003
- 2003-01-16 CN CN 03114937 patent/CN1431327A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304605C (en) * | 2003-09-17 | 2007-03-14 | 南京理工大学 | Process for preparing block nano crystal alloy by deep over cold melting body |
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