CN109881125A - A method of widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section - Google Patents
A method of widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section Download PDFInfo
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- CN109881125A CN109881125A CN201910307234.3A CN201910307234A CN109881125A CN 109881125 A CN109881125 A CN 109881125A CN 201910307234 A CN201910307234 A CN 201910307234A CN 109881125 A CN109881125 A CN 109881125A
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Abstract
The invention discloses a kind of methods for widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section, it is characterised in that (1) using Al, Ni, Y, Co, La metal as raw material, prepares just crystal form amorphous alloy component；(2) melt high-temperature resistivity is tested using four electrode method, obtains the temperature range of Melt Structure Transition；(3) using the vacuum spun furnace for having infrared color comparison temperature measurement, the amorphous thin ribbon of 30 μ m-thicks is prepared under specific melt temperature.Compared with the existing methods, the present invention can be directed to specific amorphous alloy component, pass through the accurate determination of melt temperature, aluminium-based amorphous alloy primary crystal Precipitation Temperature section can be increased, it anneals in high temperature 590K-600K, fcc-Al is all only precipitated in the insulating process of long period, lays the foundation for subsequent preparation Al based amorphous nano composite material.
Description
Technical field
The present invention relates to non-crystalline material fields, and in particular to a kind of to widen aluminium-based amorphous alloy primary crystal by selection melt temperature
The method in Precipitation Temperature section.
Background technique
In recent years, with the fast development of Aeronautics and Astronautics and transport facility lightness, especially in international oil price hurricane
Under the overall background risen, drop can save consumption, advocate low-carbon life and have become themes of the times, this to grind high-strength low-density material
Study carefully and exploitation is paid much attention to, such as Al base noncrystal alloy material.Its corrosion resistance and specific strength are high, tensile strength
Up to 1000 MPa or more, thus have a extensive future in light-weight high-strength material field.But these amorphous alloy systems is non-
Brilliant Forming ability is very weak, not easily passs through the method quickly solidified and directly prepares block amorphous alloy, the disadvantage pole in size
Big limits the development of Al base noncrystal alloy.When by reasonable preparation process formed Al based amorphous-nano-crystalline composite material,
When so that suitable nanoscale fcc-Al particle being precipitated on noncrystal substrate, not only the intensity of material can be made to further increase
(up to 3200MPa), and it is able to maintain good toughness.
By the partially-crystallized method for preparing composite material, need to meet two necessary conditions: first, amorphous alloy
It must be first crystal form crystallization, that is, fcc-Al is only precipitated；Second, subsequent crystallization and primary crystal crystallization it
Between have biggish temperature difference.First crystal form aluminium-based amorphous alloy type is more, for a kind of specific amorphous component, does not there is correlation also
Technology can increase temperature difference (the Δ T between primary crystal crystallization and the second crystallizationx), i.e. primary crystal Precipitation Temperature section.The present invention
The quasi- reasonable change by melt temperature, is prepared with wide Δ Tx, suitable annealing temperature is then selected, in the long period
Insulating process in be all only precipitated fcc-Al, therefore answering for suitable fcc-Al size and volume fraction can be obtained to be subsequent
Condensation material lays the foundation.
Summary of the invention
The present invention (advance material research) on the basis of previous work, by Melt Structure Transition with
It prepares amorphous to combine, by selecting the amorphous of suitable melt temperature preparation, increases its primary crystal crystallization temperature section.
To achieve the goals above, aluminium-based amorphous alloy/nanocrystalline composite material of the present invention the preparation method is as follows:
(1) using Al, Ni, Y, Co, La metal as raw material, by the alloy of certain atomic ratio preparation heterogeneity, it is put into vacuum
Melting obtains master alloy in arc-melting furnace；
(2) after being crushed master alloy, alloy part is placed in electron tubes type resistance furnace, tests melt high-temperature electric using four electrode method
Resistance rate obtains the temperature range of Melt Structure Transition；
(3) part master alloy is placed in quartz ampoule, using the vacuum spun furnace for having infrared color comparison temperature measurement, in specific melt
At a temperature of the amorphous thin ribbon of 30mm thickness is prepared.
Preferably, the ingredient that step (1) selects for first crystal form al based amorphous alloy ingredient.
Preferably, detailed process is as follows for step (2): broken master alloy is put into porcelain boat, is tested using four electrode method,
Suction is 8 × 10-2It is filled with argon gas after Pa, furnace temperature is risen into 1673K with the heating rate of 5K/min, records temperature-voltage
Curve.
Preferably, in step (2) when test melt resistivity, electrode is reacted with alloy melt under high temperature in order to prevent, is adopted
With graphite electrode and melt contacts, then it is connect using tungsten electrode extraction with equipment.
Preferably, the master alloy of certain mass the detailed process of step (3): is put into the quartz ampoule that lower end has nozzle
Interior, the hot spot for adjusting infrared radiation thermometer makes it be directed at alloy, and the temperature accuracy of test can control in ± 5K. when in vacuum chamber
Vacuum degree reaches 3.0 × 10-3 After Pa, starts electrode for copper roller revolving speed and be adjusted to 3500 rpm, it is rear to connect induction coil electricity
Source master alloy melting.After the temperature of alloy melt reaches required temperature, adjustment electric current keeps the temperature 5 s, is then charged with height
Pure argon sets up certain pressure difference between quartz ampoule and furnace chamber, is ejected into alloy on high-speed rotating copper roller,
Form strip.
Preferably, the amorphous thin ribbon of step (3) is Δ TxWidest, the range of choice of annealing temperature and time are wider.
The invention has the benefit that the present invention can pass through choosing for the first crystal form aluminium-based amorphous alloy of a certain special component
Temperature difference (Δ T between primary crystal crystallization and the second crystallization can be increased by selecting suitable preparation temperaturex), method is simple and effective, into
It and is to prepare aluminium-based amorphous alloy/nanocrystalline composite material to lay a good foundation.
Detailed description of the invention
Fig. 1 is the melt resistivity curve figure of 1 ingredient of example；
Fig. 2 is the DSC curve figure of the amorphous of 1 different temperatures of example preparation；
Fig. 3 is the amorphous thin ribbon annealing curve figure that example 1 has widest primary crystal Precipitation Temperature section.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, the present invention is carried out
It is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit
The present invention.
Embodiment 1
By Al, Ni, Y, Co metal according to Al85Ni5Y8Co2Stoichiometric ratio weigh, be put into melt back 4 in vacuum arc furnace ignition
It is secondary, master alloy ingot is smashed, is partially disposed in quartzy porcelain boat, is put into four electrode of graphite at a certain distance, is drawn and perseverance with tungsten wire
Stream source and nanovoltmeter connection demarcate temperature using K-type thermocouple, and above-mentioned electrode and thermocouple use insulator to separate and prevent from connecting
Effect of Short Circuit electric current.Then the sample bound is placed in electron tubes type resistance furnace, suction to 8 × 10-2Pa, Yi Houchong
Enter argon gas, furnace temperature is risen into 1523K heat preservation 30min with the heating rate of 5K/min, so that metal molten is full of porcelain boat bottom,
It is frozen into certain shapes, subsequent furnace cooling to room temperature.It inputs and stablizes alternating current 500mA, be warming up to by above-mentioned steps
1673K, temperature collection and voltage obtain current -voltage curve and obtain Melt Structure Transition temperature range, as shown in Figure 1.
The alloy of such ingredient, the temperature after selecting Melt Structure Transition prepare the primary crystal crystallization and the second crystalline substance of amorphous thin ribbon
Temperature difference (Δ T between changex) maximum, as shown in Figure 2.Another part master alloy is placed in quartz ampoule, is put into red
In the vacuum spun furnace of outer temperature measurer, it is heated to throw away the strip of 30mm thickness after predetermined temperature.600K anneals at relatively high temperatures
All do not occur intermetallic compound in 240min, as shown in Figure 3.
Embodiment 2
By Al, Ni, Y, Co, La metal according to Al86Ni6Y4.5Co2La1.5Stoichiometric ratio weigh, be put into vacuum arc furnace ignition
Melt back 4 times, master alloy ingot is smashed, be partially disposed in quartzy porcelain boat, is put into four electrode of graphite at a certain distance, use tungsten wire
Extraction is connect with constant-current source and nanovoltmeter, demarcates temperature using K-type thermocouple, above-mentioned electrode and thermocouple are separated using insulator
Prevent connection Effect of Short Circuit electric current.Then the sample bound is placed in electron tubes type resistance furnace, suction to 8 × 10- 2Pa is filled with argon gas later, furnace temperature is risen to 1523K heat preservation 30min with the heating rate of 5K/min, so that metal molten is full of
Porcelain boat bottom is frozen into certain shapes, subsequent furnace cooling to room temperature.Sample is taken out, is invaded in 30 DEG C of water, removal covering
Agent, then drying is placed in vacuum resistance furnace again, is inputted and is stablized alternating current 500mA, is warming up to 1673K by above-mentioned steps, adopts
Collect temperature and voltage.It obtains current -voltage curve and obtains Melt Structure Transition temperature range.
The alloy of such ingredient, select Melt Structure Transition after 1673K temperature prepare amorphous thin ribbon primary crystal crystallization and
Temperature difference (Δ T between second crystallizationx) maximum.Another part master alloy is placed in quartz ampoule, is put into infrared survey
It in the vacuum spun furnace of Wen Yi, is heated to throw away the strip of 30mm thickness after predetermined temperature, 590K anneals at relatively high temperatures, can be
All do not occur intermetallic compound within the scope of 120min.
Claims (6)
1. a kind of method for widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section, it is characterised in that: the following steps are included:
(1) using Al, Ni, Y, Co, La metal as raw material, by the alloy of certain atomic ratio preparation heterogeneity, it is put into vacuum
Melting obtains master alloy in arc-melting furnace；
(2) after being crushed master alloy, alloy part is placed in electron tubes type resistance furnace, tests melt high-temperature electric using four electrode method
Resistance rate obtains the temperature range of Melt Structure Transition；
(3) part master alloy is placed in quartz ampoule, using the vacuum spun furnace for having infrared color comparison temperature measurement, in specific melt
At a temperature of the amorphous thin ribbons of 30 μ m-thicks is prepared.
2. requiring a kind of raising aluminium-based amorphous alloy/nanocrystalline preparation efficiency method according to power 1, it is characterised in that: material
The purity for expecting Al is 99.999% wt.%, and the purity of Ni is 99.99% wt.%, and the purity of Co is 99.99%, and rare-earth elements La is
99.9% wt.%, Y are 99.5% wt.%.
3. requiring a kind of method for widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section according to power 1, it is characterised in that: step
Suddenly the aluminium-based amorphous alloy prepared in (2) is first crystal form amorphous alloy.
4. requiring a kind of method for widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section according to power 1, it is characterised in that: step
Suddenly detailed process is as follows for test melt resistivity in (2): broken master alloy is put into porcelain boat, is tested using four electrode method,
Suction is 8 × 10-2It is filled with argon gas after Pa, furnace temperature is risen into 1673K with the heating rate of 5K/min, records temperature-voltage
Curve.
5. requiring a kind of method for widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section according to power 1, it is characterised in that: step
The temperature of melt can control its precision in ± 5K when preparing amorphous thin ribbon in (3) suddenly.
6. according to a kind of method for widening aluminium-based amorphous alloy primary crystal Precipitation Temperature section is required according to power 1, feature exists
In: the temperature after specific melt temperature is Melt Structure Transition in step (3), the primary crystal Precipitation Temperature section of the amorphous of preparation
It is most wide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2732809C1 (en) * | 2020-01-15 | 2020-09-22 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Тихоокеанский государственный университет" | Method of obtaining a ligature with aluminides of nickel and rare-earth metals for modifying aluminium alloys |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106868430A (en) * | 2017-02-17 | 2017-06-20 | 中国科学院金属研究所 | A kind of alloy component design method of regulation and control aluminium-based amorphous alloy Forming ability |
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- 2019-04-17 CN CN201910307234.3A patent/CN109881125A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106868430A (en) * | 2017-02-17 | 2017-06-20 | 中国科学院金属研究所 | A kind of alloy component design method of regulation and control aluminium-based amorphous alloy Forming ability |
Non-Patent Citations (1)
| Title |
|---|
| 王知鸷: "Zr/Al 基非晶合金的电阻及内耗行为与熔体状态的相关性", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2732809C1 (en) * | 2020-01-15 | 2020-09-22 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Тихоокеанский государственный университет" | Method of obtaining a ligature with aluminides of nickel and rare-earth metals for modifying aluminium alloys |
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Application publication date: 20190614 |