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CN113324877A - Ultra-low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melt - Google Patents

Ultra-low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melt Download PDF

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Publication number
CN113324877A
CN113324877A CN202110607548.2A CN202110607548A CN113324877A CN 113324877 A CN113324877 A CN 113324877A CN 202110607548 A CN202110607548 A CN 202110607548A CN 113324877 A CN113324877 A CN 113324877A
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aluminum
sealing chamber
magnesium
partial pressure
oxygen partial
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徐春
丁亚飞
孙士阳
马冰洋
彭睿智
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects

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Abstract

The invention relates to a sealing chamber seat dropping method for observing wetting angles of molten aluminum and magnesium with extremely low oxygen partial pressure. Firstly, a quartz sealing chamber with extremely low oxygen partial pressure which does not generate gas exchange with a vacuum chamber of the heating furnace is constructed in a low-vacuum heating furnace, then aluminum and magnesium metal in the sealing chamber are heated to be molten, and observation and measurement of wetting angles of aluminum and magnesium melt and a ceramic test piece in the sealing chamber are realized. The sealing chamber constructed at a lower heating temperature has extremely low oxygen partial pressure and nitrogen partial pressure, can eliminate the restriction of an oxide film on the surfaces of aluminum and magnesium to liquid drops, realizes the observation and measurement of the wetting angle of a molten metal on the surface of a ceramic test piece at a high temperature, greatly reduces the strict requirement on the required vacuum degree of observation equipment, and has the advantages of accurate and reliable observation result, convenient operation and low cost.

Description

Ultra-low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melt
Technical Field
The invention relates to a technology in the field of composite materials, in particular to a method for observing a wetting angle of aluminum and magnesium melt by obtaining an extremely low oxygen partial pressure sealing chamber.
Background
The composite material composed of metal and ceramic, whether a metal-based composite material or a ceramic-based composite material, has wide application in modern industry, and the application field of the composite material is still continuously expanded. The metal matrix composite material composed of light metal such as aluminum, magnesium, titanium and the like and a ceramic reinforcement has the characteristics of light weight and high strength, has special advantages in the field of light weight of vehicles including space flight and aviation, and is indispensable in modern industry due to the characteristics of high hardness, high modulus and the like in the ceramic matrix composite material represented by hard alloy.
The wetting behavior of molten metal and solid ceramic is of great significance in the preparation, processing and connection of composite materials, and is described and characterized by a seat drop method of a wetting angle formed after the metal is melted on the surface of the ceramic. When observing the wettability of the metal droplets by the sitting drop method, a low-pressure vacuum is the most basic gas phase environment, and the oxygen partial pressure therein is very important, and the wetting behavior of the droplets is strongly influenced by the oxide films formed on the surfaces of the solid metal and the subsequent droplets. For aluminum and magnesium which are extremely easy to oxidize, the formed surface oxide film is extremely difficult to remove, and the oxide films not only influence the accuracy of the observation result of the wetting angle of the liquid drop, but also even cause the metal liquid drop to be difficult to form.
The surface of the aluminium is covered with a layer of strong Al with a melting point up to 2050 DEG C2O3The oxide film, this dense oxide film, is extremely chemically stable and needs to be as low as 10 deg.C even at high temperatures of 1000 deg.C-30Decomposition is possible only at an oxygen partial pressure of Pa, which is not achieved by the prior art.
Magnesium is also an extremely active metal, the surface of which is also covered with an oxide film which has extremely stable chemical properties and a melting point of 2852 ℃, the loose property of the oxide film enables the thickness of the oxide film to continuously increase along with the increase of temperature and the prolongation of time under the vacuum with very low oxygen partial pressure, and the high saturated vapor pressure characteristic of magnesium metal and the volatilization generated under the conditions of high temperature and vacuum make the observation of the wetting angle of the metal difficult.
To eliminate Al2O3And the restraint of the MgO surface film on the aluminum and magnesium liquid drops, the prior art adopts an improved seat drop method, the method tears off the oxide film on the surface of the molten liquid by pressing the molten liquid of aluminum or magnesium out of a small hole and dropping the molten liquid onto the surface of a ceramic test piece, and the process and subsequent observation still need to maintain the environment in a gas phase environment with very low oxygen partial pressure. Vacuum is often used in a gas phase environment for aluminum, and inert gas at a pressure for magnesium to prevent evaporation of magnesium.
Although the improvement of the seat drop method in the prior art by adopting the drop method can tear off the surface oxide film of the active metal to obtain the drops, the drop kinetic energy of the molten metal can affect the accuracy of the obtained wetting angle, and the technology still needs to be adopted in the environment with very low oxygen partial pressure. For aluminum, only the aluminum melt and Al are satisfied2O3Capable of reacting at high temperature to form gaseous Al2The thermodynamic condition of O can prevent Al2O3The regeneration of oxide film, this reaction requires the oxygen partial pressure of vacuum environment to be as low as 10-6Pa. For magnesium, the inert gas charge also requires a very low oxygen partial pressure to prevent metal volatilization and surface MgO film formation and thickening. Due to these demanding low oxygen partial pressure vacuum environment requirements, the improved sitting drop method of the prior art still has the disadvantage of being difficult to popularize.
Disclosure of Invention
The invention provides a sealing chamber seat dripping method for observing the wetting angle of molten aluminum and magnesium metal, aiming at the defects that the prior art is difficult to remove an oxide film on the surface of the molten aluminum and magnesium and prevents liquid drops from being oxidized again and the wetting angle deviation is caused by the dripping kinetic energy of the molten aluminum and magnesium metal.
The invention is realized by the following technical scheme:
a very low oxygen partial pressure sealing chamber seat dropping method for observing wetting angles of aluminum and magnesium melts is characterized in that a very low oxygen partial pressure quartz sealing chamber which does not generate gas exchange with a vacuum chamber of a heating furnace is constructed in a low-vacuum heating furnace, then aluminum and magnesium metals in the sealing chamber are heated to be molten, and the wetting angles of the aluminum and magnesium melts and a ceramic test piece in the sealing chamber are observed and measured.
Further, the specific method for constructing the quartz sealed chamber with the extremely low oxygen partial pressure which does not generate gas exchange with the vacuum chamber of the heating furnace in the low-vacuum heating furnace is as follows: the quartz cup is placed on a metal or ceramic base with a groove in an inverted mode, indium tin alloy is placed in the groove, the vacuum chamber of the heating furnace is vacuumized and filled with inert gas, the space in the quartz cup is sealed after the indium tin alloy in the groove is melted through heating, and a sealing chamber which does not generate gas exchange with the vacuum chamber of the heating furnace is obtained.
Furthermore, a ceramic test piece is placed on the metal or ceramic base with the groove in advance, and a test piece of aluminum or magnesium or their respective alloys is placed on the ceramic test piece.
Furthermore, a small weight for generating pressure is arranged at the outer top of the inverted quartz cup.
Further, the vacuum degree in the vacuum chamber of the heating furnace is pumped to 10-1Pa。
Further, aluminum powder for further reducing the partial pressure of oxygen and nitrogen in the sealing chamber is placed in the quartz cup so as to consume the residual oxygen and nitrogen in the sealing chamber.
Further, the metal or ceramic base is made of one of steel, quartz and alumina which can be wetted by indium tin alloy.
Further, the indium content in the indium-tin alloy is 30-60%, and the melting temperature of 120-180 ℃ is obtained, so that the sealing of the sealing chamber can be realized within the temperature range.
Further, the aluminum or magnesium test block comprises pure aluminum or pure magnesium or various alloys based on the pure aluminum or the pure magnesium; the ceramic test piece is made of alumina, aluminum nitride or silicon nitride ceramic.
Further, the inert gas is filled in, and the pressure intensity is 50-500 Pa, wherein the inert gas does not generate chemical reaction with aluminum and magnesium.
The invention has the beneficial effects that:
compared with the seat drop method in the prior art and the improved seat drop method capable of enabling the molten liquid to drop, which need equipment for obtaining high vacuum and have the defect that the molten liquid drops to generate unstable data, the invention can construct a transparent sealing chamber with an extremely low oxygen partial pressure vacuum environment in a common low-vacuum heating furnace, and the sealing chamber formed at a lower temperature lower than 180 ℃ has the advantages of preventing the thickening of an oxide film on the surface of an aluminum test block and a magnesium test block before melting, preventing the oxidation of the liquid drops in the spreading process, and realizing the direct observation and measurement of the wetting angle of the liquid drops and the surface of a ceramic test block and the change of the wetting angle with the temperature and the time. The method has the advantages of convenience, accuracy, high efficiency and low cost.
Drawings
FIG. 1 is a schematic view of the apparatus for sealing according to the present invention;
in the figure: 1-base, 2-indium-tin alloy, 3-quartz cup, 4-small weight, 5-aluminum powder, 6-ceramic test piece and 7-metal test piece.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1:
as shown in FIG. 1, the method for observing the wetting angle of aluminum and magnesium melts based on the sealing chamber seat dropping method with extremely low oxygen partial pressure for the embodiment observes that pure aluminum is in Al2O3Wettability of the ceramic surface. A quartz cup 3 with a flat opening is adopted and is placed on a base 1 with a groove upside down, indium tin alloy 2 is placed in the groove, a small weight 4 is pressed on the upper part of the quartz cup, aluminum powder 5 for absorbing oxygen and nitrogen is placed on the base in the quartz cup, and a ceramic test piece 6 (Al) for testing is also placed on the base2O3) And a metal test piece 7 (pure aluminum) to be tested is placed on the ceramic test piece 6.
Placing the combination in a low vacuum heating furnace with an observation hole, and vacuumizing the vacuum chamber of the heating furnaceHollow to 10- 1And after Pa, heating to melt the indium tin alloy (150 ℃), and immersing the quartz cup into the melted indium tin alloy liquid under the pressure of a small weight to seal the inner space of the quartz cup, thereby obtaining a quartz sealing chamber which does not generate gas exchange with the vacuum chamber of the heating furnace. And continuously heating the sealed chamber to a certain temperature after the aluminum is melted, and observing and measuring the wetting angle and the change of the wetting angle along with time obtained at the temperature that the aluminum liquid is dripped on the aluminum oxide test piece through an observation hole of the heating furnace and the transparent quartz cup.
Example 2:
as shown in FIG. 1, the present example is based on a very low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melts, and pure magnesium is observed in Al2O3Wettability of the ceramic surface. A quartz cup 3 with a flat opening is adopted and is placed on a base 1 with a groove upside down, indium tin alloy 2 is placed in the groove, a small weight 4 is pressed on the upper part of the quartz cup, aluminum powder 5 for absorbing oxygen and nitrogen is placed on the base in the quartz cup, and a ceramic test piece 6 (Al) for testing is also placed on the base2O3) And a metal test piece 7 (pure magnesium) to be tested is placed on the ceramic test piece.
Placing the combination in a low vacuum heating furnace with observation holes, and vacuumizing the vacuum chamber of the heating furnace to 10 DEG- 1And Pa, filling 100Pa of argon, heating until the indium tin alloy is molten (about 150 ℃), immersing the quartz cup into the molten indium tin alloy liquid under the pressure of a small weight to seal the inner space of the quartz cup, and obtaining a quartz sealing chamber which does not generate gas exchange with the vacuum chamber of the heating furnace, wherein the oxygen partial pressure in the sealing chamber is extremely low, the argon partial pressure is kept at 100Pa, and the volatilization of magnesium can be prevented. The sealed chamber is continuously heated to a certain temperature after magnesium is melted, and the wetting angle and the change of the wetting angle along with time of the wetting angle are observed and measured at the temperature of the magnesium liquid drop on the alumina test piece through the observation hole of the heating furnace and the transparent quartz cup.
In the implementation above:
preferably, the outer top of the quartz cup is provided with a small weight for generating pressure.
Preferably, the metal or ceramic base is one of steel, quartz and alumina that is wettable by indium tin alloy.
Preferably, the indium content in the indium-tin alloy is 30-60%, and a melting temperature of 120-.
Preferably, the aluminum or magnesium coupon comprises pure aluminum or pure magnesium or various alloys based thereon.
Preferably, various ceramics such as alumina, aluminum nitride, or silicon nitride are used as the ceramic test pieces.
Preferably, the inert gas is a gas which does not generate chemical reaction with aluminum and magnesium, and the pressure range is 50-500 Pa.
The foregoing embodiments may be modified in many different ways by those skilled in the art without departing from the spirit and the principle of the invention, and the scope of the invention is not limited by the above embodiments, but rather by the claims, and all implementations that fall within the scope of the invention are to be considered limited by the scope of the invention.

Claims (10)

1. A very low oxygen partial pressure sealing chamber seat dropping method for observing wetting angles of aluminum and magnesium melts is characterized in that: firstly, a quartz sealing chamber with extremely low oxygen partial pressure which does not generate gas exchange with a vacuum chamber of the heating furnace is constructed in a low-vacuum heating furnace, then aluminum and magnesium metal in the sealing chamber are heated to be molten, and observation and measurement of wetting angles of aluminum and magnesium melt and a ceramic test piece in the sealing chamber are realized.
2. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 1, wherein: the specific method for constructing the quartz sealing chamber with the extremely low oxygen partial pressure and without gas exchange with the vacuum chamber of the heating furnace in the low-vacuum heating furnace comprises the following steps: the quartz cup is placed on a metal or ceramic base with a groove in an inverted mode, indium tin alloy is placed in the groove, the vacuum chamber of the heating furnace is vacuumized and filled with inert gas, the space in the quartz cup is sealed after the indium tin alloy in the groove is melted, and a sealing chamber which does not generate gas exchange with the vacuum chamber of the heating furnace is obtained.
3. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: the metal or ceramic base with the groove is pre-provided with a ceramic test piece, and a test piece of aluminum or magnesium or alloy based on the aluminum or magnesium or the alloy is arranged on the ceramic test piece.
4. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: and a small weight for generating pressure is arranged at the outer top of the quartz cup.
5. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: the vacuum degree in the vacuum chamber of the heating furnace is 10-1Pa。
6. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: aluminum powder for further reducing the partial pressure of oxygen and nitrogen in the sealing chamber is placed in the quartz cup so as to consume the residual oxygen and nitrogen in the sealing chamber.
7. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: the metal or ceramic base is made of one of steel, quartz and aluminum oxide which can be wetted by indium-tin alloy.
8. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: the indium content in the indium-tin alloy is 30-60%, and the melting temperature of 120-180 ℃ is obtained, so that the sealing of the sealing chamber can be realized in the temperature range.
9. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: the aluminum or magnesium test block comprises pure aluminum or pure magnesium and various alloys based on the pure aluminum or the pure magnesium; the ceramic test piece is made of alumina, aluminum nitride or silicon nitride ceramic.
10. The method for observing the wetting angle of the aluminum and magnesium melts for the pedestal drop of the sealing chamber with the extremely low oxygen partial pressure as claimed in claim 2, wherein: the filled inert gas is gas which does not generate chemical reaction with aluminum and magnesium, and the pressure range is 50-500 Pa.
CN202110607548.2A 2021-06-01 2021-06-01 Ultra-low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melt Pending CN113324877A (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT218554B (en) * 1959-12-24 1961-12-11 Voest Ag Method and device for performing metallurgical processes, in particular for refining or pre-refining pig iron, for refining and alloying steel
CN1054579A (en) * 1989-10-19 1991-09-18 艾尔坎国际有限公司 With the method for microwave heating heat-treating unstable ceramics and used receptor
CN1242715A (en) * 1997-10-28 2000-01-26 阿莫科公司 Composite materials for membrane reactors
CN1442882A (en) * 1997-10-15 2003-09-17 佳能株式会社 Formation method of indium oxide film, substrate having indium oxide film and semiconductor unit
CN101308077A (en) * 2008-06-17 2008-11-19 中国科学院过程工程研究所 Apparatus and method for measuring middle and low-temperature smelt surface tension, density and wettability
CN102484032A (en) * 2009-08-26 2012-05-30 旭硝子株式会社 Electrode for discharge lamp, process for production of electrode for discharge lamp, and discharge lamp
CN103420568A (en) * 2013-07-17 2013-12-04 戴长虹 Seal structure of vacuum glass air suction mouth and manufacturing method thereof
CN103954534A (en) * 2014-04-14 2014-07-30 上海大学 Device for synchronously measuring wetting angle and differential scanning calorimetry (DSC) curve of metals on substrate
CN106885760A (en) * 2017-04-11 2017-06-23 攀钢集团研究院有限公司 For the measure device and assay method of metal solid-liquid boundary energy
CN111910148A (en) * 2020-08-28 2020-11-10 浙江华达新型材料股份有限公司 Method for forming compact oxide film on surface of Fe-Mn-Al alloy

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT218554B (en) * 1959-12-24 1961-12-11 Voest Ag Method and device for performing metallurgical processes, in particular for refining or pre-refining pig iron, for refining and alloying steel
CN1054579A (en) * 1989-10-19 1991-09-18 艾尔坎国际有限公司 With the method for microwave heating heat-treating unstable ceramics and used receptor
CN1442882A (en) * 1997-10-15 2003-09-17 佳能株式会社 Formation method of indium oxide film, substrate having indium oxide film and semiconductor unit
CN1242715A (en) * 1997-10-28 2000-01-26 阿莫科公司 Composite materials for membrane reactors
CN101308077A (en) * 2008-06-17 2008-11-19 中国科学院过程工程研究所 Apparatus and method for measuring middle and low-temperature smelt surface tension, density and wettability
CN102484032A (en) * 2009-08-26 2012-05-30 旭硝子株式会社 Electrode for discharge lamp, process for production of electrode for discharge lamp, and discharge lamp
CN103420568A (en) * 2013-07-17 2013-12-04 戴长虹 Seal structure of vacuum glass air suction mouth and manufacturing method thereof
CN103954534A (en) * 2014-04-14 2014-07-30 上海大学 Device for synchronously measuring wetting angle and differential scanning calorimetry (DSC) curve of metals on substrate
CN106885760A (en) * 2017-04-11 2017-06-23 攀钢集团研究院有限公司 For the measure device and assay method of metal solid-liquid boundary energy
CN111910148A (en) * 2020-08-28 2020-11-10 浙江华达新型材料股份有限公司 Method for forming compact oxide film on surface of Fe-Mn-Al alloy

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