JPH08247905A - Method and equipment for detaching molten sample - Google Patents

Abstract

PURPOSE: To enable execution of a supercooling experiment of a molten sample with high accuracy by suppressing vibration and further mixing-in of impurities, in equipment for detaching the molten sample which is used for a physicochemical apparatus or the like utilizing a drop tower. CONSTITUTION: After a sample 1 having a hole 2 made is held by a fiber 3 such as a carbon fiber in an inactive gas atmosphere and melted by an infrared heating furnace 4, the fiber 3 is oxidized and evaporated completely by introducing oxygen gas into the heating furnace by an oxygen introducing mechanism 6 and thereby the molten sample is detached from the fiber without mixing-in of impurities. Accordingly, this method and equipment are supposed to be utilized not only in the field of crystal growth, but also in the field of manufacture of glass, and further development of new materials is expected, since the natural characteristics of materials are made clear by an experiment.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for releasing a molten sample. For more information,
The present invention relates to a method and a device for releasing a molten sample useful for a physics and chemistry device using a falling tower.

[0002]

2. Description of the Related Art In a containerless experiment of a molten sample using a falling tower, it is necessary to release the molten sample without applying vibration to the sample. However, in the case of the conventional method in which the molten sample held by the wire is separated by applying vibration, there is a problem that the microgravity environment cannot be fully utilized because the molten sample has an initial velocity.

Further, a method is known in which a molten sample is cut off by burning the wire by energizing the holding wire. However, this method of burning out the wire and cutting off the molten sample by energization makes it difficult to burn off the wire at the target site, and the unburned wire is mixed as impurities into the sample, which adversely affects the melting and solidifying characteristics of the sample. There are problems such as giving.

[0004] The present invention has been made in view of the above circumstances, and solves the disadvantages of the conventional method, is a method suitable for a microgravity environment, and has a new molten sample which does not cause the problem of impurity contamination. And a method of releasing the same.

[0005]

SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems by holding a hard-to-oxidize solid sample with an inorganic fiber which is more easily oxidizable than this sample and has a high melting point, and is used in an inert gas atmosphere. A method for separating a molten sample, comprising introducing an oxygen gas to completely oxidize and evaporate the fiber after heating and melting the fiber, and separating the molten sample from the fiber without mixing impurities.

As an apparatus in this case, the present invention is provided with an inert gas introducing mechanism, a mechanism for holding a solid sample by inorganic fibers, a melting heating furnace for the solid sample, and an oxygen introducing mechanism. Under an inert gas atmosphere, the solid sample held by the inorganic fiber holding mechanism is melted in a melting and heating furnace, and the molten sample is cut off by oxidizing and evaporating the fiber of the holding mechanism with oxygen introduced from the oxygen introducing mechanism. The present invention also provides an apparatus for releasing a molten sample.

[0007]

According to the present invention, the fiber holding the hard-to-oxidize solid sample is only oxidized and evaporated after the sample is melted, so that the vibration during the evaporation can be suppressed and the advantage of the microgravity environment can be utilized. . The fiber for holding the sample may be any fiber as long as it has heat resistance enough to hold the solid sample even in a molten state, and is oxidized and evaporated. For example, carbon fiber, BN fiber, S
Any suitable material such as i ₃ N ₄ fiber and SiC fiber can be used.

[0008] These fibers may have any shape such that one or a plurality of them can suspend a solid sample or mount a solid sample.
A hole may be made in the solid sample, and a fiber may be penetrated through the hole to suspend the solid sample, or the solid sample may be held by a woven mesh. In this latter case,
Since the molten sample in which the entire molten sample is held is released, it is not necessary to make a hole in the sample in advance, and the operability is excellent.

The heating means is not particularly limited, and may be an infrared heating furnace or the like. Similarly, there is no particular limitation on the oxygen introduction mechanism. When the microgravity environment is applied by using the drop tower, the sample may be released by a command signal after dropping the infrared heating furnace main body, or the infrared heating furnace main body may be dropped using the sample release as a trigger. The fiber is oxidized even after the molten sample is released.
Since evaporation continues, there is no contamination of the fiber material into the sample.

Hereinafter, this description will be described in more detail with reference to examples.

[0011]

Embodiment 1 FIG. 1 of the accompanying drawings is a schematic view illustrating a molten sample cutting and releasing apparatus using a sample holding mechanism by the fiber of the present invention. For example, as illustrated in FIG.
A sample holding hole (2) with a diameter of 0.3 mm was made in an oxide sample (1) consisting of 0 mg of BaB ₂ O ₄ and the diameter was 0.1 m.
The carbon sample fiber (3) is passed through the sample holding hole (2) to hold the oxide sample (1), and is suspended from above the infrared heating furnace (4).

The sample part of the infrared heating furnace (4) has a diameter of 10
Since it is sealed using a transparent quartz tube (5) of mm, the atmosphere can be controlled. Here, high-purity Ar gas is introduced at a pressure of 1 atm and a flow rate of 100 cc / min. By raising the temperature of the infrared heating furnace (4), the BaB ₂ O ₄ sample, which is the oxide sample (2), is melted at a melting point of 1095 ° C., and the carbon fiber fiber (3) is melted by surface tension.
Is held.

The oxygen introduction mechanism (6) introduces oxygen at a pressure of 1.1 atm and a flow rate of 100 cc / min. The diameter of the oxygen introduction mechanism around the sample is 8 m so that infrared rays can pass through it.
m, a ring-shaped transparent quartz tube (7) having a slit (8) formed in a ring shape toward the molten oxide sample (1). The carbon fiber fiber (3) is oxidized and vaporized 0.1 seconds after contact with the molten oxide sample (2) in a high temperature state, and the molten sample (2) is cut off from the holding fiber (3). It Example 2 FIG. 2 of the accompanying drawings is a schematic view showing a sample holding mechanism using a carbon fiber mesh as another example of the present invention.

In the example shown in FIG. 2, BaB ₂ O ₄ , which is a 20 mg oxide sample (1), has a wire diameter of 0.05 mm.
It is placed and held on a 100-mesh carbon fiber mesh (9) and suspended from above the infrared heating furnace (4).
When the oxide sample (1) was heated by the infrared heating furnace (4) in the same manner as in Example 1, the oxide sample (1) was melted at a melting point of 1095 ° C.,
It is held on the carbon fiber mesh (9) by surface tension.

As in Example 1, when oxygen was introduced by the oxygen introduction mechanism (6) at a pressure of 1.1 atm and a flow rate of 100 cc / min, the carbon fiber mesh (9) was oxidized and evaporated 0.1 seconds later. , The molten sample (2) is cut off.

[0016]

According to the present invention, as described in detail above, in a molten sample separation device used in a physics and chemistry device using a falling tower, vibration and furthermore contamination of impurities can be suppressed, and a highly accurate molten sample can be suppressed. Supercooling experiment becomes possible. Also, because the principle is very simple,
By slightly modifying the conventional apparatus, the present invention can be adopted, and it is possible to provide a containerless processing process that maintains a high purity suitable for a microgravity environment.

The present invention is not limited to the field of crystal growth,
It is also expected to be used in the field of glass production, and furthermore, the original characteristics of the material will be clarified by experiments, so the development of new materials is expected.

[Brief description of drawings]

FIG. 1 is a schematic view showing an example of a molten sample cutting and releasing device of the present invention using a sample holding mechanism by fibers.

FIG. 2 is a schematic view illustrating a sample holding mechanism using a carbon fiber mesh as another example.

[Explanation of symbols]

 REFERENCE SIGNS LIST 1 oxide sample 2 sample holding hole 3 carbon fiber fiber 4 infrared heating furnace 5 transparent quartz tube 6 oxygen introduction mechanism 7 ring-shaped transparent quartz tube 8 ring-shaped slit 9 carbon fiber mesh 10 inert gas introduction mechanism

Claims (3)

[Claims] 1. A solid sample that is hardly oxidizable is held by an inorganic fiber having a higher melting point than the sample, and is heated and melted in an inert gas atmosphere. Then, oxygen is introduced to oxidize and evaporate the fiber. A method for releasing a molten sample, comprising releasing the molten sample from a holding fiber. 2. The method according to claim 1, wherein the solid sample is held by inorganic fibers made of a mesh-like woven body, and the molten sample is cut off. 3. An inert gas introduction mechanism, a solid sample holding mechanism with inorganic fibers, a melting heating furnace and an oxygen introduction mechanism for the solid sample, and an inorganic fiber holding mechanism under the introduced inert gas atmosphere. An apparatus for separating a molten sample, wherein the solid sample held by the mechanism is melted in a melting and heating furnace, and the fiber of the holding mechanism is oxidized and evaporated by oxygen introduced from an oxygen introduction mechanism to cut off the molten sample.