SU1763307A1 - Container for samples of ultra-pure solids - Google Patents

Abstract

Use: materials. SUMMARY OF THE INVENTION: The container includes a hermetically sealed quartz ampoule, an insert, a guard cup, a removable cup cover, a pressure pad, installed in the ampoule. The pressure pad is placed in the glass with the possibility of contact with the lid. 1 hp ff, 1 ill.

Description

The invention relates to the field of materials of high-purity substances exposed to atmospheric air, in particular their packaging, transportation and storage.

There are several ways of packaging high-purity solids: plastic films and bags, glass cans, plastic cans, tracing paper, glass ampoules, metal containers, and others. The most widespread in the last 15 years as a packaging material received polyethylene. For example, ingots of high-purity lead of the COOOO, COOO and COO brands are wrapped with plastic wrap, then parchment; during long-term storage, the ingots are placed in bags of plastic film whose necks are welded. However, under the influence of atmospheric air, the lead ingot is covered with an oxide film, gases and water are sorbed on its surface, and the ingot is rubbed with organic impurities when rubbing polyethylene. In this form, lead ingots cannot be directly used to synthesize semiconductor compounds (for example, PbSnTe, PbSe , PbS, PbTe, etc.), because during the synthesis, oxide compounds of lead, sorbed gases and water violate the stoichiometry of the compound and form additional phase impurities. Since the amount of oxide film, sorbed gases and water on each lead ingot is different, reproducible synthesis results are not obtained, and solid and gaseous inclusions make the samples heterogeneous, which negatively affects the physico-chemical characteristics of the synthesized samples and makes it difficult to apply them. devices.

Similar packaging of polyethylene film is used for other simple high-purity substances, for example, for cadmium 1, antimony, used in semiconductor and electronic equipment, hermetic

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Thus, the packaging of high-purity substances in a polyethylene film does not preserve their purity during storage and transportation, which negates all the effort expended on cleaning. Similar drawbacks are inherent in the consistency of high purity substances (for example, elemental sulfur of grade 14–16 grade) in glass jars with ground stoppers or screw caps. Preferably, glass packaging consists in eliminating contamination of high-purity substances with organic compounds.

There is a method for packaging high purity substances in glass vials. For example, at the final stage of obtaining in vacuum a metal mouse of the brand OCh 19-5, the mouse is deposited on the walls of a glass ampoule, which is discharged after the cleaning process is completed. However, when the ampoule is opened, it is possible that the mouse gets into glass fragments, which can lead to contamination of the mouse with a hardening compound during its preparation.

It is known 2 that sealed quartz ampoules are used for packaging high-purity substances and semiconductor materials. Before sealing, the ampoule is evacuated or filled with an inert gas. To prevent the high-purity substance from rubbing against the walls of the ampoule, an insert is inserted into it from the side of the sealed end, which prevents the substance from moving and rubbing against the walls of the ampoule. Such a container design (ampoule + insert) for high purity substances preserves the purity of the substance during storage and transportation, but does not retain purity during the opening. When the ampoule with the high purity substance is opened, fragments fall onto it, which can lead to contamination and, therefore, the complex compound in which the substance is a component. The degree of contamination is especially increased if the high-purity substance is in the form of pieces or powder, since fragments of the ampoule can be lost among powder or pieces of substance.

The aim of the present invention is to reduce the contamination of samples during transportation and opening of the ampoule.

The goal is achieved by the fact that in a known container construction, which is an ampoule made with the possibility of hermetic sealing, and

an insert placed therein, a sample beaker placed under the insert and having a free-mounted lid. The container is additionally provided with a pressure pad installed in the glass with the possibility of contact with the lid.

FIG. 1 shows the container structure:

1.- high purity substance;

2.- glass;

3.- cover;

4.- ampoule;

5.- insert;

6.- clamping insert.

The most preferred material for making the container is silica glass. It is possible to use thermoplastic polymeric materials such as organic glass, polystyrene, etc. The use of plastics in the proposed design is permissible, since the high-purity substance is rigidly fixed and does not rub against the walls of the glass, lid or liner.

The packaging of the high purity substance in the container is carried out as follows. The container is prepared (washed) by one of the known methods, then it is transferred to a sealed box filled with an inert gas (for example, argon). In the box, an ingot of high-purity substance (1) is placed in a glass (2). A cap (3) is put on the beaker and a beaker with an ingot of high-purity substance and a cap is inserted into the ampoule (4). An insert (5) is placed inside the ampoule (4) so that it rests on the cover (3). The container is removed from the box, connected to a vacuum system, pumped out and sealed (for example, the walls of the ampoule (4) are deposited on the walls of the insert (5) around the entire circumference of the ampoule with a flame of a gas burner). The connection of the ampoule with the vacuum system can be carried out by one of the known methods, for example, by means of a grinding compound, a fungal seal, and the like.

Similarly, packaging of high-purity substances is made in the form of pieces or powder. After filling the glass with pieces (powder) of high-purity substance (1), the insert (6) is inserted into the glass so that part of the insert (6) protrudes above the glass (2); the cup is closed with a lid (3) and inserted into the ampoule (4), then the insert (5) is placed inside the ampoule so that it is supported on the lid (3). Further, the container is sealed as described above.

In the proposed design, the cup and the lid serve to protect the solid high-purity substance from contamination by fragments forming the ampoule upon opening. In the event that the high-purity substance is in the form of an ingot, the height of the glass must be less than the length of the ingot, thanks to which the lid rests directly on the ingot, and the lid, in turn, is supported by an insert which, when sealing the container, is rigidly attached (welded ) to the walls of the ampoule, i.e. if the proposed ratio of the length of the ingot and the height of the glass is maintained, the ingot is rigidly fixed inside the container, does not move during transportation and, therefore, does not get dirty. In the event that a high-purity substance is in the form of a powder or pieces, it is almost impossible to provide 100% filling with the substance of the glass; therefore, during transportation, the high-purity substance can be poured, rubbed against the walls of the glass and, therefore, contaminated. To eliminate this cause, the powders and pieces of high-purity substance may be contaminated, in the proposed design an insert is placed inside the glass. The bottom of the deposits lies directly on the powder or pieces, thereby virtually eliminating friction of the high-purity substance on the wall of the glass during transportation. Hard fixation of powder and pieces in the container of the proposed design also allows preserving the particle size distribution of the substance during its transportation.

Using the proposed container design, it is possible to pack solid high-purity substances of almost any mass. Such a container design ensures that the purity of the solid high-purity substances is maintained during storage, transportation and opening of the container. Hard fixation of the substance, protection from exposure to atmospheric air, protection of the substance from the fragments of the ampoule upon opening at the opening of the substance make it possible to reliably preserve the purity of the solid high-purity substance.

Claims (2)

1. The container for samples of high-purity solid substances, including a quartz ampoule, made with the possibility of hermetic sealing, and an insert placed in it to restrict the movement of samples, characterized in that, in order to reduce the contamination of the samples during transportation and opening of the ampoule, it is equipped with a glass placement of samples located under the insert and having a free-installed lid. 2. The container according to claim 1, characterized in that it is provided with a pressure insert placed in a glass with the possibility of contact with the lid.