JP2665528B2 - Detecting agent - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a detecting agent, and more particularly, to an organic tellurium used in a cadmium tellurium (CdTe) compound semiconductor manufacturing process or the like and contained in an exhaust gas or the like. The present invention relates to a detection agent for detecting a compound.

[Conventional technology and problems to be solved]

With the development of the semiconductor industry, the types and amounts of substances used for it are increasing rapidly.

Of these substances, organic tellurium compounds such as dimethyl tellurium and diethyl tellurium are not only highly toxic but also flammable, so that careful handling is required.

Therefore, the working environment must be constantly measured when handling these toxic components, and it is necessary to take measures to accurately notify the worker if these toxic components leak.

In addition, when these toxic components are contained in the gas discharged from the semiconductor process, etc., they are released to the outside after being purified using a detoxification device, etc. There is a need.

However, a detecting agent capable of efficiently detecting an organic tellurium compound such as dimethyl tellurium and diethyl tellurium is not known.

[Means and actions for solving the problem]

The present inventors have continued their research to obtain a highly sensitive detector that can be applied to the detection of these organic tellurium compounds, and as a result, have found that a mixture of a zinc salt and a gold salt is extremely excellent as a discoloration component, The present invention has been completed.

That is, the present invention is an organic gas detecting agent containing an organic tellurium compound containing a mixture of a zinc salt and a gold salt as a color-changing component.

The detecting agent of the present invention can be commonly used for detecting a gas containing an organic tellurium compound such as dimethyl tellurium and diethyl tellurium in nitrogen, hydrogen, argon, helium, air and the like.

The discoloring component of the detecting agent is sensitively discolored from pale yellow to deep green to green or reddish brown depending on the type of the carrier upon contact with a gas containing these organic tellurium compounds.

In the present invention, the zinc salt used for the color-changing component of the detecting agent is a zinc salt of an inorganic acid and an organic acid.Examples of the salt of the inorganic acid include salts of oxo acids and halides. For example, copper salts such as carbonic acid, silicic acid, nitric acid, sulfuric acid, arsenic acid, boric acid, chloric acid, perchloric acid, chlorous acid, and hypochlorous acid, and halides such as zinc chloride, zinc bromide, and zinc iodide. No. As organic acids, formic acid, acetic acid, propionic acid, oleic acid,
Aliphatic monocarboxylic acids such as stearic acid and oxalic acid,
Zinc salts of aliphatic dicarboxylic acids such as adipic acid and sebacic acid, oxyacids such as lactic acid and tartaric acid, aromatic salts such as benzoic acid and toluic acid, and various acids such as naphthenic acid.

Among them, zinc chloride, zinc bromide and the like are preferable because they are water-soluble and easy to handle.

Various inorganic and organic acid salts can be used for the gold salt, but chloroauric acid and its sodium, potassium, and ammonium salts are preferred in view of availability and water solubility.

The mixing ratio of the gold salt to the zinc salt is not particularly limited, but for 1 g of zinc in the zinc salt, gold in the gold salt is usually 0.5 to 0.0
01 g, preferably in the range of 0.3 to 0.01 g.

When the ratio of gold is larger than 0.5 g, the color of the detection agent itself becomes brown, and discoloration may be difficult to distinguish.
If it is less than 0.001 g, the discoloration sensitivity decreases.

In the present invention, the mixture itself of the zinc salt and the gold salt, which are discoloring components, may be used as a detecting agent in powder form or molded into a pellet or the like, or may be supported on a carrier or the like as a detecting agent. However, a carrier is preferable, and a carrier supported on a porous carrier is particularly preferable.

The type of carrier can be selected from a wide range,
For example, catalyst carriers such as silica gel, silica alumina and alumina, among which white or colorless ones, are suitably used. Of these, alumina is preferred, and α-alumina is particularly preferred. Various kinds of α-alumina are commercially available, and usually contain 0.1 to 15% of silica as a binder. The specific surface area of the carrier is not particularly limited, but is preferably in the range of 0.001 to 1.0 m ² / g.

As a method for supporting the color-changing component when a carrier is used, for example, the carrier may be immersed in a solution in which the color-changing component is dissolved or suspended in water or various organic solvents, or the solution may be sprayed on the carrier surface. May be carried. If an organic solvent such as ethanol is used, drying in air at 100 ° C or higher causes the discoloration component to become black.In such a case, the pressure is reduced under an inert gas atmosphere at 80 ° C or lower. dry.

The amount of the discoloring component carried on the carrier is usually 0.01 to 5.0 parts by weight, preferably 0.05 to 1.0 part by weight, per 100 parts by weight of the carrier, as a total of zinc metal and gold.

The concentration of the organic tellurium compound detected by the detecting agent of the present invention is 0.1 ppm or more.

The flow rate of the gas to be brought into contact with the detection agent is usually linear velocity 0.01 to
100cm / sec. The temperature and pressure of the gas at the time of contact are set at −20 to 100 ° C. and 0.001 to 20 kg / cm ² abc.

The detection agent of the present invention is solid and is usually used in a transparent inspection window provided in a glass detection tube, a transparent container made of transparent plastic or the like, or a gas purification cylinder, and used in the system. The presence of the tellurium compound can be known from the color change of the detecting agent.

When used together with a purifying agent, it may be inserted downstream of the purifying agent layer in the purifying column or between a plurality of purifying agent layers, or a detector tube filled with a detecting agent may be connected behind the purifying tube. used.

〔The invention's effect〕

The detection agent of the present invention has the following excellent characteristics.

It can be used commonly for detecting organic tellurium compounds used in semiconductor manufacturing processes and the like, and has extremely high sensitivity.

It may be installed at the viewing window of a gas purifier or at the exit of an abatement system to detect breakthrough of an organic tellurium compound, or it may be used to detect leakage at a workplace. wide.

〔Example〕

Examples 1-4 86% by weight of α-alumina, 12% by weight of silica and 0.005 specific surface area
~0.040m ² / g, packing density 1.1 g / ml, diameter 3/16 inch spherical α- alumina (US, Norton Co.) chloroauric acid obtained by dissolving gold 5g in aqua regia to 500 g 5 Aqueous solution of 50
ml and an aqueous solution of 10 g of zinc chloride dissolved in 50 ml of water were each impregnated. Then in the rotary evaporator
It was dried at 80 ° C. for 3 hours to prepare a pale yellow detector.

5 g of this detecting agent was packed in a hard polyvinyl chloride column having an inner diameter of 13 mmφ, and 0.1 to
A nitrogen gas containing 5.0 ppm of dimethyl tellurium or diethyl tellurium was passed through at a linear velocity of 0.1 cm / sec to make contact with the detecting agent, and the time until the detecting agent changed color was measured.
The results are shown in Table 1.

Example 5 8-10 mesh, specific surface area 280 m ² / g, pore volume 1.05 ml /
g, an average pore diameter of 100 mm, and a packing density of 0.4 g / ml in 30 g of granular silica gel (manufactured by Fuji Devison Co., Ltd.). Each was impregnated and then dried at 80 ° C. for 3 hours in a rotary evaporator to prepare a pale yellow detector.

Using this detector, a nitrogen gas containing dimethyl tellurium was flowed in the same manner as in Example 1, and the time until the color changed was examined.

 The results are shown in Table 1.

Claims (1)

(57) [Claims] 1. A harmful gas detecting agent containing an organic tellurium compound containing a mixture of a zinc salt and a gold salt as a color-changing component.