JP2002148155A - Molten metal sample collection device, its method, and gas supplying device for sample collection probe - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a molten metal collecting device and its method capable of preventing a reaction between a sample and a sample collection vessel internal air and contamination of the sample with slag or a material at the tip for collecting a contamination-free sample. SOLUTION: This molten metal collection device 80 is constructed of a probe 81 and a gas supplying device connected to it. An inert gas vessel 101 is connected to the probe 81 via a tube 105, and inert gas is fed into the probe 81 via a three-way valve 111. In this condition, the probe 81 is immersed into molten steel. The air inside the probe 81 is replaced by the inert gas, and when a protection cap 51 and a vessel cap 41 are melted, gas is jetted from an inflow port 29 of the collection vessel 21 for removing the slag or the melted protection cap 51 and vessel cap 41 existing around the inflow port 29, and consequently, only the uncontaminated molten steel is left in the vicinity of the inflow port 29. Subsequently, when the three-way valve 111 is switched for returning the inside of the probe 81 to an atmospheric pressure, the molten steel flows into the vessel 21 and the sample is collected.

Description

DETAILED DESCRIPTION OF THE INVENTION

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a molten metal sampling apparatus for sampling molten metal, for example, molten metal to analyze the composition of molten steel during refining. Molten metal sampling equipment that can collect non-contaminated samples by preventing reaction with air, mixing of dissolved matter attached to the tip of the sample collection container into the sample, and mixing of floating slag in the molten metal into the sample About. Furthermore, the present invention relates to a gas supply device that enables the sampling of a sample that is not contaminated by switching the inside of a sampling container of a sampling probe between an inert gas and an ambient atmosphere to communicate therewith. Further, the present invention relates to a method for collecting a molten metal, which enables a non-contaminated sample to be collected.

2. Description of the Related Art Conventionally, various components in molten steel have been used in each refining process.
Analysis is performed for
The sampling probe is immersed in molten steel to collect various samples.
ing. Especially with the spread of ultra-low carbon steel in recent years,
The composition ratio of carbon contained in molten steel at a very low rate
In order to analyze the rate with high accuracy, a pin type sample was collected.
It has become so. Below is a conventional sampling probe
Will be described using two examples. As a first conventional example, FIG.
1 shows a side sectional view of an atmospheric probe 1. Symbol 3 is a sample
A protective tube for holding the collection container 21 and a cylindrical paper tube 5
Outside of the ₂O₃And / or Si0₂System heat resistance
It is configured by fitting a leave 7. Collection container 21
Is the lower end of the protective tube 3 which is the side immersed in the molten steel.
1 is attached to the container attaching portion 9 at the left end of the container 1.
You. The collection container 21 is made of glass and has a through hole 23 in the axial direction.
And has a cylindrical shape. FIG. 1 of the container 21
The opening of the left end portion 25 where the molten metal flows in
The mouth 29. The container 21 is made of a refractory material such as ceramic.
Substantially cylindrical mounting member 3 with flange 33 made
1, the end on the inflow port 29 side is protruded by a predetermined length and inserted.
And is fixed by refractory cement 35. And
As shown in FIG. 1, the container mounting portion 9 of the protective tube 3
Attach the flange 33 to the end of the protection tube 3
It is fixed. The inlet 29 of the container 21 is
Is made of aluminum and has a bottomed cylindrical container cap 41
Have been. In the through hole 23 of the container 21,
Near the end 25 on the 29 side and the end 27 on the opposite side,
A rod 45 is arranged. The outer diameter of the iron rod 45 is
It is smaller than the inner diameter of the through hole 23, and the through hole 23 should not be closed.
No. Reference numerals 47 and 49 are formed on the inner peripheral wall of the through hole 23.
These projections 47 and 49 make the iron bar
45 is fixed at a predetermined position in the axial direction of the through hole 23.
You. In addition, the end of the container mounting portion 9 of the protective tube 3 is
Or a protective cap 5 made of aluminum and having a bottomed cylindrical shape
1 is attached, and the container 21 projects from the protection tube 3.
Cover the entire part. Furthermore, take out the container of protection tube 3
To the holder mounting part 11 at the end opposite to the mounting part 9
Is an iron pipe of an appropriate length as a holder (not shown).
Is attached. Using the above probe 1
To collect a mold sample, this probe 1
It is passed and immersed to a predetermined depth in the molten steel. This and
First, the protective cap 51 is dissolved, and then the container cap 4
1 melts and the molten metal flows into the container 21 through the opening 29.
Enter. The flowing molten metal enters the inside of the container 21 and
It comes into contact with the rod 45 and is thereby cooled and solidified. Predetermined
After immersion for a time, when the probe 1 is pulled out of the molten steel,
The molten metal collected in the container 21 is naturally cooled and solidified
Then, it becomes a solid pin-shaped sample. However, the conventional
When collecting using probe 1 as an example,
There is a problem as follows. The first problem is the table of molten steel.
There is the effect of slag floating on the surface. That is,
When immersing probe 1 in molten steel, probe 1
Pass through the layers. At this time, on the outer surface of the protective cap 51
Slag adheres. Adhered slag is directly in molten steel
To the protective cap 51 and the container cap in the molten steel.
And the molten metal flows into the container 21 in sequence.
At this time, it flows into the container 21 together with the molten metal. That is,
Samples taken are considered to be contaminated by slag.
Measurement of the exact amount of oxygen in the molten metal
Can not. As a second problem, there exists in the container 21
There is the influence of oxygen. That is, probe 1 is immersed in molten steel
When the molten metal flows into the container, the molten metal
Oxidation reaction with oxygen in vessel 21
I do. Therefore, the sample has a higher oxide value than the actual molten steel.
The exact total oxygen content in the molten metal
Cannot be measured. As a third problem, the container 2
There is an effect of nitrogen present in 1. In other words,
When the lobe 1 is immersed and the molten metal flows into the container 21,
At this time, the nitrogen component in the container 21 is mixed into the molten metal,
After solidification. Therefore, the sample contains the nitrogen component in the container 21.
The amount of nitrogen in the molten metal is accurate
Can not be measured. Next, as a second conventional example
FIG. 2 is a side sectional view of a conventional vacuum probe 61.
Show. The configuration of this conventional example is mostly the first conventional
The same reference numerals are given to the same members because they are the same as in the example.
The detailed description is omitted, and different points are mainly described below.
Reference numeral 63 denotes a container for collecting a sample,
3 is the same as that of the container 21 of the first conventional example.
However, the configuration is slightly different. The container 63 has an axial inside.
2 has a hole 64 extending in the direction shown in FIG.
The right end 67 is not open. Left end 65 is open
And it becomes the inlet 69 for the sample to flow in
However, as shown in the figure, the inlet 69 has a low melting point gas.
The inside of the hole 64 is kept vacuum by being sealed by the lath 71.
ing. It corresponds to the container cap 41 in the first conventional example.
Things are not used. Using the above second conventional example
The method of collecting the pin-type sample is the same as in the first example.
When the probe 61 is immersed in the molten steel, the protection tube cap 5
1 is melted, then the low melting glass 71 is melted,
Flows into the container 63. The molten metal that has flowed into the container 6
Enter within 3. After immersion for a predetermined time, the probe 61 is
When the steel is pulled out of the molten steel, the molten
The metal is naturally cooled and solidified to form a solid pin-shaped sample.
However, a probe 61 as in the second conventional example is used.
However, there are the following problems when performing sampling. first
The problems mentioned above are the same as the problems in the first conventional example.
Same, the effect of slag floating on the surface of molten steel
In other words, when the probe 61 passes through the slag layer,
The slag attached to the outer surface of the protection tube cap 51 is melted.
This is contamination caused by flowing into the container 63 together with the metal.
You. As a second problem, the influence of the low-melting glass 71
You. Protective cap 51 and low-melting glass 71 are in order in molten steel.
When the molten metal flows into the container 63,
The low melting glass 71 flows into the container 63 together with the molten metal.
Enter. That is, the sample to be collected is the low melting glass 71
Accurate tota in molten metal
The oxygen content cannot be measured.

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned problems in the prior art, and has been described in terms of melting a molten metal to be taken as a sample, a slag, a melt of a member attached to the tip of a probe, or the like. It is an object of the present invention to provide an apparatus and a method for collecting a molten metal sample in which the molten metal is prevented from being mixed, and the molten metal to be collected is not affected by oxygen or nitrogen present in the probe. It is a further object of the present invention to provide a gas supply device for supplying an inert gas to a sample-time sampling probe in order to enable sampling of a sample that is not contaminated.

In order to solve the above-mentioned problems, the present invention provides a molten metal sampling apparatus having the following configuration. That is, it is a sampling device including a molten metal sample sampling probe and a gas supply device connected thereto. The probe has a protective tube, a through hole, and one end on which an opening is formed is protruded from the protective tube, and a sample collection container inserted and attached to the protective tube, and sample collection from the protective tube. A protective cap is provided to cover the protruding portion of the container. The gas supply device connects a gas supply source for supplying an inert gas, a gas supply source and a probe, and supplies the inert gas supplied from the gas supply source through an opening opposite to the opening of the sampling container. There is provided a pipe for supplying the inside of the sampling container, and switching means for switching the inside of the sampling container between a state connected to a gas supply source and a state opened to the atmosphere. Further, the present invention provides an inert gas supply device having the following configuration. That is, a protective tube, a sample collection container having a through-hole, and having one end on which the opening of the through-hole is formed protruding from the protective tube, and inserted and attached to the protective tube, and a sample collection container A gas supply device connected to a molten metal sampling probe having a protective cap covering a portion protruding from the protective tube and supplying an inert gas into the sampling container. Gas supply source, and the gas supply source and the molten metal sampling probe are connected, and the inert gas supplied from the gas supply source is introduced into the sample collection container through the through hole opposite to the opening of the sample collection container. There is provided a piping for supplying and a switching means for switching the inside of the sample collection container between a state connected to an inert gas supply source and a state opened to the atmosphere. Furthermore, in order to solve the above problems, in the method for collecting a molten metal according to the present invention, a protective tube and a through-hole,
One end of the through-hole where the opening is formed is protruded from the protective tube to cover the sample collection container inserted and attached to the protective tube and the portion of the sample collection container protruding from the protective tube. Using a molten metal sampling probe equipped with a protective cap and supplying an inert gas to the inside of the sample collection container while applying pressure, the sample collection probe is immersed in molten steel, and after a predetermined time elapses, the sample collection container A method for sampling molten metal is provided in which the interior is communicated with the atmosphere and then a sampling probe is lifted from molten steel.

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below, but the scope of the present invention is not limited to the embodiments described below. FIG. 3 shows a molten metal sampling device 80 according to an embodiment of the present invention. Reference numeral 81
Is a probe for collecting molten metal, and the shape and material of each member may be the same as those of the probe 1 shown in FIG. In the drawing, the members of the probe 81 are denoted by the same reference numerals as those used for the corresponding portions of the probe 1 shown in FIG. 1, and detailed description thereof will be omitted. However, the probe 1 shown in FIG. 1 was used by attaching an iron pipe (not shown) of an appropriate length to the holder attaching portion 11 of the paper tube 5, but the probe according to the embodiment of the present invention was used. A gas supply device 83 described below is connected to 81. The gas supply device 83 includes a holder 9 described later.
1, mounting fitting 93, gas container 101, piping 105,
The three-way valve 111 is roughly configured. First, a cylindrical holder 91 having a proper length is inserted into the holder mounting portion 11 of the paper tube 5 via a mounting bracket 93. The mounting bracket 93 includes a conical portion 95 formed in a conical shape having a vertex in the inner direction of the protection tube 3 and a cylindrical portion 97 formed in a cylindrical shape at the bottom thereof, and has a through hole in the axial direction. As shown in the figure, the holder 91 is attached to the outer periphery of the holder 91 at a predetermined position in the axial direction by appropriate means such as bonding. The mounting bracket 93 is pushed into the holder mounting portion 11 of the paper tube 5 using the inclined outer peripheral surface of the conical portion 95, whereby the holder 91 is mounted on the paper tube 5. Reference numeral 101 denotes a gas container as a gas supply source. In the present embodiment, the gas container 101 is filled with an argon gas as an inert gas. Reference numeral 105 denotes a pipe. The pipe 105 has one end connected to the gas container 101 and the other end connected to the end opposite to the end of the holder 91 inserted into the paper tube 5. In the middle of the pipe 105, a pressure reducing valve 103 for reducing the pressure of the supplied gas to a predetermined pressure is attached. Sign 1
Reference numeral 11 is a three-way valve provided in the middle of the pipe 105.
The three-way valve 111 has a holder 9 attached to the three-way valve body 113.
1 connected to the pipe connected to the gas container 101 and the port 11 connected to the pipe connected to the gas container 101 side.
7 and a port 119 that is open to the atmosphere. The three-way valve 111 communicates between the port 115 and the port 117, disconnects the communication between the ports 115 and 117 and the port 119, communicates between the port 115 and the port 119, and communicates with the ports 115 and 119. It can be switched between a gas cutoff state in which communication with the port 117 is cut off. The state of the three-way valve main body 111 shown in FIG. 1 is a gas supply state in which the holder 91 and the gas container 101 are connected. A sampling method for sampling the molten metal using the molten metal sampling device 80 having the above configuration will be described below. First, the holder 91
Is attached to the paper tube 5 via the attachment fitting 93 as shown in the figure. Next, the three-way valve 111 is connected to the port 115 and the port 117 so as to be in a gas supply state, and the inert gas is supplied into the paper tube 5 via the holder 91. This gas naturally enters the container 21 and the inside of the container 21 is in a predetermined pressurized state. The attachment portion between the holder 91 and the paper tube 5, or the attachment portion between the container 21 and the container cap 41, and the attachment portion between the attachment member 31 and the protective cap 51 are not completely sealed, but are slightly gaseous inside. Can be leaked. Therefore, by the supply of the inert gas, the air that was initially present in the probe 81 is promptly replaced by the inert gas. Next, probe 8
1 is immersed to a predetermined depth in molten steel. During this dipping process, the protective cap 51 is melted by the heat of the molten steel, and then the container cap 41 is melted. When the container cap 41 is melted, the pressurized gas in the container 21 is released from the inlet 2.
Blow out from 9. As a result, the slag which may adhere to the protection cap 51 and be drawn into the molten steel, and the dissolved components of the protection cap 51 and the container cap 41 are removed by the pressurized gas blown out from the container inlet 29. In this state, the probe 81 is held at a position where a sample is collected. The inside of the container 21 is completely replaced with the inert gas, and there is no slag, air, components of the protective cap 51 and the container cap 41 in the molten steel near the inflow port 29. Next, the three-way valve 111 is switched, the port 115 and the port 119 are communicated, the gas is shut off and the atmosphere is opened, and the pressure in the container 21 is reduced to the atmospheric pressure. Then, the molten metal flows into the container 21 from the container inlet 29. The inflowing molten metal enters the inside of the container through-hole 23, and the leading portion contacts the iron rod 45 arranged inside the container through-hole 23, and is cooled and solidified. That is, the molten metal does not overflow from the inside of the container 21. In this state, when the probe 81 is pulled out of the molten steel, the molten metal in the container 21 is naturally cooled, and all solidifies to form a pin-type sample. Hereinafter, a sampling device 80 according to a specific embodiment of the present invention will be described.
And a molten metal sample was collected using the conventional probe 1 shown in FIG. 1 as a comparative example,
The analysis values of the total oxygen amount and the nitrogen amount contained in the raw steel were compared. Tables 1 and 2 show the results. The sampling of the molten metal sample was performed alternately 10 times.

[Table 1]

[Table 2] As can be seen from Tables 1 and 2, both the total oxygen content and the nitrogen content are closer to the analysis values of the raw steel in the examples than in the comparative examples.

As can be seen from the above description, according to the present invention, the slag or the probe 81
Of the protective cap 51 and the container cap 41 attached to the tip of the container can be prevented, and the collected molten metal can be contained in the probe 81 or the collection container 21.
It can be prevented from being affected by oxygen or nitrogen which is initially present in the inside, and a good sample can be obtained which accurately reflects the component ratio in the molten steel.

[Brief description of the drawings]

FIG. 1 is a side sectional view of a conventional atmospheric type molten metal sampling probe.

FIG. 2 is a side sectional view of a conventional vacuum-type molten metal sampling probe.

FIG. 3 is a side sectional view of the molten metal sampling apparatus according to the embodiment of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Conventional atmospheric probe 3 Protective tube 21 Sampling container 23 Through hole 29 Inlet 41 Container cap 51 Protective cap 80 Molten metal sample collecting container according to this embodiment 81 Probe 83 Gas supply device 91 Holder 93 Mounting bracket 101 Gas Container 103 Pressure reducing valve 105 Piping 111 Three-way valve

 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Masato Iizuka 4-1-1-14 Miyahara, Yodogawa-ku, Osaka-shi, Osaka Sumitomo Life Shin-Osaka Kita Building Inside Osaka Oxygen Industry Co., Ltd. (72) Keita Iwasaki, Osaka-shi, Osaka 4-1-1, Miyahara, Yodogawa-ku Sumitomo Life Shin-Osaka Kita Building Osaka Oxygen Industry Co., Ltd. F-term (reference) 2G055 AA22 BA01 DA04

Claims (3)

[Claims] 1. A sample having a protective tube, a through hole, and one end on which an opening of the through hole is formed is protruded from the protective tube, and is inserted and attached to the protective tube. A sampling container, a molten metal sampling probe including a protective cap covering a portion of the sample collection container protruding from the protective tube, a gas supply source for supplying an inert gas, and the gas supply source. A pipe for connecting the molten metal sampling probe and supplying the inert gas supplied from the gas supply source to the inside of the sampling container through an opening opposite to the opening of the sampling container. And a gas supply device including a switching unit that switches the inside of the sample collection container between a state connected to the gas supply source and a state open to the atmosphere,
Molten metal sampling equipment. 2. A sample having a protective tube, a through hole, and one end on which an opening of the through hole is formed protrudes from the protective tube, and is inserted and attached to the protective tube. A gas for supplying an inert gas into the sampling container by connecting to a molten metal sampling probe having a sampling container and a protective cap covering a portion of the sampling container protruding from the protective tube. A gas supply source for supplying the inert gas, the gas supply source being connected to the molten metal sampling probe, and supplying the inert gas supplied from the gas supply source to the sample collection container. A pipe for supplying the inside of the sampling container from the through hole on the side opposite to the opening, and switching the inside of the sampling container between a state connected to the gas supply source and a state opened to the atmosphere. Switching hand A gas supply device comprising: a step; 3. A method for collecting a molten metal sample, comprising:
The method for collecting a molten metal sample includes a protective tube, a through-hole, an end of the through-hole where an opening is formed, protrudes from the protective tube, and is inserted and attached to the protective tube. Using a molten metal sampling probe having a sampled sample container and a protective cap covering a portion of the sample sample container protruding from the protective tube, an inert gas is introduced into the sample sample container. While supplying and pressurizing,
A method for collecting a molten metal sample, comprising: immersing the sample collection probe in molten steel; allowing a predetermined time to elapse to allow the inside of the sample collection container to communicate with the atmosphere; and then pulling up the sample collection probe from the molten steel.