JPH0674949A - Disk type molten metal sample gathering device - Google Patents

Abstract

PURPOSE:To provide a molten metal sample gathering device by which residual gas and uneven distribution of deoxidizer can be prevented in a surface part supplied at least as an analyzing surface by making uniform deoxidation possible over the whole sample when a disk type metal coagulated sample is gathered. CONSTITUTION:In such a constitution as having a sampler 4a formed of a passage 5a to which molten metal is flowed in from below and an almost flat sample gathering chamber 7a in which the molten metal is filled and coagulated so as to communicate with the upper part of the passage 5a and arranging deoxidizer 18 in the passage 5a, a gas extracting means 40 is provided so that the sample gathering chamber 7a can discharge chamber inside gas to the chamber outside. A communicating part 14a between the passage 5a and the sample gathering chamber 7a is constituted to be blocked up by a closing member 19 being melted after the molten metal is flowed in the passage 5a and is filled in the passage 5a.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a disk-shaped molten metal sample collecting device for collecting molten steel, hot metal, etc. and using the collected disk-shaped solidified sample for analysis.

[0002]

2. Description of the Related Art Conventionally, a disc-shaped molten metal sampler for collecting molten metal such as molten steel or hot metal as a sample is connected to a flow path for letting the molten metal flow from below and an upper part of the flow path. It is equipped with a so-called bottom-casting disk-shaped sampler that forms a substantially flat sample collection chamber that fills and solidifies the molten metal, and in particular, in the sampler for collecting the molten metal such as carbon steel or stainless steel, It is known to provide a deoxidizer in the channel.

The deoxidizer is formed of Al, Ti or the like into a foil shape (extremely thin plate shape) or a linear shape, and is contained in the flow path.

When the molten metal is sampled by immersing the apparatus in the molten metal, the molten metal is filled in the sampling chamber through the flow path. Therefore, in the apparatus in which the deoxidizing agent is contained in the channel, the inflowing molten metal is deoxidized by the deoxidizing agent in the channel, and after being deoxidized, it is filled in the sampling chamber and solidified. The purpose of deoxidizing the molten metal in this way is to prevent formation of cavities due to residual gas inside the solidified sample.

[0005]

For the above-mentioned purpose, the amount of the deoxidizing agent is determined to be necessary and sufficient in consideration of the amount of the sample to be filled in the sampling chamber.

In the conventional structure, as soon as the molten metal flows into the flow path, the deoxidizer is melted and mixed into the molten metal. Therefore, since the channel is directly communicated with the sampling chamber, the molten metal flowing into the channel immediately enters the sampling chamber and is filled and solidified.

By the way, a disk-shaped metal sample collected by a disk-type sampler has a flat surface polished, and the polished surface is subjected to emission spectroscopic analysis. Often it is impossible to analyze due to abnormal light emission,
It was discovered that compositional segregation causes poor analysis. Therefore, conventionally, when polishing the surface of the disk-shaped sample and performing emission spectral analysis, while repeating the analysis, it has to be polished many times until the polished surface becomes a good-quality analysis surface,
Waste time and effort. Therefore, under the present circumstances, when poor analysis occurs, another sample is collected again in the expectation of a solidified sample with good analysis.

[0008] Then, as a result of investigating to find out the cause, it was found that it was caused by the following two problems.

First, as seen in AOD furnaces, secondary refining furnaces, etc., an inert gas (A
(r, N ₂ etc.) or O ₂ gas is forcedly injected from the bottom of the furnace, a large amount of gas bubbles are mixed in the bath.
The molten metal collected by the sampler contains a large amount of gas. Therefore, in the conventional sampling device, since the molten metal is allowed to flow into the sampling chamber from the flow channel and solidifies while containing such a gas, residual gas bubbles inside the solidified sample including the analysis surface. , Which is caused by being mixed in a wide area in a wide area, and therefore it is difficult to obtain an analysis surface without a nest when polishing the sample surface.
Therefore, in the case of emission spectroscopic analysis, abnormal light emission occurs in almost all cases, and stable analysis work cannot be obtained.

Secondly, in the conventional sampling device, the deoxidizer contained in the channel is melted by a small amount of molten metal that first flows into the channel, and is mixed with the molten metal. To move from the channel to the sampling chamber. That is, the deoxidizer follows the small amount of molten metal that does not sufficiently fill the sampling chamber and is drawn into the sampling chamber from the flow channel early. On the other hand, the subsequent molten metal that subsequently flows into the flow channel enters the sampling chamber without being deoxidized in the flow channel. Therefore, the sample filled and solidified in the sampling chamber is
Homogeneous deoxidation is not performed throughout, and partial segregation of the deoxidizer (for example, aluminum segregation) occurs in the sample, which causes composition segregation.

In particular, in the case of a submersible disc-type sampler, the molten metal that first flows into the sampling chamber through the flow channel first adheres to the inner wall surface of the sampling chamber to start solidification and A solidified film extending along the inner wall surface is formed. Then, the subsequent inflowing molten metal stays in the space surrounded by the solidified film and solidifies. Therefore, the sampled disk-shaped sample contains a large amount of gas in the flat surface portion used for the emission spectroscopic analysis, and the molten metal that first flows into the sampling chamber while drawing in the deoxidizer. Since it is composed of the above, the analysis surface of the sample will have a nest due to the residual gas and a composition segregation due to the unevenly distributed deoxidizing agent.

[0012]

The present invention solves the above-mentioned conventional problems and prevents the residual gas and deoxidizes the surface portion used as an analysis surface when collecting a disk-shaped sample. A molten metal sampling device capable of preventing uneven distribution of the agent.

Therefore, the present invention is configured as a first means, and a flow path for allowing molten metal to flow in from below,
In the molten metal sampling device provided with a sampler that is connected to the upper part of the flow channel and forms a substantially flat sample collection chamber for filling and solidifying the molten metal, the molten metal sampling device provided with a deoxidizer in the flow channel, The chamber has a degassing means that allows the gas inside the chamber to be discharged to the outside, and the flow channel and the sampling chamber are provided by a closing member that melts after the molten metal flows into the channel and is filled in the channel. The point is that the communication part of is closed.

Further, the present invention is configured as the second means in that the closing member is made of a thin metal plate having a wall thickness of about 0.05 to 1.0 mm.

The third aspect of the present invention is that the closing member is provided with a melting control portion selected from one or more of a protrusion, a recess, and a pinhole.

In an embodiment of the present invention, at least the sampling chamber may be constituted by a pair of butt-polymerized half-divided divided pieces, and the mating surfaces of the divided pieces may constitute the degassing means. it can. Alternatively,
It is also possible to form a gas vent hole at least at the top of the sampling chamber and to form the gas vent means by this gas vent hole.

[0017]

Embodiments of the present invention will be described in detail below with reference to the drawings.

In FIG. 1, a probe body 32 made of a paper tube having a cylindrical shape with its tip facing downward is provided with a holding member 33 and a probe body 32, which are made of a molded product such as a shell mold and installed inside the tip portion of the probe body 32. The sampler 4a is housed through a plug 34 made of a molded product such as ceramics inserted at the tip.

The sampler 4a has an inflow guide tube 6 forming a flow path 5a for allowing molten metal to flow in from below.
a and a sample collection container 8a which is connected to the upper part of the flow path 5a and forms a substantially flat sample collection chamber 7a for filling and solidifying the molten metal are arranged vertically, which is so-called. Construct a disc-type sampler of the bottom-note type.

The inflow guide pipe 6a is made of a quartz pipe, a steel pipe or the like. The inflow guide pipe 6a projects downward from the plug body 34 while being held by the plug body 34, and the inlet 11a opened at the projecting end has a thin steel plate or the like. It is encapsulated by a cap 35 made of. When the apparatus is immersed in the molten metal, the cap 35 is lost after the apparatus passes through the slag layer and sinks to a predetermined position in the molten metal bath, causing the inlet 11a to open, and melting from the inlet 11a. The metal is caused to flow into the flow path 5a.

The sampling container 8a is made of metal such as steel. In the illustrated example, the sample collection container 8a is composed of a pair of divided pieces formed in a half-divided shape, and a substantially flat sample collection chamber 7a is formed by abutting and superposing the pair of divided pieces. At this time, although not shown, the sample collection chamber 7a may have a configuration in which a thick collection chamber and a thin collection chamber that can collect a sample integrally having a thick portion and a thin portion are formed in series. In this case, the collected sample is subjected to emission spectral analysis by polishing the flat surface of the thick portion,
A part of the thin portion is punched and separated by a puncher or the like, and the separated piece is subjected to combustion analysis.

This sample collection container 8a is a sample collection chamber 7a.
Communication passage 14 for communicating the inflow guide pipe 6a
a is formed, and the communication passage 14a has a smaller diameter than the inner diameters of the flow path 5a and the sampling chamber 7a.

Further, the sample collecting container 8a is provided in the sample collecting chamber 7
Gas venting means 4 capable of discharging the gas in the chamber a to the outside
0 is set. In the illustrated example, the degassing means 40 is composed of a small degassing hole formed at least at the top of the sampling chamber 7a. However, instead of or together with the degassing hole, It may be constituted by a slight gap formed on the mating surface of the half-divided divided pieces constituting the sample collection container 8a.

In the above structure, the flow path 5a
A deoxidizer 18 is provided inside the. The deoxidizer 18 is formed in a foil shape (extremely thin plate shape) or a linear shape from Al, Ti or the like and is stored in the flow path 5a, but the storing method is not limited.

The communication passage 14a from the flow path 5a to the sampling chamber 7a is closed by a closing member 19, which is made of a material that does not affect the sample analysis value and is formed in a thin plate shape. There is. That is, this closing member 19
As will be described later, the molten metal flows into the flow path 5a and is melted after being filled in the flow path 5a. Therefore, the communication passage 14a is closed until the closing member 19 melts, and the communication passage 14a is opened after the closing member 19 melts after a predetermined time elapses.

In the embodiment shown in FIG. 1, the closing member 19 is
Is formed into a disk-shaped thin plate and is interposed between the inflow guide tube 6a and the step portion of the communication passage 14a, thereby closing the communication passage 14a from the flow passage 5a side.

By the way, for the purpose of constructing a submersible disk-type sampler, the sampler 4a of the present invention is used.
In addition to the configuration shown in FIG. 1, it is possible to construct another embodiment as shown in FIGS. 2 (A) to 2 (C) and FIGS. 3 (A) and 3 (B).

In the embodiment shown in FIG. 2A, the flow path 5a is an inflow path 11b formed by an inflow guide tube 6a.
And an inflow chamber 5b formed by an inflow guide container 6b interposed between the inflow guide tube 6a and the sampling container 8a. That is, the sampler 4a includes an inflow guide tube 6a made of a quartz tube or a steel tube, and an inflow guide container 6
b and the sample collection container 8a, the inflow guide pipe 6a constitutes the inflow passage 11b, the inflow guide container 6b constitutes the inflow chamber 5b, and the sample collection container 8a constitutes the communication passage 14a and the sample collection chamber 7a. , The inflow passage 11b and the inflow chamber 5
The flow path 5a is formed by b. In addition, the sampling container 8
Although a communication guide tube 37 made of quartz or the like is inserted in the communication passage 14a of “a”, such a communication guide tube 37 does not necessarily have to be provided. The inflow guide container 6b has a cylindrical wall 38a.
And a pair of plate walls 38b that cover the upper and lower sides of the cylindrical wall 38a,
38c and.

Therefore, in this embodiment, the deoxidizing agent 18 is contained in the inflow chamber 5b forming the flow path 5a. The closing member 19 is interposed between the plate wall 38c and the cylindrical wall 38a on the side of the sample collection container 8a, and the closing member 19 is provided.
Thus, the communication passage 14a is closed from the inflow chamber 5b side.

The embodiment shown in FIG. 2B is the same as that shown in FIG.
Is similar to that described above, but the polymerizable split piece 38 in which the plate wall 38c on the side of the sampling container 8a is split.
The connecting passage 14a is closed by interposing a closing member 19 between the two divided pieces.

The embodiment shown in FIG. 2C is the same as that shown in FIG.
As described above, but when inserting the communication passage 14a of the sample collection container 8a into the plate wall 38c on the side of the sample collection container 8a, forming a different diameter hole into which the communication passage 14a is inserted, A closing member 19 is interposed between the different-diameter step portion of the different-diameter hole and the insertion end of the communication passage 14a, and the communication member 14a is closed by the closing member 19.

In the embodiment shown in FIGS. 3A and 3B, the sampler 4a integrally formed with the inflow guide container 6b and the sample collection container 8a and the small-diameter communication passage 14a for communicating the both containers 6b, 8a. Make up. The sampler 4a is composed of a pair of split pieces formed in a half-split shape.
It is constructed by abutting and superposing a pair of divided pieces, and an inflow guide tube 6a made of quartz or the like is inserted into the inflow guide container 6b, and the inflow path 11b is constituted by this inflow guide tube 6a.

Therefore, in this embodiment, the deoxidizer 1 is placed in the inflow chamber 5b formed by the inflow guide container 6b.
8 is accommodated, a closing member 19 is fitted in the communication passage 14a, and the closing member 19 closes the communication passage 14a.

As described above, the sampler 4a is composed of half-divided pieces that are butted and overlapped with each other. Therefore, by forming a groove in the circumferential direction at the opposed position of each divided piece, the disk-shaped closure is formed in the groove. The peripheral edge of the member 19 can be fitted.

In these examples, when the apparatus is immersed in the molten metal for collecting the molten metal, the molten metal flowing into the channel 5a is sampled until the channel 5a is sufficiently filled. Do not enter the chamber 7a. That is, the molten metal is
The deoxidizer 18 immediately flows into the flow path 5a with a stirring flow and is melted while being mixed with the molten metal while being mixed, but since the closing member 19 prevents the deoxidizer 18 from entering the sampling chamber 7a, the flow path 5a is prevented. It is filled up with and is made to stay there.

Therefore, the molten metal flowing into the flow path 5a is
Immediately after the inflow, the flow path 5 whose upper part is closed by the closing member 19
The air in the flow path 5a is introduced into the inflow port 11a with a stirring flow in
It is discharged to the outside by being pushed further downward, and a part of the inert gas in the molten metal is discharged together with this air discharge. At this time, the stirring flow of the molten metal causes the deoxidizer 18 to move to the flow path 5
In a, the molten metal is mixed by a combined action due to the difference in density and the difference in concentration with the molten metal while being mixed under a homogeneous distribution state in the molten metal, and a uniform deoxidation treatment of the entire molten metal in the channel 5a is performed. I do.

The molten metal is immediately collected in the sampling chamber 7a.
Of the residual gas contained in the molten metal while being retained in the flow path 5a closed by the closing member 19 without being made to enter the above.

Therefore, after such a short residence time,
When the closing member 19 melts and the closed state between the flow path 5a and the sampling chamber 7a is released and the communication portion 14a is opened,
As described above, the molten metal that has been subjected to the separation of the gas that has floated upward and the uniform deoxidizing treatment is discharged from the flow path 5a into the sampling chamber 7a.
Enter all at once.

When the molten metal enters the sampling chamber 7a, the molten metal pushes up the gas floated upward in advance to above the sampling chamber 7a, together with the air in the sampling chamber 7a, the degassing means 40. While being discharged to the outside via, it flows along the inner wall surface of the sampling chamber 7a and is solidified there.

As described above, the molten metal that is made to flow into the sampling chamber 7a from the flow path 5a all at once flows along the inner wall surface of the sampling chamber 7a in a state in which the gas has been floated and separated and has been uniformly deoxidized. Since it solidifies, the molten metal along at least the inner wall surface of the sampling chamber 7a does not contain a large amount of gas, and the deoxidizer is not unevenly distributed. Therefore, in the metal sample filled and solidified in the sample collection chamber 7a, at least a portion corresponding to the analysis surface (a portion in the vicinity of the flat surface of the disk-shaped sample) does not have a nest due to the residual gas, and The composition segregation due to the deoxidizing agent does not occur.

Then, in the process in which the molten metal staying in the flow channel 5a flows into the sampling chamber 7a and begins to solidify along the inner wall surface of the sampling chamber 7a, further molten metal is further flowed. After passing through 5a, it enters the sampling chamber 7a, and flows into the space surrounded by the metal film at the start of solidification with stirring flow. Therefore, even if the initial molten metal retained in advance in the flow path 5a is insufficiently deoxidized and contains a deoxidizing agent and unreacted oxygen, the flow phenomenon due to the subsequent molten metal may occur. A secondary deoxidation by stirring dispersion of the deoxidizing agent based on is expected, where again a completely homogeneous deoxidation over the molten metal is applied. For this reason, the solidified sample collected by the sample collection chamber 7a is uniformly deoxidized over the entire sample including the analysis surface, and segregation of the deoxidizing agent as in the conventional case does not occur. Further, when the molten metal flows into the sampling chamber 7a and fills the sampling chamber 7a,
Even if residual gas were to be enclosed in the molten metal, such gas would only form a nest at the center of the sample, so the analysis surface (flat surface It is located away from (the vicinity of) and does not hinder the analysis.

By the way, the molten metal is thus passed through the flow path 5a.
For the purpose of filling the sampling chamber 7a with only the molten metal that has stagnated in the chamber where the gas is floated and homogeneously deoxidized, the volume of the flow channel 5a should be increased as much as possible. On the other hand, it is preferable to make the volume of the sampling chamber 7a relatively small. However, in the sampler for the purpose of sampling, if the flow path 5a is simply enlarged, not only the sample but also the amount of unnecessary solidified metal that subsequently enters the flow path 5a is increased, which is not preferable. There is a problem that it hinders downsizing of the entire device. Therefore, it is desirable to make the volume of the flow path 5a as small as possible within the scope of the object of the present invention in which the closing member 19 is provided. As described above, the present invention, among the collected coagulated samples, at least in the portion corresponding to the analysis surface, the purpose is to prevent abnormal light emission due to the occurrence of nests, composition segregation due to non-uniform deoxidation, This is because, in such a region greatly deviated from the analysis surface, even if a nest or composition segregation occurs, it does not necessarily go against the object of the present invention.

Next, as described above, the present invention provides the closing member 1.
The purpose of providing 9 and the function of this closing member 19 are to fill the flow path 5a with a necessary and sufficient amount of molten metal, and to perform the floating separation of the required gas and the uniform deoxidizing treatment in this filled state until the flow path 5a is processed. Is to control the inflow timing by delaying the entry into the sampling chamber 7a. Therefore,
The closing member 19 does not immediately melt as soon as the molten metal flows into the flow channel 5a, and the flow channel 5 does not melt even for a short time.
It is necessary that it does not melt until a is filled with the necessary and sufficient molten metal. However, on the other hand, the closing member 19 needs to be melted without delay after the necessary gas floating separation of the molten metal in the flow path 5a and the uniform deoxidation have been performed. When the lid is closed and the melting of the closing member 19 is delayed, the tendency of the molten metal to solidify in the channel 5a progresses, and as a result, the molten metal does not smoothly enter the sampling chamber 7a from the channel 5a, and This is because it becomes impossible to secure sufficient filling of the sample in the collection chamber 7a.

In this regard, the wall thickness of the closing member 19 is
Conditions vary depending on the melting point of the material, but generally 0.0
It is preferably about 5 to 1.0 mm. As a result, from the start of inflow of the molten metal into the flow path 5a, 0.5
The reason is that the closing member 19 is melted after about 3.0 seconds and the above-mentioned purpose is achieved.

According to the experiments conducted by the present inventors, the closing member 19
When the melted metal has a small thickness and melts in less than 0.5 seconds after starting to flow into the flow path 5a, it is sufficient to perform floating separation of the gas of the melted metal in the flow path 5a and homogeneous deoxidation. I don't have the time. Therefore, the melting time of the closing member 19 must be 0.5 seconds or more.

On the other hand, when it takes a long time to melt the closing member 19, the molten metal tends to solidify. For example, when the flow path 5a is made of steel, the closing member 1
If the wall thickness of No. 9 is too thick and exceeds 2.0 seconds before melting, the molten metal tends to solidify. Therefore, in this case, the melting time of the closing member 19 needs to be within 2.0 seconds. On the other hand, in the case where the flow path 5a is formed of the above-mentioned quartz tube, a refractory material such as shell mold or ceramics, the tendency of solidification of the molten metal appears after 3.0 seconds. Therefore, in this case, the melting time of the closing member 19 is 3.
Must be within 0 seconds.

Therefore, in carrying out the present invention, the closing member 19 may adopt various structures capable of controlling the melting time while keeping the wall thickness within the range of 0.05 to 1.0 mm. It is possible.

In FIG. 4 (A), the closing member 19 is provided with one or a plurality of protrusions 19a protruding toward the flow path 5a, thereby constituting a melting control section. According to this embodiment, when the molten metal M is poured into the closing member 19 from the flow path 5a side, the projection 19a is first melted to form a hole, and the closing member 19 is gradually expanded. Melt. Therefore, as compared with the case without the protrusion 19a,
By providing the protrusion 19a, the melting time of the closing member 19 can be shortened. Further, the melting time can be further promoted by increasing the number of the protrusions 19a.

In contrast to the above, in FIG. 4B, one or a plurality of small recesses 19b facing the flow path 5a are provided in the closing member 19 to form a melting control section. Also in this embodiment, the molten metal M flows from the flow path 5a side to the closing member 1
When it is poured into 9, the concave portion 19b is first melted to form a hole, and the closing member 19 is melted in a direction of gradually expanding the hole. Therefore, the same effect as the protrusion 19a can be obtained.

In FIG. 4C, the closing member 19 is provided with one or a plurality of pinholes 19c to form a melting control section. According to this embodiment, the molten metal M
Is poured into the closing member 19 from the side of the flow path 5a, the closing member 19 is melted in the direction of gradually expanding the pinhole from the portion of the pinhole 19c. Therefore, the protrusion 19a
The same effect as can be obtained.

The projections 19a, the recesses 19b, and the pinholes 19c can be selected in any one mode or in a combination of a plurality of modes, and the melting time of the closing member 19 can be controlled by design. it can.

The closing member 19 is formed in a thin plate shape with a material whose melting point is equal to or higher than that of the deoxidizer 18 and does not affect the sample analysis value. Therefore, the closing member 19 is, for example,
When the deoxidizer 18 is Al, it is preferable to use a thin plate formed of Ti. In addition, the melting point of Ti (about 1680 degrees Celsius) is higher than the melting point of Al (about 660 degrees Celsius), which meets the above-described object of the present invention and does not affect the sample analysis value. In this regard, Ti has a melting point of 1680.
Since the temperature is in degrees Celsius, when it comes into contact with a molten metal whose temperature is higher than this melting point, it melts in a desired time, and the above-mentioned closing member 1
Since it functions as 9, it is suitable for collecting such high temperature molten metal. However, the closing member 19 composed of such a thin plate of Ti has a Fe content in the molten metal flowing into the inflow chamber 5a even when the molten metal having a melting point or lower, that is, 1680 ° C. or lower is sampled.
By reacting with and other components, it becomes a compound of TiFe ₂ or TiFe, and the melting point gradually lowers from the surface and melts after a lapse of a predetermined time, so that the above-mentioned intended purpose can be achieved.

Moreover, when the closing member 19 is made of Ti, since Ti itself has a deoxidizing function and a denitrifying function, there is an advantage that this can be advantageously used. That is, according to the present invention, as described above, the molten metal flowing into the flow path 5a is subjected to a uniform deoxidizing treatment by the deoxidizing agent 18, but if the closing member 19 is made of Ti, Oxygen of the above is combined with titanium to become O + Ti = TiO ₂ , which also promotes deoxidation. Further, titanium combines with nitrogen in the molten metal to give N + Ti = TiN, so that the molten metal is denitrified to facilitate sample analysis after sampling.

By the way, when a molten metal sample is taken, it is common to use Al as the deoxidizer 18, but some sampling steel grades analyze the Al element in the molten metal. In this case, Al cannot be used as the deoxidizer 18. Therefore, in such a case, a Ti foil or a thin wire is used as the deoxidizer 18, but the closing member 19 of the present invention can be formed of a Ti thin plate in this case as well. is there. Cover with a thin foil of the deoxidizer 18 (for example, 0.05
mm) to make it easy to melt, while the closing member 1
This is because the object of the present invention can be achieved by forming the wall thickness of 9 to be 0.05 to 1.0 mm as described above.

However, the present invention does not particularly limit the material of the closing member 19. For example, when extracting molten steel having a low refining temperature, a thin plate selected from Fe or Cu can be used, and in the case of ultra-low carbon steel refining, a thin plate made of the same material as the sampled metal. May be used.
Furthermore, it is also possible to use a thin plate of Ni as the closing member 19.

Next, FIG. 5 shows the result of an experiment conducted to confirm the homogeneous deoxidizing effect of the present invention.

In this experiment, the sample collecting apparatus having the disc-type sampler of the sub-injection type shown in FIG. 1 was used, one without the closing member 19 (hereinafter referred to as a conventional example) and one with the closing member 19 ( (Hereinafter referred to as the present Example)), and the segregation state of the deoxidizer in the sample was measured by performing emission spectroscopic analysis on the samples of molten steel collected by each.

The conditions of the sampler used in this experiment were 90 g for the sample weight (sample coagulated in the sampling chamber 7a) for both the conventional example and the present example, and the volume X of the sampling chamber 7a was The volume Y of the channel 5a is Y / X =
The flow rate was 1.0, and 0.27 g (0.3% by weight based on the weight of the sample) of an Al wire was stored as the deoxidizer 18 in the flow path 5a. The closing member 19 used in this embodiment is a thin titanium plate having a thickness of 0.5 mm.

Then, using each of the conventional example and the present example, molten steel during converter refining was sampled, and the distribution of aluminum (deoxidizer) in the solidified sample sampled by each was observed. . As shown in FIG. 5A, the measurement point of this aluminum is 0.5 from the surface of the sample S.
mm (general analytical surface that appears by polishing the surface), an analytical surface corresponding to 3.75 mm, and an analytical surface corresponding to 7.5 mm are obtained. S1 to S5 for each analytical surface. The five points shown in are extracted respectively.

The measurement results are shown in FIG. 5 (B). In the sample collected by the conventional example, the precipitation value of aluminum drastically decreases from the surface of the sample to the center of the sample, and It was confirmed that there were large variations in the values at 5 points from S1 to S5 even on the same analysis surface. On the other hand, in the sample collected according to the present example, aluminum is uniformly distributed throughout the sample, and the presence of the closing member 19 causes the deoxidizer 18 to be homogeneously mixed in the sample. It was proven.

[0062]

According to the first aspect of the present invention, when the molten metal is sampled by the disk-shaped molten metal sample collecting device, the molten metal flowing into the channel 5a is closed by the closing member 1.
Since the gas is prevented from immediately entering the sampling chamber 7a by 9 and is once filled and retained in the flow path 5a, the gases such as Ar and CO ₂ in the molten metal are floated and separated there. At the same time, the molten metal is uniformly deoxidized by the deoxidizer 18 while staying in the channel 5a. When the closing member 19 melts after the short residence time, the molten metal that has been subjected to the floating separation and uniform deoxidation of the gas in the flow path 5a in advance is collected at once in the sampling chamber 7a.
And flows along the inner wall surface of the sampling chamber 7a,
At this time, the separated gas is pushed up above the sampling chamber 7a and is suitably discharged to the outside through the gas venting means 40 together with the air in the sampling chamber 7a. Therefore, in the disk-shaped solidified sample filled and collected in the sample collection chamber 7a, there is no nest at least in the vicinity of the flat surface of the disk serving as the analysis surface, so that abnormal emission as in the conventional case is caused in emission spectroscopy. In addition, since the deoxidizing agent is uniformly distributed, composition segregation as in the conventional case does not occur, and good results can be obtained for sample analysis such as emission spectroscopy. As a result, in the conventional analysis, there is an effect that time and labor are not wasted until the analysis surface of the disk-shaped sample is repeatedly polished to obtain a good quality analysis surface.

According to the second aspect of the present invention, the closing member 19 is configured such that the molten metal in the flow path 5a has a sufficient amount of time sufficient for the floating separation of the gas and the homogeneous deoxidation to pass through. Since it is melted, the communication part between the channel 5a and the sampling chamber 7a is closed during the time required for gas separation and homogeneous deoxidation of the molten metal, while before the molten metal shows a solidification tendency in the channel 5a. Has the effect that it can be melted and the communication portion can be opened to allow the molten metal to enter the sampling chamber 7a and be filled.

According to the third aspect of the present invention, it becomes possible to control the melting time of the closing member 19 in design according to the type and temperature of the molten metal, and the optimum conditions for achieving the object of the present invention can be obtained. There is an effect that the sampler can be easily provided.

According to the present invention described in claim 4, there is an effect that the structure of the gas venting means 40 is simple and the invention can be easily implemented.

According to the present invention of claim 5, the flow path 5
When the molten metal subjected to the floating separation of the gas in a enters into the sampling chamber 7a, the gas separated by the inflow of the molten metal can be suitably pushed out from the sampling chamber 7a. is there.

[Brief description of drawings]

FIG. 1 is a vertical sectional view showing an embodiment of the present invention.

FIG. 2 is a vertical cross-sectional view showing another embodiment of the sampler and a modification of the closing member according to the present invention.

FIG. 3 is a vertical sectional view showing still another embodiment of the sampler and a modification of the closing member according to the present invention.

FIG. 4 is an enlarged vertical cross-sectional view showing each embodiment of the melting control unit implemented on the closing member.

5A and 5B show analysis results of samples collected by a sampler based on an example of the present invention and a sampler based on a conventional example, FIG. 5A is an explanatory diagram showing an analysis point of the sample, and FIG. It is the diagram which compared the analysis result.

[Explanation of symbols]

 4a Sampler 5a Flow path 5b Inflow chamber 6a Inflow guide tube 6b Inflow guide container 7a Sampling chamber 8a Sampling container 11a Inlet port 11b Inflow channel 14a Communication path 18 Deoxidizer 19 Closing member 19a Protrusion 19b Recess 19c Pinhole S sample

Claims (5)

[Claims] 1. In order to collect a disk-shaped metal solidified sample having an analysis surface in the vicinity of a flat surface, a flow path into which molten metal is made to flow from below and an upper portion of the flow path are communicated with the molten metal to solidify and solidify the molten metal. In a molten metal sampler having a sampler that forms a substantially flat sample collection chamber and a deoxidizer provided in the flow path, a gas vent that enables the sample collection chamber to discharge indoor gas to the outside A disk comprising means for closing the communication part between the flow path and the sampling chamber by a closing member that melts after the molten metal flows into the flow path and is filled in the flow path. Equipment for collecting molten metal samples. 2. The closing member has a wall thickness of about 0.05 to 1.0.
2. The device for collecting a disk-shaped molten metal sample according to claim 1, wherein the device comprises a thin metal plate of mm. 3. The device for collecting a disk-shaped molten metal sample according to claim 2, wherein the closing member is provided with a melting control section selected from one or more of a projection, a recess, and a pinhole. 4. At least a sampling chamber is constituted by butting and superposing a pair of divided pieces formed in a half-divided shape, and the degassing means is constituted by a mating surface of the divided pieces. The device for collecting a disk-shaped molten metal sample according to claim 1, 2 or 3. 5. The disk shape according to claim 1, 2 or 3, wherein the sampling chamber has a gas vent hole at least at its top, and the gas vent means is constituted by the gas vent hole. Equipment for collecting molten metal samples.