JPS6293638A - Apparatus and method for measuring component of two-metal type alloy - Google Patents

Abstract

PURPOSE:To make it possible to rapidly measure the concn. of component metals constituting a two-metal type alloy with good accuracy, by regulating the tamp. of the alloy stagnated in a measuring container independently of the temp. of the alloy in a container main body. CONSTITUTION:A jet stream consisting of fine Mg-particles and oxidizing gas is allowed to flow in a Mg trap container 1 storing a molten Pb-Mg alloy 6 and this molten alloy is sent out to a Mg distillation chamber by send-out piping 11 and introducing piping 12. A heater 2 and a heater 14 are regulated to set not only the temp. of the molten alloy in the trap container 1 to about 300-750 deg.C but also the temp. of the molten alloy in a measuring container to temp. 50-100 deg.C higher than that of said alloy in the container 1 and a convection is generated by specific gravity difference to stirr the molten alloy. Next, after the heaters are cut off, cooling air is blown to the molten alloy by a cooling air blow-off apparatus 42 to cool the molten alloy in the measuring container 3 while the temp. variation thereof is measured by a thermocouple 5 to be recorded on a recorder 52 and pre-eutectoid temp. is determined to be converted to Mg-concn.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention is directed to increasing the concentration of component metals constituting a two-metal alloy.
This invention relates to a method of measuring using a thermal analysis method and an improvement of an apparatus used for the measurement.

According to the present invention, the concentration can be quickly and precisely determined by 1[I], and the durability of the measuring device bLl!
There is a good C.

[Prior Art] Methods such as thermal analysis, chemical analysis, emission spectrometry, and specific gravity measurement are known as methods for measuring the a degree of component metals constituting a two-metal alloy.

The thermal analysis method mentioned above is a measurement method that takes advantage of the property that the primary crystal temperature of the alloy differs depending on the concentration of the component metals. However, it is useful as a method that can be measured relatively quickly.

FIG. 4 is a schematic diagram of an example of a device conventionally used for implementing a thermal analysis method.

The illustrated device has a structure in which a sample collection chamber 70 is installed on the upper part of the fI device main body 1, and a collection container 71 is transferred between the sample collection chamber 70 and the B device main body 1 to obtain two metals. Series alloy 6
The method involves taking a sample and measuring its component concentration.

The concentration measuring method using the conventional apparatus shown in FIG. 4 will be described in detail below.

Inside the container body 1, a molten metal 6 of a two-metal alloy (Pb-Mg alloy) is placed at a temperature of 4°C (10mlH) to prevent reaction with oxygen.
The molten metal 1 and molten metal 6, which is stored in the lower part of J10 below Q, is sent to the tvl distillation chamber (not shown) via the communication pipe 11, and
After evaporating and removing the water, the container body 1 is removed from the communication pipe 12.
Reflux to. On the other hand, from the inlet 3 at the upper corner of the container body, oxidizing (J) and atomized Mg cooled by the heat insulation 1111 in the nozzle (shown in the figure) flow in as a jet ().
, the inflowing MO is collected in the molten metal 6. Note that the molten metal 6 of the two-metal alloy is arranged around the container body 1, and
It is heated by the ni-heater 2, and slag 61 is floating in one part of the molten metal 6.

When collecting a sample of the molten metal 6, first, the sampling chamber 7
The inside of the container 0 is depressurized to the same extent as the container body 1.

Next, listen to the partition valve 72, move the sample 1W71 down with the slide rod 73, immerse it in the molten metal 6 to collect the sample, and pull it out.
Close.

Thereafter, the sample is cooled in the sample collection chamber 70. ．． ),
The temperature change during cooling is measured with a thermocouple 5, the C primary crystal temperature is determined, and from this primary crystal temperature, a thermal analysis method is used! vHJ1
1 degree equals 17.

Alternatively, the cooled sample is taken out of the sampling chamber and Mg11 degrees is determined by a method such as chemical analysis, emission spectrometry, or specific gravity measurement.

[Problem to be solved by the invention] The conventional methods and devices described above have the following drawbacks.

(1> Problems with measurement accuracy When sampling, the slag 61 gets mixed into the sampling container 71, and the mixed Iζ slag prevents accurate measurement of 'a degrees.

Furthermore, the molten metal within the container body is segregated depending on the location due to the difference in specific gravity of the component metals. Therefore, the component ratio of the sample taken does not necessarily represent the component ratio of the molten metal 6.

(2) Problems with speed of measurement A sample is collected from the molten metal 6, and the component ratio of the sample is determined. Y! ! 8, it takes time and effort to collect samples for measurement. For this reason, feedback control of the component ratio of the molten metal is accompanied by a long time delay, resulting in inaccurate illumination control.

In addition, the measurement method is not a thermal analysis method, but a chemical analysis method.
When the emission spectrometry method and the specific gravity measurement method are adopted and the measurement is performed after taking the sample out of the collection chamber, the adverse effects caused by the time 1511 error become significant.

(3) Problems with device durability 7 Partition valve 7 that partitions the sample collection chamber 70 and the container body 1 etc.
2 and the sealing material 74, and the pressure inside the sample collection chamber 70 is adjusted 11.
The plowing valve 75, the leak valve 76, the sealing material 77 that seals the slide rod 73, etc. deteriorate due to heat, resulting in poor airtightness.

For this reason, oxidation of the molten metal 6 occurs, and in MO,
Safety issues also arise.

In addition, 18 moving parts such as valve seals and slide rods are blued with metal vapors, slag, etc. to prevent deterioration of the weather.
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The present invention was devised in response to such circumstances, and aims to provide a measuring method and a measuring device that solve the above-mentioned problems.

[Means and Effects for Solving the Problems 1] The first invention comprises: a container body for accommodating a two-metal alloy in a molten state; a heating means for heating the alloy accommodated in the container body; and the container. a measuring container that communicates with the main body and retains a portion of the alloy contained in the container main body; and a temperature that adjusts the temperature of the alloy retained in the measuring container independently of the temperature of the alloy in the container main body. An apparatus for measuring components of a two-metal alloy, comprising: a regulating means; and a temperature measuring means for measuring the temperature of the alloy remaining in the measuring container over time.

In addition, the second invention provides a method for storing a part of the molten two-metal alloy contained in the container body.
The alloy is retained in a measurement container communicating with the container body, the temperature of the alloy retained in the measurement container is changed, the primary crystal temperature of the alloy is measured, and from the primary crystal temperature, by thermal analysis method, The concentration of the component metals constituting the alloy is 1! This is a method for measuring the components of two-metal alloys that covers the cost of ¥1.

Each component of the first invention will be explained below.

The container body is a heat-resistant container that contains molten metal. As the container body, for example, a container for a collection device that collects the atomized first metal in the second metal part in a molten state, as described in claim 2, is assumed. Note that the bimetallic alloy to which the present invention is applied may be any alloy whose primary crystal temperature differs depending on the component ratio, such as Cu-Mn, Cu-Ni
SA(+-Au lFe-Mn, Mg-8i, etc.).

The heating means may be of any type as long as it can maintain the molten metal in the container body in a molten state. The heating mode may be heater heating or induction heating. Note that the heating means and the measurement container are insulated.

The measurement container is a heat-resistant container in which a portion of the molten metal within the container body remains during temperature measurements necessary to determine the primary crystal temperature of the molten metal.

Temperature g! The first section has a function of setting the temperature of the molten metal in the measurement container to an arbitrary temperature independently of the temperature of the molten metal in the container body. Therefore, it is desirable to have heating means and cooling means. Further, it is desirable that the control system is independent from the control system of the heating means of the container body. Note that the temperature adjustment means and the container body independently control the temperature of the molten metal in the container body and the temperature of the molten metal in the measurement container by 1,
11 II+ Insulate as possible.

The temperature measuring means is used to measure the temperature of the molten metal in the measuring container over time and to determine its primary crystal temperature.

A thermal lightning pair is usually used as the temperature measuring means.

Next, the second invention will be explained.

In the second invention, a member common to the first invention, or
Since the meaning of 1i-jun is the same as that of the first invention, the explanation will be omitted.

The primary crystal temperature is the temperature at which crystallization begins when the molten metal is cooled. Generally, in the case of a two-metal alloy, the primary crystal temperature varies depending on the concentration of the component metals. Therefore, by measuring the primary crystal temperature, the component ratio of the two-metal alloy can be determined. This is the principle of thermal analysis method.

The initial product temperature is detected by uniformly cooling the molten metal and measuring the temperature change over time, and finding the point where the temperature temporarily stops decreasing or the cooling rate changes. In other words, since the absolute value of the amount of heat required to crystallize a unit mass of alloy is greater than the absolute value of the amount of heat required to lower the unit temperature of a unit mass of molten metal, when cooling uniformly, The primary crystal temperature can be determined by utilizing the fact that the temperature drop temporarily stops at the primary crystal temperature.

In addition, as described in claim 4, prior to cooling, the molten metal in the container body and the molten metal in the measurement container are stirred,
By eliminating segregation, a more accurate component ratio can be obtained.

[Example] The present invention will be described below based on specific examples.

FIG. 1 is a schematic diagram illustrating the configuration of an example device.

In this example, M cooled by adiabatic expansion in the nozzle
The fine particles of a are collected from the Pb-
This is to find the MQ molten metal component ratio.

As shown in the figure, the embodiment device includes an Mg collection container 1 containing a molten metal 6 of F)b-MQ alloy, and a Mg collection container 1 disposed on the side wall and bottom wall of the collection container 1. Pb-Mg alloy 6
A heater 2 that heats and keeps it in a molten state, a measurement container 3 installed at the bottom of the collection container 1 so as to communicate with the collection container, and a heater 41 installed on the side wall of the measurement container 3. and a cold air blowing device 4 that is installed at the bottom of the measurement container 3 and blows cold air to the installation part of the heater 41.
2, a thermocouple 5 that is housed in a protective tube 51 protruding from the bottom of the measurement container 3 and measures the temperature of the molten metal in the measurement container 3; and a record that records the temperature detected by the thermocouple 5. 52 in total.

An inlet 13 is opened at the upper corner of the collection container 1 to allow a jet of Mg fine particles and oxidizing gas cooled by adiabatic expansion in a nozzle (not shown) to flow in and collect in the molten metal 6. ing. Further, the side wall of the collection container 1 is coated with molten metal 6.
A delivery piping 1] and an introduction piping 12 are installed for sending the liquid to a distillation chamber (not shown), evaporating and removing Mg, and refluxing it to the collector a 1 after IJ.

Further, a heat insulating material 20 is arranged on the outside of the heater 2 that heats the molten metal in the collection container 1, and a heat insulating material 43 is arranged on the outside of the heater 41 that heats the molten metal in the measurement container 3. has been done. The heat insulating material 43 connects the heater 2 and the heater 4.
1 is mutually insulated, and the temperature of the molten metal in the collection container and the temperature of the molten metal in the measurement container can be independently controlled.
, Liruru J: The sea urchin is turning.

The measurement method using the apparatus of the above embodiment will be explained below.

First, adjust the heater 2 and heater 41 to
The temperature of the molten metal in the measurement container 3 is set to 300-750℃.
The temperature of the molten metal inside is set to a temperature 50 to 100°C higher than the above temperature, and the molten metal is stirred by generating convection due to the difference in ratio 1b.

Next, after the heater is cut off, cold L1 air at a predetermined temperature is blown out at a constant speed from the cooling air blowing device 42 as needed, and while cooling the melt field in the measurement container 3, the temperature fluctuation is measured by thermocouples. 5 and recorded with a recorder 52.

FIG. 2 is a graph showing the temperature fluctuation of the molten metal in the measurement container 3 recorded by the record 5152.

As shown in the figure, the graph temporarily becomes flat Jff (460'C) during the descent, and then descends again while changing the cooling rate. The flat part and the part where the cooling rate is slow are the parts where the heat of cooling was spent on crystallization,
This gives the primary temperature.

In the Pb-Mg alloy, the Mg concentration corresponding to the primary crystal temperature of 460'C is io, o%.

In this way, the Mg degree of the pb-Mg alloy could be determined in about 60 minutes. Note that conversion from primary crystal temperature to MQ concentration was performed using known data.

Next, the measurement of the present invention was performed using a sample with a known Mg concentration, and the measurement results were compared with the Mo2 degree data to evaluate the accuracy of the measurement. The results are shown in FIG.

As shown, the accuracy of the measurements according to the invention is good.

[Effects] As detailed above, the present invention provides thermal analysis for 7 people, J, and 2
A method and apparatus for measuring the component ratio of metal alloys with high precision and speed.

As mentioned in the Examples, according to the present invention, there is no need to collect samples to determine 111+1. Measurements can be made quickly.

Furthermore, since the device does not need to have any moving parts for sample collection, the device has good durability.

In addition, since no slab is mixed into the molten metal to be measured, the measurement accuracy is good.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram illustrating the configuration of an example device. FIG. 2 is a graph of Table 1 showing the temperature measurement results of the molten metal. FIG. 3 is a graph showing Mq concentration data and measurement results. FIG. 4 is a schematic diagram showing a conventional measuring device. 1... Container body 2... Heating means 3... Measuring container 4... Temperature adjusting means 5... Temperature measuring means

Claims (4)

[Claims] (1) A container body containing a two-metal alloy in a molten state, a heating means for heating the alloy housed in the vessel body, and a heating means communicating with the vessel body to heat the alloy housed in the vessel body. a measurement container in which a portion of the alloy remains; a temperature control means for adjusting the temperature of the alloy remaining in the measurement container independently of the temperature of the alloy in the container body; A component measuring device for a two-metal alloy, comprising: a temperature measuring means for measuring temperature over time; (2) The device according to claim 1, wherein the container body is a container for a collection device that collects atomized first metal in a molten second metal. (3) Part of the molten bimetallic alloy contained in the container body is retained in a measurement container communicating with the container body, and the temperature of the alloy retained in the measurement container is changed to A method for measuring the components of a two-metal alloy, comprising: measuring the primary crystal temperature of the alloy; and using the primary crystal temperature to obtain the concentration of component metals constituting the alloy by a thermal analysis method. (4) Prior to the measurement of the primary crystal temperature, the temperature of the alloy in the measurement container and the temperature of the alloy in the container body are 50 to 1
Claim 3: A temperature difference of 00°C is provided to cause the alloy in the measurement container and the alloy in the container body to convect and stir.
The method described in section.