JP2007155460A - Low-temperature type hardness meter - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a low-temperature type hardness meter capable of certainly preventing the adhesion of frost to the surface of a sample at the time of measurement of hardness at a low temperature by housing a hardness meter body in a hermetic closure using a high capacity globe box without internally evacuating the hardness meter body. <P>SOLUTION: The low-temperature type hardness meter 1 is equipped with a gas supply means (an Ar gas source 5, a nozzle 6, etc.) for blowing a high-purity gas, which has a dew point temperature lower than the sample W against the sample W fixed on a sample stand 10 and the whole of the hardness meter 1 is housed in a gas replacing simple case 4 into which the high-purity gas is supplied. Accordingly, even if a slight amount of the open air penetrates in the gas replacing simple case 4, a gas which has a dew point temperature lower than the temperature of the sample W and keeps the moisture content below the saturated steam pressure (amount) at the surface temperature of the sample W comes into contact with the surface of the sample W, so that the adhesion of frost to the surface of the sample W can be prevented. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a low-temperature type hardness tester for measuring the hardness of a low-temperature sample. More specifically, the indenter is pressed against the surface of a sample cooled to a low temperature, and the size of a dent generated thereby, or the indenter against the sample surface The present invention relates to a low-temperature hardness meter that obtains the hardness of a sample at that temperature from the amount of pressing.

  From the size of the indentation that occurs on the sample surface by pressing the indenter on the sample surface, a hardness meter such as a Vickers hardness tester that calculates the hardness of the sample, or the indenter being pushed into the sample surface when the indenter is pressed against the sample surface. In a hardness meter that determines the hardness of a sample from the amount (depth), generally, as shown in a longitudinal sectional view of a schematic configuration diagram in FIG. 5, a sample stage 10 is provided on the Z and moves in the vertical direction. A stage 11 and an XY stage 12 provided on the Z stage 11 and moving on a horizontal plane are included, and the sample W is fixed on the XY stage 12 by a fixing tool (not shown). Above the sample stage 10, a load mechanism 14 that presses the indenter 13 against the surface of the sample W and a microscope 15 for observing the surface of the sample W fixed on the XY stage 12 are provided. 5 is a type in which the hardness of the sample is obtained from the amount of indentation of the indenter to the sample surface, and the amount of indentation 13 is measured by the displacement meter 20 and converted into hardness (for example, Patent Document 1). reference).

  In addition to the microscope 15, an imaging device such as a CCD camera is provided, and a recess formed on the surface of the sample W by the imaging device by switching or separating the optical path from the surface of the sample W to the microscope 15. It is also known to include a length measuring means for measuring the size of the dent using the image data and converting the size of the dent into hardness (see, for example, Patent Document 2).

Conventionally, when measuring the hardness of the sample cooled to a low temperature, a hardness tester as described above was prepared, and a cooling device was added to the sample to push the indenter in a state of cooling the sample. Measuring the size of the indentation.
JP-A-9-79963 JP 2005-172663 A

  By the way, in the conventional method for measuring the low temperature hardness of the sample as described above, there arises a problem that frost adheres to the surface of the sample, the surface cannot be observed, and the indent cannot be measured. In order to solve the problem of frost, it is necessary to place the entire apparatus in a glove box and sufficiently replace the inside of the glove box with a high purity inert gas so that the dew point temperature inside the apparatus becomes low. To that end, it is necessary to evacuate the inside of the glove box, and it is necessary to use a high-performance glove box for dealing with leakage, which is expensive.

  The present invention has been made in view of such circumstances, and without using a high-performance glove box, it is possible to reliably prevent frost from adhering to the sample surface during hardness measurement at a low temperature. It is an object of the present invention to provide a low temperature type hardness tester that can reduce the cost of the entire apparatus as compared with the conventional low temperature hardness measurement method.

  In order to solve the above problems, a low-temperature hardness tester according to a first aspect of the present invention includes a sample table on which a sample is fixed by a fixture, a load mechanism that presses an indenter against the sample on the sample table, and a sample In a low-temperature type hardness meter comprising an optical microscope for observing the surface of the sample and a length measuring mechanism for measuring a dent generated on the sample surface by pressing the indenter, and a cooling means for cooling the sample on the sample stage A gas supply means for blowing a gas having a dew point temperature lower than the sample temperature to the sample fixed on the sample stage, and a gas for covering the entire hardness meter and filling the inside with a high purity gas It is characterized by having a simple case for replacement.

  In order to solve the same problem, the low-temperature hardness meter of the invention according to claim 2 similarly includes a sample table on which a sample is fixed by a fixture, and a load mechanism that presses an indenter against the sample on the sample table. A low-temperature hardness equipped with an optical microscope for observing the surface of the sample and a length measuring mechanism for measuring the indentation generated on the surface of the sample by the pressing of the indenter, and a cooling means for cooling the sample on the sample stage The gas replacement simple case for covering the entire hardness meter and filling the inside with a high purity gas, and the ambient temperature in the gas replacement simple case is lower than the temperature of the sample on the sample stage. In this way, it is characterized by having a gas supply control means for controlling the temperature of the high purity gas supplied into the gas replacement simple case.

  On the other hand, the invention according to claim 3 relates to a hardness meter of a type in which the hardness is obtained from the indentation amount of the indenter with respect to the sample surface, and the sample is fixed to the sample table by the fixture and the sample on the sample table. A load mechanism for pressing the indenter against the optical microscope for observing the surface of the sample, and an indentation amount measuring mechanism for measuring the indentation amount of the indenter against the sample surface when the indenter is pressed with a predetermined load. A gas supply means for blowing a high-purity gas having a dew point temperature lower than the sample temperature to the sample fixed on the sample table in a low-temperature hardness meter having a cooling unit for cooling the sample on the table; It is characterized by having a simple case for gas replacement for covering the entire hardness meter and filling the inside with high purity gas.

  The invention according to claim 4 also solves the same problem in the hardness meter of the type that holds the hardness from the amount of indentation of the indenter against the sample surface, and similarly, a sample stage on which the sample is fixed by a fixture, A load mechanism that presses the indenter against the sample on the sample stage, an optical microscope that observes the surface of the sample, and an indentation amount measurement that measures the indentation amount of the indenter against the sample surface when the indenter is pressed with a predetermined load In a low-temperature hardness meter having a mechanism and a cooling unit for cooling the sample on the sample table, a gas replacement simple case for covering the entire hardness meter and filling the interior with a high-purity gas, The temperature of the high purity gas supplied into the gas replacement simple case is set so that the ambient temperature in the gas replacement simple case is lower than the temperature of the sample on the sample stage. It characterized by that it comprises a Gosuru gas supply control means.

  The present invention intends to solve the problem by eliminating the cause of frost adhering to the sample surface without using a high-performance glove box. The frost adheres to the sample surface when the amount of moisture in the atmosphere is larger than the saturated water vapor pressure (amount) of the sample surface temperature and the sample surface temperature is 0 ° C. or less.

  In the inventions according to claims 1 and 3, by spraying a high-purity gas having a low dew point temperature, the high-purity gas comes into contact with the sample surface instead of the atmosphere in the gas replacement simple case, and at least a part of the gas is contacted. When the moisture content of the high-purity gas having a low dew point is less than the saturated water vapor pressure (amount) at the sample surface temperature, it is possible to prevent frost from adhering to the sample surface.

  In the inventions according to claims 2 and 4, the atmosphere in the gas replacement simple case filled with high-purity gas is made lower than the sample temperature, so that the atmosphere in the gas replacement simple case is saturated with the sample surface temperature. It is possible to keep only water vapor that is less than the water vapor pressure (amount), thereby preventing frost from adhering to the sample surface.

  According to the inventions according to claims 1 and 3, since the high-purity gas having a dew point temperature lower than the sample temperature is sprayed on the sample fixed on the sample stage, the atmosphere in the gas replacement simple case Regardless of the amount of moisture, it is possible to prevent frost from adhering to the surface of the sample where high-purity gas is sprayed, which can reduce the cost compared to the conventional low-temperature test configuration. it can.

  According to the second and fourth aspects of the invention, the gas is contained so that the atmosphere temperature in the simple case for gas replacement in which the hardness meter is accommodated and the inside is filled with the high purity gas is lower than the sample temperature. Since the temperature of the high-purity gas supplied to the simple case for replacement is controlled, the high-purity gas can hold less water vapor than the amount of saturated water vapor at the sample surface temperature, which causes frost to adhere to the sample surface. This can be prevented, and the cost can be reduced as compared with the configuration when performing a conventional low-temperature test in the same manner as described above.

Hereinafter, embodiments of the present invention will be described with reference to the drawings.
FIG. 1 is a main part configuration diagram of an embodiment of the invention according to claim 1, and is a diagram showing a schematic diagram showing a mechanical configuration and arrangement, and a piping diagram showing an outline of refrigerant piping and gas piping. . FIG. 2 is a front view of this embodiment, and FIG. 3 is an enlarged perspective view of the upper structure of the sample table 10.

  The hardness meter main body 1 has the same basic structure as a conventional hardness meter of the type that obtains the hardness from the size of only a depression formed on the surface of the sample by pressing an indenter, and a low temperature furnace 16 is fixed on the XY stage 12. It has a structure. That is, the Z stage 11 and the XY stage 12 are placed in order on the sample stage 10, and the low temperature furnace 16 is fixed thereon. The sample W is fixed on the low temperature furnace 16 by a fixing band 17 as shown in FIG. The periphery of the low temperature furnace 16 is surrounded by a cover 16a. Although not shown in FIG. 1, the hardness meter body 1 is provided with a microscope 15 for observing the surface of the sample W, as shown in FIG. A CCD camera 18 is also provided for photographing the surface of the image and using the image data for measurement of the indentation.

  The refrigerant controlled to a required low temperature by the low-temperature controller 2 is circulated and supplied to the low-temperature furnace 16 through the switching valve unit 3 through the refrigerant supply pipe 31a and the refrigerant discharge pipe 31b, so that the sample W reaches the required temperature. To be cooled.

  The hardness meter main body 1 described above is housed in a gas replacement simple glove box 2. This gas replacement simple glove box 4 is a simple glove box which is not completely sealed and does not include a pump or the like for decompressing the inside. The gas replacement simple glove box 4 is supplied with high-purity Ar gas from the Ar gas source 5 via the switching valve unit 3 through the replacement gas supply pipe 32a, and the inside thereof is replaced with Ar gas.

  Further, high-purity Ar gas from the Ar gas source 5, that is, Ar gas having a low dew point, is introduced into the gas replacement simple glove box 4 through the blowing gas supply pipe 32b through the switching valve unit 3 as well. . A nozzle 6 is mounted at the tip of the blowing gas supply pipe 32b. The nozzle 6 opens toward the surface of the sample W fixed on the low temperature furnace 16, and a low dew point Ar is formed on the surface of the sample W. Gas is blown.

  The test procedure using the above embodiment of the present invention is as follows. First, after the gas replacement simple glove box 4 is filled with Ar gas, the refrigerant is circulated and supplied to the low-temperature furnace 16 to start cooling. Ar gas is sprayed on the surface of the sample W. Then, after the temperature of the low temperature furnace 16 reaches the set temperature, the load mechanism 14 is driven to press the indenter 13 against the surface of the sample W on which Ar gas is blown, and the test is performed.

  According to such a procedure, even if some outside air enters the simple gas replacement glove box 4, the Ar gas sprayed portion on the surface of the sample W comes into contact with the Ar gas of high purity immediately after the start of cooling. Then, by keeping the moisture content (water vapor pressure) of the Ar gas smaller than the saturated water vapor content (pressure) at the surface temperature of the sample W, frost is not generated. Accordingly, the observation of the surface of the sample W by the microscope 15 and the photographing of the dent by the CCD camera 18 do not cause the influence of frost.

  Next, an embodiment of the invention according to claim 2 will be described. FIG. 4 is a configuration diagram of the main part, and is a diagram illustrating a schematic diagram showing a mechanical configuration and arrangement, and a piping diagram showing an outline of refrigerant piping and gas piping.

  The feature of this example is that the blowing gas supply pipe 32b and the nozzle 6 in the previous embodiment are not provided, and the gas low temperature control device 7 is interposed between the Ar gas source 5 and the switching valve unit 3. And a temperature sensor 8 for detecting the atmospheric temperature in the gas replacement simple glove box 4 is provided. The temperature of the Ar gas introduced into the gas replacement simple glove box 4 by the gas low temperature control device 7 so that the atmospheric temperature in the gas replacement simple glove box 4 is always slightly lower than the temperature of the sample W. To control.

  That is, the point that the refrigerant is circulated and supplied to the low temperature furnace 16 to start cooling the sample W after the gas replacement simple glove box 4 is filled with Ar gas is the same as the previous example. The temperature detection value of the atmosphere in the gas replacement simple glove box 4 based on the output is introduced into the gas low temperature control device 7, and the gas replacement is performed so that the detection value of the atmosphere temperature is always slightly lower than the temperature of the sample W. The temperature of Ar gas to be supplied into the simple glove box 4 is controlled.

  According to this embodiment, since the atmosphere in the gas replacement simple glove box 4 can hold only water vapor that is less than the saturated water vapor amount (pressure) at the surface temperature of the sample W, frost is not generated and is the same as the previous example. In addition, frost does not affect the observation or photographing of the surface of the sample W.

  Here, in each of the above-described embodiments, an example in which the present invention is applied to a hardness meter of a type that obtains the hardness from the size of a dent generated by pressing the indenter to the sample surface has been shown. Of course, the present invention is equally applicable to a type of hardness meter that obtains sample hardness from the amount of indentation of the indenter against the sample surface.

  In addition, the detailed structure of the hardness meter body used in each of the above embodiments, the detailed structure of the gas replacement simple glove box, etc. are not particularly limited, and other known structures can be adopted. Of course.

It is a principal part block diagram of embodiment of the invention which concerns on Claim 1, It is a figure which writes and shows together the schematic diagram showing mechanical structure and arrangement | positioning, and the piping diagram showing the outline of refrigerant | coolant piping and gas piping. It is a front view of embodiment of FIG. FIG. 3 is an enlarged perspective view of an upper structure of a sample size 10 in FIG. 2. It is a principal part block diagram of embodiment of the invention which concerns on Claim 2, Comprising: The schematic which represents mechanical structure and arrangement | positioning, and the piping diagram showing the outline of refrigerant | coolant piping and gas piping are shown together. It is sectional drawing which shows schematic structure of an indenter pushing type hardness tester.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Hardness meter main body 10 Sample stand 11 Z stage 12 XY stage 13 Indenter 14 Load mechanism 15 Microscope 16 Low temperature furnace 17 Fixing band 18 CCD camera 2 Low temperature control device 3 Switching valve unit 4 Gas replacement simple glove box 5 Ar gas source 6 Nozzle 7 Low-temperature gas control device 8 Temperature sensor W Sample

Claims (4)

A sample table on which the sample is fixed by a fixture, a load mechanism for pressing the indenter against the sample on the sample table, an optical microscope for observing the surface of the sample, and a dent generated on the sample surface by the pressing of the indenter. In the low-temperature type hardness meter having a length measuring mechanism for measuring length and a cooling unit for cooling the sample on the sample table,
A gas supply means for blowing a high-purity gas having a dew point temperature lower than the sample temperature to the sample fixed on the sample stage, and for filling the inside with the high-purity gas covering the hardness meter A low-temperature hardness tester characterized by having a simple case for gas replacement. A sample table on which the sample is fixed by a fixture, a load mechanism for pressing the indenter against the sample on the sample table, an optical microscope for observing the surface of the sample, and a dent generated on the sample surface by the pressing of the indenter. In the low-temperature type hardness meter having a length measuring mechanism for measuring length and a cooling unit for cooling the sample on the sample table,
A simple case for gas replacement for covering the entire hardness meter and filling the inside with a high purity gas, and an atmospheric temperature in the simple case for gas replacement is lower than the temperature of the sample on the sample stage. A low-temperature type hardness tester comprising gas supply control means for controlling the temperature of the high purity gas supplied into the gas replacement simple case. A sample stage on which the sample is fixed by a fixture, a load mechanism for pressing the indenter against the sample on the sample stage, an optical microscope for observing the surface of the sample, and an indenter when the indenter is pressed with a predetermined load In a low-temperature type hardness tester comprising a push-in amount measuring mechanism for measuring a push-in amount with respect to the surface of the sample and a cooling unit for cooling the sample on the sample stage,
A gas supply means for blowing a high-purity gas having a dew point temperature lower than the sample temperature to the sample fixed on the sample stage, and for filling the inside with the high-purity gas covering the hardness meter A low-temperature hardness tester characterized by having a simple case for gas replacement. A sample stage on which the sample is fixed by a fixture, a load mechanism for pressing the indenter against the sample on the sample stage, an optical microscope for observing the surface of the sample, and an indenter when the indenter is pressed with a predetermined load In a low-temperature type hardness tester comprising a push-in amount measuring mechanism for measuring a push-in amount with respect to the surface of the sample and a cooling unit for cooling the sample on the sample stage,
A simple case for gas replacement for covering the entire hardness meter and filling the inside with a high purity gas, and an atmospheric temperature in the simple case for gas replacement is lower than the temperature of the sample on the sample stage. A low-temperature type hardness tester comprising gas supply control means for controlling the temperature of the high purity gas supplied into the gas replacement simple case.

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