JPH0394147A - Setting method for standard sample in local analyzing device and its setting jig - Google Patents

Abstract

PURPOSE:To exactly set a measuring position of a standard sample in a short time by storing in advance a relative coordinate of the standard sample against a position calibrating mark on a sample holder, and an actual coordinate of the calibrating mark in an analyzing device. CONSTITUTION:Plural pieces of standard sample blocks 1 in which may kinds of standard samples 11 are contained are set in a lump to a sample holder 12, fixed to a sample holding base 2, and thereafter, installed in a sample driving system 8 of a local analyzing device 4. A relative coordinate of a position calibrating mark 13 put to the upper part of the holder 12 and each sample 11 is stored in a computer 9. By using an optical microscope 5, an actual coordinate of the mark 13 is read in, and inputted to the computer 9. From a relation of both the coordinates, an actual coordinate of each sample 11 in the device 4 is calculated and stored. In the course of automatic analysis, by operating and setting the driving system 8 so as to become an actual coordinate of the sample 11 required, a call of the sample 11 concerned 11 is executed. Subsequently, by operating a z axis direction aligning mechanism 6, the holding base 2 is adjusted and aligned in the z axis direction through the driving system 8.

Description

DETAILED DESCRIPTION OF THE INVENTION <Industrial Application G; F> The present invention relates to a method for setting a standard sample in a local analysis device and a method for setting it.

<Prior Art> Local analysis devices HzHt using electrons or ions are widely used in various fields to obtain information on the shape and composition of minute regions. With such local analyzers, there are many opportunities to measure standard samples for quantitative analysis and collection of standard data, and the amount of work required for setting the sample is relatively large in daily analysis. .

Here, an X-ray microanalyzer, which is one of these local analysis devices, will be explained in a little more detail as an example.

Usually, in an X-ray microanalyzer, for example, EB
X-ray Svek1 in S-image photography or mapping
・Be sure to measure a standard sample when checking the peak of the sample or performing quantitative analysis. In particular, in quantitative analysis, the Z8F correction, which is often used in the standard correction method, requires measurement of not only the target element but also all coexisting elements under the same conditions as the analytical sample, and many standard sample measurements are required. is required.

When measuring such standard samples, in the case of manual measurement in which the operator directly controls the analyzer and performs the analysis, each standard sample is analyzed one by one while being observed using the optical microscope attached to the analyzer. This is done by searching for the location of the rust sample.

On the other hand, in the case of automatic measurement, the required standard sample is set in the sample drive system driven by a pulse motor installed in the analyzer, and the operator observes it with an optical microscope in advance to determine the position of each mark i11j sample. After checking, the coordinates are read and registered in the computer's memory, and during measurement, the computer controls the analysis position based on the coordinates and performs the measurement.

As mentioned above, measurements of such standard samples are frequently performed, and therefore, a lot of time and energy is spent on the measurements and the associated target setting work. Also, considerable care is required to accurately set the positions of a large number of standard samples.

For this reason, regarding the measurement position setting work,
As a means of improving work efficiency or reproducibility of analysis positions, for example, Japanese Patent Publication No. 6158774 discloses a method using a sample fine movement device that is installed in the atmosphere and has the same sample drive system as the main body of the analyzer. , a sample position determining device is disclosed in which all measurement positions are observed in advance with an optical microscope and the coordinate values are read in, and the position within the analyzer body is controlled based on the coordinate values. Also, in 1987,
Publication No. 9305 discloses that the origin of the coordinates, the X axis,
A sample holder has been proposed in which a mark indicating the y-axis direction is cleared and positioning is performed based on the mark.

Problems to be Solved by the Invention> However, the former sample position determination device of Japanese Patent Publication No. 61-58774 has the disadvantage that while the coordinates are set using the sample fine movement device, it can be done without using the analyzer itself. Although it is possible to improve the operating rate of the equipment,
Since the work of observing the measurement position using an optical microscope cannot be simplified, there is still the problem that it requires a lot of manpower. In addition, since this device uses a sample fine movement device separately from the main body of the analyzer, there is a potential problem in that careful attention is required to align the positions of the two and achieve positional accuracy.

In addition, it is necessary to observe the measurement position of each sample using the sample holder of the latter Japanese Utility Model Application Publication No. 52-19305, as well as Japanese Patent Publication No. 61-58774.

Furthermore, when determining the position using the coordinates automatically registered by the above two means, the registered coordinates may be changed frequently due to resetting by replacing the analytical sample or standard sample, or by repolishing the surface of the standard sample. There are also issues that need to be fixed.

As can be clearly seen in this example of an X-ray microanalyzer, even though standard samples are measured many times during analysis work using a local analyzer, the measurement position settings are made for each standard sample individually. It is necessary to observe it with an optical microscope or to automatically control the position from the coordinates determined in advance, which is not efficient as it takes a long time and requires a detailed nerve. There is a great risk of making a mistake.

The present invention has been made in view of the above circumstances, and allows the coordinates of many types of standard t% samples to be easily registered without having to observe each one, and the measurement position of the standard sample can be accurately determined in a short time. The purpose of the present invention is to provide a method for setting a standard specimen in a local analysis device and a setting jig therefor.

<Means for Solving the Problems> A first aspect of the present invention is that when setting the measurement position of a standard sample in a local analysis device, it is possible to at least 1
a step of memorizing in advance the relative coordinates of the standard sample with respect to the position calibration marks, and inserting the sample holder to which the standard sample is fixed into the local analysis device to determine the actual position of the mark in the device. a step of detecting the coordinates;
A process of calculating and registering the actual coordinates of each reference sample from the actual coordinates and the relative coordinates, and calling the actual coordinates of the corresponding standard sample when measuring the standard sample. A method for setting a standard sample in a local analysis device, comprising the steps of aligning measurement positions.

Further, a second aspect of the present invention is a standard sample setting jig in a local analysis device, which includes a standard sample block holding many types of standard samples and a 1:1 standard sample block. A plurality of sample holders are integrated and fixed, and at least one position calibration mark is provided on the sample holder at a position substantially flush with the top surface of the standard sample block.
This is a standard sample setting jig for a local analysis device, which is characterized by the following.

According to the present invention, one or more standard sample blocks holding standard samples of multiple scales are integrated and fixed in a sample holder, and at least one sample block is fixed to the upper part of the sample holder. Since a standard sample setting jig with position calibration marks is used, the individual positions of each standard sample held in the standard sample block can be expressed as relative coordinates based on the position calibration marks. can.

Next, the actual coordinates of the mark in the local analyzer are detected, and the actual coordinates of each standard sample are calculated and registered from the relationship between the two coordinates, so when measuring a standard sample, the corresponding standard The settings can be made by extracting the actual coordinates of the sample by n and adjusting the measurement position.

<Examples> Examples of the present invention will be described below with reference to the drawings:
<Explain.

FIG. 1 is a structural diagram schematically showing an example in which the present invention is applied to an X-ray microanalyzer, which is one type of local analysis device.

In the figure, reference numeral 1 denotes a standard sample block holding a plurality of standard samples, and is placed on a sample holding table 2.

3 is an electron optical system installed inside the chi-ray microanalyzer 4 to generate an electron beam and control the optical path; the electron beam 32 emitted from a filament 31 is accelerated by an anode 33, and then passed through an electromagnetic lens. 34 and 35 to form a focal point S on the standard sample surface.

Reference numeral 5 denotes an optical microscope provided inside the X-ray microanalyzer 4, which allows the sample surface to be observed through a mirror 36, thereby allowing the position calibration mark attached to the standard sample block 1 to be corrected. can detect the position of

Reference numeral 6 denotes a Z-axis positioning mechanism, which may be any mechanism as long as it has the function of correctly aligning the two-axis directions of the focal point S of the electron beam 32 irradiated onto the sample surface to the analysis {j''I. This figure uses a pattern signal detector 7 such as an autofocus mechanism to adjust the bin l position in the l-axis direction of the optical microscope 5. That is, the pattern signal detector 7 uses the optical Wn1jI!.mirror 5 The inverse 1.1 light of the pattern projected onto the standard sample surface from the light source is detected, and the detection signal is sent to the Z-axis positioning mechanism 6.
input and process the signal.

Reference numeral 8 denotes a test rice drive system installed inside the X-ray microanalyzer 4, which moves the sample holding table 2 on which the sample block 1 is set on the X-axis. The position is set in the y-axis and Z-axis directions using a pulse motor (not shown). This position setting is performed using x, y, and z coordinates, and these are stored and controlled by the computer 9. The Z-axis direction is finely adjusted by the Z-axis positioning mechanism 6 which receives a signal from the pattern signal detector 7.

The reason why it is desirable to incorporate the Z-axis positioning mechanism 6 is that in the X-ray microanalyzer 4, positional deviation in the Z-axis direction greatly affects the measured Although the position needs to be adjusted, it is difficult to register the two-coordinate position without deviation in advance, so it is best to adjust the position in the two-axis direction each time when measuring. .

Here, regarding the preparation of standard sample blank 1: Jink 1, the second
．． This will be explained in detail using Figure 3.

As shown in these figures, a plurality of standard sample blocks 1 contain, for example, 90 polygonid standard samples 11 in small quantities in a well-ordered manner.
! The sample blocks 1 are set, for example, in a sample holder 12 that is fixed to a sample holder 2 side by side.

The frame portion 12a of the sample holder l2 has at least a
Position calibration marks 13 are attached. The mark 13 and each standard sample 11 are fixed by pressing them from one surface to the opposite surface using screws 14 so that the relative coordinates of each standard sample 11 do not change at all times.

Note that the number of position calibration marks 13 is not limited to one, and may be attached, for example, to a frame 12b symmetrical to the frame 12a of the sample holder I2.

In addition, the surface of the standard sample 1L is polished to a mirror-like state, and the surface of the standard sample 1L is polished to a mirror-like state. 11! The material of the sample block 1 is preferably a conductive material such as brass.

Further, it is desirable that the standard sample block 1 be divided into groups of metal elements and non-metal elements, for example, so that when the surface of the block 1 becomes contaminated, it is easy to perform dirt polishing or vapor deposition suitable for each type.

Next, a procedure for calibrating the local analysis device using the standard sample block 1 configured as described above will be described.

■ A plurality of standard sample blocks 1 containing standard samples 11 and divided in advance are set in the sample holder 11 holder 12, and after fixing this sample holder 12 to the sample holder 2, the X-ray micro It is attached to the sample drive system 8 of the analyzer 4.

■ The relative coordinates (X+', )'+') of the position calibration mark l3 attached to the sample holder 12 and each standard sample 11 are registered in the internal memory of the computer 9. Also, each mark 14+
! Approximate two coordinates of the sample 1l are also registered at the same time.

■ Mark 13 on sample holder 12 using optical microscope 5
The actual position in the x and y axis directions +”J (xqi, 3'
MI) and input it to the computer 9.

■ In the computer 9, the x and y axes of each standard sample 11 in the X-ray microanalyzer 4 are calculated based on the actual coordinates and the relative coordinates of the marks 13 and each standard sample 11 registered in advance in the internal memory. The actual coordinates of the direction (X+, y
(direct) and register it in a separate memory from the relative coordinates.

■ During automatic analysis, the sample drive system 8 is operated and set so that the actual x, y coordinates (xi.yi) of the required standard sample 11 are set. 11 calls are made.

■ Next, operate the z-axis positioning mechanism 6゜(,
Registered ゜C7. i [L minute 4J'+f near the coordinates
1'f. The sample holder 2 is adjusted in two axial directions via the sample drive system 8 so that the sample holder 2 is positioned at the same position.

In this way, by optimizing the position of the standard sample 11 in the x, y, and z axis directions, the precepts of the corresponding standard sample 11 can be accurately measured.

In this embodiment, it takes about 2 minutes to register the coordinates of about 90 types of standard samples held in the target tll1 sample holder 12, but this is much shorter than the 40 minutes required in the conventional example. You can register by asking.

Furthermore, although the above embodiment has been described using an X-ray microanalyzer as the local analysis device, the tree starting point 1 is not limited to this, and may be applied to other local analysis devices such as an ion microanalyzer. Needless to say.

<Effects of the Invention> As explained above, according to the standard sample setting method and setting jig of the present invention, it is possible to set a large number of standard samples in a local analysis device in a straightforward and simple manner, and in a short time. Because it is possible to do so, work efficiency can be improved.

Moreover, the present invention U. For systems that automatically analyze samples with completely unknown compositions, it is important to prepare a large number of standard samples in advance so that they can be used in case any element is detected in automatic qualitative analysis. Therefore, it is indispensable to quickly carry out actual work, and its contribution is significant.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram showing the structure of the local analysis device of the present invention, FIG. 2 is a perspective view showing the structure of a standard sample block, and FIG. 3 is a plan view of FIG. 2. Sample drive system, 9... Computer, 11... Standard sample, 12... Sample holder, 13... Mark. 3
1... filament, 32... electron beam, 33...
Anode, 3/1.35... Electromagnetic lens, 36...
Mirror S...Focus. 1... Standard sample block, 2... Sample holding stand,
3... Electron optical system. 4...X-ray microanalyzer. 5... Optical w1 microscope, 6... Z-axis positioning mechanism, 7... Pattern signal detector,
8...Patent Ishiojin Kawasaki Steel Co., Ltd. 15 l6

Claims (1)

[Scope of Claims] 1. When setting the measurement position of a standard sample in a local analysis device, the above-mentioned method is applied to at least one position calibration mark placed on a sample holder that holds multiple types of standard samples at once. a step of memorizing the relative coordinates of the standard sample in advance; a step of inserting the sample holder to which the standard sample is fixed into the local analysis device and detecting the actual coordinates of the mark in the device; The process of calculating and registering the actual coordinates of each standard sample from the actual coordinates and the relative coordinates, and the process of calling the actual coordinates of the corresponding standard sample and determining the measurement position when measuring the standard sample. A method for setting a standard sample in a local analysis device, comprising: a step of combining; 2. A standard sample setting jig for a local analysis device, which includes a standard sample block that holds many types of standard samples, a sample holder that integrates and fixes one or more of the standard sample blocks, and the sample. A standard sample setting jig for a local analysis device, characterized in that at least one position calibration mark is attached to a holder at a position substantially flush with the top surface of the standard sample block.