JP2666872B2 - X-ray diffraction qualitative analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a qualitative X-ray diffraction analyzer for measuring and qualitatively analyzing a sample by X-ray diffraction.

[0002]

2. Description of the Related Art In an X-ray diffraction measuring apparatus, X-ray diffraction is determined by the type of a sample to be measured, whether the component to be identified is a main component or a trace component contained in the sample, and the configuration of the measuring device. It is necessary to set various measurement conditions such as the voltage and current of the tube, the slit angle, the scan angle, and the like, and perform the measurement. Conventionally, the setting of the measurement conditions has been performed by an operator who performs the measurement directly on the measuring device. However, the various measurement conditions to be set are often related to each other, and if an inexperienced operator sets them, restrictions between the conditions are not reflected, and as a result, the accuracy of the measurement results is reduced. In addition, an operator or the like also analyzes the measured result by looking at an output waveform or the like, and there is a problem that it is difficult for a person who is unfamiliar with such a measuring apparatus to perform the analysis.

[0003]

SUMMARY OF THE INVENTION The present invention has been made in order to solve the above-mentioned problems. Anyone can easily set measurement conditions and analyze measurement results to perform accurate measurement. It is an object of the present invention to provide an X-ray diffraction qualitative measurement apparatus capable of performing the above.

[0004]

SUMMARY OF THE INVENTION The present invention relates to an X-ray diffraction qualitative analyzer, in which an X-ray diffraction qualitative analyzer sets measurement conditions by interacting with an operator, executes measurement by the measuring device, and obtains a measurement result. And a measurement unit for displaying the analysis result, and in response to an inquiry from the measurement unit, derives measurement conditions based on predetermined input data by the operator, analyzes the measurement result, and returns the derived result and the analysis result to the measurement unit. An AI analysis unit is provided. When setting measurement conditions, the measurement unit receives the input data, sends the input data to the AI analysis unit, and derives the measurement conditions based on the input data in the AI analysis unit. Notify the result to the measurement unit, set the measurement conditions in the measurement unit,
When analyzing the measurement result, the measurement unit sends the measurement result obtained by the measurement device to the AI analysis unit, analyzes the measurement result in the AI analysis unit, and notifies the measurement unit of the analysis result. It is.

[0005]

According to the present invention, at the time of setting measurement conditions, for example, a question is presented about factors that determine the measurement conditions, dialogue with the operator is received, input data as the answer is received, and the input data is analyzed by AI analysis. To the measurement section, and the AI analysis section derives the measurement conditions based on the input data, and notifies the measurement section of the derivation result. In addition, it is possible to automatically set an appropriate measurement condition in consideration of the constraints between the measurement conditions. The automatically set measurement conditions can be modified by interaction with the operator. Also, based on the set measurement conditions,
In the measurement device, the sample is measured, and the measurement result is
The analysis can be automatically performed by the I-analysis unit, and the analysis result of the measurement result can be obtained.

[0006]

EXAMPLE FIG. 1 is a block diagram showing an example of an X-ray diffraction qualitative analyzer of the present invention. In the figure, 1 is a measuring unit, 2
Denotes an AI analysis unit, 3 denotes a knowledge base, 4 denotes a measurement device, and 5 denotes an input / output unit.

The measuring unit 1 includes an AI analyzing unit 2, a measuring device 4,
The input / output unit 5 is connected to the input / output unit 5 for setting measurement conditions, displaying a measurement result of a sample and an analysis result of the measurement result, and the like. The AI analyzer 2 transmits the answer to the question about the measurement environment input from the operator and the data measured by the measurement device, and receives the derivation result of the measurement condition and the analysis result of the measurement result. Further, the set measurement conditions are transmitted to the measurement device 4 and the measurement results are received. Further, the user interacts with the operator via the input / output unit 5 to display a question concerning the measurement environment when setting the measurement conditions, obtain the answer, and obtain the answer.
The measurement conditions sent from are displayed, and each measurement condition can be corrected. In addition, a measurement result and an analysis result of the measurement result are displayed.

The AI analysis unit 2 operates in response to a question sent from the measurement unit 1, infers a question using the knowledge base 3, and transmits the obtained answer to the measurement unit 1. . At the time of setting measurement conditions, inference is performed based on input data of an answer to an operator's question sent from the measurement unit 1 and the obtained measurement conditions are transmitted to the measurement unit 1. Further, at the time of analysis, inference is performed using the knowledge base 3 based on the measurement result, and the analysis result is transmitted to the measurement unit 1. The knowledge base 3 stores knowledge data on measurement conditions related to X-ray qualitative analysis, and is searched by the AI analysis unit 2.

The operation of one embodiment of the X-ray qualitative analyzer of the present invention will be described. FIG. 2 is a flow chart for explaining the operation of one embodiment of the X-ray qualitative analysis apparatus of the present invention. In S11, first, it is determined whether the setting of the measurement condition is automatically performed using the AI analysis unit 2 or the item of each measurement condition is set manually. When automatically using the AI analysis unit 2, in S12, some questions about the measurement environment are presented to the operator using the window, and an answer to the questions is input. In S13, the input answer is inferred by the AI analysis unit 2, measurement conditions are set, and displayed on the input / output unit 5. In S14, the operator determines whether or not to perform measurement under the displayed conditions. If measurement is not to be performed under the displayed conditions, the process returns to S11 and starts again from the selection of a method for setting measurement conditions. If manual measurement condition setting is selected in S11, the process proceeds to S1.
In step 5, each measurement condition is set manually as in the related art. When the setting of the measurement conditions is completed, S16
In, measurement is performed, and in S17, the measurement result is diagnosed. If it is determined in step S18 that the measurement needs to be performed again as a result of the diagnosis, the process returns to step S11 to start again from the selection of the measurement condition setting method. If the measurement result is found to be appropriate in S18, the measurement ends.

FIG. 3 is a flowchart for explaining the operation of the measurement environment input. This flowchart shows an operation corresponding to S12 in FIG. First,
In S21, a question to be presented is determined. Here, the question to be presented next is determined based on the answers to the questions up to that point. They may also decide that they no longer need to ask questions. In S22, the presence or absence of the question determined in S21 is determined, and when the question is presented, S
Proceed to 23, and if not presented, end the question. S2
In 3, the question determined in S21 is presented to the operator. Then, in S24, an answer to the question by the operator is obtained. Then, returning to S21, the next question is determined based on the answered contents. If it is determined in S23 that the question has been completed,
At 13, inference is performed based on the answer to the question input by the operator, appropriate measurement conditions are set, and displayed on the input / output unit 5.

Hereinafter, the above processing will be specifically described. 4 to 13 are explanatory diagrams of specific operations. Description will be made in association with each step shown in FIGS. 2 and 3. FIG. 4 shows a selection screen for a method of setting measurement conditions in S11. When the X-ray diffraction qualitative analyzer of the present invention is activated, the selection screen for the measurement condition setting method is displayed. In the guidance window at the bottom of the screen, “Please select the setting method of the measurement conditions. Do you want to use AI setting or manual?” Is displayed, and “AI setting” is displayed on the screen.
"Manual setting" is displayed, and the operator selects one of them. As a selection method, it is also possible to adopt a configuration in which a selection is made with “↑” and “↓” keys on a keyboard and confirmed with a return key, or a selection is made using a pointing device such as a mouse. This selection method can be similarly used for selecting the following items. On this screen, if you select “AI setting”,
The processing shifts to the measurement condition setting processing using the I analysis unit.

FIG. 5 shows an initial screen when setting AI measurement conditions. In the guidance window at the bottom of the screen, "Set AI measurement conditions" is displayed, and a list of measurement conditions to be set is displayed. The displayed measurement conditions are: Scan mode 2. 2. High angle (deg) 3. low angle (deg) Integration time (sec) 5. 5. Scan speed (deg / min) 6. Full scale (kcps) Comments 8. Data file number 9 Drive shaft of goniometer 10. Fixed axis and angle (deg) Tube target 12. Tube voltage (kV) 13. Tube current (mA) Divergence slit (deg) 15. 15. Air scattering prevention slit (deg) The detection slit (mm). Other items may be provided. After this initial screen is displayed, a question presentation screen for setting measurement conditions is displayed. The selected item is displayed by an appropriate method such as reverse display, blink display, or changing the display color. Since nothing is performed on this initial screen, it is possible to shift to the screen for presenting the next question without displaying this screen.

Next, a question for setting the measurement conditions shown in S12 of FIG. 2 and FIG. 3 is presented. First, FIG.
As shown in FIG. 3, a question about the selection of the type of the measurement sample is selected in S21 of FIG. 3, and in S23, it is displayed as shown in FIG. As shown, the question is displayed as a single window. In S24, the operator selects an appropriate one from the list of measurement samples displayed as shown in FIG. Here, "steel, non-ferrous metal" is selected. When the selection of the type of the measurement sample is completed, the process returns to S21, and a question about the expected X-ray intensity is selected as the next question and displayed in S23. FIG. 7 shows a screen at the time of this question. There are four options, "strong", "normal", "weak", and "don't know", and the operator selects one of them. Here, “strong” is selected. In addition, a question is asked about the component to be identified. The screen at the time of this question is shown in FIG. As the selection options, there are prepared “main component”, “trace component”, and “not specified”, and the operator selects one of them. The question continues, asking whether a monochromator is being used. The screen at this time is shown in FIG. 9, and the operator selects from two options, “used” and “unused”. In this case, "use" is selected. Since the measurement conditions can be set up to this question,
At 21, it is determined that there is no question to be presented, and S2
In 2, the end of the question item is determined, and the input operation of the measurement environment ends.

In this way, the measurement environment can be input by the operator answering the question. In the above-mentioned specific example, the following conditions were set when measuring a sample. Type of measurement sample: steel, non-ferrous metal Expected X-ray intensity: strong Component to be identified: main component Monochromator: use As described above, the question does not necessarily correspond to each item of the measurement conditions shown in FIG. For example, when the type of the measurement sample is determined, in accordance with the type of the selected measurement sample,
A plurality of measurement items such as a tube current, a divergence slit angle, and a measurement angle are changed and set. Further, the question is not always the same, and the next question is changed depending on the answer to the question. For each question, an answer such as "I do not know" or "Do not specify" is also prepared, so that it is possible to respond to an unfamiliar operator or an unknown sample. If you choose these answers,
As each measurement condition, a preset condition can be selected. This preset condition can be realized by adding a configuration for modifying the knowledge base 3 via the AI analysis unit 2.

As mentioned above, by answering the questions,
An inference is made for the measurement conditions. FIG. 10 is a display example of measurement conditions set by inference. After confirming the displayed measurement conditions, indicate whether or not to perform the measurement under the set measurement conditions. Choices in the displayed window "1. Measure", "2. Correct conditions", "3.
Select one from "Redo". The selection method is
Similarly to the input of the answer to the above-mentioned question, the selection may be made by a method of selecting with a cursor or a pointing device, or a method of inputting a number of a selection from a keyboard.
When "1. measure" is selected, actual measurement is started. When "2. Modify condition" is selected, the value of each displayed measurement condition can be modified on the screen.
When "3. Redo" is selected, the screen returns to the selection screen of the setting method of the measurement condition shown in FIG. 4 or the question screen shown in FIG. 6 and thereafter, and the settings can be redone.

When "manual setting" is selected on the measurement condition setting method selection screen shown in FIG. 4 or "2. Modify condition" is selected on the measurement condition display screen in FIG. Then, on the screen of the list of the measurement conditions similar to that of FIG. 5, it is possible to input or modify the items of each measurement condition. The selection of the measurement condition items to be input or corrected can be performed using a cursor key or a pointing device. Also,
The value to be set for each item can be input using a keyboard or the like. In the case of "manual setting", the value of each item may be left blank, or a predetermined value may be displayed and only necessary items may be modified.

When "1. measure" is selected on the measurement condition display screen in FIG. 10, the process proceeds to step S16 in FIG. 2, and the measuring device actually uses the set measurement conditions. A measurement is made. When the measurement is completed, a confirmation screen of the measurement result is displayed, and the measurement result is diagnosed in S17 of FIG. After the measurement is started, the execution of the measurement can be interrupted, the interrupted measurement can be resumed, and the measurement can be stopped by a specific input, for example, a program function key on a keyboard. When the measurement is stopped, the screen returns to the selection screen for setting the measurement condition shown in FIG.

FIG. 11 shows an example of the confirmation screen of the measurement result. Although a graph of the measurement result is displayed in the lower half of the screen, the graph is omitted in FIG. The upper half is an area for presenting a question for inferring the quality of the measurement result and inputting an answer. As in the case of setting the measurement conditions, the operator inputs answers to some questions and makes inferences based on the input answers to determine the quality of the measurement data. In FIG. 11, a question "How many peaks can be confirmed?" Is presented, and two options, "less than 1.3" and "2.3 or more", are prepared as the answer. And you will have to choose one.

When the input of the answer to the question regarding the measurement result is completed, inference is performed based on the input answer data. As a result of the inference, when the measurement result can be used as it is, an indication that "remeasurement is not necessary" is displayed. As a result of the inference, when it is determined that the measurement condition is bad and a good result is not obtained, the display of the determination result and the method of treatment are displayed to the operator. FIG. 12 is a display example when it is determined as a result of inference that the measurement angle range is too narrow. The judgment result of "the measurement angle range is too narrow" and the treatment method of "extend the measurement angle range" are displayed. And when you press any key,
Since the screen of FIG. 3 is displayed, a selection is made as to whether or not to perform re-measurement. When re-measurement is to be performed, the screen returns to the selection screen for setting the measurement conditions shown in FIG. A measurement can be performed.

FIGS. 12 and 13 have been described as separate screens in this example, but they may be displayed on the same screen. Further, the screens for displaying the question answer and the inference result shown in FIGS. 11 to 13 may be displayed as windows separate from the display part of the measurement result. In the above-described analysis of the measurement results, the determination of the measurement conditions is performed. In addition, features such as peaks are automatically extracted from the measurement results, and inference is performed based on the extracted features. It is also possible to display the analysis result of the sample.

The results obtained by the measurement and the measurement conditions used at that time can be stored as a file. Further, it is also possible to output to a printer, a plotter or the like. In addition, the measurement device can be corrected.

[0022]

As is apparent from the above description, according to the present invention, the measurement conditions can be set by answering several questions, so that anyone can easily set the measurement conditions and obtain the measurement results. Can be analyzed. In addition, it is possible to automatically set the relevant measurement condition items and check the obtained measurement results, so that highly accurate measurement results can be obtained and good qualitative analysis can be performed. There is an effect that a result can be obtained.

[Brief description of the drawings]

FIG. 1 is a block diagram showing one embodiment of an X-ray diffraction qualitative analyzer of the present invention.

FIG. 2 is a flow chart for explaining the operation of one embodiment of the X-ray qualitative analysis apparatus of the present invention.

FIG. 3 is a flowchart for explaining an operation of inputting a measurement environment.

FIG. 4

FIG. 13 is an explanatory diagram of a specific operation.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Measurement part 2 AI analysis part 3 Knowledge base 4 Measuring device 5 Input / output part

Claims (1)

(57) [Claims] 1. An X-ray diffraction qualitative analyzer which sets measurement conditions through dialogue with an operator, executes measurement by the measurement device, and displays measurement results and analysis results. Accordingly, the measurement unit derives measurement conditions based on predetermined input data from the operator, analyzes the measurement results, and has an AI analysis unit that answers the derivation results and the analysis results to the measurement unit. Receiving the input data, sending the input data to the AI analyzer, deriving measurement conditions based on the input data in the AI analyzer, notifying the derivation result to the measurement unit, and setting the measurement conditions in the measurement unit; When analyzing the measurement result, the measurement unit sends the measurement result obtained by the measuring device to the AI analysis unit, and the AI analysis unit analyzes the measurement result. An X-ray diffraction qualitative analyzer for notifying a measurement unit of the analysis result.