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XRD-DSC General (BB) D/teX Package Measurement

XRD-DSC General (medium resolution PB/PSA) Package Measurement

XRD-DSC General (2D detector) Package Measurement

Contents

XRD-DSC General (BB) D/teX / (medium resolution PB/PSA) / (2D detector) Package Measurement i

Contents

1. Package measurement flow ........................................................................................................ 1 1.1 XRD-DSC General (BB) D/teX Package Measurement ...................................................................1 1.2 XRD-DSC General (medium resolution PB/PSA) Package measurement........................................3 1.3 XRD-DSC General (2D detector) Package measurement .................................................................5

2. Measurement procedures ........................................................................................................... 7 2.1 Starting up the X-ray generator .........................................................................................................7 2.2 Hardware setup ..................................................................................................................................8 2.3 Setting Package measurement conditions ........................................................................................13

2.3.1 Setting Optics Alignment Part conditions ............................................................................13 2.3.2 Setting XRD-DSC Sample Alignment Part conditions.........................................................15 2.3.3 Setting Sample Alignment (2D detector) Part conditions ....................................................16 2.3.4 Setting D/teX Detector Center Correction Part conditions ..................................................17 2.3.5 Setting XRD-DSC Measurement Part conditions .................................................................18

2.4 Customizing Part conditions ............................................................................................................21 2.4.1 Customizing XRD-DSC Sample Alignment (BB) Part conditions.......................................21 2.4.2 Customizing Sample Alignment (2D detector) Part conditions ...........................................22 2.4.3 Customizing XRD-DSC Measurement Part conditions ........................................................24

2.5 Preparing the DSC Attachment .......................................................................................................25 2.5.1 Starting up the Bath Circulator .............................................................................................25 2.5.2 Connecting the Humidity generator HUM-SL (optional) .....................................................26 2.5.3 Connecting the Low Temperature Bath Circulator (optional) ..............................................30

2.6 Running Package measurement .......................................................................................................32 2.7 Changing configuration units ..........................................................................................................45 2.8 Removing the DSC Attachment ......................................................................................................47

2.8.1 Setting each temperature back to room temperature.............................................................47 2.8.2 Turning OFF the Low Temperature Bath Circulator(optional) ............................................48 2.8.3 Disconnecting the Humidity generator HUM-SL (optional) ................................................49 2.8.4 Turning OFF the Bath Circulator(optional) ..........................................................................50

2.9 Shutting down the X-ray generator..................................................................................................51 2.10 Sample preparation ........................................................................................................................52

2.10.1 When using powder sample ................................................................................................52 2.10.2 When using plate sample ....................................................................................................54

3. Executing Each Parts ................................................................................................................ 55 3.1 Executing Optics Alignment Part ....................................................................................................55 3.2 Executing XRD-DSC Sample Alignment Part ................................................................................57 3.3 Executing Sample Alignment (2D detector) Part ............................................................................58 3.4 Executing D/teX Detector Center Correction Part ..........................................................................59

Contents

ii XRD-DSC General (BB) D/teX / (medium resolution PB/PSA) / (2D detector) Package Measurement

3.5 Executing XRD-DSC Measurement Part ........................................................................................60

4. Troubleshooting ........................................................................................................................ 62

1.1 XRD-DSC General (BB) D/teX Package Measurement

XRD-DSC General (BB) D/teX / (medium resolution PB/PSA) / (2D detector) Package Measurement 1

1. Package measurement flow

1.1 XRD-DSC General (BB) D/teX Package Measurement

Figure 1.1.1 shows the procedural flow for an XRD-DSC General (BB) D/teX Package measurement.

Tip: In the XRD-DSC General (BB) D/teX Package measurement, the optics

alignment is done by using D/teX Ultra, then sample alignment and center

correction are done after setting the DSC attachment.

1. Select Package Measurement Task.

2. Select XRD-DSC General (BB) D/teX Package measurement.

3. Set Optics Alignment (BB) Part conditions.

5. Set D/teX Detector Center Correction Part conditions.

7. Run Package measurement.

8. Executing optics alignment.

11. Executing sample alignment.

12. Executing D/teX detector center correction.

Start

End

4. Set XRD-DSC Sample Alignment (BB) Part conditions.

User actions Guidance software actions

6. Set XRD-DSC Measurement Part conditions.

9. Mount DSCAttachment.

10. Restart the Package measurement.

13. Executing XRD-DSC Measurement.

Fig. 1.1.1 XRD-DSC General (BB) D/teX Package measurement procedural flow


2 XRD-DSC General (BB) D/teX / (medium resolution PB/PSA) / (2D detector) Package Measurement

2. Click XRD-DSC General (BB) D/teX.

1. Click Package Measurement in the Tasks menu.

3. Set the Optics Alignment (BB) Part conditions.

7. Click the Run button to run the optics alignment.

4. Set the XRD-DSC Sample Alignment (BB) Part conditions.

6. Set the XRD-DSC Measurement Part conditions.

5. Set the D/teX Detector Center Correction Part

1.2 XRD-DSC General (medium resolution PB/PSA) Package measurement


1.2 XRD-DSC General (medium resolution PB/PSA) Package measurement

Figure 1.2.1 shows the procedural flow for an XRD-DSC General (medium resolution PB/PSA) Package measurement.

Tip: In the XRD-DSC General (medium resolution PB/PSA) Package

measurement, the optics alignment is done by using the scintillation counter

(SC-70), then sample alignment is done after setting the DSC attachment.

Fig. 1.2.1 XRD-DSC General (medium resolution PB/PSA) Package measurement procedural flow



2. Click XRD-DSC General (medium resolution PB/PSA).

3. Set the Optics Alignment (PB/PSA) Part conditions.

6. Click the Run button to run the optics alignment.

4. Set the XRD-DSC Sample Alignment (PB/PSA) Part conditions.



1.3 XRD-DSC General (2D detector) Package measurement


1.3 XRD-DSC General (2D detector) Package measurement

Figure 1.3.1 shows the procedural flow for an XRD-DSC General (2D detector) Package measurement.

Tip: Before executing the XRD-DSC General (2D detector) Package measurement,

the optics alignment is done by using the scintillation counter (SC-70). After the

alignment, change the detector to PILATUS, and execute the Create Mask File

Part and the Camera Length Alignment Part.

5. Select Package Measurement Task.

6. Select XRD-DSC General (2D detector) Package measurement.

10. Run Package measurement.

11. Executing sample alignment.

Start

End

7. Set Sample Alignment (2D detector) Part conditions.

User actions Guidance software actions

12. Executing XRD-DSC Measurement.

2. Replace SC-70 with PILATUS.

8. Set XRD-DSC Measurement Part conditions.

9. Mount DSC Attachment.

3. Executing Create Mask File Part.

4. Executing Camera Length Measurement Part.

1. Executing optics alignment.

Fig. 1.3.1 XRD-DSC General (2D detector) Package measurement procedural flow



3. Set the Sample Alignment (2D detector) Part conditions.

2. Click XRD-DSC General (2D detector).

5. Click the Run button to run the sample alignment.



2.1 Starting up the X-ray generator


2. Measurement procedures

2.1 Starting up the X-ray generator

Before running the measurement, set the output of the X-ray generator (XG) as described below.

(1) Click the Startup button on the flow bar to open the Startup dialog box.

(2) Uncheck the Timer box.

Fig. 2.1.1 Startup dialog box

(3) Select an appropriate setting in the Generator usage box, based on the frequency of XG usage.

(4) Select Set in the XG set box.

(5) Enter the following values in the Voltage(kV) and Current(mA) boxes.

When using 3-kW sealed-off tube 40 kV, 30 mA When using 9-kW rotating anode tube 45 kV, 200 mA

(6) Click the Execute button.

(7) The aging operation begins. The XG output will be set to the values entered in step (5) within 30 to 60 minutes.

CAUTION: If Not used for more than 3 weeks is selected in the Generator usage box, the aging operation will take approximately five hours.

Tip: For other functions available from the Startup dialog box, refer to Chapter 21 of

the SmartLab Guidance Reference Manual (ME13365A)



2.2 Hardware setup

Before running the measurement, the hardware configuration for the XRD-DSC General (BB) D/teX / XRD-DSC General (medium resolution PB/PSA) / XRD-DSC General (2D detector) Package measurements must be set up.

The hardware setup method is described below.

(1) Select the Hardware Configuration command under the Options menu to open the Hardware Configuration dialog box.

(2) The Hardware Configuration dialog box shows the current hardware configuration.

Fig. 2.2.1 Hardware Configuration dialog box

2.2 Hardware setup


(3) Table 2.2.1, Table 2.2.2 and Table 2.2.3 show the hardware configurations that enable the XRD-DSC General (BB) D/teX / XRD-DSC General (medium resolution PB/PSA) / XRD-DSC General (2D detector) Package measurements. If the configuration units shown in the Hardware Configuration dialog box differ from those indicated in each Table, refer to SmartLab, Automated Multipurpose X-ray Diffractometer Instruction Manual and install the units indicated in each Table at the designated locations.

Table 2.2.1 Hardware configuration for the XRD-DSC General (BB) D/teX Package measurements

Hardware configuration Configuration units X-ray generator Cu target Incident optics CBO unit

Standard incident optical unit Standard incident slit box

Goniometer SmartLab Base attachment configuration Standard Z stage Attachment DSC Receiving optics Standard receiving slit box # 1

Standard receiving optical unit # 1* Standard receiving optical unit # 2 Standard receiving slit box # 2 Standard attenuator

Detector (See CAUTION below)

D/teX Ultra

* Remove the standard receiving optical unit # 1 when using the D/teX Ultra in the one dimensional mode.

For example, if the target is set to Mo in the X-Ray Generator dialog box, you must change the target setting to Cu, since the XRD-DSC General (BB) D/teX Package measurement runs only with the Cu target. For sealed-off tubes, you must replace the Mo tube with the Cu tube.



Table 2.2.2 Hardware configuration for the XRD-DSC General (medium resolution PB/PSA) Package measurements



Goniometer SmartLab Base attachment configuration Standard Z stage Attachment DSC Receiving optics Standard receiving slit box # 1

Standard receiving optical unit # 1 Standard receiving optical unit # 2 Standard receiving slit box # 2 Standard attenuator

Detector Scintillation counter SC-70

Table 2.2.3 Hardware configuration for the XRD-DSC General (2D detector) Package measurements



Goniometer SmartLab Base attachment configuration Standard Z stage Attachment DSC Receiving optics None Detector (See CAUTION below)

Scintillation counter SC-70 Pilatus

CAUTION: Before executing the XRD-DSC General (2D detector) Package measurement, perform the detector setting. Click the Detector button in the Hardware Configuration dialog box to open the Detector dialog box, and select SC-70 from the Detector #1 box and PILATUS from Detector #2 box.

2.2 Hardware setup


(4) Click the X-Ray Generator button to open the X-Ray Generator dialog box.

Fig. 2.2.2 X-Ray Generator dialog box

(5) Select Cu from the Target box. Change any other parameters such as wavelengths as necessary.

(6) Click the OK button to close the X-Ray Generator dialog box. The changes made will be registered to the Hardware Configuration dialog box.

(7) If necessary, click the Incident Optics, Receiving Optics, and Detector buttons to change configuration units. After modifying the conditions, click the OK button. The changes made will be registered to the Hardware Configuration dialog box in the same way.

(8) Click the Update button in the Hardware Configuration dialog box.

Tip: For Base Attachment Config. and Attachment, configuration units are

automatically detected.



(9) Confirm that each configuration unit displayed in the Hardware Configuration dialog box corresponds to the configuration unit indicated in Table 2.2.1, then click the Close button.


2.3 Setting Package measurement conditions



There are five Parts for XRD-DSC General (BB) D/teX, three Parts for XRD-DSC General (medium resolution PB/PSA), and two Parts for XRD-DSC General (2D detector) included in each Package measurements.

Package measurement Configuration Parts XRD-DSC General (BB) D/teX • Optics Alignment (BB)

• XRD-DSC Sample Alignment (BB) • D/teX Detector Center Correction • XRD-DSC measurement

XRD-DSC General (medium resolution PB/PSA)

• Optics Alignment (PB/PSA) • XRD-DSC Sample Alignment (PB/PSA) • XRD-DSC measurement

XRD-DSC General (2D detector) • Sample Alignment (2D detector) • XRD-DSC measurement

To run the Package measurements, you must set the conditions of each Parts individually. Described below is how to set the conditions of each Part.

CAUTION: Selecting another Package measurement or choosing another task such as the Manual Control task cancels the specified conditions. To save the specified conditions in a file, click the Export... button in each dialog box or save Package measurement conditions as described in the “Tip” in Subsection 2.3.5 (8).

2.3.1 Setting Optics Alignment Part conditions

This section describes how to set the Optics Alignment (BB) Part conditions. The Optics Alignment (PB/PSA) Part conditions are also set in the same way.

(1) Click the Optics Alignment (BB) button on the flow bar to open the Optics Alignment (BB) dialog box.

Fig. 2.3.1 Optics Alignment (BB) dialog box



(2) Uncheck the Change optics without alignment box.

Tip: Check the Change optics without alignment box when you want to switch

optics for the data measurement without running the optics alignment and by

using the alignment results stored under the selected optics alignment name.

(3) In the Optics alignment name box, select a location for storing optics alignment results.

Tip: To store optics alignment results under a new optics alignment name, click the

OK or Cancel button to close the Optics Alignment (BB) dialog box. Then,

select the Optics Alignment from the Option menu to open the Optics Alignment dialog box and add a new optics alignment name. After adding a new

optics alignment name, return to step (1) in this subsection. For more information

on creating an optics alignment name, refer to Chapter 17 of the SmartLab Guidance Reference Manual (ME13365A).

(4) To print out the optics alignment results, check the Print out results after alignment box.

Tip: If both the Change optics without alignment and Print out results after

alignment boxes are checked, the alignment results stored under the selected

optics alignment name will be printed out.

(5) Click the OK button to close the dialog box.



2.3.2 Setting XRD-DSC Sample Alignment Part conditions

This section describes how to set the XRD-DSC Sample Alignment (BB) Part conditions. The XRD-DSC Sample Alignment (PB/PSA) Part conditions are set in the same way.

(1) Click the XRD-DSC Sample Alignment (BB) button on the flow bar to open the XRD-DSC Sample Alignment (BB) dialog box.

Fig. 2.3.2 XRD-DSC Sample Alignment (BB) dialog box

(2) Select the Run recommended sequence radio button.

Tip: To confirm or set the scan conditions, etc., select the Customize conditions

radio button, then click the Customize button.

2.4.1 Customizing the XRD-DSC Sample Alignment (BB) Part conditions




2.3.3 Setting Sample Alignment (2D detector) Part conditions

This section describes how to set the Sample Alignment (2D detector) Part conditions.

Tip: Before executing Sample Alignment (2D detector) Part, execute Optics

Alignment Part, the Create Mask File Part, and the Camera Length Alignment Part. For the information on how to execute each Part, refer to the

“Optics Alignment” Part to be used, the “Create Mask File” Part , and the

“Camera Length Alignment” Part Help Topic of the online help of the SmartLab

Guidance software.

(1) Click the Sample Alignment (2D detector) button on the flow bar to open the Sample Alignment (2D detector) dialog box.

Fig. 2.3.3 Sample Alignment (2D detector) dialog box

(2) Enter the sample thickness in the Sample thickness (mm) box.

(3) Check the Direct beam half cut alignment conditions checkbox.

(4) Check the Clear omega offset and Set chi, phi=0 checkboxes.

Tip: If the result of the previous sample alignment is kept, the next sample alignment

uses this position as a reference and may not work correctly. In ordinary

cases, check the Clear omega offset and Set chi, phi = 0

checkboxes.




Tip: To confirm or set the scan conditions, etc., select the Customize conditions radio button, then

click the Customize button.

2.4.2 Customizing Sample Alignment (2D detector) Part conditions


2.3.4 Setting D/teX Detector Center Correction Part conditions

(1) Click the D/teX Detector Center Correction button on the flow bar to open the D/teX Detector Center Correction dialog box.

Fig. 2.3.4 D/teX Detector Center Correction dialog box

(2) Click the Default button. The angle at which the Si diffraction peak is detected will be set in the Theta/2-Theta position(deg) box.

Tip: If diffraction from a sample is used for the correction measurement, select the

Use diffracted beam and enter the angle at which diffraction from the sample

can be detected in the 2-theta position(deg) box. Also, if setting the scan

conditions, check the Scan conditions checkbox, and enter the scan conditions.

2.10 Sample preparation




2.3.5 Setting XRD-DSC Measurement Part conditions

(1) Click the XRD-DSC Measurement button on the flow bar to open the XRD-DSC Measurement dialog box.

Fig. 2.3.5 XRD-DSC measurement dialog box

(2) Set the folder to store the measurement data file and the name of the measurement data file in the File name box in the Save measurement data section. After completing the XRD-DSC data measurement, the measurement data will be saved as the specified file name.

1. Click the [...] button to open the Save As dialog box.

Fig. 2.3.7 Save As dialog box

2. Select the folder in the Save in and enter the file name in the File name box.

3. Click the Save button.



(3) Enter any required information in the Sample name, Reference sample name, Sample weight (mg), Atmosphere and Memo boxes (optional).

CAUTION: The information entered here will be saved to the file. There are no limits for the number of characters to be entered, but only the first 30 characters of Sample name and the first 84 characters of Memo will appear when the measurement data is printed out.

(4) In the Temperature and humidity setting box, select Varying temperature, no humidity control when not using the HUM-SL humidity generator. Select Varying temperature, humidity fixed or Temperature fixed, varying humidity when using the HUM-SL humidity generator.

(5) In the Temperature unit box, choose the desired temperature unit from deg C, F or K.

(6) Enter the start temperature and stop temperature in the Temperature range (deg C) box.


Tip: To confirm or set the scan conditions, select the Customize conditions radio

button, then click the Customize button.

2.4.3 Customizing XRD-DSC Measurement Part conditions




Tip: To save all the Part conditions set in Subsections 2.3.1 through 2.2.3 to a single

file, click the Save as button on the flow bar to open the Save As dialog box.

Enter the settings in the Save in and File name boxes, and then click the Save

button.

You can easily load conditions stored in a file by selecting the saved Package

measurement conditions file (*.sqp) shown within the box on the flow bar.

2.4 Customizing Part conditions



The user is able to set desired scan conditions and slit conditions for the XRD-DSC Sample Alignment (BB), XRD-DSC Sample Alignment (PB/PSA), and XRD-DSC measurement Parts. Use the Customize dialog box to set scan conditions and slit conditions.

Tip: To confirm the conditions set for Run recommended sequence, click the Set

recommended values button in the Customize dialog box.

2.4.1 Customizing XRD-DSC Sample Alignment (BB) Part conditions

This section describes how to customize the XRD-DSC Sample Alignment (BB) Part conditions. The XRD-DSC Sample Alignment (PB/PSA) Part conditions are set in the same way.

(1) Select the Customize conditions radio button in the XRD-DSC Sample Alignment (BB) dialog box.

(2) Click the Customize button to open the Customize dialog box.

Fig. 2.4.1 Customize dialog box



(3) If necessary, set conditions in the Direct beam half cut alignment measurement conditions and Direct beam half cut alignment measurement conditions (final conditions) sections.

CAUTION: Clicking the Set recommended values button changes settings in the Direct beam half cut alignment measurement conditions and Direct beam half cut alignment measurement conditions (final conditions) sections to recommended value for each value.

(4) After setting the conditions, click the Close button to close the Customize dialog box.


This section describes how to customize the Sample Alignment (2D detector) Part conditions.

(1) Select the Customize conditions radio button in the Sample Alignment (2D detector) dialog box.





The conditions set in the Sample Alignment dialog box are shown in the Sample information, Direct beam half cut alignment conditions, Surface normal alignment conditions sections, and Clear omega offset and Set chi, phi=0 boxes.

(3) If necessary, set the conditions in the Slit conditions, Scattering angle for alignment, Direct beam half cut alignment measurement conditions, and Surface normal alignment measurement conditions.

CAUTION: Clicking the Set recommended values button changes settings in the Slit conditions, Scattering angle for alignment, Direct beam half cut alignment measurement conditions, and Surface normal alignment measurement conditions sections to recommended values based on the values specified in the Sample information and Direct beam half cut alignment conditions. For more information, refer to “Sample Alignment Part" Help Topic of the online help section of the SmartLab Guidance software.





(1) Select the Customize conditions radio button in the XRD-DSC Measurement dialog box.



The conditions set in the XRD-DSC Measurement dialog box are shown in the DSC measurement conditions section.

(3) If necessary, set conditions in the Slit condition and XRD measurement conditions sections.

CAUTION: Clicking the Recommended measurement conditions button changes settings in the Slit condition, DSC measurement conditions, and XRD measurement conditions sections to recommended value based on the values specified in the DSC measurement conditions section. For more information, refer to “XRD-DSC Measurement Part” Help Topic of the online help section of the SmartLab Guidance software.


2.5 Preparing the DSC Attachment



2.5.1 Starting up the Bath Circulator

Tip: When you are running the measurement at temperature below room temperature,

use a Low temperature bath circulator (optional). For how to connect the Low

temperature bath circulator, refer to 2.5.3 Connecting the Low Temperature

Bath Circulator (optional).

(1) Turn ON the two power switches of the bath circulator indicated below.

(2) Confirm that "rOFF" is displayed.



2.5.2 Connecting the Humidity generator HUM-SL (optional)

When you are running a measurement in a humid atmosphere, use the Humidity generator HUM-SL.

(1) Start flowing the nitrogen gas.

(2) Connect the Transfer tube and Temperature and humidity sensor to DSC attachment.

(3) Turn ON the power switch of the Humidity generator (HUM-SL) on the side area of the generator indicated below.

Power switch

Transfer tube Temperature and humidity sensor



(4) When the Middle lamp of the Humidity generator (HUM-SL) is lit off, it means that the remaining amount of water in the tank is less than 50%. Add distilled water from the water inlet.

CAUTION: When the Upper lamp becomes lit while adding the distilled water, stop adding the distilled water immediately.

(5) Right-click Thermo Plus EVO displayed on the task bar of the Windows PC for controlling SmartLab. Select Open the dialog.

(6) Select No in the Feedback control of Current value indication dialog box, and then click the Set button.

CAUTION: Do not set high value for Humidity at this point. Dew condensation may occur when placing the sample.

(7) Enter the value 2 degrees C higher than the measurement steam temperature planned to set into the Bath circulator temp. box, and then click Set. For example, enter 57 degrees C when you plan to set the measurement steam tempeature to 55 degrees C.

Upper lamp Middle lamp



(8) Enter the value 10 degrees C higher than the measurement steam temperature planned to set into the Water tank temp. box and Transfer tube temp. box, and then click Set. For example, enter 65 degrees C when you plan to set the measurement steam tempeature to 55 degrees C.

(9) Enter the value 10 degrees C higher than the Rubber heater temperature (which is determined from the Rubber heater temp. rough indication graph) into the Rubber heater temp. box, and then click the Set button. For example, enter 80 + 10 = 90 degrees C when the measurement steam temperature is 55 degrees C.

Tip: It takes a while for the steam temperature to rise because the whole furnace needs

to be heated up by the rubber heater (temperature rises at the rate of

approximately 1 degrees C/minute).

(10) When the current steam temperature becomes 10 degrees C lower than the measurement steam temperature you plan to set, enter the rubber heater temperature into the Rubber heater temp. box. The rubber heater temperature should correspond with the measurement steam temperature you plan to set. (For example, enter 80 degrees C when you plan to set the measurement steam temperature to 55 degrees C.) Then, click the Set button.

CAUTION: The rubber heater cools down on its own. Therefore, it remains hot for awhile even after entering a lower value in the Rubber heater temp. box.

ラバーヒータ温度目安

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

80.0

90.0

100.0

20 25 30 35 40 45 50 55 60

蒸気温度℃

ラバ

ーヒー

タ温

度℃

Rubber heater temp. rough indication graph

Humidity temp. (deg C)

Rub

ber

heat

er te

mp.

(deg

C)



(11) When the steam temperature becomes stable at the planned measurement steam temperature, the measurement preparation is completed.



2.5.3 Connecting the Low Temperature Bath Circulator (optional)

When you are running a measurement at temperature below room temperature, use a Low Temperature Bath Circulator (F81-HL).

(1) Start flowing the nitrogen gas.

(2) Connect the Low Temperature Bath Circulator (F81-Hl) and tube of nitrogen gas to DSC attachment.

(3) Connect the flow meter to the DSC attachment and flow the nitrogen gas at the rate of 100ml/min.

Nitrogen gas

Low Temperature Bath Circulator (F81-HL)



(4) Turn ON the two power switches of the Low Temperature Bath Circulator (F81-HL) indicated below. Confirm that "rOFF" is displayed.


(6) Confirm that No is selected in the Current value of Humidity control in the Current value indication dialog box.

(7) Enter "30.0" in Rubber heater temp. and click Set.

(8) Enter "25.0" in Target temp., "3.0" in Heating (Cooling) rate, "0" in Holding time, and click Set.

(9) Enter "-80.0" in Bath circulator temp. and click Set. When the bath circulator temperature decreases to the range from -65.0 to -70.0 degrees C, the measurement preparation is completed.

Tip: It requires approximately an hour and a half for the low temperature bath

circulator (F81-HL) to reach -65.0 degrees C from room temperature.



2.6 Running Package measurement

Described below is the procedure for running the measurement operations in series from start to end when the XRD-DSC General (BB) D/teX Package measurement is selected; which is from the optics alignment to the XRD-DSC measurement. Measurement can be run in the same way when the XRD-DSC General (medium resolution PB/PSA) Package measurement is selected (However, skip the steps (14) to (18)).

Tip: When you are running only a single Parts measurement (either optics alignment,

sample alignment, D/teX detector center correction measurement, or XRD-DSC

measurement), refer to 3. Executing Each Parts.

(1) Click the (Show confirmation messages) button once to switch it to (Don’t show

confirmation messages).

Tip: To confirm the optics alignment results or to show the message to verify that each

Part has been completed, set the button to (Show confirmation messages).

(2) Click the Run button on the flow bar.

Tip: After running a Package measurement, the ● mark appears on the button of the

flow bar. This ● mark indicates that the Part measurement corresponding to the

button is in progress.



(3) If the following message appears, click the No button.

CAUTION: If the current hardware configuration setting is different from that for the operation of the XRD-DSC General (BB) D/teX Package measurement, the measurement will be aborted and the Hardware Configuration dialog box will open. If this happens, replace the configuration units (e.g., the attachment) as prompted by the message in the dialog box.

2.7 Changing configuration units

(4) A message will prompt you to replace optical devices while the measurement is running. Confirm the message and click the OK button.



(5) The following message will appear. Follow the message and place the height reference sample plate on the attachment. If another message appears and prompts you to replace the optical device(s) such as the selection slit at the same time, replace and mount the specified optical device(s) as indicated by the message.

Tip: If you check the Hide figures box, only the message will be displayed within the

message box without figures.

Tip: Execute the optics alignment without the standard receiving optical unit # 1 when

using D/teX Ultra in the one dimensional mode. Move the receiving slit box # 2

and attenuator to the left side, and install the detector adapter to the theta_d arm

so that the mark on the detector adapter is positioned at 351 mm on the scale of

the theta_d arm.

(6) Click the OK button to run the optics alignment. The optics alignment will be done under the recommended conditions. The sample alignment will be completed in about 10 minutes.



(7) The procedure to take in this step differs depending on whether the setting is or on

the flow bar. Follow the directions given below.

When (Don’t show confirmation messages) is set:

The optics alignment results will be registered in the optics management database.

When (Show confirmation messages) is set:

1. The following message will appear to verify that the optics alignment has been completed. Click the OK button.

2. The Optics Alignment Results dialog box will appear. Confirm the results and click the Register button. The optics alignment results will be registered in the optics management database.

CAUTION: Clicking the Do not register button sets the zero offset value for each axis, but does not register the optics alignment results in the optics management database.



Tip: After the optics alignment is completed, the ● mark indicated on the Optics

Alignment (BB) button on the flow bar moves to the XRD-DSC Sample Alignment (BB) button.

(8) The Hardware Configuration dialog box with the message "Attachment: Change Standard to DSC" will appear. Follow the steps described below to mount the DSC Attachment.

1. Use the supplied tool (hex key) to remove the standard attachment, and then mount the DSC attachment. Tighten (loosen) the screw on the left side of each attachment with the supplied tool (hex key) to mount or remove the attachment.



2. Connect the cable.

3 Click the Update button in the Hardware Configuration dialog box.

4 Confirm that the message "Hardware check OK. Resume the measurement." is displayed,

and click Close to close the Hardware Configuration dialog box.

Cables connected



(9) Restart the Package measurement which has been aborted to change the attachment. Click the XRD-DSC Sample Alignment (BB) button on the flow bar. Then, click the OK or Cancel button in the XRD-DSC Sample Alignment (BB) dialog box displayed to close the dialog box.

(10) Click the Run button on the flow bar. The following message will appear, then click the Yes button.

(11) A message will prompt you to replace optical devices while the measurement is running. Confirm the message and click the OK button.



(12) The following message will appear.

1. Use the supplied tool (cross handle driver) to loosen the two screws of the outer cover (top

jacket) of DSC attachment.

2. Shift the outer cover (top jacket) in clockwise direction and remove it. Then, remove the silver lid (inside cover).

Silver lid

Outer cover



3. Place the sample aluminum pan for sample alignment on the right part of the thermosensitive plate (heating plate). Do not place anything on the left part.

Tip: It is unnecessary to place back the silver lid (inside cover) and outer cover (top

jacket).

4. If another message prompts you to replace the optical device(s) such as the length limiting slit at the same time, install the specified optical device(s) as indicated by the message.

(13) Click the OK button to run the sample alignment. The direct beam half cut alignment will be done under the recommended conditions. The sample alignment will be completed in about 5 minutes.

Only when (Show confirmation messages) is set on the flow bar, a message will appear to

verify that the sample alignment has been completed. Click the OK button.

.



Tip: After the optics alignment is completed, the ● mark indicated on the

XRD-DSC Sample Alignment (BB) button on the flow bar moves to the D/teX Detector Center Correction button.

(14) When the XRD-DSC Sample Alignment (BB) is completed, the following message will appear. Follow the message and confirm that the mark of the detector adapter is positioned at 351 mm on the scale of the theta_d arm.

Receiving parallel slit adapter (RPS adapter)

Receiving slit box # 2

Attenuator

D/teX Ultra



(15) Click the OK button to run the center correction measurement.

Tip: After the center correction is completed, the ● mark indicated on the D/teX

Detector Center Correction button on the flow bar moves to the XRD-DSC Measurement button.

(16) The following message will appear. Follow steps 1 through 5 to place the sample. Also, follow the message to insert the specified manual exchange slit.

1. Remove the jig for Al2O3 peak measurement on the right part of the thermosensitive plate (heating plate). Then, place the aluminum pan with the measurement sample filled on the right part of the thermosensitive plate (heating plate).

While taking this step, place the measurement sample pan so the lip on the both sides of the aluminum pan with the samples faces the front and rear side of the equipment.



2. Place an aluminum pan with the aluminum lid as the reference sample on the left part of the thermosensitive plate (heating plate).

3 Place the silver lid (inside cover) so the aluminum window faces the left and right side of the equipment.

4. Place the outer cover (top jacket) so it is shifted a little in clockwise direction. Rotate it in

counterclockwise direction to attach it.

5. Use the supplied tool (cross handle driver) to tighten the two screws of the outer cover (top jacket) of DSC attachment to fix it to the DSC attachment.



(17) Click the OK button to run the XRD-DSC Measurement. The XRD-DSC measurement will be run under the specified conditions.

Tip: When you click on the X-ray profile, temperature profile, and DSC profile, the

corresponding area will be highlighted. For more information, refer to Chapter 6

of the SmartLab Guidance Reference Manual (ME13365A).

(18) After the XRD-DSC data measurement is completed, the measurement data will be saved with

the file name specified in section 2.3.5 (2).

Only when (Show confirmation messages) is set on the flow bar, a message will appear to

verify that the XRD-DSC measurement has been completed. Click the OK button.

This is the end of the XRD-DSC General (BB) D/teX Package measurement.




After running the Package (or Part) measurement, if the hardware configuration is not set for the Package (or Part) measurement, the Hardware Configuration dialog box will open. A message appears below the dialog box prompting you to change the configuration units which prevents the Package (or Part) measurement to run.

For example, if the DSC attachment is mounted, since the optical alignment parts for XRD-DSC General (BB) D/teX or XRD-DSC General (PB/PSA) Package measurement is only available with attachments other than the DSC attachment, the following message will appear: " Attachment: Change DSC to XY-20mm. ".

CAUTION: The Package (or Parts) measurement is aborted when the Hardware Configuration dialog box appears.


Change the configuration units as prompted by the message in the dialog box and update the contents of the Hardware Configuration dialog box.

The procedures are described below.

(1) Remove the DSC attachment cable.



(2) Use the supplied tool (hex key) to loosen the screw on the left side of DSC attachment, and then remove the DSC attachment.

(3) After mounting the standard attachment, tighten the screw on the left side with the supplied tool (hex key).

(4) Connect the standard attachment cable.

(5) If necessary, make changes to the Incident optics, Receiving optics, and Detector.

(6) Click the Update button in the Hardware Configuration dialog box.

(7) Confirm that the Hardware Configuration dialog box displays the message “Hardware check OK. Resume the measurement.”, and hen click the Close button.

CAUTION: To run the measurement again, click the Run button on the Package Measurement flow bar or the Run button in the applicable Part dialog box.

2.8 Removing the DSC Attachment



Follow the steps from 2.8.1 to 2.8.4 described below to remove the DSC Attachment.

2.8.1 Setting each temperature back to room temperature


(2) Select No in the Feedback control of Current value indication dialog box, and click Set.

(3) When using the Humidity generator (HUM-SL), select No in the Humidity control, and click Set.

(4) Enter "20" in Target temp., "10" in Heating (Cooling) rate, and click Set.

(5) Enter "20" in Rubber heater temp. and click Set.

(6) When using the Humidity generator (HUM-SL), enter "20" in Bath circulator temp., Water tank temp., and Transfer tube temp., and click each Set button.

Check the current value of each temperature and wait until each temperature returns to approximately room temperature.



2.8.2 Turning OFF the Low Temperature Bath Circulator(optional)

When using the Low Temperature Bath Circulator (optional), follow the steps below to turn OFF the power.

(1) Shut the valve of the nitrogen gas.

(2) Disconnect the Low Temperature Bath Circulator (F81-HL) and the tube of nitrogen gas from the DSC attachment.

(3) Turn OFF the two power switches of the Low Temperature Bath Circulator (F81-HL) indicated below.

Low Temperature Bath Circulator (F81-HL)



2.8.3 Disconnecting the Humidity generator HUM-SL (optional)

When using the humidity generator HUM-SL (optional), follow the steps below to disconnect it from the DSC attachment.

(1) Shut the valve of the nitrogen gas.

(2) Disconnect the Transfer tube and Temperature and humidity sensor from the DSC attachment.

(3) Turn OFF the power switch on the side of the Humidity generator (HUM-SL) indicated below.

Power switch

Transfer b

Temperature and humidity sensor



2.8.4 Turning OFF the Bath Circulator(optional)

Tip: When using the Low Temperature Bath Circulator (optional), refer to 2.8.2

Turning OFF the Low Temperature Bath Circulator(optional).

(1) Turn OFF the two power switches of the bath circulator indicated below.

When the steps above are completed, the DSC Attachment can be removed from the standard Z stage.

2.9 Shutting down the X-ray generator


2.9 Shutting down the X-ray generator

After all measurements are completed, follow the steps below to turn off the x-ray generator.

(1) Click the Shutdown... button on the flow bar to open the Shutdown dialog box.

(2) Uncheck the Execute box.

Fig. 2.7.1 Shutdown dialog box

(3) Select XG Off in the XG set box.

(4) Click the Execute button.

(5) The x-ray generator will be turned off in about 10 minutes.

Tip: For other functions available in the Shutdown dialog box, refer to Chapter 21 of

the SmartLab Guidance Reference Manual (ME13365A).




When running an XRD-DSC sample measurement, an aluminum pan for XRD-DSC is used to fill the powder measurement sample.

Also, an empty aluminum pan for XRD-DSC or a sample with the specific heat very close to the measurement sample is used as the reference sample.

Set the reference sample on the left part of sample position. Set the measurement sample on the right part of the sample position.

When filling the sample, it is necessary to flatten the sample.

The following section describes how to fill the sample.

2.10.1 When using powder sample

(1) Weigh an empty aluminum pan for XRD-DSC.

(direction of X-ray radiation)

Thermosensitive plate

Lips of aluminum pan for XRD-DSC (place it parallel to the long side of thermosensitive plate)



(2) Place the weighed empty aluminum pan for XRD-DSC on the sample filling jig.

(3) Use a micro spatula to fill the sample to aluminum pan for XRD-DSC.

CAUTION: When the sample sticks on the rear side of sample pan, it may cause deformation of the sample pan, a smear on the thermosensitive plate (heating plate), or error due to sample displacement.

(4) Hold the lip of the aluminum pan for XRD-DSC with tweezers. Remove extra powder

sample by using the flat side of the supplied micro spatula and flatten the powder sample.

Sample filling jig

Aluminum pan for XRD-DSC

Sample

Micro spatula

Sample filling jig

Sample Micro spatula

Aluminum pan for XRD-DSC

Place the aluminum pan for XRD-DSC so its lips are vertical to the long side of the groove of the sample filling jig

Aluminum pan for

XRD-DSC Sample filling jig



(5) Weigh the aluminum pan for XRD-DSC filled with sample. Calculate the difference between the empty aluminum pan for XRD-DSC weighed in step (1). The difference will be the sample weight.

2.10.2 When using plate sample

When using a plate sample, the sample is cut into squares the size of 6.5 to 6.7 mm and is placed on the aluminum pan for XRD-DSC.

CAUTION: Samples such as polymer film, which curves due to heat, can reduce the curve by folding the edge. However, when you are using the sample auto changer (SmartLoader), you cannot fold the edge of the aluminum pan for XRD-DSC.

3.1 Executing Optics Alignment Part


3. Executing Each Parts

This chapter describes how to execute the following each Parts.

Optics Alignment (BB) Part

XRD-DSC Sample Alignment (BB) Part

Sample Alignment (2D detector) Part

D/teX Detector Center Correction Part

XRD-DSC Measurement Part

3.1 Executing Optics Alignment Part

This section describes how to execute the Optics Alignment (BB) Part. The Optics Alignment (PB/PSA) Part conditions are executed in the same way.

(1) Click the Optics Alignment (BB) button on the flow bar to open the Optics Alignment (BB) dialog box.

Fig. 3.1.1 Optics Alignment (BB) dialog box

(2) Uncheck the Change optics without alignment box.

Tip: Check the Change optics without alignment box to switch optics for the data

measurement without executing the optics alignment and by using the alignment

results stored under the selected optics alignment name.



(3) In the Optics alignment name box, select a location for storing optics alignment results.

Tip: To store optics alignment results under a new optics alignment name, click the

OK or Cancel button to close the Optics Alignment (BB) dialog box. Then,

select the Optics Management from the Option menu to open the Optics Management dialog box and add a new optics alignment name. After adding a

new optics alignment name, return to step (1) in this subsection. For more

information on adding an optics alignment name, refer to Chapter 17 of the

SmartLab Guidance Reference Manual (ME13365A)

(4) To print the optics alignment results, check the Print out results after alignment box.

Tip: If both the Change optics without alignment and Print out results after

alignment boxes are checked, the alignment results stored under the selected

optics alignment name will be printed out.

(5) Click the Execute button in the Optics Alignment (BB) dialog box.

(6) Execute the optics alignment by following step (5) through (7) in Section 2.6.

CAUTION: If the current hardware configuration setting is different from that for the operation of the Optics Alignment (BB) Part, the measurement will be aborted and the Hardware Configuration dialog box will open. If this happens, replace the configuration units (e.g. attachment) as prompted by the message in the dialog box.


3.2 Executing XRD-DSC Sample Alignment Part


3.2 Executing XRD-DSC Sample Alignment Part

This section describes how to execute the XRD-DSC Sample Alignment (BB) Part. The XRD-DSC Sample Alignment (PB/PSA) Part is executed in the same way. For information on XRD-DSC Sample Alignment (2D Detector) Part, refer to the manual of XRD-DSC Sample Alignment (2D Detector) Part.

(1) Click the XRD-DSC Sample Alignment (BB) button on the flow bar to open the XRD-DSC Sample Alignment (BB) dialog box.

Fig. 3.2.1 XRD-DSC Sample Alignment (BB) dialog box

(2) To print out the sample alignment results, check the Print alignment result box.




2.4.1 Customizing the XRD-DSC Sample Alignment (BB) Part conditions

(4) Click the Execute button in the XRD-DSC Sample Alignment (BB) dialog box.

(5) Execute the sample alignment by following step (12) through (13) in Section 2.6.

CAUTION: If the current hardware configuration setting is different from that for the operation of the XRD-DSC Sample Alignment Part, the sample alignment will be aborted and the Hardware Configuration dialog box will open. If this happens, replace the configuration units (e.g., the attachment) as prompted by the message in the dialog box.




3.3 Executing Sample Alignment (2D detector) Part

(1) Click the Sample Alignment (2D detector) button on the flow bar to open the Sample Alignment (2D detector) dialog box.

Fig. 3.3.1 Sample Alignment (2D detector) dialog box

(2) Enter the sample thickness in the Sample thickness (mm) box.

(3) Check the Direct beam half cut alignment conditions checkbox.

(4) Check the Clear omega offset and Set chi, phi=0 checkboxes.

Tip: If the result of the previous sample alignment is kept, the next sample alignment

uses this position as a reference and may not work correctly. In ordinary cases,

check the Clear omega offset and Set chi, phi = 0 checkboxes.





(6) Click the Execute button in the Sample Alignment dialog box.

(7) Execute the sample alignment by following step (10) through (13) in Section 2.6.

3.4 Executing D/teX Detector Center Correction Part


3.4 Executing D/teX Detector Center Correction Part

(1) Click the D/teX Detector Center Correction button on the flow bar to open the D/teX Detector Center Correction dialog box.

Fig. 3.4.1 D/teX Detector Center Correction dialog box

(2) Click the Default button. The Use direct beam radio button will be selected in the Peak measurement conditions section.

Tip: If diffraction from a sample is used for the correction measurement, select the

Use diffracted beam and enter the angle at which diffraction from the sample

can be detected in the 2-theta position(deg) box. Also, if setting the scan

conditions, check the Scan conditions checkbox, and enter the scan conditions.


(3) Click the Execute button in the D/teX Detector Center Correction dialog box.

(4) Execute the D/teX detector center correction measurement by following step (14) through (15) in Section 2.6.

CAUTION: If the current hardware configuration setting is different from that for the operation of the D/teX Detector Center Correction Part, the D/teX detector center correction measurement will be aborted and the Hardware Configuration dialog box will open. If this happens, replace the configuration units (e.g., the attachment) as prompted by the message in the dialog box.




3.5 Executing XRD-DSC Measurement Part

(1) Click the XRD-DSC Measurement button on the flow bar to open the XRD-DSC Measurement dialog box.

Fig. 3.5.1 XRD-DSC measurement dialog box

(2) Set the folder to store the measurement data and the name of the measurement data file in the File name box in the Save measurement data section. After the XRD-DSC data measurement is completed, the measurement data will be saved with the specified file name.

1. Click the [...] button to open the Save As dialog box.

Fig. 3.3.2 Save As dialog box

2. Enter the settings in the Save in and File name boxes.

3. Click the Save button.

3.5 Executing XRD-DSC Measurement Part


(3) Enter any required information in the Sample name and Memo boxes (optional).

CAUTION : The information entered here will be saved to the file. Any number of characters may be entered, but only the first 30 characters of the sample name and the first 84 characters of the memo will appear on the measurement data printed out.

(4) In the Temperature and humidity setting box, select Varying temperature, no humidity control when not using the HUM-SL humidity generator. Select Varying temperature, fixed humidity when using the HUM-SL humidity generator.

(5) In the Temperature unit box, choose the desired temperature unit from deg C, F or K.

(6) Enter the start temperature and stop temperature in the Temperature range boxes.


Tip: To confirm or set the scan conditions, select the Customize conditions radio

button, then click the Customize button.


(8) Click the Execute button in the XRD-DSC Measurement dialog box.

(9) Execute the XRD-DSC measurement by following step (16) through (18) in Section 2.6.

CAUTION: If the current hardware configuration setting is different from that for the operation of the XRD-DSC Measurement Parts, the measurement will be aborted and the Hardware Configuration dialog box will open. If this happens, replace the configuration units (e.g., the attachment) as prompted by the message in the dialog box.



4. Troubleshooting

Problem Solution Previously saved conditions cannot be imported through the Optics Alignment (BB) / Optics Alignment (PB/PSA) dialog box.

• Confirm that the user name displayed on the title bar of the main window is correct.

• Add the name of the optics alignment again in the Optics Management dialog box.

Previously saved conditions cannot be imported through the XRD-DSC Sample Alignment (BB) / XRD-DSC Sample Alignment (PB/PSA) dialog box.


Previously saved conditions cannot be imported through the D/teX Detector Center Correction dialog box.


Previously saved conditions cannot be imported through the XRD-DSC Measurement dialog box.


Package measurement cannot be run.

• Check to see if the XG output has reached the specified level. • Check to see if the door of the radiation enclosure is closed.

When optics alignment is executed, the goniometer moves slightly and the operation immediately stops.

• Confirm that the Change optics without alignment box in the Optics Alignment (BB) / Optics Alignment (PB/PSA) dialog box is unchecked.

The same message box appears even after clicking the OK button.

• Confirm that the specified slit and other devices are installed correctly. Also, make sure that the necessary devices have not been removed.

Sufficient intensity cannot be obtained for measurement.

• Check to see if an absorber is not inserted in the receiving slit box.

• Confirm that the XG output has reached the specified level. • Measure the Si powder sample (Si powder reference sample)

using the Run recommended sequence mode and check the intensity.

xrd-dsc general (bb) d/tex package measurement xrd … · 2.10.2 when using plate sample ... user...

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