Siroquant Version 3 User Manual
Published by:
Sietronics Pty Limited
Unit 3/22 Walder St
PO Box 3066
Belconnen ACT 2616
Email: spl@https://www.doczj.com/doc/cc11601090.html,.au
Web: https://www.doczj.com/doc/cc11601090.html,.au
Copyright ? 2007 Sietronics Pty Limited. All rights reserved. First edition: December 2006, minor revisions, March 2007.
Siroquant Version 3 User Manual
Table of Contents Introduction (1)
Manual Overview: (1)
Manual Conventions: (1)
1.Siroquant Overview (2)
1.1Software Description (2)
1.2Siroquant Objectives (2)
1.3.Software License, Trademark and Copyrights (2)
1.4Computer Specifications (2)
1.5Installation Instructions (3)
1.6Folders (4)
2.Siroquant Files (5)
2.1Task Files (*.TSK files) (5)
2.2Task Option File (5)
2.3Data Files (various types) (5)
2.4Databases and Databanks (6)
2.4HKL files (6)
3.Siroquant User Interface (9)
3.1Main Application Window (9)
3.2Task Display (10)
3.3Main Application ToolBar (12)
4.Basic Level Operations (16)
4.1Preparing Calculated *.HKL Files (16)
4.2Preparation of An Analytical Task (18)
4.3Task Parameters Dialog (21)
4.4Phase Dependent Parameters Dialog (23)
4.5Stage Control and Refinement dialog (26)
4.6Background Refinement dialog (28)
4.7Background Subtract dialog (29)
4.8Excluded Regions form (31)
4.9Calibration form (32)
4.10Advanced Halfwidths (33)
4.11Editing the Current Task (35)
4.12Starting a refinement (38)
4.13Displaying hkl Bars (38)
4.14HKL Bar Palette (39)
4.15Quantitation Results (40)
4.16Quantitation Charts (41)
4.17Refinement Statistics χ2 (42)
4.18Overview of Intermediate level features (43)
4.19Overview of Advanced level features (44)
5.Intermediate Level Operations (45)
5.1Extra Display Features (45)
5.2Template Tasks (46)
5.3New Task Wizard (48)
5.4Phase Status (52)
5.5Phase Preview (52)
5.6Print Out (54)
5.7Calculate Menu Functions (56)
5.8Long Results Dialog (58)
5.9Phase Profiles (58)
5.10Information Menu (59)
5.11Options (61)
5.12Verify Task Phases (64)
6.Advanced Level Operations (65)
6.1Tools Menu (65)
6.2Advanced hkl Preparation (65)
6.3Refinement History (65)
6.4Overlay Scan (66)
6.5Refinement Extras (66)
6.6Search Match (67)
6.7Composition Analysis (67)
6.8Brindley Trials (67)
7. A step by step guide to quantifying a sample: (69)
Introduction
Siroquant Version 3.0 is an integrated 32-bit program for use with 32 bit Windows
operating systems and modern PCs. All the elements of the previous 16 bit Windows
interface and the Fortran calculation programs have been merged into a single application
and the entire program has been rewritten into a new programming language.
Siroquant Version 3.0 incorporates new features requested previously but which could not
be incorporated because of programming language constraints. It also has new ways of
doing some operations, mainly because it is now a fully integrated program and better
software controls are now available. There are more user settable options in version 3
than were previously available. The initial default values for these are consistent with
version 2.5 as far as practical.
Manual Overview:
This manual is divided into seven chapters:
? Chapter 1 contains basic information on the program, copyright and installation
instructions.
? Chapter 2 contains information on the various files used by the program.
? Chapter 3 contains information on the user interface.
? Chapter 4 has a description of the basic operations needed to use version 3
effectively.
? Chapter 5 contains a detailed description of the intermediate operations of
Siroquant.
? Chapter 6 contains a detailed description of the advanced operations of Siroquant.
? Chapter 7 contains a description of the process of analyzing a sample using the
quartz/zincite demo scan.
Manual Conventions:
Icons are used in this manual to identify various types of information as follows:
Significant differences between version 3 and previous versions with
an explanation of the difference between the versions for the benefit of
Siroquant users familiar with previous versions.
Useful hints
1. Siroquant Overview
1.1 Software
Description Siroquant Version 3.0 is written for Quantitative Phase Analysis from X-ray Powder Diffraction Patterns of mixtures of solid phases such as found in many scientific and industrial applications. It is compatible with Microsoft Windows XP, 2000 and NT. Version 3.0 is a fully integrated 32-bit application (or program) with a Multi Document Interface (MDI) style user interface. The application has been written in Delphi 6 and uses the TeeChart control for all graphics support.
The software principally uses the “Rietveld” technique. The 32 bit extended DOS programs TRACSCAL, PREP & STRUCT and the 16-bit SQWIN interface have now been integrated into one 32-bit program.
The MDI style interface now allows more than one task to be open at
the same time. Working files are handled very differently to earlier
versions. 1.2 Siroquant Objectives
Sietronics is committed to the long-term development and support of Siroquant. Our
objective is to continue to develop the software to be as scientifically accurate as the
powder XRD technique will allow, while retaining its user-friendliness and suitability for
accurate solid phase analysis.
1.3. Software License, Trademark and Copyrights
The use of copies of the Siroquant? software is limited to purchasers of copies with the
WIBU protection device that is required to operate the software.
Windows is the registered trademark of Microsoft Corporation. Copyright (c) 1985-2007
Microsoft Corp.
WIBU is the registered trademark of WIBU Systems AG. Copyright ? 2007 Wibu
Systems AG.
Siroquant? is the registered trademark of CSIRO Australia.
Delphi is a registered trademark of Borland Software Corporation.
TeeChart is a registered trademark of Steema Software.
Adobe Acrobat is the registered trademark of Adobe Systems Incorporated.
Manual Contents Copyright (c) 1988-2007 Sietronics Pty Ltd. All Rights Reserved.
1.4 Computer Specifications
A Pentium III PC with at least 256 megabytes of RAM, recommended is a Pentium IV 2
GHz (or better) with 512 megabytes of RAM. Extra memory may be needed if multiple
tasks analyzing patterns with many step points or with many phases are open at the
same time. Windows 98, NT, 2000 or XP are required for operation. The minimum
screen resolution required is 800 X 600 (1024 x 768 or better is recommended) and a
CD-ROM drive is required for the installation of the software. The computer must have
either a spare USB port or a parallel port for the dongle.
The program is compatible with dual monitor displays (e.g. 1600 x 600). The program
can also take advantage of computers with multiple processors, dual core processors or
single processors with hyper-threading.
Important notes:
?
If you are using the Windows XP, 2000 or Windows NT operating systems, you will
need to be logged in with administrative privileges to install the dongle driver. ? If you are using the Windows NT or Windows 98 operating systems, you may need to
install the ADO driver to utilize the database. Please check the Microsoft website
(https://www.doczj.com/doc/cc11601090.html,) and search for the “MDAC Redistributable” for the latest
release and install this.
? If you have an Iomega Zip drive located on the parallel port, place the dongle after
the zip drive. You should also not try to access Siroquant files (task, scan or HKL
files) from the Zip drive, as the dongle will not work properly under these
circumstances.
?
If you have a printer attached to the PC working in bi-directional mode, you may need
to have this printer switched on for the dongle to operate correctly. 1.5.2 WIBU Dongle
A correct dongle must be present at all times on the computer on which Siroquant Version
3 is running. The program will not start without the dongle present and if the dongle is
removed while the program is running, the program may terminate. Siroquant v3 may be
installed on as many computers as desired but only one computer can run it at any one
time with only one dongle. If additional licenses are required, please contact Sietronics.
If you do use more than one computer with one dongle ensure that
Siroquant v3 is closed before removing the dongle. It may be easier to
connect USB dongles via an extension cable on each computer.
1.5.3 Manuals on CD-ROM
The full text of the manuals is available on the installation CD-ROM in the “Manuals”
folder. The manuals include this manual, Technical, Clay and File Formats manuals. The
latest version of the Adobe Acrobat ? reader software is also available on the CD-ROM.
The manuals can also be viewed from inside the program’s user interface as well.
1.5.4 Siroquant Updates
An Internet web page has also been established for the download of program updates.
This is designed to ensure that users keep up to date with the latest version of the
program. The web address is:
https://www.doczj.com/doc/cc11601090.html,.au/siroquant
The Internet address for updates can also be called from the Help Menu within Siroquant.
1.6 Folders
Depending on the installation parameters used, the installation program will have created
a directory structure similar to that shown below. The default installation folder is
“C:\Program Files\Siroquant\v3” and is recommended. An alternative folder may be
specified when installing Siroquant. The main installation folder has various subfolders.
These folder names must not be changed or deleted.
Note: The terms ‘folder’ and ‘directory’ are the same in Siroquant the former being the
latest used by Microsoft.
Because Version 3.0 is a 32 bit application it fully supports long file
names including folder names. Users should avoid the use of
extensions in folder names or file names with more than one
extension, that is two or more periods. 1.6.1 \Database
This folder holds the registered database including the Standard database “Quantlib
v3.mdb”. User databases are pairs of database (.mdb) and databank (.dat) files. An
example user database Quantv3.mdb & Quantv3.dat is supplied. The subfolder
“\Templates ” contains an Access database file that is used as a template for user
databases and “\Removed ” contains any user database removed from the parent folder
(under control of supplied software).
1.6.2 \Output Templates
This folder contains text template files for formatting output when printing results.
1.6.3 \Manuals
This folder holds the manuals as .pdf files.
1.6.4 \Display Settings
This folder is not currently used.
1.6.5 \Examples
This folder and its subfolders contain various examples for use with version 3. The user should create their own folders for storage of user task files and HKL files.
2. Siroquant Files
2.1 Task Files (*.TSK files)
Task files are the ‘document’ files of Siroquant. After installation ‘opening’ a task file in
Explorer will open Siroquant and the task file just like opening a .doc file opens Microsoft Word. Task files contain information necessary for the analytical task, most importantly the scan to be analysed, the phases to be quantified and refinement data. Task files are text files arranged in a similar way to an .ini type file. Long file names are allowed for tasks. The characters ampersand (‘&’) and hash (#) should be avoided in task file names as they are for special use in Siroquant. Tasks have a version number that is found on the first line of the task and for version 3 it is 10005.
Task files in version 3 have a different format to earlier versions
(10003 & 10004). When version 2.0 and Version 2.5 task files are
opened they will be automatically converted to Version 3 task files and
‘v3’ will be added to their name part of the file name. 2.1.1 Template tasks
Template tasks can be set up to provide a common starting point for similar analyses.
They have the same format as a task file but their extension is .tmk and version number is
20005. A task file and a template task file must not have the same name in a folder.
Template tasks are further discussed in Section 5.2.
2.1.2 Ancillary Task Files Tasks will have extra files associated with them for extra information associated with a task. These are described in detail in the File Formats manual and they will be mentioned elsewhere in this manual. They have extensions .cps, .cpd, .cpk and .nnn where n is 0 to 9. They are always placed in the same folder as the task.
In earlier versions of Siroquant various intermediate files were
generated during a refinement and were overwritten by every
refinement whether it was the same or different task. The equivalent
of some of these are now included in the ancillary files. Also the
calculated pattern, the background profile and the difference pattern files now have the same name as the task and not necessarily the same as the pattern. This is all a consequence of Siroquant v3’s being able to have open and refine more than one task at a time. 2.2 Task Option File One of the ancillary files is an .ini type file (extension .998) that is used to save various information and options related to the task. What is saved and how it is used can depend on how options have been set.
An example of one these options is that every task maintains its own
hkl options and hkl colors. 2.3 Data Files (various types)
XRD analysis begins with an XRD pattern collected as (preferably) a step scan from an
automated XRD instrument. The raw data files from most common diffractometer
software packages can be read by SQv3. When a task is set up the raw data file is
specified into the task and, if necessary, is converted into a ‘.cpi format. This is called the
‘original’ pattern.
The original pattern may be calibrated and can have the background subtracted. These
result in the ‘active’ pattern with extensions of either .cpc or .cpb. An alternative to
subtracting the background is to use background refinement; either method may be
appropriate depending on the pattern type. The ‘active’ pattern is the pattern used for
refinement.
In earlier versions all raw data files were automatically converted to
*.cpi format (which is easy to read or edit) but in Version 3 this is only
done if the raw data file has or is capable of storing more than one
pattern or if extra information not present in the raw data file is
required. A cpi format file can be saved by selecting the Save Scan
action and then ‘Original Scan’.
The term ‘active scan’ in version 3 refers to the scan that is used in the
refinement. 2.4 Databases and Databanks
Databanks are files (.dat) that hold crystallographic data for phases. Phases are the
components of a sample that will be will quantified. Microsoft Access databases (.mdb)
are used to hold further information about the phases. These databases are used by
Siroquant for the selection of the phases to form part of the task.
2.4.1 Standard Database
A Standard Database (“C:\Program Files\Siroquant\v3\Database\Quantlib v3.mdb”) with
over 1500 phases is provided as part of Siroquant v3. There is no corresponding
databank file (.dat) because the crystallographic data is stored inside the database itself.
Version 2.0 and 2.5 databases can be converted using “ConvertToV3.exe”. This program can also be started from the Tool
menu using the “Convert v2 & v2.5 Database to v3” menu item.
2.4.3 Example User Database
The files “Quant v3.mdb” and “Quant v3.dat” contain the first 300 phases of the standard
databank. This is the databank that was available with version 2.0.
database can be specified directly in the task in which case the equivalent of an hkl file is
generated each time the task is opened*. HKL files are text based files. The version 3 hkl
file (10005) is in an .ini style format. Version 2 & 2.5 hkl file (other than the Clay Pack
files) are compatible. HKL files basically consist of phase parameters and the reflections
for the phase.
* This has been made possible by the integration of the previous DOS programs and by
faster modern computers.
2.4.1 Observed HKL Files
Siroquant is able to substitute F o (hkl) for F c (hkl) in the Rietveld calculation allowing
quantification of phases for which there is no published crystal structure. Observed *.hkl
files have been prepared for many common clays which have very disordered and ill-
defined structures. These are included in the Standard database and are specified in the
companion “Clay Package Manual”. The Siroquant user cannot prepare (hkl) files from
the structure database for these structurally disordered mineral phases; these are already
supplied for use with Siroquant. In version 3 supplied observed HKL files are included in
the Standard database. Also non-Clay Pack observed phases are supplied as hkl files
installed with the program.
Supplied observed hkl files are included in the Standard database and
have a reference ID > 5000 and are also supplied as disk HKL files
except for the Clay or any other special package files. These files
have a reference ID number > 8000. The non-clay phases for which no crystal structure data could be found also have
observed (hkl) files and are listed below. These are located, for the standard setup, in the
directory “C:\Program Files\Siroquant\v3 \Observed”. Special Phase
(No Crystal Structure Data)
Standard Database Serial #
Name of “Observed” (hkl) File para-Spurrite 5197 pspurr1.hkl Pyrrhotite-5c 5199 pyrr5c_1.hkl
CaSiF6 5235 CaSiF61.hkl Theta-alumina 5299 thal1.hkl Talc, disordered 5320 talb1.hkl
2.4.2 Clay Pack Observed hkl
Clays often have very disordered and ill-defined structures - many common types of clay
listed below have been included in the databank and these are also specified in the
companion “Clay Package Manual”.
Clay phases with imperfect or unknown crystal structures are included in Siroquant
Version 3.0: When a Clay Pack phase is added to a task it must be specified directly from
the Standard database. HKL files in Version 3 are not supplied separately for Clay Pack
phases but included in the Standard database.
Do not use Clay Pack files from previous versions of Siroquant as they
are no longer valid in version 3. When an earlier version task is
converted any Clay Pack, observed hkl files are automatically
referenced to the Standard database.
The Clay Pack phases are:
Clay Mineral in Siroquant Clay Package Crystal Structure Status Clay Package
Demonstration Task
Filenames
Ref. ID
Number
Antigorite Modulated
structure (unknown) Antig, Antig18 8237
Halloysite Curved lattice (unknown) Halloy, Halloy18 8161
Illite Mica-like
(unknown) Illite,
Illite20
8146
Moderately Ordered 1Tc Kaolin, No 1. Unknown Kaoord,
Kaoord13
8240
Moderately Ordered 1Tc Kaolin No 2 Unknown Kaodis1,
Kaodi120
8440
Disordered 1Tc Kaolin
produced by grinding
Kaolin No 2
Unknown Kaodis2, Kaodi220 8441
Highly Disordered 1Tc Kaolin Unknown Kaodisor,
Kaodis50
8442
Highly Disordered 1Md Kaolin Unknown Kao1Md,
Kao1Md36
8239
Montmorillonite Poorly Known Mont, Mont24 8137 Amorphous Opal,
Tridymite-based
Amorphous, Tridymite-like regions SI02FUM 8101 Palygorskite (Attapulgite) Poorly Known Paly, Paly27 8237
Mixed-Layer Illite- Smectite Unknown Mixlayer,
Mixlay18
8236
Meta-Kaolin Unknown Metako,
Metako30
8274
3.
Siroquant User Interface
To effective utilize this part of the manual you should have Siroquant v3 installed and the dongle attached. There may be slight inconsequential differences between what may be shown on your computer screen and what is shown in the text. Some differences may be due to how Windows is set up. There may also be some color differences to the default setup.
3.1 Main Application Window
The main Siroquant application window is a multiple document interface (MDI) application. It features (from the top):
Caption
The number in the brackets is the session number. This is incremented for a user each time Siroquant v3 is started. Main Menu
Shows the menu commands available when no tasks are opened. Tool Bar Siroquant for Windows allows shortcuts for frequently used functions via
a tool bar (button bar). If no tasks are open very few buttons are
enabled. Some buttons have a drop down menu for additional actions.
The top most item of the drop down menu is the same action as the
button itself.
Client Area The main area of the application window is the client area where the child
windows of the MDI are placed. The only type of child window in is the
dialog that displays each open task.
Status Bar The bottom most part is the status bar. It is divided into four panels:
1. Hint for a selected action from the main menu and toolbar.
2. Identifies whether the active task is saved or not.
3.
Identifies the active task. Each task is identified by a letter enclosed in square brackets (e.g. [A]). Every open window or dialog associated with the task has its caption preceded by this identification. 4. The folder (directory) where the active task resides and therefore the current directory.
In earlier versions of Siroquant the current directory was
the Siroquant directory. In v3, no working files need to be
placed in the program directory.
3.2 Task Display
For the following example open the task (press Ctrl-O) and open the following task:
“C:\Program Files\Siroquant\v3\Examples\Manual Demos\ Demo Task Display.tsk”.
The above shows the task window maximized in the MDI client area. The captions for the
main application window and the task window have been combined.
There are significant differences in operation between version 3 and
earlier versions. The following should be read by users of earlier
versions of Siroquant. The display of hkl bars is discussed in Section 4.13. Extra display features are discussed in section 5.1.
3.2.1 General Description
The plot above is what is displayed after a refinement. The calculated pattern (red) is overlaid on the active pattern (yellow). The difference pattern (blue) is shown below the other plots. The difference trace is the active trace with the calculated trace subtracted. Also shown is a magenta trace for the background profile because background refinement was included.
The first four panels of the status bar show the position of the last left mouse click. Two more panels indicate the status of the keyboard Ctrl, Alt and Shift keys.
3.2.2 Zooming & Unzooming
To zoom a section of the plot, draw a rectangle from the top-left to the bottom-right by holding down the left mouse button. The plot may be further zoomed in the same
manner. To unzoom reverse the operation, that is draw a rectangle anywhere from the
bottom left to the top right.
The plot returns to the original, not to the previous zoom operation.
The difference trace is not zoomable. 3.2.3 Scrolling
There are two methods of scrolling. Firstly: you will notice that on a zoomed plot red arrows appear at each end on the two-theta axis. The left most shifts the current scan graph to the left (displaying lower 2θ angles) and the right most shifts the current scan graph to the right (higher 2θ angles). The range of the intensity values is not affected. Secondly: hold the middle mouse button (or scroll wheel) down and move the mouse. To
recover from scrolling unzoom the display (i.e. draw a rectangle from the bottom left to top right while holding down the left mouse button).
3.2.4 Reading the Position Points on the Plot and Traces
When certain actions are executed the first four panels of the status bar at the bottom of the task display window show the two-theta angle, d-spacing, reading and the relative intensity to either of the active, calculated or difference traces. The various types are:
A. Any point on the plot area.
Click the left mouse button on the plot: The x-values of the angle and d-spacing will always be shown. The y-value shown depends on which zone of the plot area is clicked. The relative intensity is either relative to the active trace or the difference trace. If the shift key on the keyboard is held down the calculated trace, if present, will be used instead of the active trace.
B. Points on a Trace.
If you hold down the Ctrl key and click the left mouse button or move the mouse a point on the active or difference trace will have a small circle drawn around it and its coordinates will be shown in the status bar. If the Shift key is also held down then the calculated trace, if present, is used instead of the active trace. In these
circumstances no zoom box can be drawn unless the Alt key is held down as well.
The above emulates facilities available in the earlier versions of
Siroquant. The right mouse button in v3 is used for other purposes
(usually to show a popup menu) and there is no ‘active’ trace selection
in the pre v3 style. 3.2.5 Chart Popup Menu
If the mouse is right clicked over the chart area a popup menu related to the chart is
displayed. Access to the OEM (original equipment manufacturer) controls is supplied on an ‘as is’ basis. They are beyond the control of Sietronics and limited assistance can be
provided in their use.
3.2.5.1 Popup Menu item: Edit
This is an OEM chart editing tool supplied by TeeChart. It can be used to edit various chart features. Changes made are not remembered and could be lost when the chart is redrawn. Care should also be taken as some deletions could cause program exceptions. The principle use would be to ready the chart for print out.
3.2.5.2 Popup Menu item: Print
This is an OEM print preview tool supplied by TeeChart. It can be used to print out the chart as it is currently displayed as. The user should experiment with the various controls on the print preview dialog for best results. See also Print Colors below.
3.2.5.3 Popup Menu item: Export
This brings up the part of the OEM chart editor related to export of the chart and its data.
3.2.5.4 Popup Menu item: Print Colors
Clicking this item changes the colors to those suitable for printing. Clicking the item a second time reverts to the original colors. The print colors can be edited in the main menu item Options/Main Display & Colors/Print set page.
3.2.5.5 Popup Menu item: hkl Bar Options
This is equivalent to the main menu item Display/hkl Bar Options. Note that changes to these options only affect the active task window and other tasks are unaffected.
3.2.5.6 Popup Menu item: Cross Hairs
Cross hairs can be displayed on the main of difference plots with the coordinates of the cross hairs being displayed on the Task Window’s status bar. Cross hairs commands are:
Off No cross hairs are displayed
On Active The Relative Intensity will be with respect to the active trace.
On Calculated The Relative Intensity will be with respect to the calculated trace.
On Diff.The cross hairs will be displayed on the difference trace and the
relative intensities will be with respect to that trace.
Stick to Trace If selected the cross hairs will stay on the trace as determined
above.
3.2.5.7 Popup Menu item: Add Annotation
Annotations can be added to the plot. These are stored and are redisplayed each time the task is opened. As annotations are labels for one series they are the same font and color. The following dialog is brought up:
The initial coordinates are those of the last left mouse click on the chart. Annotations can be edited with the Main Menu Command Display/Annotation List. See Section 5.1.1. 3.3 Main Application Toolbar
In earlier versions, this was referred to as the button bar. Version 3
uses smaller buttons similar to standard Windows applications.
The toolbar has short cuts for the most frequently used functions in Version 3. The toolbar is not customizable. Some buttons have a drop down menu for additional actions. The
top most item of the drop down menu is the same action as the button itself.
d indicates that th
e button includes a drop down menu.
1. New Task : Prepare a new analytical Task. You will be asked to specify the phases,
the pattern and the task file name. (Menu equivalent: File | New | New Task). The drop down menu has actions for:
a. New Task : as above.
b. New Template Task : Similar to New Task but the task will be saved as a
template task. (Menu equivalent: File | New | New Template Task).
c. Use Template : A new task will be set up using a specified task as a template.
You will be asked for the template task, the pattern and new task file name.
(Menu equivalent: File | New | Use Template).
d. From Current Task : [Only available if a task is open] A new task will be set up
using the active task as a template. You will be asked for the pattern and new
task file name. The current task will remain open.
Use this menu item rather than Load Scan to refine a new pattern. (Menu equivalent: File | New | From Current Task).
e. Duplicate Current Task : [Only available if a task is open] The active task will be
duplicated and a new window opened. You will be asked for a new task file
name. (Menu equivalent: File | New | Duplicate Current Task).
f. New Task Wizard : Sets up a new task in a series of next/back steps. (Menu
equivalent: File | New Task Wizard). 2. Open Task : Opens an existing task into a new task window. The task must not be
already open. (Menu equivalent: File | Open Task).
3. Save Task : The active task is saved using its current name. If there have been no
changes then this action will be disabled. There is no acknowledgement of a
successful save other than the action’s being disabled. (Menu equivalent: File | Save Task).
4. Load Scan : Replaces the current pattern in the active task with a new pattern while
retaining current parameter settings in the same task window.
Use From Current Task if you to open another task window or safeguard the previous task. (Menu equivalent: File | Load Scan). 5. Close : This action closes the active task window. If the task is unsaved a query
message will be displayed. This command does not exit Siroquant.
6. Prepare hkl File : Displays the Prepare hkl File dialog. (Menu equivalent: File |
Prepare hkl File or Tools | Prepare hkl File).
7. Edit Task Phases : Brings up a three page dialog to control what phases are in a task,
their order and status [‘phase status’ will be discussed later]
This is equivalent to Edit Task in version 2.5 but with increased
functionality. It has also been moved from the file menu to the
Parameters menu. 8. Background Subtraction : Brings up a dialog to subtract the background from a
pattern.
Combines two previous menu items into one. Note also that a
separate dialog is used rather than the main display. (Menu
equivalent: Parameters | Background Subtraction).
The drop down menu has actions for:
a. Background Subtraction : as above.
b. Calibration : Brings up a dialog similar to the Background Subtraction dialog
where the pattern can be calibrated. (Menu equivalent: Parameters | Calibration)
Note also that a separate dialog is used rather than the main
display.
c. Excluded regions : Brings up a dialog to specify the excluded regions. (Menu
equivalent: Parameters | Excluded Regions).
The excluded regions are first displayed on a separate chart.
9. Edit Phase Dependent Parameters : Brings up a dialog where the phase dependent
parameters may be edited. (Menu equivalent: Parameters | Phase Dependent).
10. Stage Refinement Control : Displays the stage and refinement control parameters
dialog. (Menu equivalent: Parameters | Stage Refinement).
11. Start Refinement : The ‘Go’ button to start a refinement by executing the TRACSCAL
portion of the program. (Menu equivalent: Refinement | Go).
12. Restore Previous : Restores the active task to the state it was in immediately before
the last refinement. New feature in v3. (Menu equivalent: Refinement | Restore | Previous). The drop down menu has actions for:
a. Restore Previous : as above.
b. @Pre : Only available if an option enabled. The action restores the active
window with the contents of a task that was last saved to file immediately before the last refinement. (Menu equivalent: Refinement | Restore | @Pre).
c. @Post : Only available if an option enable
d. The action restores the active
window with the contents of a task that was last saved to file, immediately after
the last successful refinement. (Menu equivalent: Refinement | Restore |
@Post).
d. Clear Refinement : Removes the calculated and difference traces from the active
display. Refinement | Clear Refinement).
13. Restore Redo : Undoes a Restore Previous action to state immediately before that
action. These commands are complementary to each other. (Menu equivalent: Refinement | Restore | Redo).
14. Quantification Results : Displays the quantification results dialog. (Menu equivalent:
Results | Quantification). The drop down menu has actions for:
a. Quantification Results : as above.
b. Charts : Brings up a dialog to display various charts of the quantification. . (Menu
equivalent: Results | Charts).
c. Long Results : The term ‘Long Results’ in earlier referred to a text file that
contained information how parameters varied during a refinement. In v3 the
term is reserved for a dialog that displays these parameters. (Menu equivalent:
Results | Long Results).
d. Refinement History :
have varied between refinements. (Menu equivalent: Results | Refinement
History).
e. Composition : Shows a dialog that does elemental or oxide composition analysis
based on the results of the refinement. (Menu equivalent: Results |
Composition).
15. Chi Squared Plot : Brings up a chart dialog showing the refinement statistics. (Menu
equivalent: Results | Chi Squared)
In previous versions this item was in the Display menu. In v3 it is
moved to Results. 16. Display Reset : Completely redraws the display. While can be used to unzoom the
display it will reset temporary changes to the chart. (Menu equivalent: Display |
Display Reset).
17. hkl Bars On/Off // Turns the hkl bars for the phases alternately on and off. The button
remains depressed in the On state. Note that the hint will be what happens after the button is pressed
18. hkl Bar Palette : Alternately shows and hides the hkl bar palette dialog. If the button is
in the ‘depressed’ state then the dialog is showing. (Menu equivalent: Display | hkl Bars Palette).
19. Series Listing : Displays the Series Listing dialog. The term ‘series’ is a TeeChart’
referring to line (or trace), set of bars (hkl bars) and similar items showing on the plot. If the button is in the ‘depressed’ state then the dialog is showing. (Menu equivalent: Display | Series List).
20. Cascade : All the task windows will be partially overlapped so that each window’s
caption is visible. (Menu equivalent: Window | Cascade).
21. Tile Horizontally : The open task windows are tiled one above the over. Menu
equivalent: Window | Tile Horizontally).
22. Tile Vertically : The open task windows are tiled side by side. (Menu equivalent:
Window | Tile Vertically).
23. Help : Opens the help file for SIRQUANT Version 3. (Menu equivalent: Help | Index).
4. Basic Level Operations
This chapter will give the basic menu operations needed to setup a task, refine the pattern and view the results. Additional operations will be in the Intermediate and Advanced sections. A full outline of all menu operations in order is available in the online help. An overview of Intermediate and Advanced level features is given in sections 4.18 and 4.19.
4.1 Preparing Calculated *.HKL Files
Menu: File - Prepare HKL file or Tools - Prepare HKL file
Toolbar button:
While it is not strictly necessary to prepare hkl files for phases in the Standard database, the principles of it should still be understood. In version 3 hkl files can either be loaded from a disk hkl file or the equivalent can be regenerated when a task is loaded or set up. If the phase is from a user database and databank pair, the HKL file must be prepared in the standard way.
Siroquant is provided with a crystal structure databank stored in the Standard database. User database store the equivalent information in database and databank pairs. The characteristic HKL lines of a phase can be calculated from this information. The dialog is shown below:
For a full description of what all
the controls on this dialog
perform, press the Help button.
The available phases will be
shown in a table. Click the
column header to change the
sort order. A second click on the
same header will reverse the
sort. You can choose one or
more groups to limit the number
of phases. Right clicking over
the group box allows you to
select whether you want to list
the phases that can be found in
one (or more selected groups
(Union) or phases that are
common to all selected groups
(Intersection). The number of
phases in the table is shown in
brackets after Phase List.
The Phase Search text box
provides a rapid method of
searching for the particular
phase – the user types the
criteria in the form of the phase or mineral name, the Siroquant reference number or the chemical formula into the box and the entries in the Mineral list are narrowed to match the criteria. To specify which fields are to be searched press Options and then check the appropriate boxes in Phase Find Search Options.
Ensure that the correct wavelengths are used when preparing the hkl file, by selecting the appropriate tube anode. To change the selected tube anode simply click the anode symbol required.
现在将通过实例初步介绍jade5.0的基本操作步骤。 1、数据输入 由于不同的X射线衍射仪输出的数据类型不同，但都可以将数据转换成txt 文档或Ascii格式的文档（文件名为*.txt或*.asc），为提高软件的通用性jade5.0提供了以txt文档或Ascii格式输入数据。运行jade5.exe首先进入以下界面 中间的窗口用于选择需打开文件，左侧选择文件路径与资源管理器的操作相同， 右侧选择打开文件的类型，一般选择XRD Pattern files(*.*)，这时在右下方 的窗口中将显示左侧被选择文件夹中所有能被该软件识别的文件，然后选择需要
分析的数据文件，点击菜单栏Read进入主窗口，此选择窗口可以通过主窗口中file/patterns进入。 2、背景及Ka2线扣除 在主菜单栏中选择analyze/fit background进入如下窗口： 该窗口用于设置扣除背景时的参数，一般选择默认值直接选择apply，回到主窗口，此时软件自动运行Edit bar/B.E按钮，用于手动修改背景， Edit bar工具栏如下：
此工具栏提供了放大、标定峰位等操作，当鼠标移动到按钮上时软件将自动提示。在该软件中的所有按钮对鼠标左右键操作都有不同效果，一般左键为确定或正向操作，右键为取消或反向操作。 3、确定峰位 在主菜单栏中选择analysie/find peaks，进入确定峰位所需的参数设置窗口，如下图，一般选择默认值，选择apply回到主窗口，选择Edit bar左第三个按钮可手动编辑。 在手动编辑过峰个数或峰位后，同样可以选择analyze/find peaks，选择Report，进入如下界面：
1.做XRD有什么用途啊，能看出其纯度?还是能看出其中含有某种官能团？ X射线照射到物质上将产生散射。晶态物质对X射线产生的相干散射表现为衍射现象，即入射光束出射时光束没有被发散但方向被改变了而其波长保持不变的现象，这是晶态物质特有的现象。 绝大多数固态物质都是晶态或微晶态或准晶态物质，都能产生X射线衍射。晶体微观结构的特征是具有周期性的长程的有序结构。晶体的X射线衍射图是晶体微观结构立体场景的一种物理变换，包含了晶体结构的全部信息。用少量固体粉末或小块样品便可得到其X射线衍射图。 XRD（X射线衍射）是目前研究晶体结构(如原子或离子及其基团的种类和位置分布，晶胞形状和大小等)最有力的方法。 XRD特别适用于晶态物质的物相分析。晶态物质组成元素或基团如不相同或其结构有差异，它们的衍射谱图在衍射峰数目、角度位置、相对强度次序以至衍射峰的形状上就显现出差异。因此，通过样品的X射线衍射图与已知的晶态物质的X射线衍射谱图的对比分析便可以完成样品物相组成和结构的定性鉴定；通过对样品衍射强度数据的分析计算，可以完成样品物相组成的定量分析； XRD还可以测定材料中晶粒的大小或其排布取向（材料的织构）...等等，应用面十分普遍、广泛。 目前XRD主要适用于无机物，对于有机物应用较少。 关于XRD的应用，在[技术资料]栏目下有介绍更详细的文章，不妨再深入看看。 如何由XRD图谱确定所做的样品是准晶结构？XRD图谱中非晶、准晶和晶体的结构怎么严格区分？ 三者并无严格明晰的分界。 在衍射仪获得的XRD图谱上，如果样品是较好的"晶态"物质，图谱的特征是有若干或许多个一般是彼此独立的很窄的"尖峰"（其半高度处的2θ宽度在0.1°~0.2°左右，这一宽度可以视为由实验条件决定的晶体衍射峰的"最小宽度"）。如果这些"峰"明显地变宽，则可以判定样品中的晶体的颗粒尺寸将小于300nm，可以称之为"微晶"。晶体的X射线衍射理论中有一个Scherrer公式，可以根据谱线变宽的量估算晶粒在该衍射方向上的厚度。 非晶质衍射图的特征是：在整个扫描角度范围内（从2θ1°~2°开始到几十度）只观察到被散射的X射线强度的平缓的变化，其间可能有一到几个最大值；开始处因为接近直射光束强度较大，随着角度的增加强度迅速下降，到高角度强度慢慢地趋向仪器的本底值。从Scherrer公式的观点看，这个现象可以视为由于晶粒极限地细小下去而导致晶体的衍射峰极大地宽化、相互重叠而模糊化的结果。晶粒细碎化的极限就是只剩下原子或离子这些粒子间的"近程有序"了，这就是我们所设想的"非晶质"微观结构的场景。非晶质衍射图上的一个最大值相对应的是该非晶质中一种常发生的粒子间距离。 介于这两种典型之间而偏一些"非晶质"的过渡情况便是"准晶"态了。 在做Ｘ射线衍射时，如果用不同的靶，例如用铜靶或者Cr靶，两者的谱图会一样吗？如果不同的话，峰的位置和强度有啥变化吗？有规律吗？ 不同的靶，其特征波长不同。衍射角（又常称为Bragg角或2θ角）决定于实验使用的波长（Bragg方程）。使用不同的靶也就是所用的X射线的波长不同，根据Bragg方程，某一间距为d的晶面族其衍射角将不同, 各间距值的晶面族的衍射角将表现出有规律的改变。因此，使用不同靶材的X射线管所得到的衍射图上的衍射峰的位置是不相同的，衍射峰位置的变化是有规律的。
XRD分析软件有4种 1.pcpdgwin 有人认为是最原始的了。它是在衍射图谱标定以后按照d值检索。一般可以有限定元素、按照三强线、结合法等方法。所检索出的卡片多时候不对。一张复杂的衍射谱有时候一天也搞不定。 2.search match 可以实现和原始实验数据的直接对接可以自动或手动标定衍射峰的位置对于一般的图都能很好的应付。而且有几个小工具使用很方便。如放大功能、十字定位线、坐标指示按钮、网格线条等。最重要的是它有自动检索功能。可以帮你很方便的检索出你要找的物相。也可以进行各种限定以缩小检索范围。如果你对于你的材料较为熟悉的话对于一张含有45相的图谱检索也就3分钟。效率很高。而且它还有自动生成实验报告的功能 3.High Score 几乎search match中所有的功能highscore都具备而且它比searchmatch更实用。 1它可以调用的数据格式更多。 2窗口设置更人性化用户可以自己选择。 3谱线位置的显示方式可以让你更直接地看到检索的情况 4手动加峰或减峰更加方便。 5可以对衍射图进行平滑等操作是图更漂亮。 6可以更改原始数据的步长、起始角度等参数。 7可以进行0点的校正。 8可以对峰的外形进行校正。 9可以进行半定量分析。 10物相检索更加方便检索方式更多。 11可以编写批处理命令对于同一系列的衍射图一键搞定。 4.jade 和highscore相比自动检索功能少差但它有比之更多的功能。 1它可以进行衍射峰的指标化。 2进行晶格参数的计算。 3根据标样对晶格参数进行校正。 4轻松计算峰的面积、质心。 5出图更加方便你可以在图上进行更加随意的编辑。 其实学化工和材料的人对这个软件HighScore是很熟悉的还有一个软件数据分析与科学绘图软件origin 是搞材料研究算是必备的软件。对于学材料学生可能毕业写论文要用到这些软件。 Jade5.0的使用初步说明 1、数据输入由于不同的X射线衍射仪输出的数据类型不同但都可以将数据转换成txt文档或Ascii格式的文档文件名为.txt 或.asc为提高软件的通用性jade5.0提供了以txt文档或Ascii格式输入数据。运行jade5.exe首先进入以下界面图片一在后面的压缩文件里面下同中间的窗口用于选择需打开文件左侧选择文件路径与资源管理器的操作相同右侧选择打开文件的类型一般选择XRD Pattern files.这时在右下方的窗口中将显示左侧被选择文件夹中所有能被该软件识别的文件然后选择需要分析的数据文件点击菜单栏Read进入主窗口此选择窗口可以通过主窗口中file/patterns进入。 2、背景及Ka2线扣除在主菜单栏中选择analyze/fit background进入如下窗口图片二该窗口用于设置扣除背景时的参数一般选择默认值直接选择apply回到主窗口此时软件自动运行Edit bar/B.E按钮用于手动修改背景 Edit bar工具栏如下图片三此工具栏提供了放大、标定峰位等操作当鼠标移动到按钮上时软件将自动提示。在该软件中的所有按钮对鼠标左右键操作都有不同效果
如何使用XRD分析软件Jade5.0解谱？ Jade5.0的使用初步说明1、数据输入 由于不同的X射线衍射仪输出的数据类型不同，但都可以将数据转换成txt文档或Ascii格式的文档（文件名为*.txt或*.asc），为提高软件的通用性jade5.0提供了以txt文档或Ascii格式输入数据。运行jade5.exe首先进入以下界面中间的窗口用于选择需打开文件，左侧选择文件路径与资源管理器的操作相同，右侧选择打开文件的类型，一般选择XRD Pattern files(*.*)，这时在右下方的窗口中将显示左侧被选择文件夹中所有能被该软件识别的文件，然后选择需要分析的数据文件，点击菜单栏Read进入主窗口，此选择窗口可以通过主窗口中file/patterns进入。 2、背景及Ka2线扣除 在主菜单栏中选择analyze/fit background进入如下窗口： 此工具栏提供了放大、标定峰位等操作，当鼠标移动到按钮上时软件将自动提示。在该软件中的所有按钮对鼠标左右键操作都有不同效果，一般左键为确定或正向操作，右键为取消或反向操作。 3、确定峰位 在主菜单栏中选择analysie/find peaks，进入确定峰位所需的参数设置窗口，如下图，一般选择默认值，选择apply回到主窗口，选择Edit bar左第三个按钮可手动编辑。
在手动编辑过峰个数或峰位后，同样可以选择analyze/find peaks，选择Report，进入如下界面： 在此窗口中显示了以上操作中所确定的峰位置、强度、半峰宽（FWHM）等参数，其中FWHM将时计算晶粒度的主要参数。 选择analyze/find peaks，在此窗口中选择Labeling标签，可以选择峰的标示方式，如下图：
1.用Highscore软件打开XRD文件，在第一个表格界面下选定.XRDML和.ASC，点击OK 即可。然后将该文件另存为.asc格式的文件。 2.用Micro soft excel软件将.asc文件中的数据导入，这样就可以将数据在excel表格中复 制下来粘到origin里，进一步作图分析了。 3.可以利用Highscore分析XRD谱图。 （1）将XRD的数据库（即PDF2文件夹）导入到highscore软件里。 ●将PDF2文件放在不含有汉字的（纯英文）的路径里，比如直接放在D盘的 话，路径即为D:/PDF2，这是可以的。 ● b.在highscore软件的上方的Customize里找到program setting …。在program setting的对话框里点击Reference Patterns，在这个界面下找到database conversion下方的PDF2，点击，并通过这下方的一个空白条目后的browse（浏 览）里在电脑找到PDF2文件夹。选定后在其下方的Extract user data from existing reference database打勾。 ●点击start conversion of ICDD Database。 这个导入的过程可能花费半个小时的时间。 （2）分析XRD数据 ●利用highscore软件打开XRD源文件， ●在Analysis的下拉菜单里面找到Search&March，然后在它的后拉条目中选Execute Search&March。 ●在弹出的对话框中点击restrictions，在Edit Restriction Sets…里找到Periodic Table…并 点击。select restriction set使用default选项 ●按照提示选择可能含有或者一定含有的元素，然后点击close。即会返回到Search&Match 的对话框，点击search。 ●寻峰完后，在lists pane里面出现一列表，表分为上下两部分。下部分都是具体数据。 上部分是空的。把自己想知道的元素的数据拖到上方表格中。谱图中就会出现与该元素拟合的峰。可以双击该元素的那行数据，查看有关该成分的具体情况。
[一般问题] 做XRD有什么用途啊，能看出其纯度?还是能看出其中含有某种官能团？ X射线照射到物质上将产生散射。晶态物质对X射线产生的相干散射表现为衍射现象，即入射光束出射时光束没有被发散但方向被改变了而其波长保持不变的现象，这是晶态物质特有的现象。 绝大多数固态物质都是晶态或微晶态或准晶态物质，都能产生X射线衍射。晶体微观结构的特征是具有周期性的长程的有序结构。晶体的X射线衍射图是晶体微观结构立体场景的一种物理变换，包含了晶体结构的全部信息。用少量固体粉末或小块样品便可得到其X射线衍射图。 XRD（X射线衍射）是目前研究晶体结构(如原子或离子及其基团的种类和位置分布，晶胞形状和大小等)最有力的方法。 XRD特别适用于晶态物质的物相分析。晶态物质组成元素或基团如不相同或其结构有差异，它们的衍射谱图在衍射峰数目、角度位置、相对强度次序以至衍射峰的形状上就显现出差异。因此，通过样品的X射线衍射图与已知的晶态物质的X射线衍射谱图的对比分析便可以完成样品物相组成和结构的定性鉴定；通过对样品衍射强度数据的分析计算，可以完成样品物相组成的定量分析； XRD还可以测定材料中晶粒的大小或其排布取向（材料的织构）...等等，应用面十分普遍、广泛。 目前XRD主要适用于无机物，对于有机物应用较少。 关于XRD的应用，在[技术资料]栏目下有介绍更详细的文章，不妨再深入看看。 如何由XRD图谱确定所做的样品是准晶结构？XRD图谱中非晶、准晶和晶体的结构怎么严格区分？ 三者并无严格明晰的分界。 在衍射仪获得的XRD图谱上，如果样品是较好的"晶态"物质，图谱的特征是有若干或许多个一般是彼此独立的很窄的"尖峰"（其半高度处的2θ宽度在0.1°~0.2°左右，这一宽度可以视为由实验条件决定的晶体衍射峰的"最小宽度"）。如果这些"峰"明显地变宽，则可以判定样品中的晶体的颗粒尺寸将小于300nm，可以称之为"微晶"。晶体的X射线衍射理论中有一个Scherrer公式，可以根据谱线变宽的量估算晶粒在该衍射方向上的厚度。 非晶质衍射图的特征是：在整个扫描角度范围内（从2θ 1°~2°开始到几十度）只观察到被散射的X射线强度的平缓的变化，其间可能有一到几个最大值；开始处因为接近直射光束强度较大，随着角度的增加强度迅速下降，到高角度强度慢慢地趋向仪器的本底值。从Scherrer公式的观点看，这个现象可以视为由于晶粒极限地细小下去而导致晶体的衍射峰极大地宽化、相互重叠而模糊化的结果。晶粒细碎化的极限就是只剩下原子或离子这些粒子间的"近程有序"了，这就是我们所设想的"非晶质"微观结构的场景。非晶质衍射图上的一个最大值相对应的是该非晶质中一种常发生的粒子间距离。 介于这两种典型之间而偏一些"非晶质"的过渡情况便是"准晶"态了。 在做Ｘ射线衍射时，如果用不同的靶，例如用铜靶或者Cr靶，两者的谱图会一样吗？如果不同的话，峰的位置和强度有啥变化吗？有规律吗？ 不同的靶，其特征波长不同。衍射角（又常称为Bragg角或2θ角）决定于实验使用的波长（Bragg方程）。使用不同的靶也就是所用的X射线的波长不同，根据Bragg方程，某一间距为d的晶面族其衍射角将不同, 各间距值的晶面族的衍射角将表现出有规律的改变。因此，
相对于其它XRD分析软件，JADE系列软件应该说是做的最好的，它囊括了从定性，指标化，峰型拟合（JADE5.0）到无标定量，晶体结构分析（Jade6.0）等一系列的功能。我个人以为，只要有Jade5.0就够了，至于后面两项功能，最好是用其它免费软件执行（在https://www.doczj.com/doc/cc11601090.html,上应有尽有），傻瓜相机虽然好用，但要拍出好照片，还是专业相机好。NO1.Jade5.0的安装和设置 Jade5.0都是自动安装的，这不成问题。要把PDF卡片引入，先将ICDD的光盘插入，然后pdf/setup/select all/,其它按提示进行。 可以对优选项进行设置：EDIT/preference/,里面包括了对显示窗口的设置，仪器参数的设置，打印输出的设置等，一般来说按默认就行，我本人则喜欢将MISC栏里的“Materials Data, Inc.”改为我自己的大名 No2 数据的输入 Jade软件可以直接读取Rigaku、Bruker、Philips、Scintag等很多衍射仪的原始数据。打开File\patterns,将出现如附件中所示画面，先（I）找到你文件位置，从（III）的下拉框中选择你的数据格式，按（II）选择。很多仪器输出文件的格式都是*.raw,实际上都是不一样的，但格式选错了也没关系，软件会给你自动转到合适的格式中去的。 高级一点的：有一些数据格式在（III）的下拉框中没有，比如最常见的txt，xy等，此时你可以自己动手设置，在以上的数据输入面板中，点击工具栏上的“import",进入格式设置画面，如附件所示，a区为注释区，b区为数据格式区，对于最简单的一列角度，一列强度的数据格式，a区不用填写，b区在” angle column“前打上勾，数据从第1行开始读，每行1列数据，强度数据从第8行开始（角度不算），角度从1至6列，所得数据格式即为附件中所示的数据格式。你也可以按照自己的数据格式进行自由改动，如果a区中表明第1行有说明文字，则数据从第2行读入，相应在b区就将data starts改成2。 No 3 基本功能使用：平滑，扣背底 一张XRD图谱出来，往往因为有空气散射，漫散射，荧光以及样品结晶差等等原因而造成图谱上存在许多“毛刺”和较高的背底，虽然提高X光强度能成倍提高信噪比，然而有时受仪器和样品所限，这两项功能需要用到。但根据我个人的经验，要尽量少使用平滑和扣背底，因为这两项操作带来的可能后果就是将一些微弱的有用信息一概抹掉了，特别注意的是，如果将数据用来做Rietveld精修，更不要进行这两项操作。当然，如果是将图谱打印出来给别人看，适当进行平滑和扣背底也是个不错的选择。 1 平滑 打开Filters/smooth pattern或在快捷工具栏中右键点击也可。随后将出现一个悬浮框，最上面的一栏中方块可以直接用鼠标拖动，大家试试看图谱会有什么变化，拖到什么位置，根据情况而定，我的经验是将方块拖到尖峰的底部出现倒生的毛刺之前。再下面有“parabolic filter"和”quartic filter"的选择，选择后一个的效果稍好。再下面还有选择框，我一般都不管它。作完以上操作后，再用鼠标左键点击快捷工具栏中的平滑图标即可。 2 扣背底 打开analyze/fit background或在快捷工具栏中右键点击也可。随后也出现一个如附件中所示的悬浮框，（I）处所示代表了背底拟合的级数，点击越靠前，该级数越高，也可在右边选择是一次拟合，抑或二次和三次拟合，试情况而定，背底偏离线性越远，则拟合的级数要求越高。 背底曲线用黄线表示，红点代表了背底在局部的最高点，左键点击图谱上的某一处便可在此
常用的XRD分析软件有4种： 1.pcpdfwin 有人认为是最原始的了。它是在衍射图谱标定以后，按照d值检索。一般可以有限定元素、按照三强线、结合法等方法。所检索出的卡片多时候不对。一张复杂的衍射谱有时候一天也搞不定。 2.search match 可以实现和原始实验数据的直接对接，可以自动或手动标定衍射峰的位置，对于一般的图都能很好的应付。而且有几个小工具使用很方便。如放大功能、十字定位线、坐标指示按钮、网格线条等。最重要的是它有自动检索功能。可以帮你很方便的检索出你要找的物相。也可以进行各种限定以缩小检索范围。如果你对于你的材料较为熟悉的话，对于一张含有4，5相的图谱，检索也就3分钟。效率很高。而且它还有自动生成实验报告的功能！ 3.High Score 几乎search match中所有的功能，highscore都具备，而且它比searchmatch更实用。（1）它可以调用的数据格式更多。 （2）窗口设置更人性化，用户可以自己选择。 （3）谱线位置的显示方式，可以让你更直接地看到检索的情况 （4）手动加峰或减峰更加方便。 （5）可以对衍射图进行平滑等操作，是图更漂亮。 （6）可以更改原始数据的步长、起始角度等参数。 （7）可以进行0点的校正。 （8）可以对峰的外形进行校正。 （9）可以进行半定量分析。 （10)物相检索更加方便，检索方式更多。 （11）可以编写批处理命令，对于同一系列的衍射图，一键搞定。 4.jade 和highscore相比自动检索功能少差，但它有比之更多的功能。 （1）它可以进行衍射峰的指标化。 （2）进行晶格参数的计算。 （3）根据标样对晶格参数进行校正。
XRD分析软件介绍及使用 1.XRD分析软件 常用的软件一共有四种。 1.pcpdgwin 有人认为是最原始的了。它是在衍射图谱标定以后，按照d值检索。一般可以有限定元素、按照三强线、结合法等方法。所检索出的卡片多时候不对。一张复杂的衍射谱有时候一天也搞不定。 2.search match 可以实现和原始实验数据的直接对接，可以自动或手动标定衍射峰的位置，对于一般的图都能很好的应付。而且有几个小工具使用很方便。如放大功能、十字定位线、坐标指示按钮、网格线条等。最重要的是它有自动检索功能。可以帮你很方便的检索出你要找的物相。也可以进行各种限定以缩小检索范围。如果你对于你的材料较为熟悉的话，对于一张含有4，5相的图谱，检索也就3分钟。效率很高。而且它还有自动生成实验报告的功能！ 3.High Score 几乎search match中所有的功能，highscore都具备，而且它比searchmatch更实用。 （1）它可以调用的数据格式更多。 （2）窗口设置更人性化，用户可以自己选择。 （3）谱线位置的显示方式，可以让你更直接地看到检索的情况 （4）手动加峰或减峰更加方便。 （5）可以对衍射图进行平滑等操作，是图更漂亮。 （6）可以更改原始数据的步长、起始角度等参数。 （7）可以进行0点的校正。 （8）可以对峰的外形进行校正。 （9）可以进行半定量分析。 （10)物相检索更加方便，检索方式更多。 （11）可以编写批处理命令，对于同一系列的衍射图，一键搞定。 4.jade 和highscore相比自动检索功能少差，但它有比之更多的功能。 （1）它可以进行衍射峰的指标化。 （2）进行晶格参数的计算。 （3）根据标样对晶格参数进行校正。 （4）轻松计算峰的面积、质心。 （5）出图更加方便，你可以在图上进行更加随意的编辑。 /@g2385945/680997.topic 整个网址上可以下X'Pert HighScore Plus(XRD分析软件)及其XRD卡片 其实什么软件都一样用，关键还是要下的到，不过这里可以下到PDF2—2004标准卡片库。在宿舍用EMULE下的很快的，如果没有装EMULE，右击直接下载就可以了。网页里面有导入标准卡片库的方法。 2.XRD文件转换器
X’Pert HighScore X’Pert HighScore Plus
目录 1. 约定术语 (1) 1.1. 动作术语 (1) 1.2. 指令与说明 (1) 1.3. 按钮与表单域 (1) 1.4. 菜单项与按键 (1) 2. 启动HS+并启用示例数据库 (2) 2.1. 介绍 (2) 2.2. 启动X’Pert HighScore Plus (2) 2.3. 启用数据库 (4) 3. 载入及显示数据 (6) 3.1. 介绍 (6) 3.2. 载入扫描 (6) 3.3. 显示扫描 (7) 3.4. 检索参考卡片 (8) 3.5. 显示参考卡片 (10) 4. 图谱处理 (12) 4.1. 介绍 (12) 4.2. 确定背景 (12) 4.3. 寻峰 (14) 5. 进行物相鉴定 (17) 5.1. 介绍 (17) 5.2. 物相检索 (17) 5.3. 物相鉴定 (18) 6. 改变评分 (21) 6.1. 介绍 (21) 6.2. 改变评分 (21) 7. 运行用户批处理 (22) 7.1. 介绍 (22) 7.2. 运行用户批处理 (22) 8. 检索及精修晶格 (23) 8.1. 介绍 (23) 8.2. 准备 (23) 8.3. 载入图谱 (23) 8.4. 寻峰 (25) 8.5. 检索/精修晶格 (27) 8.6. 保存结果 (30) 9. 自动Rietveld精修 (31) 9.1. 介绍 (31) 9.2. 载入数据 (31) 9.3. 自动精修 (32) 9.4. 更好的精修 (32)
9.5. 注解及建议 (33) 10. 物相鉴定策略及疑难解答 (35) 10.1. 介绍 (35) 10.2. 图谱处理顺序 (36) 10.3. 物相鉴定 (37) 10.4. 疑难解答 (37)
XRD分析软件及使用说明汇总 XRD是我们晶体分析中最常用的分析方法，我们常常会借助与各种软件来分析我们的实验数据，而这些软件有很多，每种都有不同的使用方法，下面我把自己珍藏的各种XRD分析软件共享给大家，希望能对大家有用：我都上传到纳米盘了，不需要金币，可以免费下载： 一、MDI Jade 5安装程序 地址： https://www.doczj.com/doc/cc11601090.html,/d/c818c4f ... 1096c189163f39b7900 jade 5.0还是我们比较常用的，虽然也有6.0但是由于破解方法等现在使用的较少，还不是很完美，我个人感觉5.0足够用了，没有必要最求最新。 二、MDI.jade5.0 使用说明 地址： https://www.doczj.com/doc/cc11601090.html,/d/0a41e12 ... 89d6dcbb6717faf4c00 这其中包含多个版本的说明，比较全面。 三、PDF2004 地址： https://www.doczj.com/doc/cc11601090.html,/d/964291b ... 9bfa054cc26f1a3dc0a 我相信这个是大家最想要的，我看到很多人都在求助这个卡片库，这个版本是全库的，大家可以 放心使用，解压之后大约900M。 四、晶粒大小计算 地址： https://www.doczj.com/doc/cc11601090.html,/d/1834ddc ... fdafc7f1c11dd170000 一个比较实用的小软件，根据谢乐公式编写，直接求出颗粒粒径尺寸。 五、search-match
地址： https://www.doczj.com/doc/cc11601090.html,/d/d06af98 ... fab0d7427a49e8a5b00 也是常用的分析软件，里面包含有使用说明。 六、XRD文件转换 地址： https://www.doczj.com/doc/cc11601090.html,/d/79f9293 ... 366fbe4fcb01d130300 七、分子三维结构计算和预测软件地址： https://www.doczj.com/doc/cc11601090.html,/d/e0ca0e5 ... 52301a470bd0f545a00 八、rigaku 地址： https://www.doczj.com/doc/cc11601090.html,/d/6a39530 ... 8ce627de0082640c900 九、Mercury 1.4.1 地址： https://www.doczj.com/doc/cc11601090.html,/d/007e31e ... 344caa3c042fca1d000 十、Atoms_V6.1 地址： https://www.doczj.com/doc/cc11601090.html,/d/c8e4c85 ... 84a9cd9e9c9b1793d00 十一、SHELXTL 地址： https://www.doczj.com/doc/cc11601090.html,/d/7844e1b ... 6d333f55e41da194301 十二、Diamond2.0 地址： https://www.doczj.com/doc/cc11601090.html,/d/7c99e9c ... deab92d3e56603b5000 十三、Diamond 3.1 地址： https://www.doczj.com/doc/cc11601090.html,/d/2012c71 ... 2ba8f23e420d98d0802
Siroquant Version 3 User Manual
Published by: Sietronics Pty Limited Unit 3/22 Walder St PO Box 3066 Belconnen ACT 2616 Email: spl@https://www.doczj.com/doc/cc11601090.html,.au Web: https://www.doczj.com/doc/cc11601090.html,.au Copyright ? 2007 Sietronics Pty Limited. All rights reserved. First edition: December 2006, minor revisions, March 2007.
Siroquant Version 3 User Manual Table of Contents Introduction (1) Manual Overview: (1) Manual Conventions: (1) 1.Siroquant Overview (2) 1.1Software Description (2) 1.2Siroquant Objectives (2) 1.3.Software License, Trademark and Copyrights (2) 1.4Computer Specifications (2) 1.5Installation Instructions (3) 1.6Folders (4) 2.Siroquant Files (5) 2.1Task Files (*.TSK files) (5) 2.2Task Option File (5) 2.3Data Files (various types) (5) 2.4Databases and Databanks (6) 2.4HKL files (6) 3.Siroquant User Interface (9) 3.1Main Application Window (9) 3.2Task Display (10) 3.3Main Application ToolBar (12) 4.Basic Level Operations (16) 4.1Preparing Calculated *.HKL Files (16) 4.2Preparation of An Analytical Task (18) 4.3Task Parameters Dialog (21) 4.4Phase Dependent Parameters Dialog (23) 4.5Stage Control and Refinement dialog (26) 4.6Background Refinement dialog (28) 4.7Background Subtract dialog (29) 4.8Excluded Regions form (31) 4.9Calibration form (32) 4.10Advanced Halfwidths (33) 4.11Editing the Current Task (35) 4.12Starting a refinement (38) 4.13Displaying hkl Bars (38) 4.14HKL Bar Palette (39) 4.15Quantitation Results (40) 4.16Quantitation Charts (41) 4.17Refinement Statistics χ2 (42) 4.18Overview of Intermediate level features (43) 4.19Overview of Advanced level features (44) 5.Intermediate Level Operations (45) 5.1Extra Display Features (45) 5.2Template Tasks (46) 5.3New Task Wizard (48) 5.4Phase Status (52) 5.5Phase Preview (52) 5.6Print Out (54)
XRD分析软件简介 1.XRD分析软件 常用的软件一共有四种。 1.pcpdgwin 有人认为是最原始的了。它是在衍射图谱标定以后，按照d值检索。一般可以有限定元素、按照三强线、结合法等方法。所检索出的卡片多时候不对。一张复杂的衍射谱有时候一天也搞不定。 2.search match 可以实现和原始实验数据的直接对接，可以自动或手动标定衍射峰的位置，对于一般的图都能很好的应付。而且有几个小工具使用很方便。如放大功能、十字定位线、坐标指示按钮、网格线条等。最重要的是它有自动检索功能。可以帮你很方便的检索出你要找的物相。也可以进行各种限定以缩小检索范围。如果你对于你的材料较为熟悉的话，对于一张含有4，5相的图谱，检索也就3分钟。效率很高。而且它还有自动生成实验报告的功能！ 3.High Score 几乎search match中所有的功能，highscore都具备，而且它比searchmatch更实用。 （1）它可以调用的数据格式更多。 （2）窗口设置更人性化，用户可以自己选择。 （3）谱线位置的显示方式，可以让你更直接地看到检索的情况 （4）手动加峰或减峰更加方便。 （5）可以对衍射图进行平滑等操作，是图更漂亮。 （6）可以更改原始数据的步长、起始角度等参数。 （7）可以进行0点的校正。 （8）可以对峰的外形进行校正。 （9）可以进行半定量分析。 （10)物相检索更加方便，检索方式更多。 （11）可以编写批处理命令，对于同一系列的衍射图，一键搞定。 4.jade 和highscore相比自动检索功能少差，但它有比之更多的功能。 （1）它可以进行衍射峰的指标化。 （2）进行晶格参数的计算。 （3）根据标样对晶格参数进行校正。 （4）轻松计算峰的面积、质心。 （5）出图更加方便，你可以在图上进行更加随意的编辑。 https://www.doczj.com/doc/cc11601090.html,/groups/@g2385945/680997.topic 整个网址上可以下X'Pert HighScore Plus(XRD分析软件)及其XRD卡片 其实什么软件都一样用，关键还是要下的到，不过这里可以下到PDF2—2004标准卡片库。在宿舍用EMULE下的很快的，如果没有装EMULE，右击直接下载就可以了。网页里面有导
xrd分析软件Jade5.0和Highscore 转载 xrd分析软件有4种： 1.pcpdgwin 该软件是最原始的了。它是在衍射图谱标定以后，按照d值检索。一般可以有限定元素、按照三强线、结合法等方法。所检索出的卡片多时候不对。一张复杂的衍射谱有时候一天也搞不定。 2.search match 可以实现和原始实验数据的直接对接，可以自动或手动标定衍射峰的位置，对于一般的图都能很好的应付。而且有几个小工具使用很方便。如放大功能、十字定位线、坐标指示按钮、网格线条等。最重要的是它有自动检索功能。可以帮你很方便的检索出你要找的物相。也可以进行各种限定以缩小检索范围。如果你对于你的材料较为熟悉的话，对于一张含有4，5相的图谱，检索也就3分钟。效率很高。而且它还有自动生成实验报告的功能！ 3.high score 几乎search match中所有的功能，highscore都具备，而且它比searchmatch更实用。 （1）它可以调用的数据格式更多。 （2）窗口设置更人性化，用户可以自己选择。 （3）谱线位置的显示方式，可以让你更直接地看到检索的情况 （4）手动加峰或减峰更加方便。 （5）可以对衍射图进行平滑等操作，是图更漂亮。 （6）可以更改原始数据的步长、起始角度等参数。 （7）可以进行0点的校正。 （8）可以对峰的外形进行校正。 （9）可以进行半定量分析。 （10)物相检索更加方便，检索方式更多。 （11）可以编写批处理命令，对于同一系列的衍射图，一键搞定。 4.jade 和highscore相比自动检索功能少差，但它有比之更多的功能。 （1）它可以进行衍射峰的指标化。 （2）进行晶格参数的计算。 （3）根据标样对晶格参数进行校正。 （4）轻松计算峰的面积、质心。 （5）出图更加方便，你可以在图上进行更加随意的编辑。 Jade5.0的使用初步说明 1、数据输入 由于不同的X射线衍射仪输出的数据类型不同，但都可以将数据转换成txt文档或Ascii格式的文档（文件名为*.txt 或*.asc），为提高软件的通用性jade5.0提供了以txt文档或Ascii格式输入数据。运行jade5.exe首先进入以下界面 中间的窗口用于选择需打开文件，左侧选择文件路径与资源管理器的操作相同，右侧选择打开文件的类型，一般选择XRD Pattern files(*.*)，这时在右下方的窗口中将显示左侧被选择文件夹中所有能被该软件识别的文件，然后选择需要分析的数据文件，点击菜单栏Read进入主窗口，此选择窗口可以通过主窗口中file/patterns进入。 2、背景及Ka2线扣除 在主菜单栏中选择analyze/fit background进入如下窗口：