1. The Powder Diffraction File Release 2006
PDF-4+
The Powder Diffraction File
Release 2006

2. Index – Use direct links to skip to the section
Fundamentals
Design and Purpose
Data sources and collaborations
Quantitative Analysis with PDF-4+
Material Data Sets (Entries)
Pattern Simulations
Molecular Display
Searches and Data Mining
Pattern Fitting
Combining Tools – Analyzing polymorphs

3. Notice This presentation gives an overview of features and
capabilities found in the Powder Diffraction File (PDF),
specifically PDF-4+ Release 2006.
This presentation represents a small portion of the
capabilities in the database. The presentation
focuses on the database and not on the capabilities
of the database when combined with the world’s leading
data analysis programs.
The database itself contains over 500 pages of help
file documentation. This includes definitions and terms
of the classifications and calculations used in the database.

4. Fundamentals

5. PDF-4+ Basic Capabilities
PDF-4+ contains 254,873 entries.
Entries contain > 85 data fields, some fields
such as d, I, h,k,l and atomic parameters may
contain dozens to hundreds of data points.
There are 65 different data display options.
There are 44 search options.
Display and search options can be combined and permuted
using a JAVA interface. This results in nearly endless combinations
for data display and analysis, only a few of which are described here.

6. Powder Diffraction File (PDF)
PDF Databases are designed to work with most
commercial diffraction analysis software packages.
The ICDD works with software distributors so
that the PDF seamlessly interfaces to their software.
Many features in the database are specifically designed
for distributor use.
A list of compatible software and distributors can be found here.

7. Diffraction Analysis Software interfaced to PDF Databases
Company Software
Bede Bede Search/Match
Bruker AXS EVA, DiffractPlus,
PolySNAP, Topas
Bruker AXS SAS DiffractPlus, EVA
(formerly Socabim)
Crystal Impact Match, Endeavor
Digital Data Corp MacPDF
EDAX ACT, OIM
GE Inspection Rayflex Search/Match
GBC Traces
HKL Technology Flamenco
Inel WinFit
ITAL Structures WinDust32, WinSearch32
Kratos (Shimadzu) PDF-2 Search Software
Company Software
MDI JADE, jPOWD RIQAS, RUBY
Overseas X-ray PDF Plus
Oxford Instruments Flamenco
Oxford Cryosystems Crystallographica
PANalytical X’Pert Highscore Plus
Rigaku JADE, jPOWD, RIQAS, RUBY
RMS Kempten ADM/PADS
Sine Theta 2TdST
STOE & Cie GmbH WinX Pow
Tasker Applications TXRDWIN
Thermo Electron WinXRD
ZDS SEARCH/MATCH,
QUANT
Please check with the vendor to match their software with the specific release of the PDF database (year and type, i.e. PDF-4+ Release 2006).

8. Design & Purpose

9. All PDF Databases are designed for rapid material identification
All PDF Databases are designed for rapid material identification. This differentiates a PDF database from all other databases of crystallographic or physical property data. If you are working on a known material another database may be more appropriate for your work.

10. Powder Diffraction File
Rapid Material Identification with the PDF
The database is designed to use input data and match it to
candidate reference materials.
Most matching is done by comparing sets of d-spacing and Intensities,
however it can also be done by chemistry, properties, structural
and crystallographic classifications – using dozens of different
searches.
All data are converted to a standardized format for rapid search.
There are many embedded indexes facilitating searches.
Data entries are extensively cross referenced to other entries and to
physical and chemical measurements.
Data are extensively classified by chemical and structural types;
each classification can be searched.

11. Sources of Data

12. The Powder Diffraction File PDF-4+ Database
Data Sources for the Database
1) Publications, journals, scientific periodicals and theses
2) ICDD Grants for new materials (~60 annual grants)
3) Data collections donated by companies or individuals
4) Data from other Database organizations that they
collect from scientific publications
The Powder Diffraction File contains a compilation of data
from 5 global databases. PDF-4+ uses 4 database sources.

13. PDF Databases – Continuous growth and change
Data on new materials are being constantly collected and published by laboratories around the world so the PDF database continually grows.
With time, data quality has steadily improved in both accuracy and precision. (Better hardware, optics, software and computational power as a function of time). This leads to improved accuracy in the database and the diffraction method of analysis.
A major function of the ICDD editorial system is to evaluate quality and standardize data that has been collected by global sources over decades of time. The quality evaluations and standardization processes are also
updated continually and the entire database gets reviewed each time.

14. Powder Diffraction File – Database Collaborators
Cambridge Structural
Database (CSD)
ICSD
NIST
Linus Pauling File (LPF)

15. Each PDF database contains data from several database sources
254,873 Entries
PDF-4/ Organics
312,355 Entries
Release 2007
PDF-2
186,107 Entries
ICDD, NIST, ICSD + LPF
ICDD-organics + CSD
ICDD, NIST, ICSD

16. PDF-4+
The PDF-4+ and its subset, PDF-4/Minerals, are the only PDF databases that contains data from the Linus Pauling File (LPF). The LPF is currently the largest single global source of inorganic atomic coordinates and crystallographic parameters.
It is also a large source of data on inorganic materials, many
with unique compositions. This data is added to inorganic materials data from ICDD, NIST and ICSD to form the comprehensive data collection in PDF-4+.

17. 500,000 Material Data Sets and Growing
500,000 Material Data Sets and Growing! Data from global sources – collected, translated, edited and standardized
PDF-4/
Organics
60 Years
PDF-4+

18. PDF-4+ More Data and New Data
Distribution of data by number of
elements, PDF-2 and PDF-4+
Unique Formula

19. Database Codes
The first two digits in any PDF number contains the database
Code. For example PDF is the PDF number for
an Fe3O4 entry that is sourced from the Linus Pauling File
(04-LPF).

20. Material Data Sets (Entries)
Each entry contains
Chemical information and nomenclature
Experimental conditions
Diffraction data including d,I and h,k,l listings
Journal reference and bibliographic citations
Crystallographic data
Individual entries, such as the one for
Acetaminophen, PDF , displayed
on the left may contain thousands of
alphanumeric data fields.
Print display of a
PDF entry

21. Acetaminophen
PDF
A multi-page nested display, shown below, is used to display the data in PDF-4+.
Printed Form for Data

22. Quantitative Analysis with PDF-4+

23. PDF-4+ The PDF-4+ database is designed for rapid identification
and quantitative analysis.
Quantitative analysis can be performed by any of three different methods and the database provides the properties required these analysis techniques.

24. Quantitative Analysis and PDF-4+
Method Database Quantity Required by
of Quantitation the Method
Reference Intensity Ratio 165,923 Entries with I/Ic
Rietveld Analysis 98,291 Structures with atomic
parameters and unit cells
Full Pattern Analysis 254,873 entries all with full
digital patterns that can be
modified for wavelength,
radiation (x-rays, neutrons, electrons) instrumental and specimen effects

25. Full Pattern Analysis
Digital patterns of ~150 A Cellulose II and Ib, with crystalline
stearic acid. Experimental data on a natural product tablet in blue.

26. Automated Quantitative Analysis by XRD
PDF-4+ databases provide reference data, viewing software, critical physical properties and crystallographic properties required for quantitative analysis.
The database is designed to work with many software
packages, including those of all major global instrument
manufacturers. These software packages provide the
required calculations and refinements for automated
quantitation utilizing the data in PDF-4+. With modern software and databases this operation is seamless and can be often be done in minutes.

27. Features – The PDF Entry

28. 1
The main entry
page includes
several display
options 1
and data in
nested display
Pages. 2 2
These are activated
by the “point” and
“click” of a mouse.

29. Display Options Pattern Simulations 1 Digital Diffraction Pattern
Electron Diffraction
Simulation
Electron Backscatter
Pattern
Digital Diffraction Pattern

30. Molecular Dimensions & Graphics1
Display Options
Molecular Dimensions & Graphics
Molecular Graphics
Bond Angles & Distances

31. Pattern Simulations 1 Options for the addition of multiple phases,
instrument and specimen factors, wavelengths.
Options for import/export and graphic display
Calculations.
Crystallite size
simulation

32. Display Options – d,I Listings
Right click the mouse to Undock pattern listing and compare data
with different instrument configurations.
Fixed Slit
Variable Slit
Integrated I
Note how the intensities changes as
a function of optical configuration, resolution.

33. 2
Data in Nested Display
Print Forms

34. Data in Nested Display – Computer Display 2
Subfile designations, pattern
cross references (active link),
Pearson symbol and
prototype assignment
Experimental and
Bibliographic reference
Opening page – status,
formula, quality mark
Structure, symmetry,
atomic positions,
active link to atomic
environment display
Editors evaluation
and database cross references

35. Display Fields in PDF-4+
Color Coding Key
Fields filled in >80% of the 254,873 entries
Fields filled when the data is provided by the original source
Fields filled by an field expert editor, consultant or volunteer editorial task team
Quality indicator measurements

36. Display Fields Accessible from the Main Entry page through nested page displays
PDF
PDF#
Status
Quality Mark
Pressure/Temperature
Chemical Formula
Weight %
Atomic %
ANX
Compound Name
Mineral Name
Common Name
Experimental
Radiation
Wavelength
Filter
d-spacing type
Cutoff
Intensity type
I/Ic
Camera Diameter
Reference
Title
Author
Citation
Physical
System
Space Group
Aspect
Author Cell
Volume
Reference
D calc
D meas
D structure
SS/FOM
Melting Pt Z
R-Factor
Error
Crystal
Space Group Z MW
Crystal Cell
Crystal Volume
Crystal axial ratio
Reduced Cell
Reduced Volume

37. Display Fields Accessible from the Main Entry page through nested page display
Only in PDF-4+
Optical
alpha
beta
gamma
Sign 2V
Reference
Structure
TF type
Coordinate Table
Atom
Number
Wyckoff Position
Symmetry
x,y,z
SOF (Site Occupancy)
ITF (Isothermal TF)
AET (Atom Environment)
Symmetry Operator
Anisotropic Temp Factors
Miscellaneous
CAS #
PDF Cross References
and status
Pearson Symbol
Prototype Structure
LPF Prototype
Mineral Classification
Zeolite Classification
Subfiles
Entry Date
Last Modification Date
Editorial
Editors Comments
includes comments
generated by statistical
analysis of the data
User Comments
Shared Comments
98,291 Structures in PDF-4+

38. Display Fields in PDF-4+
Expanded views
of the d, I, h,k,l
listing
and
stick figure.
Both are interactive
displays where the
user can expand,
sort and scale the
data.

39. Searches and Data Mining

40. Searches and Data Mining
ICDD problem solving software
Completely re-written in Java
Powerful search and retrieval
Numerous display options
Flexible user-interface
Features based on our extensive RDB knowledge and user feedback
Java
Faster database access
Portable code for Web (WebStart)
Cross-platform (Linux/Unix)
User feedback
Customers
Members
Employees

41. Searching Opening screen menu Main Search Page Search Icon
“Point and Click”
Opening screen menu
Main Search Page
Searches are performed by
using the search option on the
program DDView+. This
program is embedded in the
database. If you use vendor
display software you may have
to start the program “ICDD
PDF ” from your
program menu to see the options
described here. Every PDF-4+
database has this program. (It is
an option for PDF-2).

42. Search Central input form (Main Search Page)
45 unique criteria in 7 categories
Multiple input methods:
Lists
Text
Numeric
Estimated Standard Deviation (ESD)
Ranges
Periodic Table
Composition Table
Logical Boolean operators
Powerful cumulative searches
Criteria selection awareness
Criteria Examples
Subfile
Empirical formula
Composition
Reference data
Cell axis/volume (author, crystal, reduced)
Space group
Long/Strong lines
Categories
Subfiles/Database Filters
Periodic Table
Elements
Names
References
Structures
Miscellaneous

43. Searches are activated
by point and click operations
or alphanumeric entry. Activated
fields become highlighted in red.
Multiple fields can be active.
In this example
search fields for LPF,
star quality, primary,
ambient data for Si and O
were activated.

44. This search activated an empirical formula combined
an elemental composition analysis
with a specific space group
and compound name.
Input element composition
analysis with error limits

45. Search Display - Results2
The criteria
matched 1,817
entries in PDF-4+
Alphabetical Formula Index sort: Formulae are sorted on 1 common
Formulae are sorted by elements alphabetically starting with the sort element.
If 2 formulae elements are alphabetically equal and contain 2 or 3 elements, they are sorted by the ratio of the second-to-last divided by the last atomic weight from largest to smallest.
If formulae elements are alphabetically equivalent and higher than a ternary system, atomic weights are sorted alphabetically.
Quality Mark (proprietary sort): Star, Indexed, Blank, Low-Precision, Calculated, Prototyping, Rietveld, Hypothetical
All 1,817 entries
search results can
be accessed through
the scroll bar. 3 1
The search criteria are given in
the search description.

46. Search Results - User Preferences
Click on the
“Preferences”
Icon or
Use the Fields
drop down menu
User selection of the display fields can be
done by point and click interfaces or a drop
down menu. The menu above allows the user
to add, drop and change the display order.

47. Search Results Same search criteria as before but now
the user defined order preferences are
displayed:
Mineral name,
Quality mark,
Reduced cell
parameters,
Pearson symbol
and chemical
formula.
Minerals sorted
Alphabetically.
Reverse order by
clicking on the
Header.

48. Search Results – Display Algorithms & Calculations
Sorting algorithms:
Alphabetical
Alphabetical Formula Index
Numerical
Proprietary
Calculations:
Mean
Median
ESD
Calculations
Displayed
Same search, the user can highlight
any numerical field and obtain a
mean, median and ESD for the entries.

49. Application Example 1: Phase Identification
From research we obtain the following data:
Pattern is cubic
Lattice parameter a=12.348(.010) Å
Pattern density is ρ=4.9(.1) g/cm³
Pattern color is red
Pattern melting point is 677(5) °C
We then input these user data into DDView+ and look for possible solution(s).
Author’s Cell Axis: Cubic, a: (.01) Å
Density: 4.9(.1) g/cm³
Color: Red
Melting Point: 677(5) °C

51. Problem 1 – Results (Answer)
With the given input data there are only 2 search hits out of 254,873 entries in the database.
One entry is from the experimental collection (PDF 00); the other from the LPF collection (PDF 04).

52. Application: Problem 2 From research we obtain the following data:
Powder Pattern Space Group is Fm-3m
Pattern only contains elements Cu and Zn
Input user data into DDView+
Additionally:
If we measure the lattice parameter:
a=3.640 Å, what is the likely concentration of Zn in the alloy?
Space Group: Fm-3m
Periodic Table: Only (Cu, Zn)

53. 1 2 3
Search input
provide search criteria
with results
displayed 1 2 3

54. Problem 2 – Results (Answer)4
(Obeys Vegard’s Law)
Answer: Estimated Zn weight concentration is 15%
The data from the
search form
were exported and
plotted to identify the composition based on lattice parameter.
(Composition plot not done by the database)
Non-ideal solution behavior 3

55. Application Problem 3 – Answer shown, sequence described
FERRO-PARA ELECTRIC TRANSITION IN BaTiO3
Sequence of 1) Search by composition 2) Search by temperature
3) Display results, 4) Compare cell parameter with temperature*,
5) Plot the results.
* Specific temperature given in the comments section of the entry, so you
would need to display the comment section.

56. Pattern Fitting and Simulations

57. Pattern Simulations Point & Click Click on this icon brings
up the “Preferences” menu
options for display features

58. Diffraction Pattern Options
Radiation Settings
Anodes
X-Ray Diffraction
Neutron Diffraction
Electron Diffraction
Types
Kα1
Kα2 Kβ
Kα(avg)
Kα1+2
Kα1+2+Kβ
Custom wavelength

59. Diffraction Pattern Options
Geometry Settings
Bragg-Brentano
Debye Scherrer

60. Diffraction Pattern Options
Profile settings
pseudo-Voigt
Modified Thompson-Cox-Hastings pseudo-Voigt
Gaussian
Lorentzian
Particle Size
To change to a user
defined crystallite size
enter a value, hit return
and then click apply.

61. Graph Icon 1 Click once 1 Get digital pattern Click again
Add, subtract, scale
input other ref. patterns
or experimental data. 1 2 2 3
Crystallite size series
Data input
console, provides
data input and
pattern options,
each pattern can be
adjusted separately.

62. Application Example 1 Pattern simulation of complex mixtures
using PDF-4+, DDView+
Data input
console, goes
to pattern options
Raw Data
6 Phase solution used data from 3 different databases
ICDD-powder, ICSD – single crystal, LPF- single crystal

63. Application Example 2 Full pattern analysis, mixed crystallite sizes
Digital patterns of ~150 A Cellulose II and Ib, with crystalline
stearic acid. Experimental data on a natural product tablet in blue.

64. Combining Tools – Analyzing Polymorphs

65. Example – Examining the Polymorphs of SiO21 1
Execute a Search - Primary patterns, star quality, ambient conditions,
2 elements, formula SiO2

66. Display the results 2
37 star
quality,
primary
patterns
Search Summary

67. Customize the results
Why are there so many primary star patterns for SiO2?
To study this, customize the display by selecting preferences. 3

68. Customized results 4
SiO2 polymorphs – differences in Mineral Name, Common Names,
Space Groups, Unit Cell Volumes, Pearson Symbols.

69. Analyze SiO2 polymorphs4
Highlight a selection
of data entries in the
results, then right click to
provide a menu of options.
CTRL and Shift Key can both be used to highlight user specific entries.
From the menu, diffraction pattern is
selected 5

70. Polymorphs of SiO2
All eight highlighted entries are simultaneously plotted. The data
clearly show that these are polymorphic materials with different
characteristic diffraction patterns for each polymorph.

71. Customize the results
Why are there multiple primary star quality patterns
for same polymorph?
To study this, use the prior results (37 SiO2 primary star patterns) and
look at entries with the same space group, Pearson symbol and
reduced cell volume.
Three entries for Stishovite - why?

72. Three entries for Stishovite - why? Examine the Comments!
Single Crystal
Synthetic Powder
Mineral
High quality data on three different
specimens taken by three different
Laboratories. Mineralogists typically
prefer known minerals, chemists may
prefer high purity synthetic or single
crystal – if different in source or properties
ICDD editors will keep all entries.
Examine properties
Slight difference
in density, I/Ic

73. SiO2 Why are there 37 primary, star patterns?
Answer
Polymorphs, a primary pattern is selected for each different
polymorphic form (~24 different polymorphs).
Different physical properties – the same polymorph may
have slightly different physical properties or chemistry
(i.e. due to calcination). This is especially
common in minerals from different geographic localities.
Difference source, for example mineral or synthetic, powder
or single crystal.