CIC Photonics

1
CIC Photonics

• IRGAS Training

2
Schedule - Day 1

• FTIR analysis
• IR spectrum
• Michelson interferometer
• Fast Fourier transform and corrections
• Interferogram, single beam spectrum, absorption
  spectrum and transmission spectrum
• Beers law
• Instrument resolution
• Quantification analysis-Classical Least Squares
  introduction
• Hardware description
• Bomem WorkIR
• Instrument purge
• Manual manifold
• SPGAS software
• IRGAS 100
• IRGAS configuration manager
• Data retrieval

3
Schedule - Day 2

• SPGAS software cont.
• Qmax quantification manager
• IRGAS spectra reprocessing software
• Hardware installation
• System power
• Pipe installation
• Instrument purge
• Software installation
• IRGAS software
• Bomem Ethernet drivers
• System verification
• System maintenance

4
Schedule - Day 3

• IRGAS worksheet
• IRGAS options
• IRGAS product array
• Marketing and selling strategies and techniques
• Competitors and competing products
• Service and maintenance

5
FTIR Analysis

• Tab 1

6
Light Spectrum

• Infrared is invisible light ranging from 1mm to
  750nm in wavelength
• Infrared light can be divided into three parts
• Far infrared -1mm to 10µm
• Mid infrared - 10µm to 2.5µm
• Near infrared - 2.5µm to 750 nm

7
Infrared (IR) Spectrum

• IRGAS System mid infrared range
• 2.5µm 25µm in wavelength
• 4000 cm-1 400 cm-1 in wavenumbers
• Wavelength (?)
• Wavelength (1/wavenumber)10,000
• Wavenumber (cm-1)
• Wavenumber (1/?)10,000

8
IR Molecules

• Not every molecule absorbs infrared light
• Monoatomic
• He, Ar, Ne, etc
• Homoatomic diatomic
• N2, O2, H2, etc
• N N
• Molecules that do absorb infrared light
• Water is a good example
• O
• H H

9
Michelson Interferometer
2
1
3
4

• Step 1 Beam leaves IR source and hits
  beamsplitter where it is sent straight through
  and at a 90 angle
• Step 2 The 90 angle beam hits a fixed mirror
  and is sent back to the beamsplitter
• Step 3 The beam that went straight through hits
  a movable mirror and is sent back to beamsplitter
• Step 4 The two beams recombine, go through the
  gas cell and travel to the detector

10
Michelson Interferometer

• When ABAC the phase of the frequencies look the
  same
• When ABAC1/4?, then the phase of the
  frequencies are opposite in regards to maximums
  and minimums

11
Michelson Interferometer

• When ABAC and the two recombine you get stronger
  maximums and minimums
• When ABAC1/4? and the two recombine they cancel
  one another out and result in a flat line

12
ABB Bomem Michelson Interferometer

• It has two sets of mirrors that move by a
  pivoting motion
• This design is called a wishbone configuration
• This configuration is more robust
• It can be placed in any orientation
• This configuration only has to be smooth at one
  point vs. the traditional interferogram that has
  to be smooth along a rail

13
ABB Bomem Michelson Interferometer
14
ABB Bomem Michelson Interferometer
Laser
15
Fast Fourier Transform

• The highest peak intensity is attained when ABAC
• The maximum of the highest intensity peak is
  called the zero path difference (ZPD) point
• After the interferogram has been created by the
  instrument, the Fourier transform is applied to
  it, which then results in a single beam spectrum

16
Single Beam Spectrum
17
Single Beam Spectrum
18
Single Beam Spectrum
19
Single Beam Spectrum
20
Transmission

• The ratio between the sample and the background
  spectrum

21
Transmittance Spectrum
22
Chemometrics

• Based on the transmission spectrum chemometrics
  can be applied
• Chemometrics The application of statistical and
  mathematical methods for the design or
  optimization of chemical experiments and for the
  efficient extraction of information from chemical
  data
• Two types of chemometrics
• Qualitative (identification)
• Quantitative (quantity)

23
Absorbance
24
Beers Law

• Says that concentration is directly proportional
  to absorbance (linearity)
• Beers law equation is A abC
• Where A absorbance
• a absorptivity of the molecule
• b pathlength that the light travels
• C concentration

25
Instrument Resolution

• The more points per peak the higher the
  resolution
• The higher the resolution the more noise, but the
  better peak separation
• Common resolution used for an ABB Bomem
  instrument is 2 cm-1
• Ranges between 1 cm-1 to 128 cm-1

26
Why Do We Need a Gas Cell

• Intensity of a peak is directly related to the
  of moles in a sample
• In the same area
• Solid will be very packed
• Liquid will be less packed
• Gas will be even less packed

27
Long Path Gas Cell
28
4Runner 6 Meter Gas Cell
29
Gas Cell Mirrors
Top view of field mirror
30
IR Beam Path
31
Classical Least Squares (CLS)

• The base equation is As AcK e
• Where As sample absorption
• Ac calibrated absorption
• K concentration
• e noise
• Using the above equation find K that minimizes e
• To minimize e we use the CLS method
• In this situation there are more equations then
  variables

32
Classical Least Squares (CLS)

• To simplify matters we assume that e 0
• The equation then becomes As AcK
• Matrix form

33
Classical Least Squares (CLS)

• In order to solve for K (Ac-1As K), Ac needs
  to be an inverse matrix
• Therefore AcTAs (AcTAc)K
• (1x1) (1x1)K

34
Problems with Initial CLS Approach

• Baseline becomes unstable throughout the day
• It can shift, slope, or curve
• These changes can be compensated for in the
  calibrated absorption matrix

35
Classical Least Squares (CLS)

• Accounting for these baselines changes the
  equation
• The eqn. becomes As AcK1 K2 K3
  K4
• The calibrated absorption matrix can be increased
  to accommodate the number of species being tested

36
Weighted Multi-band CLS

• A more complex version of the standard CLS
• The spectrum is separated into bands
• Each band is then calculated
• After all the bands are calculated they are added
  in a weighted averaged fashion
• The ones with the highest error and lowest signal
  are counted for less then the ones with the
  lowest error and highest signal

37
Hardware Description

• Tab 2, 3, 4

38
IRGAS Systems

• Thus far the oldest system in the field without
  maintenance is 4 yrs
• Out of 20-30 systems, there has only be a need to
  perform maintenance on 3 of them
• The Bomem spectrometer is high in reliability and
  low in maintenance
• There has been 2 hardware failures
• There was a burned out IR source

39
IRGAS Systems

• There is one basic package that can be dressed up
  in several different ways
• One reason our throughput is higher than
  competitors is because of mirror quality and
  coating
• Our objective mirrors are adjustable
• Sideways
• Rotational
• Competitors have mirror that are locked into
  place

40
ABB Bomem WorkIR
41
Manual Manifold
42
Manifold Parameters

• Flow Restrictor
• A flow of 30 psi in will give a flow of 5 slpm to
  the instrument
• Purifier
• Gives dry N2 to below 2 ppb
• Has a lifetime of more than a year if it is used
  24/7

43
Vibrations

• There are a number of designs of suspension
  systems to counteract vibrations
• These designs help to keep the data from being
  affected by a simple bump of the instrument bench

44
Typical Gas Cells

• Have a flow similar to turbulent flow and have a
  longer residence time

45
Laminar Flow Gas Cells

• The flow is like a waterfall
• Therefore there will be less turbulence
• Heated laminar flow gas cells
• The gas is in contact with the walls letting it
  reach a temperature similar to the gas cell prior
  to entering the cell

46
Gas Cell Flow Diagrams
47
f/5 Beam Geometry

• The higher the f / , the smaller the objective
  mirrors, the more light that is lost, the smaller
  the throughput

48
SPGAS Software

• Tab 6, 7, 8, 9, 10

49
Specialty Gas Analysis Software (SPGAS)

• IRGAS 100 system
• Collection quantification
• Qmax
• Quantification manager
• IRGAS Configuration Manager
• Configures parameters
• Quantification Reprocessing Tool
• Recalculating spectra

50
IRGAS 100 System

• After opening the software the first window is
  the monitor screen
• On the right side there is the available species
• On the bottom is the legend of the species that
  are being shown in the top window
• The top shows the concentration of all the
  species over time

51
IRGAS 100 Monitor Screen
52
IRGAS 100 System

• Collecting a background
• After opening the program, pressing the start
  button will automatically send the spectrometer
  to collect a background and then begin collecting
  a sample
• Seeing the sample
• Clicking on the desired species tab at the top
  will show you that species in real time
• That screen shows the fast concentration tracker
  (FCT) and the averaged sample

53
Advantages to Spectra Stream

• Provides high sensitivity detection of impurities
  (low ppb)
• Reduces the time response typically associated
  with FTIR (from minutes to seconds)
• Continuous collection of background
• Running average spectra
• Reduction in spectrometer drift
• Reduction of contribution of moisture
• System is very easy to use

54
IRGAS Configuration Manager
55
IRGAS Configuration Manager
56
IRGAS Configuration Manager
57
IRGAS Configuration Manager
58
IRGAS Configuration Manager
59
Data Retrieval

• Data storage
• By default the data gets stored on the C drive
• C\Program Files\CIC Photonics\IRGAS
• IRGAS data
• Quantification log
• Spectral records

60
Quantification Log Folder

• Data stored as a text file
• Can be converted to an excel file
• Copy file, paste in the same folder, rename with
  an .xls extension
• In the excel file
• Data storage names
• Folder with YY-MM
• Folder with Quan YY-MM-DD.log

61
Spectral Records Folder

• Stored with a .spc extension
• All market software writes and reads this format
• This was created by Galatic, now ThermoGalactic
• Data storage names
• Folder with YY-MM-DD
• Absorbance File
• Abs YY-MM-DD HHMM.zip
• Background File
• Bck YY-MM-DD HHMM.zip
• Sample File
• Smp YY-MM-DD HHMM.zip
• Residual File
• Res YY-MM-DD HHMM.zip

62
QMax

• Using existing calibration file

63
QMax
Quantification Set
Spectral Set
Calibrated Spectral Record of specific molecule
64
Non-linear Behavior

• As a rule of thumb a species behaves non-linear
  when it is higher than 0.1 a.u.
• The non-linear correction graphs curve is
  modeled by ax3bx2cxd 0
• In this equation the values that are necessary to
  find are a, b, and c
• To do this non-linear correction there needs to
  be at least 3 spectral records
• In general when the residual curve is flat line
  that indicates that there is non-linear behavior

65
QMax

• Starting a calibration from scratch

66
Synthetic Calibration Set

• Instrument Line Shape (ILS)
• Each instrument has its own
• HITRAN database
• Contains the absorption coefficients of different
  components
• Doesnt contain the ILS of specific instruments
• MALT software
• Created by Dr. David Griffith from the University
  of Wollongong in Australia
• Models ILS parameters

67
MALT

• Calculates spectra for single homogeneous path or
  for multiple layers
• Includes instrumental parameters into the
  calculations so the calculated spectra match the
  line shape, resolution and wavelength shift of
  the measured spectra
• Uses HITRAN molecular spectroscopy databases

68
Gas Calibration

• When a gas is not in the HITRAN system, it is
  necessary to produce the calibration
  non-synthetically
• Start collecting data
• Flush the gas cell several times with the gas
• During this time find the equilibrium point of
  each flush
• Take these points and average them to use for the
  calibration
• This will give a better signal to noise ratio

69
HITRAN/MALT vs. Actual Calibration

• Advantages
• Calibration data free of noise
• Best match to the measured spectrum according to
  the least squares criteria
• Operational costs reduction
• Non-time consuming calibrations
• Precision at least as good as that of traditional
  methods ( ? 3)

70
HITRAN/MALT vs. Actual Calibration

• Disadvantages
• Provides analysis only over gases included in the
  HITRAN database
• System requires regeneration of calibration data
  if spectrometer or gas cell change

additional gases by standard calibration
procedures
71
IRGAS Spectra Reprocessing
72
IRGAS Spectra Reprocessing
73
Gas Analysis Modules
74
Absorbance Data _at_ 1ppm/meter
75
Software Installation
76
Software Installation

• The installation window should automatically
  pop-up
• After the installation has been completed, check
  that the computer and spectrometer are
  communicating with each other

77
Establishing Communication

• Network
• Instrument address 192.168.0.127
• Computer address 192.168.0.YYY
• Where YYY is any number between 0 and 225 that is
  not 127

78
Establishing Communication

• Two Ethernet configurations
• Straight through
• Crossover

79
Ethernet Connection

• Straight through configuration
• 1 1
• 2 2
• 3 3
• 4 4
• 5 5
• 6 6
• 7 7
• 8 8

80
Ethernet Connection

• Crossover configuration
• 1 1
• 2 2
• 3 3
• 4 4
• 5 5
• 6 6
• 7 7
• 8 8

81
Verifying Communication

• Changing network address
• Control panel
• Network connection
• Local network
• Properties
• Last check for communication
• Control panel
• ABB Bomem

82
Marketing and Selling Strategies and Techniques

• Tab 13

83
Worldwide Customers
84
Semiconductor Applications

• Wafer yield enhancement
• By reducing O-atom defects
• Process reaction monitoring
• By confirming reactants/products
• Supply gas quality monitoring
• Abatement tool efficiency

85
Semiconductor Dry Process
http//www.jp.horiba.com/semicon_e/measurement/gas
.htm
86
Semiconductor Industry
87
Semiconductor Applications

• A large amount is spent on equipment in the fab
  area
• In-situ monitoring is being looked at to prevent
  the damage of large quantities of goods
• The equipment section is also supplying the raw
  materials section, not just the Semi fab
• Getting the companies to upgrade current
  equipment is difficult but results is a large
  sale

88
Chemical Applications

• Specialty gas purification
• Combustion thermodynamics
• Aero-engine optimization
• Destructive testing release of hazardous gases
• Gas blending

89
Environmental Applications

• Plant air monitoring
• Stack gas emissions
• PFC emissions
• Homeland Security
• Chemical Weapon Agents
• Toxic Industrial Chemicals
• Illicit Drugs

90
Our Product Line

• FTIR gas analyzer systems
• Long and short path gas cells
• Custom gas cells
• Fiber optic probes (UV/VIS/NIR)
• Resell UV/VIS FO spectrometers
• FTIR sampling accessories
• ATR, transmission, reflectance, M-Press

91
Competitor Analysis
Research conducted by Los Alamos National
Laboratories marketing interns
92
Competitors and Competing Products

• Tab 5,12,14

93
Competitors

• FTIR gas analyzers
• MKS Instrument
• MIDAC
• Thermo Nicolet
• Other technologies
• Tiger Optics
• Delta F

94
Other Technology Competitors

• Tiger Optics
• Cavity Ring Down Spectroscopy (CRDS)
• Single gas at a time
• Delta F
• Tunable laser
• Single gas at a time

95
Differentiators
96
Gas Cells

• Laminar flow
• Faster gas exchange
• Eliminates dead space
• 316L Stainless steel / Nickel plated body
• More chemically resistant to acid gases and
  retain less moisture
• 304 Stainless steel mirror
• Proprietary fabrication and coating process
• Radius of curvature
• Surface finish smoothness
• 98.5 reflectivity
• High pressure tolerance
• 20 atm, 300 psi
• Hand aligned by expert personal to maximize
  throughput

97
IRGAS System

• Spectrometer
• ABB Bomem WorkIR
• Industrial ruggedness
• Compactness
• Very low failure rate
• Cost competitive
• Software
• Unique because it offers the weighted multi-band,
  multi-variant classical least squares method
• Patented on Spectra Stream w/ the fast tracker
  for early warning
• User friendly
• Configurations
• One package that can be dressed different ways
• Pre and post technical support

98
Scientific Package

• 4Runner gas cell
• ABB Bomem WorkIR spectrometer
• Coupling optics
• Suspension system

99
The 4Runner

• 0.6 liter volume
• 125 mm base path
• 304 stainless steel body
• Metal and Kalrez seals
• Welded VCR fittings for gas porting
• Heatable to 260C
• Integrated purge box with movable reference
  optics
• MgF2 protected, gold-coated stainless steel
  mirrors
• Evacuable pressurizable 10-4 Torr to 300 psig

100
Ranger-EN

• 9.6 meter fixed pathlength
• 1.7 liter cell volume
• 0.05 sq. m/L surface/volume
• Gold-coated SS mirrors
• All-metal, electropolished SS body
• External transfer optics
• Heatable to 200C
• Optional aluminum body glass mirror

101
Pathfinder-EN

• 0.4-10 meter variable pathlength
• Pressurizable to 50 psig
• Heatable to 200C
• Gold-coated SS mirrors
• All-metal, electropolished SS body
• Very high energy throughput
• Extremely chemically-inert

102
Scout-EN

• Nickel plated stainless steel 10cm gas cell for
  toxic and corrosive gas analyses heated and
  unheated versions.
• 28-cm3 volume
• Teflon-encapsulated Viton, Viton, or Kalrez
  O-rings for chemical resistance and temperature
  considerations
• KBr, CaF2, ZnSe, quartz, or sapphire window
  materials for UV-VIS and FTIR applications
• Evacuable and pressurizable 10-4 Torr to 150
  psig
• Heatable to 200C with heating mantle, tape, or
  dual bands
• 5 cm 15 cm pathlength versions also available
• Optional temperature controller
• Easy adaptation to all spectrometers

103
Montero

• 1.0 meter fixed pathlength
• 82.6 mm basepath
• Anodized aluminum cell body
• Gold-coated Pyrex mirrors
• Internal transfer optics
• Low 600 ml volume
• Purgeable beam conduits
• Swagelok (tm) gas ports
• Viton O-rings
• Choice of windows
• High energy throughput
• Unheated and heated versions
• Fits totally inside FTIR compartments

104
CR-V

• Extremely short path length
• 0.5mm to 1cm
• High Pressure
• Up to 100 atm
• Heated Option

105
IRGAS Options

• Tab 11

106
O-Ring Material Working Temperature Ranges
107
Window Thickness
108
Options

• Pressure and temperature based on ideal gas
  parameters
• Automated manifold systems
• System outputs
• Text based
• Analog and digital outputs

109
IRGAS Moisture Plus
110
IRGAS-SP
111
IRGAS EPI
112
IRGAS 100T
113
IRGAS 100MT
114
IRGAS 200RM
115
IRGAS 400
116
IRGAS XFlo
117
IRGAS Worksheet

• Tab 13

118
IRGAS Worksheet

• Important because it guides us in system
  parameters, options, and price quoting
• Important parameters
• Gases present in the mixture
• Estimated concentrations
• Temperature and pressure range
• Sampling time
• The parameters help to determine
• O-Ring material
• Window material
• Gas cell
• All of these can really vary the price of the
  product

119
IRGAS Worksheet

• Part A of the worksheet is for customers that
  only want a gas cell
• The entire worksheet is necessary for customers
  that want the whole IRGAS system
• Customers should fill out as much of the
  worksheet as possible

120
Warranties and Technical Support

• Tab 16

121
Warranty

• 1 yr parts and labor for gas cell and software
• 30 day on critical optical elements, ex. mirrors
• This is because we have no control over how the
  system is treated by the user
• 1 yr telephone and e-mail technical supprt

122
Technical Support

• 24/7 technical support is provided to the best of
  our abilities

123
System Maintenance

• Tab 15

124
Service and Maintenance

• Handled on a case to case basis
• Repair, test, ship
• System repaired
• Quality tested
• Shipped back to customer
• CIC Photonics pays the shipment back to customer
  if still under warranty, if not it is paid both
  ways by the user

125
Contact Information [phone](505)
343-9520 TechSupport_at_cicp.com