AD-R148 783 NULTIPHOTON PHOTOCHENICAL AND COLLISIONAL EFFECTS i/iDURING OXYGEN ATOM FLAK-.(U) ARMY BALLISTIC RESEARCHLAB ABERDEEN PROVING GROUND MD A N MIZIOLEK ET AL.

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IR TECHNICAL REPORT BRL-TR-2604

MULTIPHOTON PHOTOCHEMICAL ANDCOLLISIONAL EFFECTS DURING OXYGEN

ATOM FLAME DETECTION

Andrzej W. Miziolek

l-_ Mark A. DeWilde

C,October 1984

US ARMY BALLISTIC RESEARCH LABORATORY ,ABERDEEN PROVING GROUND, MARYLAND

84 11 27 055

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Destroy this report when it is no longer needed.Do not return it to the originator.

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V. FinalMI' LT I PHOTON PHOTOCHEMI CAL AND COLL I SIONALEFFECTS I)URINC OXYGEN ATOM FLAME DETECTION t, PERFORMING ORG. REPORT N,'AER

7. AL' THOR,. S. CONTRACT OR GRANT NUM6-:R'.

Andrzej W. ",iziolekM irk A. VeLde

9 P- RF3RMING O-IGANIZATION NAME AND ADDRE_.. 10 PROGrAM EEMENT.PROJ.E-r TASK

1"T Army Ballistic Research Laboratory AREA WORK uNIT NUMSE'V.AI N: AVIXBR - IBD 1L161102AH43A\-rdeen Proving Ground, M4D 210(5--5066

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IR IPPL FMFNTARr NOTES

'9 ( F Y wQPDS If r-,-', #,d *V y f .. v Ie esr- 1 , deni'lt h,- Mock nambeef

¢'" Pl tt-hem is trv 'Muliphoton Fluorescence!-'i,,r .v Transfr Oxygen Detect ionF' ,im %ton.

2r0 AP R wc Ct-m., - rierse .,aft of ,...ar d 14ontify twn bi.,k .Ieb*.) me

A Nd:YA; ptmpod dyo Iaser system was used to two-photon excite oxygen atomst .25.6 n," in ;in atmospheric pressure CH,/N 9 O/N., flame. Subsequent

I- is,;'io, at 844.7 nm from the dlrectl populated state, as well as a stronger(i1ission at 777.5 nm tue to the O(3p P-*3p P) collisional energy transfer

- pror's. s, w,- monitord. Two-photon resonant oxygen atom and hydrogen atom('1h.3 nm) omissi)ns were also observed in the absence of a flame. CloserI0 .amin;itirn revealed that the tightly focussed probe beam was producing

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20. Abstract (Cont'd):

these atoms by promoting multiphoton photolysis of the oxidizer, as well asfuel molecules. Thus, this type of laser diagnostic probe is potentially

-. quite intrusive depending on the combustion region that is probed, as well asthe laser energies used.

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TABLE OF CONTENTS%4*%

-A Page

[,NTROOUCTION ....... ...... ...... ...... ...... ...... ...... ...... 5

I I EXPERIMENTAL .................... .. ...................... 6

LI. RESULTS AND rD[SCLISS[ON............................... ... . ... .. . .. .. . .. .6

IV. rIS oNS ............................................ . . . . .. 3

S. d

ACKNOWLEDGEMENTS................................................... 14

REFER:NCES 15............................................... o ... 15

DSTR[BU TION LIST ................... ........... ... ........... 17

Accession For

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I . INRODUCTION

Propc 1 1 1t combust ion is a process of considerable complexity in whichhii h temperittir, chemical reactions play a major role. in order to understandthe actu.il htat releasing chemical steps that are involved, an extensiveprogram h.i' hen ongoing at BRL, as well as in other combustion researchinstitrltlon', where much simpler laboratory model flames are studied indetail. Stich studies involve the interplay of flame diagnostics (usuallybased on la.--r spectroscopy techniques) with flame modeling work, as well asallied kin ,tics efforts to supply necessary elementary reaction rate constantsrl s-h detaliled chemical flame models. In the area of flame diagnostics,las;er spectroscopy techniques such as absorption, Raman, laser inducedfluoresc'ence ([F), coherent anti-Stokes Raman spectroscopy (CARS), etc., havebeen able to detect the stable major flame species as well as many reactivemolecilar intermediates. There is, however, an important class of combustion

* *iitorneli,-tes, i.e., the flame atoms, such as H, 0, and N, which hashistoricallv eluded direct detection due to the lack of accessible energy

levels for single photon excitation.

Very recently, though, multiphoton excitation techniques have been

siuccessful in detecting the hydrogen and oxygen atoms in a flame. So far, twodistinct detection approaches have been demonstrated, one involvingmultiphoton eonission (MPE) 1 ,2 and the other multiphoton ionization (MPI), 3'4' 5

the latter allo referred to as optogalvanic detection. In the case of the

oxv en atoms, however, direct detection in a flame was first accomplished byspontaneous Raman scattering 6 and coherent anti-Stokes Raman spectroscopy

C,. (CARS). 7 Apparently, sensitivity limits and spectral interferences have" prevented further development of these spectroscopies for atomic flame

I etect 1on.

•1",e, - 3,Tdner, P . Gfrfstrom, and S. Sovanberg, "7loo-Photon Excitation ofAt?7-r','c Ox~jgen ~na Flame," Opt. Comm.n., Vol. 42, p. 244, 1982.

i 2 . uc' t, J.T. ,i inon, G.. King, O.W. Weeney, and N.M. Laur'endeau, "Too-I. P ton- xe ted F! escenzce Measurement of Hydrogen Atoms in Flames,"

- '. )pt. r"tt., Vol. 8, o. 365, 1983.

-" . *.4 oi0 itk, "Resonant 4uttiphoton Optogalvanic Detection of AtomicJ?yd.rogen ! z Flames," Opt. Lett., Vol 7, p. 437, 1982.

4.7.L.M ;olTs-ith, "Resonant Afultiphoton Optogaloanic Detection of Atomic

2ixyjen 7n V1 Zaes," J. Chem. Phys. Vol. 78, p. 1610, 1983.

":).,[Tioe;3., and T.4. Cool, "Detection of Atomic Hydrogen in Flames by* 1 .P JW? 'our-Photon Ton zation at 365 nm," Chem. Phys. Lett., Vol. 100,

' ... , .7.11. Hechtel, "Spontaneous Raman Scattering by Ground-State-'O r,,',n te Ot, L gett., Vol. 6, p. 36, 1981.

7R.,. Tqect ani *T.Il. Rechtel, "Coherent Anti-Stokes Raman Spectra of OxygenA.,-mr in ,amps," Ot. Lett.- Vol. 6, p. 458, 1981.

5* L'f,*':

. Both the MPI and the MPE approaches suffer certain limitations MPE

always has quenching considerations as well as photometric inefficiencies,while MPI lacks selectivity in signal detection, and is thus quite susceptibleto background ionization. In either approach, the nonlinear signals whichusually depend on the number of photons, n, required for the given transition,are generally low due to the characteristically small multiphoton absorptioncross sections. Thus, tight focusing and maximum laser energy extraction istypically desirable. We have made recent observations in our laboratory,however, whic'h suggest that at sufficiently high laser energies, the flamediagnostic probe can become substantially intrusive by promoting multiphoton

dissociation of the parent fuel and oxidizer molecules, in this case intohydrogen and oxygen atoms. Also, we have observed very efficient collisionalenergy transfer from the two-photon populated oxygen level to a neighboringlevel, as well as energy transfer from the excited oxygen to hydrogen atoms(see Fi.-ure ). The two-photon excitation scheme for oxygen atoms using225 nm photons, followed by detection of emission at 845 nm (see Figure 1),was initially demonstrated in a low pressure discharge 8 and then appliedsuccessfully for the first time lo a combustion environment in an experimentinvolving the C2 H2 /02 flame.1

II. EXPERIMENTAL

Figure 2 shows the experimental schematic. A Nd:YAG laser is used topump a dye laser in which R590 dye is circulated. The output is frequencydoubled and mixed with the 1.06 micron Nd:YAG fundamental in a commercialwavelength extender to produce tunable radiation in the 225 nm range. Thisbeam is then focussed with a 100 mm focal length lens into a curved knife-edgeburner, whose edges are separated by 3 mm from each other, and in which a fuelrich CH4 /N20/N 2 flame (0.14:0.38:0.48) is stabilized. Laser pulse widths of5 nsec and energies up to 1.5 mjoules/pulse at 10 pps were employed. The

emitted radiation from the flame was collected by a lens system and passedthrough a broadband filter into a 0.3 in monochromator whose slits wererelatively wide (ca. 2 nm) and finally detected by a photomultiplier tube (EMI

9659QA). The PMT output was fed into a 7912AD Tektronix transient digitizer,which was interfaced with a PDP 11/04 computer. Typically 50-300 laser shotswere averaged per data point.

III. RESULTS AND DISCUSSION

Figure 3 shows an 0 atom emission profile through the curved knife-edgeburner. A well-defined flame front is quite evident while the second peak isinterpreted as resulting from entrained air further reacting with the fuel-rich post-flame gases. Figure 3 is based on monitoring the 777.5 nm line,which is actually a grouping of three closely spaced lines originating fromthe three 5P upper states to the common S state. The emission intensity of

2this group as measured in the primary flame zone was about an order of

8"W.K. Ri,;ch.1, B.E. Perry, and D.R. mrosley, "Tvo-Photon Laser-Induced

Fluorescence in Oxygen and N~tojen to's," Chem. Phys. Lett., Vol. 82,p. 85, 198!.

120

100 1 -n31P~,2 5S2 6563A

5 P12,38447AifH

0 S

60

60

Z 40

2256Ad~20

202

0I Hi01 __ 0pal,2 - n:

S P D S0

.1 ~ Figure 1. Partial Energy Level Diagram for 0 and H Atoms

7

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Figure 3. 0 Atom Emission Profile at 777.5 nm in a Curved Knife-Edge Burner Supporting a Fuel-Rich CH4/N20/N2 Flame

9

magnitude greater than the emission at 844.7 nm. When photometric wavelengthdifferences, such as grating and PMT quantum efficiencies are taken into

account, the 777.5/844.7 emission ratio is still about 3. This indicates anefficient energy transfer process and has desirable analytical implicationssince now two different wavelengths are available for 0 atom detection. Dueto the fact that low signal levels were usually a problem, most of theexperiments were done monitoring the 777.5 nm line.

Figure 4 shows the 0 atom two-photon excitation spectra where the ground

spin-orbit states are resolved. The observed ratio of 9.5:4.1:1 can becompared to a Boltzmann calculated ratio of 5.8:3.1:1 for an adiabatic flametemperature of 2290*K. This, in turn, can be compared to the ratio of1.6:l.:I,which was observed in optogalvanic experiments on the H2/02/Arflame.4 The reason for these discrepancies is not clear at this time, butrecently there have been further theoretical efforts to substantiate the two-photon absorption cross sections which were found to be equal for each of thethree fine-structure components involved in this transition.9 A roughestimate of 0.0001% for the deteclion limit is based on the emission intensityin the primary flame zone (see Fig ,i, 3) and a calculated 0 atom mole fractionof 0.005% (NASA/Lewis equilibrium progirri). This number should be improved byat least an order of magnitude by optimizing the optical collectionefficiency, as well as using a red-sensitive PMT. This detection limit can becompared to 0.01% indicated in the trevious MPE experiment, 1 parts-per-millionsensitivity 4o5 the MPI experiment, as well as 0.01-0.1% for the two Ramanexperiments.

Further spectral investigations revealed another emission line centeredat 656.3 nm, which was generally as intense as the 777.5 nm line and wasresonant with 0 atom two-photon excitation. We have identified this emissionas the H transition in the hydrogen atom Balmer series (see Figure 1

• .However, the mechanism for populating the n=3 level, which is 8861 cm- higherin energy than the laser populated 0 atom level, was quite unclear for sometime. Another even more surprising observation was the detection of the two0 atom emission lines, as well as the 656.3 nm H-atom line in the absence of aflame when only room temperature premixed gases were flowing through theburner. In order to understand these findings, a determination of the orderof nonlinearity, n, of these signals under different conditions was initiatedand the results are given in Table 1. The uncertainties for the value of nare based on a number of different runs in which the Nd:YAG amplifier lampenergy was varied to yield energies between 0.2-1.5 mjoule/pulse. Clearly,this is not the best way to vary the probe laser energy since the output pulsetime profile may change somewhat. Unfortunately, intensity attenuationattempts using polarizers available in our laboratory were unsuccessful sincethe coatings could not withstand the high peak intensities and shortwavelengths used. Nevertheless, the results listed in Table 1 are consistentwith a qualitative picture of multiphoton induced photolysis of the fuel andoxidizer parent molecules followed by a 0 atom two-photon resonant formationof a microplasma. In the preheat region the value of n=4 is close to what isfound for the N20 room temperature flow where n=5, suggesting that multiphoton

9D.R. Croeley and W.K. Rischel, "On Relative Fine-Structure Intensities inTwo-Photon Excitation," Phys. Rev., in press 1984.

10

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NOO

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--- 7- 77 7 .-. 1-- -- U:*- .. '.4 - -. -T

TABLE 1. ORDER OF NONLINEARITY (n) OF MULTIPHOTON INDUCED

EMISSION SIGNALSa

Atom (Emission X) Flame Region Probed n

0 (777.5 nm) Preheat 4 ± 0.5Primary 2 ± 0.5Post-Flame 1.8 ± 0.5

Room Temp. Flow 5 ± 1

H (656.3 nm) 10 +4%.

a - Where emission signal a (laser energy)n

photolysis of N20 is contributing significantly to the total 0 atom emissionsignal. In the primary and post- iL:, regions, however, the value of n=2 isjust what one would expect for a two-pliton generated signal where thephotolytic parent, N20, has already reacted away and the native 0 atom flamepopulation is relatively high. The highest order of nonlinearity is found for

N71 the H atom emission which is expected since it takes some number of photons tophotolyze C"4 , and more.for N2 0, and finally two to excite the 0 atoms. Thelack of uncertainty limits for the li-atom case attests to the difficulty(i.e., long averaging times and high degree of scatter) involved in makingmeasurements on very high orders of nonlinearity.

A microplasma is not surprising since the absorption of the third photonionizes the 0 atoms4 and the temperature in the focal volume may be muchhotter than even the flame temperature, thus promoting collisional energy

transfer from 0 to H atoms. An alternative to multiphoton photolysis might beplasma chemistry involving highly excited states or ion-molecule reactions,but these explanations seem less likely since all of the emissions are prompt,i.e., 5 nsec or less apart from each other. Again, it should be stressed thatthe results in Table 1 are qualitative in nature since signal levels,especially where n is high, were quite low, requiring laser energies overI mjoule/putse, and they are based on the collisionally induced 777.5 nm linewhere the rates of collisional energy transfer may not be constant for thedifferent experimental conditions. Clearly, this is a complex situation which

0 deserves further study. Nevertheless, the potential for the multiphotondiagnostic probe to be intrusive certainly exists and thus appropriate caution

A should be exercised in these types of experiments. The implication of our

4% results to previous multiphoton 0 atom flame studies cannot be readily.4% assessed since those were done on flame systems other than the CH4 /N20/N 2 and

thus photochemical effects (if any) are probably quite different. Finally,6 multiphoton induced photolysis should, in fact, not be too surprising since

recent literature in chemical physics has many examples of such, even

12

involving typical flame molecules like H210 or C2H2 . There is even a recent

flame paper where laser probe intrusion (presumably photochemical) wasnoted. On the other hand, as pointed out by those authors, there may be new

opportunities to expand our knowledge of combustion by exploitingI photochemistry.

IV. CONCLUSIONS

The following conclusions can be reached on the basis of our experiments.

1. Oxygen atoms can be detected in a CH4 /N2 0/N2 flame by two-photon

excitation at 225.6 nm and emission detection at 844.7 nm.

2. The collisional energy transfer between the directly populated 3pexcited oxygen atom state and the neighboring 5p state is very efficient.

This is quito surprising since the process involves the change of spinmultiplicities. For a given experimental condition, the resulting emission at777.5 nm can be much more intense than the one at 844.7 nm and thus be more

useful for sensitive analysis of 0-atoms.

3. Hydrogen atom emission at 656.3 nm is detected, which is resonantwith 0 atom two-photon excitation. This may result from an endothermic

collisional energy transfer process occurring in the microplasma formed in theSfocal volume of the laser whose temperature is hotter than the flame

temperature. Alternative explanations, however, for the H-atom emission such

as plasma chemistry/fast ion-molecule reactions, cannot be ruled out at thistime.

4. Since both oxygen atom and the single hydrogen atom emissions weredetected without a flame, the multiphoton photolysis of the atom precursors,N2 0 and CH4 , was indicated. This was substantiated by a study of the order of

nonlinearity of the emission signal.

5. The above observation indicates that the laser multiphoton flamediagnostic probe is potentially quite intrusive, depending on the region of

the flame being studied (i.e., the relative concentration of photochemicalprecursors), as well as the laser energies utilized (i.e., the higher thelaser energy, the more prominent the higher order processes become). Thus,appropriate caution should be exercised in these kinds of experiments.

1 0 S.T. Pratt, P.M DehLer, and J.L. Demer, "Resonant Multiphoton Ionization

of i )i the B Z + , v=7, J=9, and 4 Levels with Photoelectron EnergyAnalsis," J. Chem. Phys., Vol. 78, p. 4315, 1983.

11'.B. Craig, W.L. Faust, L.S. Goldberg, and R.G. Weiss, "TV Short-PulseFragmentation of Isotopically Labeled Acetylene: Studies of Emission with

Sd),anose!ond Resolution," 7. Chem. Phyu., Vol. 76, p. 5014, 1982.

1 2 M. Alden, 1. Edner, and S. 69anberg, "Simultaneous Spatially Resolved

Monitoring of C2 and O in a C 2 H2 /0 2 Flame Using a Diode Array Detector,"Aj2p. Phya,.-A Vol. 29, p. 93, 1982.

13

-9o

S'-ACKNOWLEDGEMENTS

The authors would like to express their gratitude to the BRL Director,Dr. R.J. Eichelberger, for supporting this research under the ILIR Program.Also, numerous discussions with Professors Paul J. Dagdigian, Johns HopkinsUniversity, and Millard H. Alexander, University of Maryland, College Park,were quite stimulating and helpful.

4~14

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REFERENCES

I. M. Alden, H. Edner, P. Grafstrom, and S. Svanberg, "Two-Photon Excitation

of Atomic Oxygen in a Flame," Opt. Comm., Vol. 42, p. 244, 1982.

2. R.P. Lucht, J.T. Salmon, G.B. King, D.W. Sweeney, and N.M. Laurendeau,"Two-Photon-Excited Fluorescence Measurement of Hydrogen Atoms inFlames," Opt. Lett., Vol. 8, p. 365, 1983.

3. J.E.M. Goldsmith, "Resonant Multiphoton Optogalvanic Detection of AtomicHydrogen in Flames," Opt. Lett., Vol 7, p. 437, 1982.

4. J.E.M. Goldsmith, "Resonant Multiphoton Optogalvanic Detection of AtomicOxygen in Flames," J. Chem. Phys., Vol. 78, p. 1610, 1983.

5. P.J.H. Tjossem and T.A. Cool, "Detection of Atomic Hydrogen in Flames byResonance Four-Photon Ionization at 365 nm," Chem. Phys. Lett., Vol. 100,

p. 479, 1983.

6. C.J. Dasch and J.H. Bechtel, "Spontaneous Raman Scattering by Ground-

State Oxygen Atoms," Opt. Lett.- Vol. 6, p. 36, 1981.

" . 7. R.E. Teets and J.H. Bechtel, "Coherent Anti-Stokes Raman Spectra ofOxygen Atoms in Flames," Opt. Lett., Vol. 6, p. 458, 1981.

8. W.K. Bischel, B.E. Perry, and D.R. Crosley, "Two-Photon Laser-InducedFluorescence in Oxygen and Nitrogen Atoms," Chem. Phys. Lett., Vol. 82,

p. 85, 1981.

9. D.R. Crosley and W.K. Bischel, "On Relative Fine-Structure Intensities inTwo-Photon Excitation," Phys. Rev., in press 1984.

10. S.T. Pratt, P.M. Dehmer, and J.L. Dehmer, "Resonant Multiphoton

Ionization of H2 via the B1 Z , v=7, J=2, and 4 Levels with Photoelectron

Energy Analysis," J. Chem. Phys., Vol. 78, p. 4315, 1983.

It. B.B. Craig, W.L. Faust, L.S. Goldberg, and R.G. Weiss, "UV Short-Pulse

Fragmentation of Isotopically Labeled Acetylene: Studies of Emissionwith Sabnanosecond Resolution," J. Chem. Phys., Vol. 76, p. 5014, 1982.

12. H. Alden, H. Edner, and S. Svanberg, "Simultaneous Spatially Resolved

Monitoring of C2 and OH in a C2H2/02 Flame Using a Diode Array Detector,"Appl. Phys. B, Vol. 29, p. 93, 1 82.

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