I!- · temperature ranges on the oxidation reactions of refractory free radical species. Various...
Transcript of I!- · temperature ranges on the oxidation reactions of refractory free radical species. Various...
I!- AD-AI12 275 QUEEN MARY COL.L LONDON (ENGLAND) DEPT OF CHEMISTRY F/s 7/3I KINETICS OF OXIDATION REACTIONS INVOLVING S AND Al CHALCONIDES. (U)
MOV SI A FORTN1'J M A CLYNE AFOSR-81-00OS5
UNWCLASSIFIEDFOSR TR-820131 NL
L' 122
1.8ai
4.51111 ItI4111111. 2 hi 1 .6=
MICROCOPY RESOLUTION TEST CHART
NAIIONAL prijAL[ OF IANI,)ARIlF' 6 A
AFOSRTL 8 2-0131
L Grant Number AFOSR-81-0035
KINETICS OF OXIDATION REACTIONS INVOLVING
B AND Al CHALCONIDES
Arthur Fontijn and the late Michael A. A. Clyne,Department of Chemistry,
Queen Mary College,Mile End Road,London El 4NS, UK
November 1981
Final Report, 1 October 1980 - 30 September 1981
Approved for public release; distribution unlimited
Prepared for: 12.1b
Air Force of Scientific Research, .. . ).
Bolling AFB, Washington DC 20332 -
and
European Office of Aerospace Research and DevelopmentLondon, England.
GXUAA Approyd for publie releuseAA distribut ion unIfted.
AIR FOP=~C D'PFIc ' Sr~rrpC FiSAFr
This techn~ical report has been revieioqd and i.: t-
approved for publtc release IAW Ayp ,~2Distribution is unlImItad.
TABLE OF CONTENTS
Page
I. INTRODUCTION - SCIENTIFIC OJECTIVES 1
II. BIBLIOGRAPHY OF PUBLICATIONS 2
III. DISCUSSION 3
A. Temperature range 3
B. Production and monitoring offurther radical species 4
IV. CONCLUSIONS 6
V. REFERENCES 7
Figure 1 9
Figure 2 10
"Kinetics of the ReactionBO + 02 + B02 + 0" (Appendix A) 11
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UNCLASSIFI~h" 'ECURITY CLASSIF ICA TI ON OF THIS'PAGE (Iii.,, Data, Kriter..d,
REPORT DOCUMENTATION PAGE READ INSTRUCTIONS________________________________________BEFORECOA~PLETING FORM
R ~2. GOVT A' -SS4jN No. 3. RECIPIENT'S CATALOG NUMBERl*R ~ -1R- 8 2 -01 3 1 4 9N 175-
4. TITLE (and Subtitle) 5. TYPE OF REPORT & PERIOD COVERED
1 Oct 80 - 30 Sep 81FINAL
KINETICS OF OXIDATION REACTIONS INVOLVING B AND 6. PERFORMING 01G. REPORT NUMBER
Al CHALCONIDES ________________
7. AUTHOR(s) 8. CONTRACT OR GRANT NUMBER(s)
ARTHUR FONTIJNMICHAEL A A CLYNE AFOSR-8 1-0035
9. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT. PROJECT, TASKAREA & WORK UNIT NUMBERS
QUEEN MARY COLLEGE610F#DEPT OF CHEMISTRY 6102FA sab'MI-LE END RD. LONDON, El 4NS, UK 2308/A
It. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE
AIR FORCE OFFICE OF SCIENTIFIC RESEARCH/NA NOV 81BOLLING AIR FORCE BASE, DC 20332 .1 13. NUMBER OF PAGES
_____ ____ 16:0) 15. SECURITY CLASS. (of this report)
'~UNCLASSIFIED
I5a. DECL ASSI FIC ATI ONDOWN GRADING-SCHEDULE a~
16. DISTRIBUTION STATEMENT (of this Report)
Approved +for public release; distribution unlimited.
17. DISTRIBUTION STATEMENT (of the abstract entered in Block 20, If different from Report)
IS. SUPPLEMENTARY NOTES-
19. KEY WORDS (Contlinue on reverse side it necessary and Identify by block number)
BORON OXIDATIONREACTION KINETICSREFRACTORY FREE RADICALS
20. ABSTRACT (Continue on reverse side If necessary end Identify by block number)
Work on various problems in solid and air-breathing rocket development, e.g.,submicron particulate formation, requires the input of kinetic data over widetemperature ranges on the oxidation reactions of refractory free radical species.Various approaches for producing these species and investigating tieir kinetics,using laser-induced fluorescence and hl~h-temperature fast-flow reactors, arediscussed. To demonstrate the feasibility of a new discharge-flow reactormethod for producing such radicals~for kinetic studies, the kinetics of B0 + 0 2
LB07+0 was investimated- A r~t r -r 4XIO_ 12 CM3 molecule- i'it 2 9 5k
DID I ~PIrAR7 1473 EWOtr0 Of I NOVA ISOSOLETEUNCLASq'I Ft F
SECURITY CLASSIFI ATION OF THIS PAGE (When Data Entered)
I. INTRODUCTION - SCIENTIFIC OBJECTIVES
The need for a reliable kinetic data base on reactions
of refractory metal atoms, metal oxide radicals and metal
halide radicals* for various aspects of solid and air
breathing rocket development has frequently been expressed,
e.g. Ref. 1. To provide such data for metal atoms, one of
us (AF) previously developed the HTFFR (High-Temperature
Fast-Flow Reactor) technique,2-4 which is uniquely useful
for measuring rate coefficients and their temperature
dependence within the temperature range of approximately
300 - 1900 K. Some data on a metal oxide radical, AlO, were
also obtained through the convenient expedient of observing
the two-step oxidation of Al atoms with the same oxidiser.
However, the need for more systematic means of studying
reactions of metal radicals in HTFFRs was obvious4 . The
visit, during the grant year, of AF to the laboratory of the
other of us (MAAC), with its state-of-the-art equipment for
laser-induced fluorescence (LIF) detection of free radicals,
presented a natural opportunity for such more systematic ex-
ploration. LIF currently represents the most sensitive
technique for monitoring of such radicals. Consequently,
the objectives for this program were to make a kinetic study
of a reaction of a refractory oxide radical (BO + 02 + B02 + 0)
*The word "metal" is used here in its propulsion technologysense, thus specifically including B, which is not ametallic element in the usual physico-chemical sense.
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and to explore means for future kinetic studies of
refractory radical species of significance to Air Force
development programs.
II. BIBLIOGRAPHY OF PUBLICATIONS
The present one year effort has resulted in the
following publication (Appendix A of this report):
I. P. Llewellyn, A. Fontijn and M. A. A. Clyne,wKinetics of the Reaction BO + 02 + B02 + 00,Chemical Physics Letters, in press.
"The reaction of BC13 + N + 0 was used to produce80 X2E+ radicals for study in a fast-flow reactor.Laser-induced fluorescence was used to follow theBO X2E+ radicals. The feasibility of kinetic studieson these radicals was demonstrated through a kineticstudy of the BO + 02 reaction, giving a rate
+4.7coefficient kI equal to ((4.4 ) x 10- 12 cm3
-3. 2
molecule-1 s-1 at 295 K."
Additionally considerable progress was made in the pre-
paration of a book chapter which discusses the status of
theory, experiments and predictive ability on the influence
of temperature on rate coefficients of bimolecular
reactions. The type of metal and metal radical reactions of
interest to the Air Force form an important subset of the
reactions discussed. This chapter and book are scheduled
for publication in late 1982. The reference will be:
A. Fontijn and R. Zellner, "Influence of Temperature onRate Coefficients of Bimolecular Reactions" inReactions of Small Transient Species (M. A. A. Clyneand A. Fontijn, Eds.), Academic Press, London, Chap.2.
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"Kinetic studies in recent years covering widetemperature ranges, have shown that the traditional expec-tations of near-Arrhenius behaviour, k - A T exp(-Ea/RT),are often unwarranted. Available data are reviewed in thelight of current theoretical and semi-empirical understanding."
III. DISCUSSION
The major complete results of the present work are
given in a publication (Appendix A). In addition to
providing ap important rate coefficient, this work has
demonstrated the practicality of a chemical production
method for a highly refractory oxide species (BO),
compatible with its subsequent kinetic studies in a
fast-flow reactor. This demonstration was made for one
species using a room temperature reactor. The two obvious
questions raised for future work thus are:
(i) what is the temperature range for which this type
of approach can be used, and
(ii) how can other radicals similarly be studied?
A. Temperature range
Figure 1 shows a simple means for extending the
temperature range of the studies. Compared to the work of
Appendix A, the Pyrex reactor has been replaced by a ceramic
reactor, surrounded by a high temperature furnace. At the
upstream end the free radical species (MeX) flows in from a
preparation line, which for BO would be identical to that of / --s
the present work. Any desired oxidant Oz, C02, NO2 , HCl, / .-"
etc. can be introduced, generally independent of the MeX
production method. An HTFFR based on this model was
COP ',ls c O _ .. . . . -
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designed, constructed and tested during the course of the
grant, but insufficient time was available to study the
BO/O2 reaction in this apparatus. The reaction tube and BO
inlet were made from impervious mullite (Morgan Refractories
Ltd.) and the three-zone furnace was made of Kanthal-A
elements (Bulten-Kanthal AB) surrounded by Triton blanket
and board insulating material (Morgan Refractories Ltd.).
This combination of materials allows work up to about 1500
K. The observation fluorescence cell was replaced outside
the heated zone. This was done to facilitate joining of the
reactor to existing laser-induced fluorescence apparatus at
Queen Mary College, not because of a principal advantage. A
previously used 3,4 modular HTFFR is shown in Figure 2. It
is obvious that the "source section" of that reactor can be
removed and the reactor section joined to a preparation line
as in Figure 1, resulting in a constant high temperature
zone including the observation region.
Thus there appears to be no reason in principle why the
metal radical work could not be extended over the full
temperature range of some previous HTFFR work (300 - 1900 K)3,4 .
The choice of apparatus design will depend on the radical of
interest, as will be discussed now.
B. Production and monitoring of further radical species
The traditional way of producing metal oxide and halide
radical species is by evaporation of inorganic compounds5 .
This approach could be practised with an original 3'4 modular
BTFFR, Figure 2, in which the vaporizer contains the
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inorganic parent compound. Thus, SnO can be produced by
dissociative evaporation of SnO2 , or else from Sn/SnO 2
mixtures where the Sn acts as a reducing agent; these
methods can be used at about 1400 K(6). Such vaporization
methods are in principle similar to those used in metal atom
HTFFR work 3'4 .
A number of methods for refractory radical production
have been developed in recent years in the area of
preparative metal-organic chemistry. These can best be
utilized with a preparation line approach, Figure 1. They
can be divided into two groups: gas-solid reactions and
pyrolysis5 7. An example of the former is the production of
BF by passage of BF3 through solid B granules at - 2000 K,
and one of the latter is the production of BC1 by passing
B2C14 through a quartz tube at - 1300 K (also yielding
BCl3). In HTFFR studies it is of course necessary to
ascertain that the other species present, BF3 and BC1 3 in
these examples, do not interfere with the reactions studied,
which is in general not likely for such thermally rather
stable compounds. These groups of methods can be expanded
by the use of laser photolysis, a method apparently not yet
used in studies of reactions of inorganic free radicals, but
one for which the basic technology has reached a high degree
of development in recent years 8 ,9.
It is important to note that neither the literature on
evaporative, nor on the preparative, methods appears to
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contain any information on the production of BO, the species
investigated experimentally in the current study (Appendix
A). Only B202 could be produced in metal-organic synthesis
work7 . The discharge-flow reaction method developed here
for BO, i.e. reacting BC1 3 with a flow of N/O/N2, was
attempted on the basis of observations that BO emission
spectra can be produced in the reaction of BC13 with active
nitrogen containing traces of oxygen i0 , while the reaction
Of BC3 with 0/02 mixtures only appears to produce B02.11
For many radicals such emission spectroscopic observations1 0
could be adapted to discharge-flow methods for production of
their respective ground states. Often the yields will be
very low, as was found to be the case for BO. However,
coupled with the extremely sensitive monitoring method,
which is LIF, low radical concentrations need not be a
drawback.
In the above we have emphasised the preparation and
monitoring of diatomic radicals. However, triatomic
radicals can be produced by similar methods and again LIF
offers currently the most sensitive detection technique.
For these larger species there is currently less information
available from earlier work. That this situation is
changing may be illustrated from the above mentioned Ba2
studies1" and the recent work by Hirota 12 on BOCI.
IV. CONCLUSIONS
In this work the practicality of producing a highly
refractory fret, radical species, BO, by a preparation line
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method has been demonstrated and k,.netic data on its
reaction with 02 have been obtained. The technical
possibilities for more extensive studies of rate
coefficients, and their temperature dependence, for
refractory radical species of Air Force interest are highly
promising. A large variety of radical production methods
can be combined with HTFFR methodology and laser-induced
fluorescence monitoring to achieve this goal.
V. REFERENCES
1. Air Force Sxstems Command Research Planninz Guide,HQ AFSC TR 80-01, February 1980, Sections 5.1 and 5.2
2. A. Fontijn and S. C. Kurzius, "Tubular Fast-Flow ReactorStudies at High Temperatures. 1. Kinetics of the Fe/0 2Reaction at 1600 KO, Chem. Phys. Lett., 13, 507 (1972).
3. A. Fontijn, "High-Temperature Fast-Flow Reactor Studiesof Elementary Reactions", in High Temperature Metal HalideChemistry, (D. C. Hildenbrand and D. D. Cubicciotti,Eds.), The Electrochemical Society, Princeton, 1978, p.484.
4. A. Fontijn and W. Felder, "High Temperature Flow Tubes.Generation and Measurement of Refractory Species", inReactive Intermediates in the Gas Phase. Generation-and4norin,(D. W. Setser, Ed.), Academic Press, New York,
TM, lap.2.
5. K. J. Klabunde, Chemistry of Free Atoms and Particles,Academic Press, New York, 1980.
6. J. M. Dyke, University of Southampton, Private Communi-cations to the authors.
7. P. L. Timms, "Techniques of Preparative Cryochemistry"in Cryochemistry (M. Moskovits and G. A. Ozin, Eds.),6hn Wiley, New York, 1976, Ch.3.
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8. M. N. R. Ashfold and G. Hancock, "Infrared MultiplePhoton Excitation and Dissociation: Reaction Kineticsand Radical Formation" in Gas Kinetics and EnergyTransfer, Vol. 4 (P. G.-shmore and R. J. Donovan,Eds.), The Royal Society of Chemistry, London, 1981,Chap. 3.
9. R. J. Donovan, "Ultraviolet Multiphoton Excitation:Formation and Kinetic Studies of ElectronicallyExcited Atoms and Free Radicals", Ibid., Chap. 4.
10. R. W. B. Pearse and A. G. Gaydon, The Identificationof Molecular Spectra, 4th ed., Chapman and Hall,London, 1978.
11. M. A. A. Clyne and M. C. Heaven, "Laser-InducedFluorescence of the BO and 802 Free Radicals",Chem. Phys., 51, 299 (1980).
12. E. Hirota, Discussion comment in Faraday Discussions71, to be published.
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TABrLE 1
Susiy of 30 + 02 _. .02 + 0 Rate Coefficient Eeaeuremsas
) "N flw A flo ;(b -t021 r ( kRCau3 (TP
a ) (cm 3 ) (SI))
l ) (a s2) (--) (10 -3) (arbitrary units) (10-12 3
(cm3(STP~m-) (0-a a-) m (0is
mole cle-1 2-u)
2.8 16 67 89 2.2 0.6 - 20 0.18 3.9 -0.962.7 16 67 90 3.1 3 - 34 0.20 9.6 -0.99
2.3 16 33 s0 S.5 1 - 14 0.23 1.-1 -0.992.9 16 67 87 2.9 8 - 21 0.23 3.7 -0.90
2.8 16 33 53 S.5 7 - 13 0.40 0.7 -0.972.8 16 33 53 5.9 S - 22 0.43 4.3 -0.982.8 16 33 53 6.1 3 - 40 0.54 1.8 -0.94
2.8 14 33 53 4.8 2 - 40 0.62 1.5 -0.98
2.7 is 18 37 7.0 3 - 40 0.46 0.7 -0.862.8 15 18 35 9.1 2 - 50 1.0 1.5 -0.982.6 27 18 S1 6.0 4 - 50 1.0 7.4 -0.81
2.6 27 18 52 5.2 4 - 25 0.30 7.S -0.98
2.6 27 18 52 4.8 2 - 23 0.41 3.7 -0.99
2.5 27 18 S3 4.3 2 - 30 0.39 10.6 -0.96
2.7 28 35 69 3.5 0.7 - 4 0.12 9.3 -0.9s1.9 22 18 65 3.7 2 - 20 0.20 7.7 -0.99
2.0 22 18 60 5.3 0.7 - 4 0.14 8.6 -0.934.1 22 18 30 9.3 2 - 12 0.23 1.9 -0.914.0 22 18 30 7.9 2 - 20 0.12 5.0 -0.944.1 22 18 30 6.7 4 - 40 0.13 5.6 -0.905.3 22 96 64 1.2 1 - 20 0.29 2.2 -0.965.5 22 96 64 3.6 2 - 13 0.64 2.0 -0.99
5.5 22 96 63 2.9 1 - 17 0.89 1.0 -0.89
all Torr 133.3 Pa b)mean pluq flo velocity c) intia. Be, ofuoriscenceiatensity
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