chemical physics of discharges - Argonne National Laboratory

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(-1) \'ariation of 1'l;iting Conditions. Comliining thc iniorm:ition obtained in the previous tests, several runs irere macle using.-vnri,:itions of the- pl;itinfi conditions. ohtainctl are prcscnte!l in Table 5 and in Fig. 5. Some of thc, results The current-tinic :intl.voltage-time chnr:ictkkistics for t\ro runs :ire indicated in Fig. 8.' TIIC fil:imcnt oI1t:iincd in Ilun 73- 1 (T:il)Ie 5) \vas cvenly and uniformly coated similar to thc filamcnt picturcd.in Fig. 5. Except for oiic defect, the filnmcnt obtained from Run 74-1 (Tablc 5) \v:is evenly and uniformly coated similar to the filament pictured in Fig. 7. As indicated in Fig. 8, the defect probably occurred after an elapsed time of ?bout 21 min at a cell voltage of about 23,600 V. Thc results obtained.indicate that the best process conditions and plating procedure for boron deposition on a stationary 0.5-mil'tungsten !\ire, are as indicated in Fig. 8. Discussion Thc morphology of the deposit obtainecl reflects, in general, the morphology of the substrate. 'I'hc coating is essentially amorphous in nature although there is indication of anisotropy. One set of operating conditions giving ;I .satisfactory coating of boron on tungsten is presented graphically in 13g. 8. In general, good coatings have been obtained at high boron tribromideto-hydrogen ratios and relatively low currents. Furthermore, if the flowrate is too great, the corona tends to break up into points, resulting in nonuniform deposits. Other effects of varying operation conditions which suggest limitations for deposition, and which also tend to verify the mechanism for deposition .. .. presented previously, include: . . (a) The voltage requirements increase as the boron tribromide to hydrogen ratio increases.. ._ (b) The voltage requirements increase as the system pressure increases. (c) The substrate is etched with.little or no boron deposited as the boron tribromide- to-hydrogen ,ratio decreases. '.. CONTINUOUS. BORON DEPOSITION ON A MOVING FILAMENT ,. Experimental Work .. . . ._ A system was designed, assembled, and tested for. continuous boron deposition on a moving filament. Figure 9 is a schematic of the apparatus. The design resembles that for the batch plating process (Fig. 1);. ,The filament is pulled through the system with a Graham constant speed motor. The spool is mounted ,on a shaft and suspended in;such a manner as to offer minimum friction.. The seal and,electrical contact between cells is a unique arrangement such that the filament moves through the seal in a vertical direction without breaking .. . . ., I' the seal. : I .I. . j .. The power for the ceils has been obtained'in a manner similar to that used for the batch plating process (big. 2). There has been a, considerable problem with 60-cycle pickup in the measurement system, Shielding;-ahd grounding, at various critical positions were necessary to elimin- . I ate this problem. 2. . IIydrogen-boron trichloride was 'chosen ab the'reactant 'system'. The reactant mixture has bccn obtained by bubbling hydrogen through boron trichloride maintained at about -2O'C. Thc reaction cells havemot been heate$ externally, and the vapor flow was split between all three cells. .,. ... . The etching cell was n& Zil as'such;'arid Was eventually converted to use for cleaning ) the substrate filament by the hot-wire technique. Thus,, the chemical cleaning train was eliminated. Hydrogen only was passed through the cleaning cell and the substrate heated to I , . . _'. I, .. "3:. :_ ~ ,,. _. , . .. t i 6
\ E ‘ 1 TIME FOR RUN 13-1 14-1 - 1 0 0 a 1 b 2 c 3 d 4 e 5 H2 FLOW BUBBLER (M L/MIN) 160 160 95 50 50 e H2 FLOW BBr3 BYPASS TEMPERATURE LML/MW (* C) 270 -22 270 Htrs. on . 95 -35 0 -50 0 -72 Shut down I I 1 I I I 1 I 4 8 12 16 20 24 28 32 PROCESSING TIME (MIN) 28 24 S 2o 3 B 16 0” Fig. 8 Electrical Characteristics During Deposition of Boron on 0.5-mil Tungsten Wire in a Corona Discharge 12 E 4 w’ 0 4 s cl w u
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)i 1 reesonably complete and accura
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3 inquire about the component of ve
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4 I I 5 To find (t2)av, we assume t
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\ vnich, it is noted can be negativ
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I 7 than or smaller than the second
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i I i I I I ) ) i L , I I . INT1:OD
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13 field per electron is and per co
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. 11. 5. CharRe-Transfer and Ion-Mo
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17 In the followin:: sections much
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above. With that EIN, an estimate o
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21 region in w!iich large, nighlv l
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i ’ understanding: 23 (a) Electro
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Obviously, the secondary ion must h
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27 (22) Franklin, J. L., Munson, M.
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Tables 1-6 present examples of rela
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Table 8 Some Ions Formed by Process
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33 velocity of the reacting partn r
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35 must be added to the Langevin cr
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37 In our laboratory a microwave di
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+ . 4 . r 39 as well as N in a cor0
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ION-MOIECULE REACTION RATES MEASUFI
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43 excitntion 2onditions so that th
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45 In 2 like manner Fig. 3, showing
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47 Absorption Spectra of Transient
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50 maximum fiela. In this manner, a
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52 3 % %- %- 5- a- 7 h W P H 0 L v)
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References I I . A.B.Callear, J.A.G
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._ . _-.. - , , . . ,. . The Pyrex
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58 0 0 0 VI J > I cv . u H a
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.... . 0 2 e I / m 0 H F4 : 1
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\ 0.9 0.8 0.7 06 0.5 0.4 0.3 0.2 01
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65 ' cause of the reduction in the
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INTRODUCTION I' Attachment of polar
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I 69 EXPERIMENTAL The mass spectrom
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+ Figure 1 Mixed water and methanol
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73 ' , radius might be expected bec
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75 Negative Ion Mass Spectra of Som
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A b 1 1 I H I I I FILAMEN T CONTINU
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79 for positive and negative ions,
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51 out to answer some of the questi
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93 INTERACTIONS OF EXCITED SPECIES
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L 4 I*C z 0'2 = a, a U x I m 4 m 0
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I L I, ; > > E Fig. 3 I50 200 150 1
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I 300 r 1 - 200 i io ;' a cn I I. 0
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where DISCUSSION OF XESULTS PERTAIN
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93 where the bar indicates values c
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'I i 'I 0 2. 4 6 8 2 [ N]* x' I 0-2
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Fig. 14 IO 8 6 4F [NO] x IO-" (mole
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for chemiluminescent excitation in
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101 Chemiluminescent Reactions of E
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103 All gases were taken directly f
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10; He: + N2 -. 2He + h': (8) whi!?
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description for both diffusion and
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B. Ions and Electrons I Consider a
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' 112 axial diffusion through the d
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the tube walls occurs continuously
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E2R M ' $6"
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1. 2. 3. 4. 5. 6. 7. 8. 9- 10. u. -
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120 . Dlschorge zone Reactor zone 1
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122 In radiation chemistry the cust
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124 4. chemistry seem limited essen
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126 Conversion of Mixtures into Mor
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Hydrazine Synthesis in A Silent dle
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{;I . - . .. . - .., . . .. _- .. .
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1 \ \ \ , \ , \ \ Pmer hnrity K.W.
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. I operating fact that the sloGe i
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_- of ' . 8. - 7 6, Residence Time
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135 Ionic Reactions in Corona Disch
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GAS OUT GAS IN i.ho QUADRUPOLE MASS
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- + ( ~ ~ + 0 H ) ~ O ~ ( H~o)~H+ +
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144 i I , , , , . + 1- u 3c w Inu c
Page 146 and 147: 146 SYNTHESIS OF ORGANIC COIGhTDS B
Page 148 and 149: mi5 a- dz CI n I a I n +4 - 0 -I- k
Page 150 and 151: 0 z cu I I I
Page 152: I- I - t d m a .rl Y x c, t-' d k
Page 155 and 156: , 155 This result is significant in
Page 157 and 158: Compound Bond he rgy Li I 82 UBr 10
Page 159 and 160: , ”..’ 3or 25 - 5 20 - s 3 w Y
Page 161 and 162: I 161 THE GLOW DISCHARGE DEPOSITION
Page 163 and 164: Fig. 1 Process Apparatus -__l.ll__
Page 165 and 166: v) t- at- InIo Io0 t-Q) loo lcua O
Page 167 and 168: This study is only an approximation
Page 169 and 170: Mole Reaction Material ratio time e
Page 171 and 172: \ i (4) Effect of System Pressure T
Page 173 and 174: 173 Pressure. Since pressure is a c
Page 175 and 176: 175 Table VI X-RAY DATA OF DEPOSIT
Page 177 and 178: 177 Another source of weakness is t
Page 179 and 180: 179 PLATING IN A CORONA DISCHARGE R
Page 181 and 182: \ 3 , ,\ 110 v 60 CPS MANOMETER . F
Page 183 and 184: I i , \ I i & a - P Fig. 3 Reaction
Page 185 and 186: \ \' C 0 .d * d .- C U d 0) c( 1) L
Page 187 and 188: I i I . Q) I, s w 0 v) Y 0 a w W a
Page 189 and 190: I (b) Polarized Light Fig. 6 Cross
Page 191 and 192: i m v) Y C i! u o) 23 a a- + 191 m
Page 193 and 194: i, d C .d c c W Q ) 0 0 L1Y 0 000 0
Page 195: i e 4 0 wcr -4 4 al 0 0 0 c) cr 13:
Page 199 and 200: 199 a red heat in this cell using d
Page 201 and 202: \ , t j \ I, v) 2 Y . C 0 u m .I C
Page 203 and 204: 203 VAPOR PHASE FORMATION OF NONCRY
Page 205 and 206: BELL JAR STANC TO VACUUM SYSTEM U T
Page 207 and 208: 207 of the boron oxide film, the fi
Page 209 and 210: i I, 4 I.( Y I- * 0 i f i 3 0.t I I
Page 211 and 212: 211 The Reacticn 3f Oxygen with Car
Page 213 and 214: 2 E, W t- a Z 9 I- a 2 X 0 I50 too
Page 215 and 216: 'i' 100 50 IC 21 5 2.0 2.5 SURFACE
Page 217 and 218: I- z W 0 w a a 100 80 60 40 20 215
Page 219 and 220: s., Literature Cited Berkley, C. ,
Page 221 and 222: 7 h \ F 221 600°C and 1 atmosphere
Page 223 and 224: 223 e I'
Page 225 and 226: R L ' -1 9mm O.D. 5mm I.D. 45mm 0.D
Page 227 and 228: Figure 5.- Paschen's law curves. 2-
Page 229 and 230: \ '? I The water-free product gases
Page 231 and 232: N I + 0" ON i I + 0 u / 0 0 I 0 cu
Page 233 and 234: - 233 SOME PROBLEMS OF THE KINETICS
Page 235 and 236: .. . :. ,. .I , . i ? .. . , ... .
Page 237 and 238: 237 Table 2 Experimental Variables
Page 239 and 240: 239 Zhbie I Eerccnt Consumption of
Page 241 and 242: 241 Discussion The systematic varia
Page 243 and 244: I \ 1 243 FORMATION OF HYDROCARBONS
Page 245 and 246: h z - a o m a 20 T IME, minutes . F
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I 1 I I I I 0 I 2 3 4 5 TIME, minut
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The next five coluws in table 1 sho
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\ .\ t 251 Given the existence of t
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I L 253 Epple, R. P. and C. M. Apt.
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1 ' Fig. 1 Schematic of flow discha
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5' . ' I 1 257 co, with excess H2,
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1 1 1 moo 1400 1300 c V' I IPOO I I
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i 25i The Dlssocfatior of ToIuere V
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L ! , c PRODUCTS FROM A 28 MC. DISC
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'\ J ?. , .. . : PRODUCT FORMATION
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'9 / I '\ "1 BENZYL CATION AND RADI
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a
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271 tube serve? as the high voltare
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273 ion (1L.). Zxcitei-ion by colli
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Apparatus and Procedure 275 EXPERIM
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. 277 6. A freshly prepared sam le
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observed. The polystyrene (10% solu
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i i (12) c (11) (14) I 281 LITERATU
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FLOW- METER I ADDITIVE SUPPLY * ,28
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285 TABLE 2 Effect of Haloqenated A
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ANALYTICAL RESULTS Some evidence wa
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DISCUSSION 289 The salient features
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? ~ MENBERSHIP IN THE DIVISION OF F
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292 flow of the reactant gas stream
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294 have suitable residence times i
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0 E < h( E l! d K c 0 .- Y 0 t u t
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298 yields of many chemical product
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- ;i Y . 15. Pressure lOmm 5 > 10-
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302 the best and in many practical
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GENERATION AND MEASUREMENT OF AUDIO
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. The transformer secondary and the
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Vaccum-Tube Amplifier The mobile co
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310 f = Power supply frequency in c
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FUFARCI! INSTITUTE OF TFYDLC UNIVER
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J # I / 4) I . . '8 r4 0 r( P
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317 i Cuencb svsten w.nnar;itus use
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epcrte? the noss~kil.itv of nroduct
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1' b t +
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323 ....... - . . . . . . . . . . .
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1 \ i I i , / / / 8 3 1 325 To205 +
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- .- - - . - - . . . - . 327 n + c
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' POWER PLASMA GAS l e , ' I ! I I
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331 f'ENI?AL PF'FCLCCFC Dernis, P.R
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i J 333 ; mosphere (as opposed to a
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; it raised the question, still &?z
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p .I V I .= - - HCN/C(CALC. WITH C
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1 1 339 atmospheric ressure and ach
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RESULTS 341 Composition Dependence
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0.09 0.08 0.07 9 0.06 2 U - .$ 0.05
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II \ to the Slot So that less of th
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i 4 2 HYDROCARBON-NITROGEN REACTION
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I 1 349 c M m ; a e, k M x
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1.0 I - a. I n TEMPERATURE - OK Fig
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353 the experimental results in the
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,) 355 The ceaswed conversion cf ni
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1 6 357 Freezing. 3jpotnesise thzf
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359 \ Frozen Compositior: Calcillat
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I 1 \ 361 -. ne reaction proceecis
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\ 36 3 ' h, I 26. H. Purnell, Gas C
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In experiments on the direct conver
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367 used as blnders, with different
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369 ' i 1. REFERENCES Berber, John
Page 372 and 373:
Distribution and yield rates of pro
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. . I . I 370 . . . . ., . . .. . .
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4 372 090- > E w - m c N O - 0 z :
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A-Feed tank 6-Thermocracker GReceiv
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80 \ 0 70 60 e 40 a U VI 9 30 20 10
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COAL DEASH& AND HIGH-PURITY COKE Wa
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3Pn _. -. - L -J:,J.-;~~~L, ):as se
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S ~ l ~ o n~pg:ading r is the resul
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The range ~f temperatures and gener
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. .. 386 9 * - r. Y 2 .' d a f' r.
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.) .L m 388 I
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TABLE 4 390 DELAYED COKING OF DEASH
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, ! I- on '---
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394 The present method is to keep t
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396 ‘c erperature, while the pres
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2, '! ! Proximate Analysis, wt $ Mo
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0 IS 0 14 LL 9 013 e \ 3 b- m *- 01
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402 HYDROGEN CYANIDE PRODUCED FROM
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404 Before startup, the system is p
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4 OL. ' , I. . TesCs. With.Coals .o
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Table 3.- Product Gas Analyses and
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410 BIBLIOGRAPHY 1. American Public
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Figure 2. Enclosure surrounding hyd
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0 0 f v) C 0 u m I z 2 c 2 r d J w
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0. E c .4 7 .. .c . I ( - Low tempe
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418 cual. A mjor aa\;antage or' the
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420 Ir ?Y ? ? 9 9 9 pc rod n o c o
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422 Table 3. Room-texperature M'dss
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424 state, depending on the strengt
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Table 4. Room-?;ergerature isomer s
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I' 1.3 . /o 9 IO 9 6 a 425 F F 33 I
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Brooks J.D. and Sternhell S. (1957)
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(52) Gib3 T.C. and Greenwood N.N. (
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434 transducer vas then introduced
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436 yield is quite similar. The con
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?-!??? 0 mv, Uh\OhIe . . . . eirlrl
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4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 4
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442 CHEMICAL REACTIONS IN A CORONA
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helium 444 CORONA REACTOR SYSTEM Fi
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446 The ultraviolet spectrum. for t
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Biphenyl Fraction 448 The low molec
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LUd The actual structural definitio
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I I I I I In m 9 In 2 , I: r- In m
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’. 454 Mechanism I The available
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456 , , . The relatively low yield
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458 h/lethylacetylene, allene and b
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Introduction VAPOR PHASE DECOMPOSIT
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462 more efficient hydrogenation. T
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464 place in parallel with fragment
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466 P rl 0, k 7 rnI rn al k a I hl
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458 TABLE I. COMPOSI'IION OF GASEOU
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REFERENCES 1. C. Hirayama and D. A.
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i 472 Reciprocal Arc Enthalpy ,-> F
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474 be pumped down without altering
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476 Instead a hydrogen deficient fi
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i 478
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480 FATTY ACIDS AND n-ALKANES IN GR
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482 TA5L,E 2. - Carbon number distr
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6. 7. a. 9. 484 Lawlor, D. L., and
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' I ' Sample No. 6 ' 12 IO 8 6 z 4
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. 488 uiolecular weight of which ca
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Xississippi (Sample GS). Stock solu
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492 found at 5.7 and 4.9& for the W
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494 mechanisms. However, the voltad
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For pure polynuclcar arom.i;ic hydr
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- '-'. . ' . . values are listed in
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500 (1;) Ten, T. 17.: a;1d,Dic;
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- ~ Resistivity Czlculation 2: 1 j:
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504 o ' C 0s 2 0 v x i 8 2 0 ! P -
Page 510 and 511:
506 i
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d 601 L P LL
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I I I I I I I I m W N W N 0 (D ? 0
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514 was heated under nitrogen in a
Page 520 and 521:
The line broadening at 79OK of the
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13. 14. 15. 16. 17. 18. 19. 20. 21.
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W L, Z 6 m (1: 0 6 d j o 2 ' 1 0.0
Page 526 and 527:
Coals 522 Studies of the 1600 cm-l
Page 528 and 529:
L in ole i c a c id - 0' Two sample
Page 530 and 531:
526 Table 1.- Ultimate analyses of
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528 6. Friedel, R. A., and H. Retco
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egeneration. The system can be seen
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532 and can be expressed in terms o
Page 538 and 539:
534 in the vapor increases with inc
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NH3 NH3 NH3 NH3 Pyridine Pyridine P
Page 542 and 543:
Mole Ratio of Test No. Quinoline to
Page 544 and 545:
IXPROFJCTION D; M. Mason Institute
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-4:c~rciiny to recent studies o ;i4
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544 Table 1. LIGHT EMISSION OF Y"TR
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emission in a few cases may be by d
Page 552 and 553:
LITERATUR2 CITED i. C. -. .' * il.
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co, CH,,OR 1 - OTHER ADDITIVE FRITT
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FRIT 'TED CO, CH,.OR 4 ___ OTHER AD
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340 350 300 400 4 50 500 600 700 80
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0 554 WITH COOLING (PLATE AT 40°C)
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5 56 then t = to when e = 0 2) the
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5 58 The surface heat transfer coef
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Discussion and Results 560 Three br
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__- ._ 562 Table I THERMAL AND PHYS
Page 570:
ln 4 I 0 4J v \ 1.0 0.8 0.6 L - 0.4
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