chemical physics of discharges - Argonne National Laboratory
chemical physics of discharges - Argonne National Laboratory chemical physics of discharges - Argonne National Laboratory
160 change in field through the corona, but very little change over the remaining distance to the opposing electrode. Most studies of corona discharges have been in inert gas systems, and have been generated at a point electrode. This study has been directed toivard the tletcrmination of the feasibility for depositing :1 coating, c.g., boron, on a suitablc substrate in :I corona discharge. A further object has becn to determine some of the critical pnramctcrs and a possible indication of the mechanism and characteristics of this technique for coating the substrate material. ; EXPERIMENTAL WORK A schematic diagram of the system used in this study is indicated in Fig. 1. The system pressure was controlled with a Cartesian Manostat GA (Manostat Corporation) and a Welch mechanical pump Model 1402 (W. M. Welch Manufacturing Company). The discharge was initiated and sustained with a 7,000/12,000 V Jefferson luminous tube outdoor-type trans- former (Jefferson Electric Company) connected to GO-cps 110-V power source through a Variac variable transformer. To dcterrnine the effect of alternating and direct current, an RCA CR 212 half-wave recti- fier \vas added to the circuit. At the same time a resistance bridge, a current measuring rcsistor, and an ammeter were added to the circuit. A schematic of the circuit is presented in Fig. 2. The resistance bridge consisted of six 2-W 2-megohm resistors (R2) and one 2-\V 1,000-ohm resistor .(R1), all in series; the total voltage being 11,775 times the voltage across the 1,000-ohm resistor. The current measuring resistor ,was a 2-W 10.075-ohm resistor. The voltage measurements were made with a Hewlett-Packard Model 130B oscilloscope, and alternating current measurements were made with a Simpson Model 378 milliammeter. The reactants utilized in this study were hydrogen, helium, or argon, and boron tribromide. The hydrogen was passed through a ffDe-oxo'7 unit (Engelhard), through a drying column of magnesium perchlorate, and then through a flowmeter. After the flowmeter, the hydrogen was split into two streams, one of which was bubbled through the boron tribromide, and then recombined into one stream before entering the reaction chamber or cell. The temperature of the bubbler, and of the cell, was controlled by wrapping each (and the associated gas lines) with heating tape and controlling the power input with a Variac variable transformer. The system was maintained at or below atmospheric pressure for this study, with most of the data being obtained at 2 to 3 in. of mercury below atmospheric pressure. Tungsten wire was chosen as the substrate material, This wire was cleaned by passing it successively through a train consisting of concentrated nitric acid, a distilled water rinse, and an acetone rinse. Using the hydrogen-boron tribromide reactant system and 60-cps alternating current to develop n corona, approximately a dozen cell designs were tried. The cell design which 1 appears to be the most satisfactory is pictured in Fig. 3. This cell consists of a 2-in.long pyrex glass tube with a neoprene O-ring inside each end and wrapped with eight turns of 3-mil tungsten wire along the tube length such that the wire is parallel and concentric to the axis of the tube. The wire is 0.9 cm from the axis. This assembly is then inserted in a 5-in.-long pyrex glass tube 1.5-in. in diameter and supported such that the tubes are concentric. A tungsten wire lead is then extended out of the tube, and neoprene rubber stoppers inserted in each end. Each stopper has a capillary tube through its center such that there are approximately 3 in. between the capillaries, and the filament enters and leaves the cell through these capillaries. The reactants also enter (and leave) the cell i! through the stoppers. I 4 1 , I
\ 3 , ,\ 110 v 60 CPS MANOMETER . Fig. 1 Schematic of System Utilized for Plating in a Corona Discharge 7 300 TO 15 000 V TRANSFORMER VARIAC MILLIAMMETER Fig. 2 Schematic of Power Input and Measuring Circuit Used With the Corona I' Discharge Plating Apparatus i I I
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160<br />
change in field through the corona, but very little change over the remaining distance to the<br />
opposing electrode. Most studies <strong>of</strong> corona <strong>discharges</strong> have been in inert gas systems, and<br />
have been generated at a point electrode.<br />
This study has been directed toivard the tletcrmination <strong>of</strong> the feasibility for depositing :1<br />
coating, c.g., boron, on a suitablc substrate in :I corona discharge. A further object has<br />
becn to determine some <strong>of</strong> the critical pnramctcrs and a possible indication <strong>of</strong> the mechanism<br />
and characteristics <strong>of</strong> this technique for coating the substrate material. ;<br />
EXPERIMENTAL WORK<br />
A schematic diagram <strong>of</strong> the system used in this study is indicated in Fig. 1. The system<br />
pressure was controlled with a Cartesian Manostat GA (Manostat Corporation) and a Welch<br />
mechanical pump Model 1402 (W. M. Welch Manufacturing Company). The discharge was<br />
initiated and sustained with a 7,000/12,000 V Jefferson luminous tube outdoor-type trans-<br />
former (Jefferson Electric Company) connected to GO-cps 110-V power source through a<br />
Variac variable transformer.<br />
To dcterrnine the effect <strong>of</strong> alternating and direct current, an RCA CR 212 half-wave recti-<br />
fier \vas added to the circuit. At the same time a resistance bridge, a current measuring<br />
rcsistor, and an ammeter were added to the circuit. A schematic <strong>of</strong> the circuit is presented<br />
in Fig. 2. The resistance bridge consisted <strong>of</strong> six 2-W 2-megohm resistors (R2) and one<br />
2-\V 1,000-ohm resistor .(R1), all in series; the total voltage being 11,775 times the voltage<br />
across the 1,000-ohm resistor. The current measuring resistor ,was a 2-W 10.075-ohm<br />
resistor. The voltage measurements were made with a Hewlett-Packard Model 130B<br />
oscilloscope, and alternating current measurements were made with a Simpson Model 378<br />
milliammeter.<br />
The reactants utilized in this study were hydrogen, helium, or argon, and boron tribromide.<br />
The hydrogen was passed through a ffDe-oxo'7 unit (Engelhard), through a drying column <strong>of</strong><br />
magnesium perchlorate, and then through a flowmeter. After the flowmeter, the hydrogen<br />
was split into two streams, one <strong>of</strong> which was bubbled through the boron tribromide, and<br />
then recombined into one stream before entering the reaction chamber or cell.<br />
The temperature <strong>of</strong> the bubbler, and <strong>of</strong> the cell, was controlled by wrapping each (and the<br />
associated gas lines) with heating tape and controlling the power input with a Variac variable<br />
transformer.<br />
The system was maintained at or below atmospheric pressure for this study, with most <strong>of</strong><br />
the data being obtained at 2 to 3 in. <strong>of</strong> mercury below atmospheric pressure.<br />
Tungsten wire was chosen as the substrate material, This wire was cleaned by passing it<br />
successively through a train consisting <strong>of</strong> concentrated nitric acid, a distilled water rinse,<br />
and an acetone rinse.<br />
Using the hydrogen-boron tribromide reactant system and 60-cps alternating current to<br />
develop n corona, approximately a dozen cell designs were tried. The cell design which 1<br />
appears to be the most satisfactory is pictured in Fig. 3. This cell consists <strong>of</strong> a 2-in.long<br />
pyrex glass tube with a neoprene O-ring inside each end and wrapped with eight turns<br />
<strong>of</strong> 3-mil tungsten wire along the tube length such that the wire is parallel and concentric<br />
to the axis <strong>of</strong> the tube. The wire is 0.9 cm from the axis. This assembly is then inserted<br />
in a 5-in.-long pyrex glass tube 1.5-in. in diameter and supported such that the tubes are<br />
concentric. A tungsten wire lead is then extended out <strong>of</strong> the tube, and neoprene rubber<br />
stoppers inserted in each end. Each stopper has a capillary tube through its center such<br />
that there are approximately 3 in. between the capillaries, and the filament enters and<br />
leaves the cell through these capillaries. The reactants also enter (and leave) the cell<br />
i!<br />
through the stoppers.<br />
I<br />
4<br />
1<br />
,<br />
I