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Oom O#00Noo-O March 9, 1943. H, wALTHER 2,313,410 PREPARATION OF BORON COMPOSITIONS Filéd March 31, 1959 O00NoO-OomOO# SWHO Nl SQNVLS/SSH .7/dl33d5 /N VE/V TOR H. WAL THER BV mgm ATTORNEY Patented Mar. 9, 1943 2,313,410 UNITED STATES PATENT OFFICE 2,313,410 PREPARATION 0F BORON COMPOSITIONS Henry Walther, Millburn, N. J., assignor to Beil Telephone Laboratories, Incorporated, New York, N. Y., a cgrporation of New York Application March 31, 1939, Serial No. 265,183 14 Claims. (Cl. 117-107) This invention relates to the preparation of tallic halide combines with the hydrogen in the resistor elements which have a negative tem proximity of the filament to deposit the metal perature coefllcient of resistance and more par thereon simultaneously with the formation of ticularly to the preparation of boron thermistors. the boron. The resulting product is homoge An object of this invention is to modify a mass neous and the ñlament upon which the boron of boron to change the characteristics thereof for and metal is deposited serves as a convenient rendering it suitable for use as a thermistor. guide for securing a required length of resist Another object of this invention is to incor ance unit. Alternatively, other metals or silicon porate throughout a mass of boron homogeneous or nitrogen may be incorporated with the boron ly another element. ‘ ~ ¿ 10 by subjecting boron trichloride, a reducing me A more particular object of this invention is dium and elemental nitrogen or a vaporized com to prepare simultaneously boron and another ele pound of the metal or silicon, such as a metal ment to produce a homogeneous substance adapt lic halide or silicon tetrachloride, to a heated sur ed for use as a thermistor. face such as an incandescent iìlament. The boron Boron has an exceptionally high negative tem 15 and metal or silicon or nitrogen is deposited on perature coeñ'icient of resistance. The conduc the filament simultaneously to form a homoge tivity of pure boron doubles for a 17° C. tem neous unit. perature rise in the range from zero to 100° C. A more comprehensive understanding of this This property is of special value in electrical sys invention is obtained by reference to the accom tems in which temperature control devices are 20 panying drawing, in which: required. However, the resistivity of pure boron Fig. 1 shows diagrammatically apparatus which is too high to be of practical use for this pur may be employed in the method of incorporat pose. The resistivity of a boron unit employed as ing a- metal with boron by the use of the ele a. thermistor may be materially lowered by in mental metal; corporating with it a small quantity of another 25 Fig. 2 represents portions of apparatus which element, such as aluminum. While boron with may be used in a modification of the method. ap certain amounts of other elements, such as mag paratus for which is shown in Fig. l; nesium, or aluminum, cr both, has been hereto Figs. 3 and 4 are views of a thermistor pro fore prepared, the resulting product is hetero duced by the method of this invention; and geneous. The grain size of such products ranges 30 Fig. 5 is a graphic representation of the tem from relatively large crystals to a fine powder and perature-resistance characteristics of the ther the crystals are extremely irregular. mistors shown in Figs. 3 and 4. In accordance with this invention, small quan In the apparatus of Fig. 1 a supply of a reduc tities of metals or silicon or nitrogen are intro ing medium such as hydrogen is indicated by the duced into boron to form a homogeneous mass 35 block labeled “Hydrogen” The hydrogen passes which is admirably adapted for use as thermistors. through a stop-cock l0 to a means for freeing The grain size and crystals of the product result the hydrogen from any contaminating materials, in'g from the practice of this invention are uni such as oxygen. This means is represented by form. The metal or silicon or nitrogen is in the block labeled “Purifier” and may comprise troduced when the boron is formed by the inter 40 heated capper gauze. From the puriñer the hy action oi‘ boron halide and a reducing agent when drogen passes to a drier comprising, for example, subjected to a suitable heated surface. Prefer phosphorus pentoxide or other efficient de ably, the metal if it is above hydrogen in the hydrating agent. The hydrogen then passes electrochemical series is disposed in the form oi through a flow meter to a mixing chamber. a shield around a heated surface comprising a 45 A boron halide such as boron trichloride is heated filament of tungsten. A boron halide, contained in a flask i2 which is cooled by solid such as boron trichloride, and a reducing mate carbon dioxide I3 in a Dewar flask I4. From the rial, such as hydrogen or carbon monoxide, are' ñask l2 the boron trichloride passes through a then passed over the heated filament. The re mercury valve i 5 containing two fritted glass ducing material interacts with the boron trichlo 50 filters I6 and il and thence through a iiow ride or other halide of boron to form boron and meter Yto the mixing chamber. The fritted glass hydrochloric or hydrohalogen acid. The boron filters I6 and i'l-are fused in the valve l5. The is deposited on the filament. The halogenated pores of these filters are so iine that mercury at product. such as hydrochloric acid, reacts with vacuum or at a pressurel even in excess of one the metal to form a halide thereof. The me 55 atmosphere cannot pass through, while gases 2 2,313,410 readily pass. A convenient fluid for the flow to a reservoir 38 containing mercury 39. A three meter in the hydrogen line is alpha monobromo way stop-cock 40 associated with the reservoir naphthalene. In the boron trichloride line no 38 is capable of applying pressure to the mer such organic liquid may be employed since the cury by means of air through a line 4I or re boron trichloride reacts with these materials. ducing the pressure thereof by connection to the Mercury is employed in the flow .meter vof the atmosphere through line 42. boron trichloride line and is also employed in A source of nitrogen gas may be employed for the valve I5. The valve I5 is supplied with mer flushing the apparatus. In the illustrated ap cury I8 contained in a reservoir I9 through a paratus the nitrogen passes through a stop-cock stop-cock 20 to control the fiow of boron trichlo 10 44 through the puriñendrier, flow meter to the ride to the mixing chamber. mixing chamber and thence through the deposit To eiiectuate this control, a three-way stop chamber 24, ‘ivalve 33 to the exhaust tube 39. cock 23 is connected to the reservoir I9 to con After the apparatus has been flushed, it is de trol the pressure on the mercury by means of sirable to remove the nitrogen in the system be air pressure supplied through a tube 2| from a fore heating the filament 21, since the nitrogen source not shown, or to reduce the pressure would combine with the boron deposited on the thereon to that of the atmosphere `through a filament. Accordingly the nitrogen is turned off tube 22. When it is desired to stop the flow of by means of a stop-cock 44 and hydrogen passed boron trichloride to the mixing chamber the through the system until the system is entirely stop-cock 20 is opened to permit the mercury freed of nitrogen. from the reservoir I9 to flow into the two arms If the shell 43 be of aluminum, for example, of the valve I5. The stop-cock 23 is opened to the hydrochloric acid resulting from the inter allow air pressure to be applied to the mercury action of boron trichloride and hydrogen reacts I8 in the reservoir I9. Under these conditions with the aluminum to form aluminum chloride. the mercury is forced up the two arms of the This aluminum chloride in turn is decomposed valve I5 to the height of that of the glass filters to form aluminum as a result of the interaction I6 and I1. When it is desired that the boron of aluminum chloride with the hydrogen present. trichloride be passed to the mixing chamber, the When boron trichloride and hydrogen pass over air pressure is removed and the pressure exerted a heated surface such as hot tungsten filament on the mercury I8 reduced to atmospheric by 30 the reaction is' turning the stop-cock 23 to connect the reser voir I9 to the tube 22. When this condition pre vails, the mercury in the arms of the valve I5 To deposit boron on the tungsten filament the flows back to a point below the junction of the temperature of the filament is preferably main two arms. Preferably, the boron trichloride in tained between 800° C. and 1500" C. Toward the flask I2 is free of chlorine. While chlorine either end of this temperature range the time does not constitute a harmful impurity from the rate of deposit decreases, at the lower end due to standpoint of >the boron to bedeposited, its pres slow chemical reaction and at the higher end due ence contaminates the mercury and may render to excessive evaporation. ’I'he most suitable tem the mercury seal valve l5 inoperative. 40 perature was found to be approximately 1300" C.
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