U.S. patent number 3,635,824 [Application Number 04/838,862] was granted by the patent office on 1972-01-18 for resistance heater and method for preparation thereof.
This patent grant is currently assigned to Bell Telephone Laboratories, Incorporated. Invention is credited to Raymond G. Brandes, Charles M. Pleass.
United States Patent |
3,635,824 |
Brandes , et al. |
January 18, 1972 |
RESISTANCE HEATER AND METHOD FOR PREPARATION THEREOF
Abstract
A resistance heater comprising a sintered mass of refractory
particles, each particle comprising an insulating core coated with
a thin film of an electrically conducting material, is obtained by
a processing sequence involving coating the particles of interest,
compacting the coated particles to form a pellet and sintering the
pellet. Devices produced in accordance with the described technique
manifest enhanced reliability and uniformity as compared with prior
art heaters, and permit a new degree of freedom in the design of
heating elements.
Inventors: |
Brandes; Raymond G.
(Meyersville, NJ), Pleass; Charles M. (Reiffton, PA) |
Assignee: |
Bell Telephone Laboratories,
Incorporated (Murray Hill, NJ)
|
Family
ID: |
25278242 |
Appl.
No.: |
04/838,862 |
Filed: |
July 3, 1969 |
Current U.S.
Class: |
252/512; 427/229;
219/209; 219/543; 338/223; 338/308; 392/438; 427/215; 427/383.3;
427/58 |
Current CPC
Class: |
H05B
3/00 (20130101) |
Current International
Class: |
H05B
3/00 (20060101); H01b 001/02 () |
Field of
Search: |
;252/512,513,514,515,518,520,521 ;117/227 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Drummond; Douglas J.
Claims
We claim:
1. A method for the fabrication of a resistance heater comprising
the steps of (a) coating the major faces and periphery of a
plurality of individual particles of an electrically insulating
refractory material with a thin layer of an electrically conducting
metal material, (b) compacting the resultant powder comprising the
coated particles to form a pellet in which a plurality of contacts
are formed between the conductive material of adjacent particles,
and (c) sintering said pellet at elevated temperatures in a
reducing ambient, so resulting in the growth of said contacts into
electrically conductive necks between adjacent particles.
2. Method in accordance with claim 1 wherein sintering is conducted
at a temperature greater than one-half the melting point of the
said conductive material.
3. Method in accordance with claim 1 wherein compacting is effected
by pressing techniques.
4. Method in accordance with claim 1 wherein said insulating
material is aluminum oxide and said conductive material is
molybdenum.
Description
This invention relates to a technique for the fabrication of a
resistance heater and to the heaters so produced.
Heretofore, it has been widely recognized by those skilled in the
art that the total exploitation of the resistance heat concept in
electron device technology has been limited by certain inherent
drawbacks. Among the most severe of such drawbacks is the fact that
the resistive element used to carry current and develop heat in
consequence is restricted in geometry by the fundamental
relationship W I.sup.2 R, where W represents power or heat output,
I represents current and R resistance. Accordingly, if the
resistance, R, of the element is low, the current, I, flowing in
the element must be proportionately high to maintain a given
output. Unfortunately, power sources capable of sustaining high
currents are intrinsically expensive and undesirable currents in
excess of about 10 amperes being generally avoided. Thus, in order
to fabricate a useful resistive heating element from a metal, its
aspect ratio must be increased to the point which we recognize as a
wire.
Although wire configurations are useful as resistance heaters in
numerous applications, they cannot be efficiently employed for the
purpose of heating objects, whose dimensions are large, with
respect to typical wire diameters, uniformly by direct contact with
the object surface. This end may only be obtained by interposing a
thermal conductor between the object and the wire, such thermal
conductor acting as a thermal diffuser. Additionally, metal heating
elements in which at least one dimension is very small are prone to
mechanical damage, local variations in resistivity drastically
reducing the useful life and reliability of the element.
Recognizing these limitations, workers in the art focused their
attention upon thin sheets and the concept of passing current
therethrough. Unfortunately, it was found that the only technique
for limiting current levels involved causing current flow along a
major dimension of a very thin sheet, the limits on thickness being
such as to make fabrication of reproducible, high reliability
elements almost impossible. This obviates the likelihood of using
the configuration for heating systems other than those which are
linear and which function at low temperature.
More recent investigations of the resistance heater technology have
concentrated upon the synthesis of composite materials manifesting
resistivities intermediate that of a metal and an insulator. This
concept has typically taken the form of a mechanical mixture of
metal and insulator but it too has been handicapped by practical
limitations such as the establishment of complete conducting paths,
the likelihood of creating reproducible resistances, etc.
In accordance with the present invention these prior-art
difficulties are successfully overcome by a novel processing
sequence which results in the formation of a resistance heater
comprising a sintered mass of electrically insulating refractory
particles individually coated with a thin film of an electrically
conductive material. The described structure includes a continuous
chain of such metal coated particles which are held together by the
sintering action of the metal films at the points of contact, such
chain manifesting a resistance determined by the thickness of the
applied metal film and the diameter of the conductive necks formed
between each particle, that is, the conductive region formed by
migration of metal from the surface of the films on adjacent
particles into the contact region under the influence of the
cohesive force induced between metal surfaces in contact with each
other at elevated temperatures. In light of the fact that these
variables are controllable, the technique permits the formation of
composites evidencing resistivities suitable for a wide range of
applications. Studies of the characteristics of the resultant
devices have revealed that not only have all the prior-art
limitations been overcome but also that there is obtained a
structure manifesting enhanced reliability and uniformity as
compared with the prior art structures.
The invention will be more readily understood from the following
detailed description taken in conjunction with the accompanying
drawing, wherein:
FIG. 1 is a cross-sectional view of a resistance heater of the
present invention;
FIG. 2 is a front elevational view of a sphere bearing a resistance
heater of the present invention; and
FIG. 3 is a front elevational view in cross section of a typical
device heated by the resistance heater of the invention.
A general outline of the procedure employed in fabricating the
novel structures described herein will now be given.
The first step in the practice of the present invention involves
coating a plurality of independent particles of an electrically
insulating refractory material with a thin film of an electrically
conducting material. Typically, the insulating material is selected
from among ceramic materials, for example, alumina, beryllia,
magnesia, zirconia, etc., the choice of a particular insulating
material being dependent upon the intended use of the resultant
structure. More specifically, the insulating material must be
capable of withstanding the temperatures to which the desired
structure will be heated without chemically reacting with the
conducting material. Thus, a suitable choice of materials for one
desiring to fabricate a structure capable of heating uniformly at
1,800.degree. C. might be tungsten and alumina, such materials not
reacting at an appreciable rate until a temperature of
2,000.degree. C. is reached. Accordingly, the only limitation on
the insulating material is that it not react with the conducting
material at the desired temperature of operation.
Particle size of the insulating material is of no criticality.
However, a preference exists for the use of crushed polycrystalline
material having particle size ranging from 80 mesh to Fischer
subsieve size average 7.0.
The electrically conducting materials found suitable for coating in
accordance with the present invention may be selected from among
the transition metal elements of groups 6B and 8 of the Periodic
Table of the Elements (see Handbook of Chemistry and Physics, 45the
Edition, 45th by the Chemical Rubber Company). Materials found to
be particularly useful for this Chemical include iron, nickel,
tungsten, molybdenum, platinum, iridium, etc.
Coating of the insulating particles may be effected by any
conventional coating or plating technique, for example,
fluidization by dry or wet methods, electroless plating, etc. A
particularly useful method for effecting this end when particle
diameters less than 10.mu. are desired, the wet fluidization
procedure, is described by D. W. Maurer et al. in U.S. Pat. No.
3,404,034 which issued on Oct. 1, 1968. It will be appreciated by
those skilled in the art that the thickness of the metal film so
deposited is not critical and may vary from a few monolayers to
thousandths of an inch, such range being dictated by considerations
relating to end use and the resistivity of the conductive element.
The particles so coated are not in the form of a powder and are
ready for the next stage of processing.
Following, the coated particles, either alone or in combination
with a binder, are compacted by any well-known compacting procedure
such as pressing, electrophoresis, etc. The most convenient
procedure, pressing, involves insertion of the coated particles in
a suitable die followed by pressing at pressures up to 150,000
p.s.i.g., thereby resulting in the formation of a pellet comprising
a plurality of individually metal-coated electrically insulating
refractory particles wherein metal contacts are formed between
metal layers of adjacent particles.
The compacted pellet is then placed in a suitable boat which is
inserted in a furnace maintained at room temperature. Then, the
furnace is purged with an inert gas such as purified dry nitrogen,
argon or helium for several minutes and the inert gas replaced by a
reducing gas such as hydrogen. The furnace is then put into
operation and is heated to a temperature such to effect sintering
of the powders contained within the pellet. For the purposes of the
present invention, it will be understood that the sintering
temperature varies with the metal of the coating but typically
occurs at temperatures above one-half the melting point of the
metal. A typical sintering temperature with molybdenum involves
heating to a temperature within the range of 1,300-1,600.degree. C.
for a time period ranging from 1 to 180 minutes, the shorter time
period corresponding with the higher temperature. The sintering
operation, as described, results in the growth of the metal
contacts alluded to above into electrically conductive necks
between adjacent compacted particles. The binder, if used, will be
volatilized at low temperature during the warmup to the sintering
temperature.
With reference now to FIG. 1, there is shown a cross-sectional view
of the resistance heater of the present invention. Shown in the
Figure is a sintered body 11 comprising a plurality of electrically
insulating particles 12, each of which is coated with a thin film
of an electrically conductive material 13, adjacent particles being
in contact with each other by means of conductive necks 14.
The unique application of the instant invention will be more fully
appreciated by reference to FIGS. 2 and 3. In FIG. 2, there is
shown an elevational view of a sphere 21 having a pair of
electrodes 22 and 23 wound around the circumference thereof and
intermediate said electrode pair a laminated layer 24 of a sintered
mass of electrically insulating coated particles coated with a thin
layer of an electrically conductive material. It is evident by
reference to the drawing that uniform resistive heating of the
sphere will be obtained by passage of current through the
electrodes. The principle embodied can clearly be extended to
irregularly shaped bodies of any kind, the only limitation being
that the geometric magnitude of the irregularity should be large
compared to the particle size of the cermet powder employed.
FIG. 3 is a front elevational view in cross section of another
embodiment of the present invention wherein an electronic device
31, such as a semiconductor device, is heated by resistance heater
32 laminated between metal film electrodes 33 and 34.
An example of the present invention is set forth below. It is
intended merely as an illustration and it is to be appreciated that
the process described may be varied by one skilled in the art
without departing from the spirit and scope of the invention.
EXAMPLE
A plurality of particles of crushed polycrystalline aluminum oxide
obtained from commercial sources and ranging in particle size from
1 to 10 microns was suspended in silicone oil and charged to a
fluidization column which was immersed in a constant temperature
oil bath. Fluidization was initiated by admitting a stream of
hydrogen containing molybdenum carbonyl vapor into the column and
coating attained by refluxing for 6 hours, thereby causing
decomposition of the carbonyl and coating of the aluminum oxide
with a thin film of molybdenum. The coated particles were then
cooled, separated from the oil by filtration, washed with acetone
and dried in air.
The coated particles in powder form were then intimately mixed with
1 milligram of stearic acid per gram of powder and inserted in a
conventional hydraulic press. Then, 85,000 p.s.i.g. of pressure
were applied by actuating the press, so resulting in the formation
of a pellet. The pellet was then positioned in a furnace and, with
hydrogen flowing, was fired for 30 minutes at 1,600.degree. C. Upon
cooling, the resultant pellet evidenced a resistivity of
approximately 5 ohm-centimeter and upon the application of
evaporated molybdenum electrodes thereon was available for use as a
resistance heater in a configuration of the type disclosed in FIG.
3. During operation of such a structure, it was determined that the
device of interest could be heated at a temperature of
1,050.degree. C. over a time period of 9,000 hours without
significant change in uniformity or electrical characteristics.
* * * * *