U.S. patent number 3,618,753 [Application Number 04/760,356] was granted by the patent office on 1971-11-09 for large flake reconstituted mica insulation.
This patent grant is currently assigned to Minnesota Mining and Manufacturing Company. Invention is credited to David W. Glasspoole.
United States Patent |
3,618,753 |
Glasspoole |
November 9, 1971 |
LARGE FLAKE RECONSTITUTED MICA INSULATION
Abstract
A reconstituted mica insulation sheet comprising large mica
flakes has improved physical properties, particularly resistance to
cut-through and sever mechanical abuse without danger of electrical
failure. The sheet can be impregnated with resin, laminated to
webs, adhesive-coated, slit, and coiled to form insulating
tapes.
Inventors: |
Glasspoole; David W.
(Stillwater, MN) |
Assignee: |
Minnesota Mining and Manufacturing
Company (Saint Paul, MN)
|
Family
ID: |
25058853 |
Appl.
No.: |
04/760,356 |
Filed: |
September 17, 1968 |
Current U.S.
Class: |
428/324; 428/363;
428/451; 428/906; 428/447; 428/483; 428/910 |
Current CPC
Class: |
H01B
3/04 (20130101); Y10S 428/906 (20130101); Y10T
428/31797 (20150401); Y10T 428/251 (20150115); Y10S
428/91 (20130101); Y10T 428/31663 (20150401); Y10T
428/2911 (20150115); Y10T 428/31667 (20150401) |
Current International
Class: |
H01B
3/04 (20060101); H01B 3/02 (20060101); B32b
019/00 (); B32b 019/02 (); B65d 085/67 () |
Field of
Search: |
;161/163,171
;206/59 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Goolkasian; John T.
Assistant Examiner: Moxon, II; George W.
Claims
I claim:
1. In a self-supporting reconstituted mica insulation sheet
comprising an overlapping arrangement of unimpregnated mica flakes,
the improvement comprising:
the mica flakes having at least 40 percent by weight of the
individual flakes larger than 14 mesh,
at least 70 percent by weight of the individual flakes larger than
35 mesh, and
at least 90 percent by weight of the individual flakes larger than
60 mesh,
whereby the insulation sheet has increased density, excellent
tensile strength, outstanding electrical properties and resistance
to cut-through and physical abuse.
2. The insulation sheet of claim 1 impregnated with resin.
3. The insulation sheet of claim 2 wherein the resin selected from
the class consisting of epoxy resin, polyester resin, silicone
resin, alkyd resin, and acrylic resin.
4. The insulating sheet of claim 3 laminated to a fibrous web.
5. The laminate of claim 4 wherein the web is polyethylene
terephthalate.
6. The insulation sheet of claim 3 laminated to a polymeric
film.
7. The laminate of claim 6 wherein the polymeric film is biaxially
oriented polyethylene terephthalate.
8. As a new article of commerce, an insulating tape wound
convolutely upon itself in roll form and capable of being unwound
therefrom without delaminating or offsetting, said tape comprising
the insulation sheet of claim 1 or 2 laminated to one side of a
thin flexible web, whereby said insulating tape has increased
specific gravity, excellent tensile strength, outstanding
electrical properties, and resistance to cut-through and physical
abuse.
9. The tape of claim 8 wherein the insulation sheet has a second
thin flexible web laminated on its other side.
Description
BACKGROUND OF THE INVENTION
This invention relates to reconstituted mica insulation. More
particularly, it relates to reconstituted mica insulation sheets
and tapes having improved physical properties, particularly
resistance to cut-through and severe mechanical abuse.
Cut-through of electrical insulation occurs when, during
application or use, a sharp edge or corner of an insulated part
forces its way through and physically separates the insulation,
causing electrical failure. A particularly acute cut-through
problem exists in high voltage turbine generators having
rectangular copper conductors which must be insulated from each
other and from ground. The insulation utilized must have
exceptional electrical and mechanical properties, particularly
resistance to cut-through and severe mechanical abuse, and must
withstand being wrapped around small angle bends and being forced
into tight crevices without cracking, splitting, or developing
voids which would cause electrical failure. It has been found that
resistance to this type of failure can be predicted from the
results of a laboratory test which measures the force, in pounds,
required to force a sharp edge through an electrical
insulation.
Mica has excellent electrical, mechanical, and thermal properties,
but is thick and inflexible in its naturally occurring state.
Laminar mica crystals have been manually delaminated into
noncohesive splittings, laid in overlapping pattern by hand or
machine, and bonded with resinous material to form an insulation
sheet having resistance to mechanical abuse and cut-through
adequate for most purposes. However, machine laid sheets are thick,
often discontinuous, have a tendency to flake, are not uniform and
must be used in thick layers to obtain adequate electrical
properties. Hand-laid insulation sheets, are expensive, difficult
to make, have a tendency to flake, are in short supply domestically
and consequently must be obtained from import sources.
U.S. Pat. Nos. 2,405,576, 2,549,880, and 2,614,055 disclose
reconstituted mica insulation sheets made by reducing naturally
occurring mica into thin cohesive flakes, in the absence of a
deactivating atmosphere, pressing the flakes together, and drying
under heat and pressure. U.S. Pat. No. 3,131,114 discloses the
broad flake size range, about 3.5 to 400 mesh, utilized in
reconstituted mica flake insulation sheets having glass flakes
included therein. Such prior art reconstituted mica insulation
sheets have good electrical properties and are considerably more
flexible and uniform than sheets of mica splittings, but are opaque
and are dependent upon an impregnating resin for resistance to
cut-through and to physical abuse. When impregnated with soft resin
the sheets lack resistance to physical abuse and deformation while
sheets impregnated with hard resin crack and split during use with
a resultant decrease in electrical insulation properties.
Despite the long-recognized desirability of mica sheet or tape
insulation having both the resistance to cut-through and physical
abuse of mica splittings, and the electrical superiority,
uniformity, low caliper and flexibility of reconstituted mica, such
a product has never heretofore existed.
SUMMARY
This invention provides reconstituted mica insulation sheets and
tapes that combine excellent resistance to cut-through and physical
abuse with the electrical superiority, uniformity, low caliper, and
flexibility of reconstituted mica.
Insulation sheets and tapes prepared in accordance with this
invention have excellent electrical and physical properties. They
are flexible, dense, uniform, continuous, translucent, nonflaky,
and retain their electrical properties such as arc and corona
resistance, dielectric strength and low power factor, in severe
use. Further, these sheets are ideally suited for insulating
sheets, wrappers, and tapes having substantially improved
resistance to cut-through and mechanical abuse during application
and use. The insulation sheets of the invention are admirably
suited for commercial use in insulating direct current traction
motors, alternating current motors, and transformers, and are
particularly well suited for insulating the rectangular conductors
of high-voltage turbine generators. These mica insulation sheets
can be bent around sharp angle bends, including the right angle
bends at the edges of rectangular stator conductors, and can be
forced into small crevices without danger of electrical
failure.
Surprisingly, it has been discovered that a reconstituted mica
insulation sheet can be made from large mica flakes so as to have a
resistance to cut-through, when unimpregnated, more than 200
percent greater than broad flake size prior art reconstituted mica
sheets, while retaining the advantageous uniformity, flexibility,
and electrical properties. The mica flakes used to make these
sheets are considerably larger than the average size of mica flake
used to make prior art sheets. At least 40 percent by weight of the
flakes are larger than 14 mesh, at least 70 percent are larger than
35 mesh and at least 90 percent larger than 60 mesh. Preferably, at
least 50 percent of the flakes are larger than 14 mesh, at least 80
percent larger than 35 mesh and at least 95 percent larger than 60
mesh. Prior art reconstituted mica insulation sheets utilize a
broad flake size distribution from about 3.5 to 400 mesh, primarily
from about 35 to 400 mesh. It is believed that the large surface
area of individual flakes permits a large overlap area which
increases cohesion between flakes, eliminates internal voids in the
sheet to increase the specific gravity and provides a continuous
sheet. It is also thought that the large surface area of the large
flakes contributes the excellent resistance to cut-through and
physical abuse.
The strength and resistance to abuse of mica insulation sheets are
illustrated by tensile strength (ASTM Test D-828). Prior art
insulation sheet made with a broad flake size range ("Acim" Brand)
has an average tensile strength of about 400-500 p.s.i. Prior art
insulation sheet made with very small flakes ("Samica" Brand) has
an average tensile strength of about 1,200-2,400 p.s.i., while
sheets made according to this invention have an average tensile
strength of about 3,500-5,000 p.s.i.
The freedom from internal voids which characterizes the sheet of
this invention is illustrated by its specific gravity of about
1.6-2.5, which approaches the 2.7-2.8 specific gravity of solid
muscovite. Prior art reconstituted mica insulation sheet has a
specific gravity of about 0.9-1.5, which clearly indicates the
large number of voids contained therein. The specific gravity of
mica insulation sheets is readily determined by the Mercury
Intrusion Method described in Bulletin 2405-A of the American
Instrument Company.
Muscovite and phlogopite mica larger than about 3 mesh can be
utilized to produce these large mica flakes. After a preliminary
water washing to remove dirt and debris, the mica blocks are split
by means of water jets striking the mica blocks at an angle
substantially parallel to the plane of cleavage as disclosed in
U.S. Pat. No. 2,405,576. The flakes are classified with the proper
mesh in U.S. standard sieve and reconstituted by standard
papermaking techniques into a mica insulation sheet having an
overlapping arrangement of large mica with their surface in
contiguous relation. Flakes split in this manner are very thin and
have a large surface area as compared to their thickness. When
reconstituted, the individual mica flakes adhere to each other by
natural cohesive forces, as contrasted with mica splittings which
must be bonded together with resin.
After the reconstituted mica insulation sheet is made, it may be
impregnated with inorganic resin such as boron phosphates and
potassium borates and organic resin such as shellac, epoxy, alkyd,
polyester, silicone, etc., the choice of resin depending on a
balance of cost, temperature resistance, flexibility, and
electrical resistance required. Inorganic or organic binders,
fibers, and filaments may be incorporated into the sheet, if
desired. For some industrial applications, it is desirable to
laminate the large flake impregnated mica insulation sheet to a web
such as polymeric film and woven or nonwoven fabrics, either by
using the impregnating resin as an adhesive or by applying a
separate adhesive between the web and the insulation sheet. The
improved cut-through resistance of large flake reconstituted mica
insulation sheet is not dependent upon the saturating resin or
backing web, whereby permitting the utilization of numerous soft
resins which retain the flexibility of the insulation sheet.
Resistance to cut-through is determined by installing a 1/2" x 1/2"
x 3" mild steel bar, having a 32 micro inch finish on all sides, in
each jaw of an "Instron" tensile tester containing a compression
cell. Both bars are installed on edge at right angles to each other
so that only point contact will occur when the bars touch. The
sample specimen is placed between the bars and the machine jaws
closed at the rate of 0.5 inch/minute. The right-angle edges of the
steel bars are forced through the mica sheet until they contact
each other closing an electrical circuit to light a bulb which
indicates when cut-through is complete. The "Instron" recorder
provides an accurate reading of the force, in pounds, required to
force the sharp edges through the mica sheet.
The following examples, in which all parts are by weight unless
otherwise noted, illustrate preparation of the insulation sheets
and tapes of this invention without limiting the scope thereof.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
EXAMPLE 1
This example describes splitting mica-blocks into flakes and making
a reconstituted large flake mica insulation sheet. Indian muscovite
punch scrap is split into thin flakes by subjecting it to jets of
water as described in U.S. Pat. No. 2,405,576. The slurry of wet
mica flakes was classified by washing the flakes through a series
of U.S. standard screen sieves, all flakes below 140 mesh being
discarded. The classified flakes are recombined in a 1 percent mica
slurry in water such that 52 percent by weight of the flakes in the
final slurry are larger than 14 mesh, 85 percent are larger than 35
mesh and 93 percent are larger than 60 mesh.
The reconstituted sheet was then made by using commercial paper
mill equipment comprising, in connected series, an agitator, a
storage chest, and a cylinder-type paper machine having an endless
wet press belt which transfers the wet mica flake layer from the
cylinder screen to a steel wet press roll. The speed of the
cylinder screen was 16 ft./minute. An endless woven cotton belt
transferred the wet paper web into a drying section of the machine
where the paper was dried by passing through a series of steel
cylinders heated to between about 140.degree. F. and 180.degree. F.
The delivery rate of mica flake slurry to the paper machine
determines the thickness of the insulation sheet obtained. Sheet
thickness can be varied from about 0.5 mil to about 30 mils. If
thicker sheets are desired, sheets can be laminated or sandwiched
together. Mica insulation sheets produced in this manner have an
unusually high degree of uniformity of flake structure as is
evident from the uniform translucency observed when a sheet is held
up to a light source.
An insulation sheet made in the aforedescribed manner had an
average thickness of 2.47 mils when tested according to ASTM Test
D-374, Method C, a tensile strength of about 4,000 p.s.i. when
tested according to ASTM Test D-838, a dielectric strength of about
643 volts per mil when tested according to ASTM Test D-149, a
cut-through resistance of about 7 lbs., a specific gravity of about
1.7, and provided a useful insulation sheet without impregnation.
This mica sheet was impregnated, laminated, coiled and slit as
described in examples 2-5.
An insulation sheet utilizing the broad 3.5 to 400 mesh flake size
distribution of the prior art, disclosed by U.S. Pat. No.
3,131,114, was made and tested in the same manner. It has an
average thickness of 2.85 mils, a tensile strength of about 200
p.s.i., dielectric strength of about 350 volts per mil, a
cut-through resistance of about 2 lbs., and a specific gravity of
about 1.2.
EXAMPLE 2
This example describes impregnation of a portion of the large flake
reconstituted mica insulation sheet of example 1 with a
polyester/epoxy resin. A mixture of 100 parts of polyester/epoxy
resin and 1 part of tertiary amine [tris-(2,4,6-dimethyl amino
methyl)-phenol] was prepared according to example 2 of U.S. Pat.
No. 3,027,279. The impregnating resin was diluted to 25 percent
solids with methyl ethyl ketone and applied to the mica sheet by
means of a conventional dip and flow method. The impregnated paper
was then dried at 150.degree. F. for about 15 minutes and
subsequently cured for 10 minutes at 400.degree. F. The resultant
insulation sheet was tough, flexible, and in a fully cured state.
The resin content of the impregnated sheet was determined by
weighing a sample both before and after coating and was found to be
about 20 percent by weight.
The impregnated sheet, when tested in the manner of example 1, was
found to have an average thickness of 4.4 mils, a tensile strength
of about 10,400 p.s.i., a dielectric strength of about 690 volts
per mil, and a cut-through resistance of about 7.7 lbs.
Impregnation of a reconstituted mica insulation sheet utilizing the
broad 3.5 to 400 mesh flake size distribution of the prior art in a
similar manner with the same resin produced a sheet that was 4.7
mils thick, contained 20 percent resin and had a cut-through
resistance of 3.6 lbs.
EXAMPLE 3
A portion of the reconstituted large flake mica insulation sheet of
example 1, was impregnated in the manner of example 2, with an
isooctyl acrylate/acrylic acid/epoxy terpolymer resin and 0.45
percent uranyl nitrate hexahydrate catalyst.
The copolymer resin was made by first mixing 1,997.5 pounds of
isooctyl acrylate, 29.0 pounds of acrylic acid, and 17.9 pounds of
tertiary dodecyl mercaptan in a stainless steel tank. A charge of
2,787.5 pounds of toluene was then placed in a 1,500 gallon
glass-lined kettle, after which 147 pounds of the mixture in the
tank was added. The kettle was purged with nitrogen and heated to
175.degree. F. with constant agitation, all the while maintaining a
slight nitrogen flow through the kettle. Next, three separate
22-pound charges of azo-bisisobutyronitrile dissolved in toluene
were added at equal intervals over a period of approximately 50
minutes; each charge being 22 percent solids. During this period
the mixture from the tank was continuously added at a rate of about
37 pounds per minute. After waiting another 50 minute period, 20
pounds of 20 percent azo-bis-isobutyronitrile in toluene was added
and the temperature maintained at 175.degree. F. for 21/2
additional hours. Then, 124.1 pounds of
3,4-epoxycyclohexylmethyl-3,4-epoxy-cyclohexanecarboxylate having
an average molecular weight of about 260 and a viscosity of about
500 centipoises at 24.degree. C. (Union Carbide ERL-4221) was added
and thoroughly mixed. The mica sheet was impregnated as in example
2, and after drying for 10 minutes at 220.degree. F., and curing 10
minutes at 400.degree. F., the resin content was determined to be
20 percent. The tacky impregnated insulation sheet was then joined
to a 1.5 mil nonwoven web of heat bonded polyethylene terephthalate
fibers by means of laminating rolls.
The cut-through resistance of this laminate is substantially
greater than that of a prior art mica insulation sheet, as
described in example 1, similarly impregnated and laminated.
EXAMPLE 4
This example illustrates the impregnation of a portion of the mica
insulation sheet of example 1 with soft flexible silicone resin by
lamination to a resin impregnated woven glass cloth and subsequent
lamination to polyethylene terephthalate film.
Polysiloxane resin (General Electric SR-32) was diluted to 35
percent solids in toluene. A 2 mil woven glass cloth was
impregnated with this resin by the common dip and flow method and
laminated to a portion of the mica sheet of example 1 by means of
laminating rolls, and the laminate dried for 4 minutes at
400.degree. F. The laminate contained 10 percent resin, was 7.5
mils thick, and had a cut-through resistance superior to that of a
prior art mica insulating sheet, as described in example 1,
similarly saturated and laminated.
The unlaminated exposed mica surface was then coated with the
silicone resin saturant disclosed above, by reverse roll coating
technique, and dried for 4 minutes at 250.degree. F. The tacky mica
surface was then laminated to 0.25 mil biaxially oriented
polyethylene terephthalate film by means of laminating rolls,
coiled into a jumbo roll, and subsequently slit into 3/4 wide rolls
of tape. The resin content of the laminate was 15 percent and the
cut-through resistance was superior to that of a prior art mica
insulating sheet, as described in example 1, similarly impregnated
and laminated.
EXAMPLE 5
This example illustrates the lamination of a polyester film web to
the impregnated large flake reconstituted mica sheet of example 2.
After impregnation and following drying at 150.degree. F. for 15
minutes, the impregnated mica sheet was cooled and laminated to 0.5
mil biaxially oriented polyethylene terephthalate film by means of
rotating pressure rolls. The cut-through resistance of the laminate
was superior to that of a prior art mica insulating sheet, as
described in example 1, similarly impregnated and laminated.
* * * * *