U.S. patent number 3,689,608 [Application Number 05/048,825] was granted by the patent office on 1972-09-05 for process for forming a nonwoven web.
This patent grant is currently assigned to E. I. du Pont de Nemours and Company, Wilmington, DE. Invention is credited to Herbert John Hollberg, John Edward Owens.
United States Patent |
3,689,608 |
|
September 5, 1972 |
PROCESS FOR FORMING A NONWOVEN WEB
Abstract
A process for spreading, electrostatically charging, and
forwarding a fibrous web concomitantly formed with a vapor blast.
The web is charged by passing it through a highly ionized zone
created by a corona discharge between an ion gun and a target
plate. The electrical potential between the ion gun and target
plate causes current to flow which is sufficient to deposit a
charge on the web which is preferably 75 to 100 percent of the
maximum sustainable charge, but low enough to avoid loss of web
charge through secondary corona discharge between the target plate
and the web.
Inventors: |
Herbert John Hollberg
(Richmond, VA), John Edward Owens (Hockessin, DE) |
Assignee: |
E. I. du Pont de Nemours and
Company, Wilmington, DE (N/A)
|
Family
ID: |
26726566 |
Appl.
No.: |
05/048,825 |
Filed: |
June 10, 1970 |
Current U.S.
Class: |
264/441; 264/121;
264/53; 264/465 |
Current CPC
Class: |
D04H
3/16 (20130101); D01D 5/04 (20130101); H01T
19/04 (20130101); D01D 5/11 (20130101) |
Current International
Class: |
D04H
3/16 (20060101); D01D 5/00 (20060101); D01D
5/04 (20060101); D01D 5/11 (20060101); H01T
19/00 (20060101); H01T 19/04 (20060101); D04h
003/03 () |
Field of
Search: |
;264/24,53,205,DIG.75
;18/8E,8W,8B ;28/72.12,76 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Robert F. White
Assistant Examiner: W. E. Hoag
Attorney, Agent or Firm: Howard P. West, Jr.
Parent Case Text
CROSS REFERENCES TO RELATED APPLICATIONS
This application is a continuation of U.S. application Ser. No.
735,889, filed June 10, 1968 and now abandoned, which is a
continuation-in-part of U.S. application Ser. No. 372,623, filed
June 4, 1964 now U.S. Pat. No. 3,387,326.
Claims
1. A process comprising: flash extruding a solution of organic
polymeric material into a gaseous atmosphere to form a
plexifilamentary web; spreading the web; passing the spread web
through an ionized zone created by a corona current between a
multi-point ion gun and a grounded target electrode to charge the
web, said web being passed in brushing contact with said target
electrode, said ion gun being connected to an electric potential
for initiating and maintaining said current; maintaining said
current at a level for depositing a charge on said web of from
about 75-100 percent of a peak charge, said level being below that
level for producing said peak charge and depositing the web on a
moving collecting
2. The process of claim 1 wherein said gaseous atmosphere is at
least about
3. The process of claim 2 wherein said gaseous solvent is
4. The process of claim 1 including the step of applying a
potential on said collecting surface which is opposite in polarity
to the charge on the
5. The process of claim 1, said current being maintained at a level
of from about 225- 325 microamperes.
Description
This invention concerns a novel and useful process for charging
fibrous webs in an electrostatic field and depositing the webs
uniformly in overlapping layers on a moving surface to form a
nonwoven sheet.
The process described and claimed herein is particularly useful in
charging webs of a continuous fibrillated strand described in U.S.
Pat. No. 3,081,519 to Blades and White. This web is prepared by
flash extrusion of a solution of crystallizable polymer. In the
"flash extrusion" process the strand is formed by extruding a
homogeneous solution of a fiber-forming polymer dissolved in a
liquid. The solution, at a temperature above the normal boiling
point of the solvent and at autogeneous or greater pressure, is
extruded into a medium of lower temperature and substantially lower
pressure. The vaporizing liquid within the extrudate forms bubbles,
breaks through confining walls, and cools the extrudate, causing
solidification of the polymer.
The resulting fibrous web is a multifibrous yarn-like strand having
an internal fine structure or morphology which may be characterized
as a 3-dimensional integral plexus consisting of a multitude of
essentially longitudinally extended interconnecting, random-length
fibrous filaments, hereafter referred to as film-fibrils. These
film-fibrils have the form of thin ribbons with an average
thickness less than about 4 microns. The film-fibril elements often
found as aggregates, intermittently unite and separate at irregular
intervals called "tie-points" in various places throughout the
width, length, and thickness of the strand to form an integral
3-dimensional plexus. The film-fibrils are often rolled or folded
about the principal film-fibril axis, giving the appearance of a
fibrous material when examined without magnification. The strand
comprising a 3-dimensional network of film-fibril elements is
referred to as a plexifilament. The plexifilaments are unitary,
i.e. the strands are one continuous piece of polymer, and the
elements which constitute the strand are interconnected. They can
be produced in essentially endless lengths in deniers as low as 15
or as high as 100,000 or even higher.
The plexifilament of Blades and White may be collected in the form
of a nonwoven fibrous sheet and may be consolidated by cold or hot
calendering to provide useful sheet products. These products and
the process for making them are described in Steuber U.S. Pat. No.
3,169,899. This patent describes an electrostatic device for
promoting attraction of the strand to a collecting belt. The device
is very satisfactory for preparing nonwoven fibrous sheets with
exceptional strength. However, in further developing the process,
it has become evident that improvements are needed to provide a
high degree of dispersion and uniformity in sheets destined for
certain uses. These improvements are needed particularly when the
sheet is to be used in printing papers, book covers and wall
coverings. It has been discovered that the requirements for
aerodynamic stability of the fine fibril network and the
requirements for uniform electrostatic charging are somewhat in
opposition to each other. These requirements must therefore be
carefully matched for production of uniform sheets.
The purpose of the present invention is to provide an improved
aerodynamic and electrostatic process for spreading and charging a
plexifilament strand and for depositing the strand in the form of a
nonwoven sheet with a high degree of dispersion and uniformity.
In the process of the invention the flash spinning, spreading, and
depositing operations are conducted in a closed chamber to provide
a uniform high dielectric atmosphere. A freshly spun plexifilament
strand and the accompanying expanding solvent gas are directed from
the spinneret to a spreading zone created by a baffle or other
confining surface whereby the plexifilament strand is opened into a
wide configuration. The spread strand is passed in a path of
advance directly from the spreading means into a highly ionized
zone created by corona discharge in the atmosphere between an ion
gun and a flat target plate. The electric potential between the ion
gun and target plate is sufficient to generate a current flow to
deposit a charge on the spread strand which is preferably 75 to 100
percent of the maximum sustainable peak charge, but is low enough
to avoid disruptive spark discharge or secondary corona discharge
between the thin trailing edge of the target plate and the strand.
The target plate is placed immediately adjacent to the mechanical
spreading means in such manner that the vapor blast from the
spinneret guides the web to provide brushing contact with the
target. The surface of the target plate is of planar construction,
particularly in the area just upstream of the trailing edge. The
target plate terminates in a thin trailing edge to provide uniform
but minimum aerodynamic turbulence at this point during operation.
The ion gun is a structure supporting a plurality of charging
needles disposed across the path of advance. The gun is placed
opposite the target and mounted in a manner that permits
circulation of vapor around it, since during operation the confined
gases tend to flow toward the path of advance over the top of the
gun. Preferably the face and the top of the gun housing are smooth
and shaped to minimize aerodynamic turbulence. The needles are
aimed at points which are uniformly spaced from the trailing edge
of the target plate by a technique described hereinafter. The
spread and charged fibrous web is then deposited on a continuously
moving surface, electrically discharged and collected by
conventional means such as windup in a roll.
FIG. 1 is a cross-sectional schematic elevation of an apparatus
embodiment useful in the practice of the invention.
FIG. 2 is a partial cross-sectional schematic elevation of another
apparatus embodiment useful in the practice of the invention.
FIG. 3 is an elevation showing the relative positions of the ion
gun, rotary baffle and target plate of FIG. 2, the spinneret nozzle
being removed for clarity.
FIG. 4 is an enlarged partially sectioned fragmentary view of FIG.
2, showing the relationship of the conducting needles to the target
electrode.
FIG. 5 is a partial cross-sectional schematic elevation
illustrating a shrouded spinning orifice useful in separating the
plexifilament as spun.
FIG. 6 is an enlarged partially sectioned front elevation of the
shrouded opening orifice and target plate of FIG. 5.
FIG. 7 is a curve wherein web charge, percent peak web charge, and
belt current are plotted as ordinate vs. ion gun current as
abscissa.
FIG. 8 is a series of curves wherein web charge is plotted as
ordinate vs. target plate current as abscissa.
DETAILED DESCRIPTION OF THE ILLUSTRATED EMBODIMENTS
Referring to FIG. 1, a spinneret device 10, connected to a source
of polymer dissolved in an organic solvent is shown. Polymer
solution 12 under pressure is fed through spinning orifice 14 into
web forming chamber 16. The extrudate from spinning orifice 14 is a
plexifilament 7. Due to the pressure drop at spinning orifice 14
vaporization of solvent creates a vapor blast which, by virtue of
impingement upon baffle 18 concomitantly with plexifilament 7,
generally follows the path of advance of the plexifilament 7 from
spinning orifice 14 to collecting surface 9, thereby creating a
flow pattern within chamber 16 as indicated by the arrows. Baffle
18 is oscillatably mounted and is powered to oscillate by means not
shown. While oscillation of the baffle is not essential, it is
preferred for the preparation of wide sheets.
As shown target plate 20 and ion gun 22 are disposed on opposite
sides of the path of advance of the plexifilament web 7 and
downstream from the web forming and mechanical separating devices.
Target plate 20 is connected to ground by wire 24 and microammeter
26 which indicates target plate current. Ion gun 22 contains
multiple needles 25, one of which is shown in FIG. 1. Each needle
25 of ion gun 22 is connected to a negative D.C. source 35 through
resistor 19. Each of the resistors is connected to the source of
power through conductor 21. Millameter 23 serves to measure ion gun
current. A negative D.C. source in the range of from 45 to 70
kilovolts may be used. Target plate 20 is so disposed that the
vapor blast originating at spinning orifice 14 and the air flow
pattern in Chamber 16 carries plexifilament web 7 in brushing
contact with its charging surface. After passing through an ionized
charging zone created by a corona discharge between ion gun 22 and
target plate 20, the charged plexifilament web 7 is deposited on
collecting surface 9. The surface illustrated is a continuous belt
forwarded by drive rolls 36. The belt is given an opposite charge
to that imposed on web 7 by means of D.C. source 37 which is
connected to the collecting apparatus through milliameter 29 and
lead 27. Due to the opposite polarity between web 7 and surface 9
the web in its arranged condition clings to the surface as sheet 38
with sufficient force to overcome the disruptive influences of
whatever vapor blast may reach this area. Surface 9 carries sheet
38 past compacting roll 44 and feeds the sheet out of chamber 16
through port 39 where it is collected on windup roll 42. Flexible
elements 40 across port 39 assist in the retention of vapor within
chamber 16. Roller seals or labyrinth seals may also be used. A
conventional solvent recovery unit 43 may be beneficially employed
to improve economic operation.
Alternate apparatus embodiments useful in the practice of the
invention are shown schematically in FIGS. 2-6. Referring to FIG.
2, the extrudate from orifice 14' is carried around the curved
surface of a lobed baffle 18' into brushing contact with the
surface of an annular target electrode 20'. Baffle 18' is
continuously rotated to impart oscillatory movement to the network
of film fibril material as it is deflected from the lobed surface.
Annular target electrode 20' is coupled, for rotary movement about
baffle 18' by means of ring 50 and pinion gear 52 attached to
driven shaft 54. Target electrode 20' is connected to lead 24
through a contacting carbon brush 56. Ion gun 22' is U-shaped and
is connected to a negative D.C. source through lead 24. FIG. 3
shows the arrangement of U-shaped ion gun 22' opposite annular
target electrode 20' with the baffle 18' centered within the
electrode. Needles 25' are arranged in the lower tubular portion of
the ion gun 22' such that the axes of the needles are generally
perpendicular to the surface of target electrode 20' (FIG. 4).
An alternative mechanical spreading arrangement is illustrated in
FIGS. 5 and 6 where spinning orifice 14 is surrounded by a shroud
15 having a stepped slot 17 therethrough. The plexifilament on
extrusion tends to open and follow the stepped contour of slot 17.
The extrudate can be impinged on a fixed or moving baffle or
directed along the path of advance without baffling (as shown) when
the shrouded orifice is employed to spread the web. Other shapes
for slot 17 may be successfully employed as for example, a bell or
a conical shape. Positioning of ion gun 22 is important to obtain
maximum charging efficiency and also to avoid web bunching and
flicking which are detrimental to sheet uniformity. "Bunching" is a
small pileup which occurs when a web passing down a target plate is
slowed by pinning forces. "Flicking" occurs when fast moving web
hits this bundle and flips it away from the target plate, sometimes
resulting in hangup on the needle point 25 and always discharging
the web unevenly. Thus, although a short distance between
needlepoint 25 and target plate 20 provides a relatively low
voltage requirement to produce a given target plate current, close
spacing can only be tolerated if web flicking and bunching is held
to a minimum. The problems are particularly acute in the production
of sheets from plexifilamentary structures due to the fluffy nature
of the plexifilament which makes it particularly susceptible to
irregularities caused by non-uniform aerodynamic or electrostatic
patterns. Use of a baffle or spinneret shroud helps to spread and
thereby dissipate the vapor blast that flashes from the spinneret.
A high velocity vapor stream at the collecting surface otherwise
disarranges deposited webs and causes them to roll. Thus a smooth
pattern of vapor flow within chamber 16 is important to assist in
the orderly forwarding of plexifilament 7 along its path of advance
from spinning orifice 14 to collecting surface 9 while avoiding
interference with the plexifilament at the collecting surface.
Equipment shapes to promote these aerodynamic desirata are
important for efficient and high speed operation. For instance the
targets 20, 20' shown in FIGS. 1 and 4 terminate in a thin edge,
and the target surface is planar just upstream of the edge, such a
shape being important to promote smooth vapor flow despite the
electrical discharge known to be associated with sharp edges. A
thin layer 58 of epoxy resin at the outer edge of the target
electrode 20' as illustrated in FIG. 4 is useful in reducing
secondary ionization at the edge of the target electrode by
eliminating a sharp conductive edge. Use of a resistor 19 in series
with each needle has been found to provide needle-to-needle current
uniformity important in the production of uniform sheet products
especially when operating at a low current per needle. Operation
below about 10 microamperes per needle is desirable when using an
ion gun with resistors separating each needle from the current
source. With needle separation of about three-eighths inches in an
ion gun of this type, between about 6 and 8 microamperes per needle
is used for depositing a linear polyethylene plexifilament. The ion
gun with a resistor in series with each needle provides a high
impedance circuit to each needle point so that normal fluctuations
in the effective dynamic resistance of corona discharge have little
effect on emitted current. In a typical ion gun/target
configuration the effective dynamic resistance of corona discharge
is about 60 megohms, whereas the resistance 19 placed in series
with each point is typically 600 megohms. Use of the resistors
makes the needle-to-needle current variations much less sensitive
to such factors as point/target spacing, point wear, point
contamination, and point-to-point spacing.
The position of needles 25 with reference to target plate 20 is
important for efficient operation. It will be apparent that the
clearance between the needle points and plate 20 should be as small
as efficient operation will permit. Generally a clearance of from
about 0.4 to about 2 inches (1 to 5 cm.) is satisfactory although
this will vary with the design and capacity of the particular
equipment. It has been found convenient in adjusting positioning of
gun 22 opposite to target plate 20 to create a carbon black deposit
on target plate 20 by spraying powdered carbon black into the
operating area between the plate and the gun. An oval pattern is
outlined by carbon deposits opposite each needle indicating the
area of electrostatic influence of each needle under the particular
conditions employed. Such a pattern of carbon deposit 13 is shown
in FIG. 6. The patterns laid down by single points are centered the
same distance apart as the needles, are oval shaped, and have a
height of about 2.5 cm. and a width of about 0.6 cm. Smoothest
operation of the equipment with uniform laydown occurs when the
above-mentioned test patterns are centered at a distance between
one-half in. (1.3 cm.) and three-fourths in. (1.9 cm.) from the
bottom edge of the target. Placement of the ion gun at a point
further upstream results in pinning or clinging of the web to the
target plate because of field concentration between the already
charged fiber and the thin edge. This results in bunching for an
instant, an uneven discharge across the web width, and a falling
free of the bunched web to give a nonuniform sheet. In addition,
when the gun is aimed further upstream on the target plate, the web
charge curve is very abrupt as will be demonstrated hereinafter,
making the process more difficult to control. On the other hand if
the ion gun is aimed too near the trailing edge of the target
plate, secondary ionization will develop at the edge of the target
plate providing positively charged ions which will discharge the
web unevenly. The web will then collapse and give a ropey strand
which in turn gives a nonuniform sheet. In addition the discharged
web will not pin well to the belt because it has lost most of its
charge. In general the target plate must be of such dimensions that
in cooperation with the vapor blast, it will guide the mechanically
opened web into the electrostatic charging zone, which zone must be
sufficiently removed from possible interfering grounded structures
such as spinneret 10 or baffle 18 so that shorting out of the gun
does not occur.
In general, in providing field-assisted laydown of plexifilament 7,
three methods may be used to produce strong electrostatic pinning
forces on the charged fibers: 1. Use of a conductive laydown roll
or belt, insulated from ground and raised to a high potential
(e.g., 60 KV). 2. use of a semiconductive laydown belt, in contact
with a stationary electrode to which a high potential is connected.
3. Use of a porous woven belt of insulating material in contact
with an electrode to which a high potential is connected.
The two critical electrostatic requirements placed upon the laydown
surface are: 1. That an intense electric field can emanate from or
be transmitted through the laydown surface toward the approaching
fibers. 2. That the current produced by neutralization of charged
fibers at the laydown surface have a path to ground. In the case of
method 3 above, the path is through the interstices of the woven
belt, wherein vapor is made conductive as a result of ionization
occurring at the laydown surface.
Two requirements for effective charging are a high density of ions
of a single polarity and a high electric field intensity in the
vicinity of the fibers. For a given ion gun-target plate geometry,
ion density is determined primarily by the value of corona current.
Web charging results from impingement of ions onto the fibers as
the ions move toward the grounded target electrode. Approximately
10-15 percent of the total corona current is carried away as charge
on the fibers because the projected web area is small compared to
the cross-section of the ion stream. To place the highest charge on
a given mass of web it is necessary to have the fibers close to the
target electrode so that the field force lines from the charges on
the fiber are directed preferentially toward ground, This
directionality of field force in effect reduces the field force
component that tends to repel additional ions and prevent them from
depositing on the fiber surface. Very little charge is lost through
web contact with the target electrode surface. The negative ions
impinge on the side of the fibers away from ground, and
conductivity of the fibers is too low to leak much of the charge to
the target. In addition, it is probable that a thin layer of
solvent vapor lubricates the target, keeping most of the fibers out
of direct contact with it.
The optimum web charge for a given combination of apparatus,
polymer and solvent may be determined by considering the
relationship of target plate current versus web charge. Three
relationships are shown in FIG. 8 for two different ion guns, the
equipment being otherwise identical, where one gun is operated
during two different polymer flow rates. In each instance the
clearance between the points of needles 25 and target plate 20 is
1.5 inches. Other dimensional and operational variations for each
of curves A, B and C are listed in Table I below, where polymer
flow rate is in pounds per hour and "target aim" is the distance in
inches from a point on target plate 20 directly opposite the point
of needle 25 to the bottom edge of target plate 20.
TABLE I Polymer Curve Needles on Gun Flow Rate Target Aim
_________________________________________________________________________
_ A 19 42 2.5 B 25 29 0.5 C 25 45 0.5
_________________________________________________________________________
_ the necessary data are obtained from spinning experiments wherein
the electric potential (in kilovolts) between ion gun and neutral
ground is increased incrementally, and the target plate current
(observed at 26 in microamperes) and the web charge (in
microcoulombs/gram) are determined and recorded. Web charges are
determined by collecting the web after it leaves the target plate
and before it reaches the collecting belt for a given period of
time in a Faraday pail. The potential relative to ground to which
the pail rises during the collecting period is measured by an
electrostatic voltmeter (e.g. Rawson type 518, Rawson Electrical
Instruments Co., Cambridge, Mass.). A high quality capacitor is
connected across the input terminals of the voltmeter to provide an
on-scale deflection of the voltmeter corresponding to the
accumulated charge. This value of capacitance is normally
substantially larger than the total other capacitances in the
metering circuit. From the well known relationship between voltage,
charge and capacitance, the charge collected per gram is calculated
as follows:
q = (CV/tw)
where: q = web charge level, microcoulombs/gm C = capacitance,
microfarads V = indicated voltage, volts t = sampling time, seconds
W = throughput of the web gm/sec From a consideration of the curves
it will be noted that increasing web charge is obtained with
increasing target plate current (obtained by increasing potential)
until a peak is reached. Thereafter secondary ionization becomes
significant and it becomes then increasingly difficult to retain a
charge on the web. Secondary ionization is characterized by a glow
discharge at the trailing edge of the target plate between the
target plate and film-fibrils as they leave the target plate. For
uniform web formation it is preferred to operate at a voltage
between ion gun and neutral ground that will provide a web charge
between about 75 percent and 100 percent of peak value under
non-secondary ionization conditions. The sharp peak of curve A is
typical of the condition wherein needles 25 are aimed too far
upstream from the edge of target plate 20. Under these conditions
it is relatively difficult to maintain a constant charge on
successive portions of the web and across the width of the web.
Much more satisfactory control is obtained in situations such as
those shown in curves B and C. In all of the curves A, B and C
increasing the target plate current above the peak charge level for
the web has detrimental effects in that the web tends to pin or
cling to the target plate resulting in bunching and flicking which
are detrimental to the sheet uniformity. This occurs because of
secondary ionization which causes non-uniform loss of charge,
uneven collapse, and uneven laydown, the plexifilament 7 tending to
roll during laydown if it is not properly electrostatically held to
the collecting belt. This causes a sheet of poor uniformity and
rope-like fiber bundles appear in the sheet.
It is to be noted that very high charge levels are obtained on
plexifilamentary webs compared to solid fibers melt-spun at the
same corona current level. For example, one can obtain a charge of
5 microcoulombs/gram on linear polyethylene plexifilament with only
150 microamperes of current with a 25 point gun (6 microamps per
corona point). Typical melt spun fibers such as those described in
U.S. Pat. No. 3,341,394 to Kinney require a current of 50 to 75
microamperes/point to obtain charges at this level.
The process and apparatus of this invention are particularly useful
for flash-spinning in a solvent laden atmosphere. It is desirable
to spin into an atmosphere containing less than 30 percent air
(more than 70 percent gaseous solvent). Spinning of this type must
be done with polymer/solvent combinations that separate rapidly on
cooling. It is then possible to spin into a closed chamber and have
adequate solidification and crystallization of the fiber structure.
Thus, a solution of linear polyethylene and trichlorofluoromethane
(Freon-11 of Du Pont) may be spun into a closed chamber, whereupon
the web is spread by a baffle or shroud, is charged
electrostatically, and is deposited on a moving belt. The gaseous
solvent may then be recovered by compression and condensation
without difficulty. In the open ventilated cells previously used
this would have been much more difficult because of the large
amount of air present.
EXAMPLE
A plexifilament of linear polyethylene was spun from a solution
containing 12.5 percent .+-. 0.3 percent linear polyethylene by
weight, and 87.5 percent .+-. 0.3 percent trichlorofluoromethane
(Freon-11), and 1,750 ppm of an antioxidant (Irganox No. 1010). The
solution was pumped continuously through a pipeline to a single
spinneret pack. The solution was delivered to the spinneret pack at
a temperature above the boiling point and at a pressure close to
the critical pressure of the solvent. The solution was spun through
a spinneret of the type shown in FIGS. 2, 3 and 4 at a rate
equivalent to 35.0 - 35.8 lbs./hour of polymer. As the solution
passed in a horizontal direction through orifice 14' into the
atmosphere of the enclosure, the solvent evaporated and a
plexifilament was formed. This plexifilament was spread and
directed downward into a vertical path by passage over the rotary
baffle 18'. At the same time the combined action of the expanding
solvent gas and the curved surface of the baffle spread the
plexifilament into a wide web. This web then traversed annular
target plate 20'. The target plate outer diameter was 19.0 cm. and
the inner diameter was 14.0 cm. The outer trailing edge of the
target plate comprised a bead of non conductive epoxy resin set
into the rim of the target plate as shown in FIG. 4. The bead width
in the plane of the target face was 0.32 cm. The web was directed
downward across the trailing edge 58 and continued toward a
continuously moving collecting belt of wire mesh traveling at 60
ft./min.
The spread web was exposed to the ionized atmosphere between
negatively charged ion gun 22' and target plate 20' during passage
and thereby collected a negative charge. The ion gun was a U-shaped
device having 24 needles spaced 0.95 cm. apart. In this experiment
the needles were attached directly to a common power source and no
resistors were used in the needle connections. The curved portion
of the U-shaped ion gun was semi-circular and concentric with the
annular target plate. The needle points were located opposite the
target plate 1.43 cm. from the outer edge (including 0.32 cm of
epoxy rim and 1.11 cm. of metal). The needle points were 1.59 cm.
from the target plate surface. The collecting belt was either
positively charged or was neutral (grounded), depending upon the
particular test items. A number of test conditions were studied and
are recorded in Table II.
The spinneret pack included a letdown chamber and a letdown orifice
upstream of the final orifice 14'. The letdown orifice was 0.035
inch (0.889 mm.) in diameter and passed through a land 0.025 inch
thick (0.635 mm.). The letdown chamber volume was 24 cm..sup.3. The
final orifice was 0.030 inch (0.762 mm.) in diameter and the land
for the final orifice was 0.25 inch (0.635 mm.). The solution was
provided to the letdown orifice at a temperature of 185.5.degree.C.
and a pressure of 1,750 - 1,800 psig (123.5 to 127.0
kg./cm..sup.2). It passed then through the letdown orifice into the
letdown chamber, which was maintained at a pressure of 1,050 psig.
Finally, the solution passed from the spinneret orifice into a
cylindrical tunnel (not shown) in the conical end of the spinneret
pack. The tunnel was concentric with the orifice hole. The tunnel
diameter was 0.188 inch (0.478 cm.) and the length was 0.188 inch
(0.478 cm.). The spinneret pack was located with the orifice 13
inches (33.0 cm.) above the belt. The bottom of the target plate
was 2.7 inches (6.86 cm.) below the orifice.
During the spinning operation the Freon concentration in the closed
chamber surrounding the spinneret pack was about 93 to 96 percent
by volume, the remainder being mostly air. The charged web was
collected on the moving belt and was consolidated by passage under
a roll at the end of the belt which provided a pressure of about 34
lbs./linear inch (6.1 kg./cm.). The roll diameter was 9.65 inches
(24.5 cm.). The roll temperature was about 55.degree. C.
Baffle 18' as shown in FIG. 3 contains three lobed fillet portions.
As the baffle turned about its axis, these lobed portions diverted
the plexifilaments either to the left or right of the center line,
providing an oscillating motion in the strand. The fibrous strand
was therefore deposited in oscillating fashion on the belt in
multidirectional over-lapping layers. The belt was forwarded at a
speed of 60 ft./min. and the baffle turned at a speed of 1,400
revolutions/min.; consequently several multidirectional layers were
collected at each point along the length of the sheet at its center
of width. In a commercial operation sheet of much greater width may
be obtained by depositing overlapping layers of plexifilaments from
many spinnerets on a single belt.
The annular target plate 20' was adapted to rotate at a speed of
2.3 revolutions/min. about an axis concentric with the rotating
baffle axis. The target plate was provided with a wicking device
(not shown) which coated the surface of the target with Zelec U.N.
lubricant, a conductive liquid which was beneficial for maintaining
a uniform conductive path to ground during the test. The target
plate was grounded through conductor 24. A microammeter was
provided between a power pack and U-shaped ion gun 22'. In
addition, a microammeter was provided between the conductive
collecting belt and either ground potential or a positive DC
source.
In this series of experiments the spinneret pack of FIGS. 2 to 4
was located over a moving belt similar to the one shown in FIG. 1.
The belt current measured by microammeter 29 was used to indicate
extent of fiber charging. Some of the test items were run with no
applied voltage on the belt and others were run with 15 kilovolts
positive potential applied (oppositely charged relative to fiber).
In either case the belt mechanism was electrically insulated from
ground except for the path through microammeter 29 or through both
microammeter 29 and positive direct current source 37. It has been
found that substantially all of the current flowing from the ion
gun is collected by either the target plate or by the collecting
belt; thus
I.sub.g - I.sub.tp = I.sub.b where I.sub.g equals the ion gun
current, I.sub.tp equals target plate current to ground, and
I.sub.b equals belt current to ground. The charge on the fibers was
calculated from the belt current I.sub.b and the polymer flow rate
W by means of the equation:
(I.sub.b /W) = Q wherein I.sub.b is the belt current in
microamperes, W is the weight in grams of fiber passing between the
ion gun and target plate per second, Q is the charge expressed in
microcoulombs per gram.
The data from this series of experiments are reported in Table II.
The various items in Table II are listed in order of increasing ion
gun current. The suffix letters A to V indicate the chronologic
order, A being first and V being last. It has been found that this
order is important in cases where the target plate accidentally
becomes coated with polymer residues. These residues may form a
hard varnish which in turn tends to change the conductivity of the
target plate or tends to promote the formation of high current
densities in pin-point areas or cavities on the target plate. This
in turn causes spark discharge, low web charge level, and low belt
current. A comparison of Items 10A and 11V shows that this
condition was avoided. In addition the data in Table II indicate
that the current from collecting belt to ground was substantially
the same with or without belt potential applied. Compare, for
example 10A with 9B or 8U with 11V.
Now considering the effect of various ion gun current levels on
quality of the deposited sheet, Table II shows the width of the
deposited swath and the range in width with ion gun currents from
100 up to about 500 microamperes. The sheet width was measured
outside the spinning enclosure over a period of time and the
maximum and minimum values were recorded. The width of the sheet
included all of the deposited web regardless of thickness. In Table
II no range is shown when the width varies less than 0.5 inch.
The basis weight averages for the sheets reported in Table II were
obtained from circular samples each 1 inch (2.54 cm.) in diameter.
The samples were cut from approximately the center of the collected
sheet width. In each case the basis weight average was determined
from 120 samples in three rows of 40, the samples in each row being
taken 6 inches (15.24 cm.) apart along the length of the sheet. The
rows were 3 inches (7.62 cm.) apart in the cross-sheet
direction.
The basis weight uniformity was established by calculation of
standard deviation .sigma. defined by the formula:
where X = average basis weight in oz./yd..sup.2 X = individual
basis weight in oz./yd..sup.2 n = number of samples and .SIGMA. (X
- X).sup.2 = the summation of the square of the differences between
X and X.
The data recorded in Table II show that the standard deviations
were at a minimum with Items 3E through 12I (ion gun current 200 to
325 microamperes). In this same range the maximum sustainable swath
width was between 18 and 21 inches (45.8 and 53.2 cm.). In multiple
spinneret operations the highest possible swath widths are most
desirable since less equipment is required. For this reason in this
example Items 4Q through 12I are especially preferred (ion gun
currents 225 to 325 microamperes and swath widths 19.5 to 21 inches
(49.6 to 53.2 cm.). In the discussion of FIG. 7 which follows it
will be shown that Items Q through I were obtained under charging
conditions which give 75 to 100 percent of the maximum sustainable
charge (peak charge).
The uniformity of the swath was determined both by swath width
uniformity in the deposited sheet and by visual observation of the
network midway between target plate and collecting belt. Uniformity
was satisfactory for ion gun currents of 100 to 325 microamperes.
With still higher ion gun currents the fiber appeared to be
non-uniformly distributed in the swath. Also under conditions of
ion gun current greater than 325 microamperes a continuous spark
discharge occurred between the target plate trailing edge and the
fiber which had already left the edge. This was readily observed by
darkening the spinning cell. These observations are recorded in
Table II. It is believed that this "lightning" or spark discharge
is responsible for a loss in fiber charge. A discharge of lesser
significance occurs at lower ion gun currents usually in the form
of an even glow from the trailing edge of the target when viewed in
the dark. All of these discharges from the target plate edge are
termed "secondary corona".
FIG. 7 is a curve plotted from the data of Table II for items with
zero belt potential.
In FIG. 7, the abscissa indicates the ion gun current as measured
by a microammeter in the negative DC power supply to the ion gun.
Three ordinates dimensions are shown on the figure. One of these is
"belt current". The "belt current" was the current measured by the
microammeter 29 between the belt structure and positive DC source
37 as shown in FIG. 1 or it was the current measured by
microammeter 29 directly to ground when the belt was not charged.
Other parameters which were derived from belt current are shown in
FIG. 7. These are "Web Charge", as determined by the formula
already described and "Percent Peak Web Charge". The peak web
charge is identified by Point 12I in FIG. 7. It will be obvious
that Point 12I indicates not the maximum charge recorded, but the
maximum sustainable charge. For operating conditions to the right
of Point I the measured belt current fluctuates when measurements
are taken over a period of time. It is believed that the
fluctuations are due to differences in web charge which is brought
to the belt by the plexifilament material. A high charge is carried
to the belt when the amount of "lightning" discharge is low. Such
conditions are represented by the upper curve marked "moderate
secondary corona". If a greater amount of "lightning" discharge
occurs while the belt current is being measured the current levels
indicated by the lower curve will occur. In practice of course the
charge level for conditions to the right of Point 12I oscillates
randomly between the upper and lower curve. For the purpose of
clarity the peak charge is identified as the maximum sustainable
charge as represented by Point 12I. The percent of peak charge at
any operating condition is determined by dividing the given charge
by the peak charge and multiplying the resulting fraction by 100.
The charge level is calculated from belt current by use of the
formulas already described.
By comparison of the swath width and standard deviation values of
Table II with the curves of FIG. 7, one may determine optimum
operating conditions for the process. In order to achieve maximum
swath width while still obtaining low standard deviation in basis
weight (Items 4Q to 12I of Table II) the process of Example I must
be operated at conditions represented in FIG. 7 by ion gun currents
between 225 and 325 microamperes. In this operating range the fiber
accumulated a charge of 6.75 to 9.00 microcoulombs per gram which
is 75 to 100 percent of the maximum sustainable charge for the
system operating with belt at ground potential. ##SPC1##
The process of the invention may be operated with a conductive
target plate having either a non-conductive trailing edge as in the
example, or a conductive trailing edge. In operating with a target
plate that has a conductive trailing edge, "lightning" occurs at a
lower current level than for a plate having an insulated trailing
edge. Charging curves obtained with a target plate having
conductive trailing edge are depicted in FIG. 8. While this target
plate is very satisfactory, the target plate with an insulated rim
is preferred, since a higher peak charge may be obtained. This
follows from the fact that there is no longer a conductive sharp
edge to permit high field concentration between the plexifilament
web and the target plate edge or between the ion gun and the target
plate edge. Higher charge levels are beneficial for obtaining
greater spreading of the network. Of course when operating the
target plate with a non-conductive edge, one should be especially
careful to operate under conditions on the left side of the
charging curve depicted in FIG. 7. In this way "lightning" is
avoided and a higher peak charge is obtained than can be obtained
with a conductive edge.
It should be noted that the target plate should be kept clean
during operation, and efficient conductive paths to ground should
be maintained. The target plate can be provided with a scraper to
remove deposits at a point outside of the corona discharge area.
The target plate should have a smooth surface to avoid field
concentrations at pits or points. For example, the surface may be
coated with a liquid conditioning material supplied through a wick.
Because of the importance of a clean, smooth surface, the target
plate should preferably be pre-conditioned by lapping with an
abrasive material such as a 500 grit abrasive cloth before use in
the spinning apparatus.
While the present invention has been described with particular
reference to the formation of sheet products from plexifilaments of
polyethylene, it is obvious that the nature of the polymer, the
solvent, in which it is dissolved and the particular extrusion
equipment is not critical. Some suggested alternatives may be found
in U.S. Pat. No. 3,081,519 to Blades and White dated Mar. 19, 1963.
While the target plate has been described as presenting a "flat"
surface to the path of advance of the web and the ion gun, plate
curvatures and other constructions which do not interfere with the
smooth flow of gases and the mechanically opened web across the
target plate may be used. It is important for avoiding turbulence
as the web leaves the target plate, that the trailing edge of the
plate be flat. While the flat edge is illustrated to be either
straight or circular, other edge shapes may be used, provided
aerodynamic and electrostatic non-uniformity is avoided.
Mechanical separation of the elements of the web may be
accomplished in any manner. A fixed or oscillating baffle is
suitable as is a shrouded spinneret device or combination of shroud
and baffle. Arrangement of the mechanical opening means and target
plate in such manner as to prevent recycling vapors from lifting
the web away from the plate during its advance is particularly
desirable. While the system illustrated shows the imposition of a
negative charge on the web while it travels its path of advance,
and a positive charge on the collecting surface, these polarities
may be reversed.
* * * * *