U.S. patent application number 13/829351 was filed with the patent office on 2013-08-22 for seamless fuser member process.
This patent application is currently assigned to XEROX CORPORATION. The applicant listed for this patent is Xerox Corporation. Invention is credited to Jonathan H. Herko, Francisco J. Lopez, Dante M. Pietrantoni, Michael S. Roetker, Kyle B. Tallman, Jin Wu.
Application Number | 20130214454 13/829351 |
Document ID | / |
Family ID | 45696063 |
Filed Date | 2013-08-22 |
United States Patent
Application |
20130214454 |
Kind Code |
A1 |
Wu; Jin ; et al. |
August 22, 2013 |
SEAMLESS FUSER MEMBER PROCESS
Abstract
Described herein is a method forming a belt suitable for use
with an image forming system. The method includes coating a
composition of a polyimide, a phosphate ester and a solvent onto an
outer surface of a rotating metal belt, and subsequently curing and
releasing the composition from the metal belt.
Inventors: |
Wu; Jin; (Pittsford, NY)
; Herko; Jonathan H.; (Walworth, NY) ; Lopez;
Francisco J.; (Rochester, NY) ; Tallman; Kyle B.;
(Farmington, NY) ; Pietrantoni; Dante M.;
(Webster, NY) ; Roetker; Michael S.; (Webster,
NY) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Xerox Corporation; |
|
|
US |
|
|
Assignee: |
XEROX CORPORATION
Norwalk
CT
|
Family ID: |
45696063 |
Appl. No.: |
13/829351 |
Filed: |
March 14, 2013 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
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12868362 |
Aug 25, 2010 |
8414815 |
|
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13829351 |
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Current U.S.
Class: |
264/300 |
Current CPC
Class: |
B29C 2791/001 20130101;
B29C 41/28 20130101; B29C 33/68 20130101; Y10T 428/31721 20150401;
B29K 2105/24 20130101; B29K 2079/08 20130101; B29D 29/00 20130101;
B29C 35/02 20130101 |
Class at
Publication: |
264/300 |
International
Class: |
B29D 29/00 20060101
B29D029/00 |
Claims
1. A method of forming a seamless belt suitable for use with an
image forming system, comprising: flow coating a composition of a
polyimide, a phosphate ester internal release agent and a solvent
onto and directly contacting an outer surface of a rotating
substrate; fully curing the coating at a temperature of from about
125.degree. C. to about 190.degree. C. for a time of from about 30
to about 90 minutes, and then at a temperature of from about
250.degree. C. to about 370.degree. C. for a time of from about 30
to about 90 minutes to form a seamless belt; removing the fully
cured belt from the rotating substrate.
2. The method of claim 1, wherein the composition further comprises
a polysiloxane polymer selected from the group consisting of a
polyester modified polydimethylsiloxane, a polyether modified
polydimethylsiloxane, a polyacrylate modified polydimethylsiloxane,
and a polyester polyether modified polydimethylsiloxane.
3. The method of claim 1, wherein the phosphate ester is selected
from the group consisting of an alkyl alcohol ethoxylate phosphate,
an alkyl phenol ethoxylate phosphate, an alkyl polyethoxyethanol
phosphate, and an alkylphenoxy polyethoxyethanol phosphate, and
said polyimide and said phosphate ester are present in a weight
ratio of about 20/80 to about 80/20.
4. The method of claim 1, wherein the solvent is selected from the
group consisting of tetrahydrofuran, methyl ethyl ketone, methyl
isobutyl ketone, N,N'-dimethylformamide, N,N'-dimethylacetamide,
N-methylpyrrolidone and methylene chloride.
5. The method of claim 1, further comprising: coating an
intermediate layer on an outer layer of the cured belt, wherein
said intermediate layer comprises silicone.
6. The method of claim 5, further comprising: coating a release
layer on the intermediate layer, wherein said release layer
comprises fillers and a fluoropolymer.
7. The method of claim 6, wherein the fillers are selected from the
group consisting of carbon blacks, carbon nanotubes, metal oxides,
doped metal oxides, polyanilines, polythiophenes, polyacetylene,
poly(p-phenylene vinylene), poly(p-phenylene sulfide), pyrroles,
polyindole, polypyrene, polycarbazole, polyazulene, polyazepine,
poly(fluorine), polynaphthalene, salts of organic sulfonic acid,
esters of phosphoric acid, esters of fatty acids, ammonium or
phosphonium salts, and mixtures thereof, and wherein the
fluoropolymer comprises a fluoroelastomer or a fluoroplastic.
8. The method of claim 1, wherein the substrate comprises a metal
belt, said belt possessing an Ra of from about 0.01 micron to about
0.5 microns and an R.sub.max of from about 0.02 micron to about 4
microns.
9. A method of forming a seamless fuser member, comprising: flow
coating a composition of a polyimide, a phosphate ester internal
release agent, a polysiloxane polymer and a solvent onto and
directly contacting an outer surface of a rotating substrate; flow
coating a composition of a polyimide, a phosphate ester internal
release agent and a solvent onto and directly contacting an outer
surface of a rotating substrate; fully curing the coating at a
temperature of from about 125.degree. C. to about 190.degree. C.
for a time of from about 30 to about 90 minutes, and then at a
temperature of from about 250 .degree. C. to about 370.degree. C.
for a time of from about 30 to about 90 minutes to form a seamless
belt; removing the fully cured belt from the rotating substrate;
coating a intermediate layer on an outer layer of the cured belt;
and coating a release layer on the intermediate layer.
10. The method of claim 9, wherein the solvent is selected from the
group consisting of tetrahydrofuran, methyl ethyl ketone, methyl
isobutyl ketone, N,N'-dimethylformamide, N,N'-dimethylacetamide,
N-methylpyrrolidone and methylene chloride.
11. The method of claim 9, wherein the polysiloxane polymer is
selected from the group consisting of a polyester modified
polydimethylsiloxane, a polyether modified polydimethylsiloxane, a
polyacrylate modified polydimethylsiloxane, and a polyester
polyether modified polydimethylsiloxane.
12. The method of claim 9, wherein the phosphate ester is selected
from the group consisting of an alkyl alcohol ethoxylate phosphate,
an alkyl phenol ethoxylate phosphate, an alkyl polyethoxyethanol
phosphate, and an alkylphenoxy polyethoxyethanol phosphate.
13. The method of claim 9, wherein the substrate comprises a metal
belt, said belt possessing an Ra of from about 0.01 micron to about
0.5 microns and an R.sub.max of from about 0.02 micron to about 4
microns.
14. A method of forming a seamless belt suitable for use with an
image forming system, comprising: flow coating a composition of a
polyimide, a phosphate ester internal release agent, a polysiloxane
polymer and a solvent onto and directly contacting an outer surface
of a rotating substrate wherein the rotating substrate comprises a
metal belt, said metal belt possessing an Ra of from about 0.01
micron to about 0.5 microns and an R.sub.max of from about 0.02
micron to about 4 microns; fully curing the coating at a
temperature of from about 125.degree. C. to about 190.degree. C.
for a time of from about 30 to about 90 minutes, and then at a
temperature of from about 250.degree. C. to about 370.degree. C.
for a time of from about 30 to about 90 minutes to form a seamless
belt; removing the fully cured belt from the rotating
substrate.
15. The method of claim 14, wherein the composition further
comprises a polysiloxane polymer selected from the group consisting
of a polyester modified polydimethylsiloxane, a polyether modified
polydimethylsiloxane, a polyacrylate modified polydimethylsiloxane,
and a polyester polyether modified polydimethylsiloxane.
16. The method of claim 14, wherein the phosphate ester is selected
from the group consisting of an alkyl alcohol ethoxylate phosphate,
an alkyl phenol ethoxylate phosphate, an alkyl polyethoxyethanol
phosphate, and an alkylphenoxy polyethoxyethanol phosphate, and
said polyimide and said phosphate ester are present in a weight
ratio of about 20/80 to about 80/20.
17. The method of claim 14, wherein the solvent is selected from
the group consisting of tetrahydrofuran, methyl ethyl ketone,
methyl isobutyl ketone, N,N'-dimethylformamide,
N,N'-dimethylacetamide, N-methylpyrrolidone and methylene
chloride.
18. The method of claim 14, further comprising: coating an
intermediate layer on an outer layer of the cured belt, wherein
said intermediate layer comprises silicone.
19. The method of claim 18, further comprising: coating a release
layer on the intermediate layer, wherein said release layer
comprises fillers and a fluoropolymer.
20. The method of claim 19, wherein the fillers are selected from
the group consisting of carbon blacks, carbon nanotubes, metal
oxides, doped metal oxides, polyanilines, polythiophenes,
polyacetylene, poly(p-phenylene vinylene), poly(p-phenylene
sulfide), pyrroles, polyindole, polypyrene, polycarbazole,
polyazulene, polyazepine, poly(fluorine), polynaphthalene, salts of
organic sulfonic acid, esters of phosphoric acid, esters of fatty
acids, ammonium or phosphonium salts, and mixtures thereof; and
wherein the fluoropolymer comprises a fluoroelastomer or a
fluoroplastic.
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application relates to commonly assigned co-pending
application Ser. No. 12/868,362, entitled SEAMLESS FUSER MEMBER
PROCESS, filed simultaneously herewith and incorporated by
reference herein.
BACKGROUND
[0002] 1. Field of Use
[0003] This disclosure is directed to a fuser member and a method
of manufacture.
[0004] 2. Background
[0005] Centrifugal molding is used to obtain seamless polyimide
belts useful as fuser members. Typically, a thin fluorine or
silicone release layer is applied to the inner surface of a rigid
cylindrical mandrel. A polyimide coating is applied to the inner
surface of the mandrel containing the release layer. The polyimide
is cured and then released the mandrel.
[0006] There are drawbacks to this process. The length of the
polyimide belt is determined by the size of the mandrel. The
requirement of a release layer on the inner surface of the mandrel
is an additional process step.
SUMMARY
[0007] Described herein is a method forming a belt suitable for use
with an image forming system. The method includes flow coating a
composition of a polyimide, a phosphate ester and a solvent onto an
outer surface of a rotating substrate. The coating is partially
cured at a temperature of from about 125.degree. C. to about
190.degree. C. for a time of from about 30 to about 90 minutes to
form a belt. The partially cured belt is removed from the rotating
substrate. The partially cured belt is tensioned and rotated at a
temperature of from about 250.degree. C. to about 370.degree. C.
for a time of from about 30 to about 90 minutes to cure the
belt.
[0008] Described herein is a method of forming a belt suitable for
use with an image forming system. The method comprises flow coating
a composition of a polyimide, a phosphate ester and a solvent onto
an outer surface of a rotating substrate. The coating is cured at a
temperature of from about 125.degree. C. to about 190.degree. C.
for a time of from about 30 to about 90 minutes, and then at a
temperature of from about 250.degree. C. to about 370.degree. C.
for a time of from about 30 to about 90 minutes to form a belt. The
fully cured belt is removed from the rotating substrate.
[0009] Described herein is a method of forming a fuser member. The
method comprises flow coating a composition of a polyimide, a
phosphate ester, a polysiloxane polymer and a solvent onto an outer
surface of a rotating substrate. The coating is partially cured at
a temperature of from about 125.degree. C. to about 190.degree. C.
for a time of from about 30 to about 90 minutes to form a belt. The
partially cured belt is removed from the rotating substrate. The
partially cured belt is tensioned and rotated at a temperature of
from about 250.degree. C. to about 370.degree. C. for a time of
from about 30 to about 90 minutes to cure the belt. An intermediate
layer is coated on an outer layer of the cured belt; and a release
layer is coated on the intermediate layer.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The accompanying drawings, which are incorporated in and
constitute a part of this specification, illustrate several
embodiments of the present teachings and together with the
description, serve to explain the principles of the present
teachings.
[0011] FIG. 1 depicts an exemplary fusing member having a belt
substrate in accordance with the present teachings.
[0012] FIG. 2 depicts a tensioning of a fusing member for final
curing.
[0013] It should be noted that some details of the FIGS. have been
simplified and are drawn to facilitate understanding of the
embodiments rather than to maintain strict structural accuracy,
detail, and scale.
DESCRIPTION OF THE EMBODIMENTS
[0014] Reference will now be made in detail to embodiments of the
present teachings, examples of which are illustrated in the
accompanying drawings. Wherever possible, the same reference
numbers will be used throughout the drawings to refer to the same
or like parts.
[0015] In the following description, reference is made to the
accompanying drawings that form a part thereof, and in which is
shown by way of illustration specific exemplary embodiments in
which the present teachings may be practiced. These embodiments are
described in sufficient detail to enable those skilled in the art
to practice the present teachings and it is to be understood that
other embodiments may be utilized and that changes may be made
without departing from the scope of the present teachings. The
following description is, therefore, merely exemplary.
[0016] Furthermore, to the extent that the terms "including",
"includes", "having", "has", "with", or variants thereof are used
in either the detailed description and the claims, such terms are
intended to be inclusive in a manner similar to the term
"comprising." The term "at least one of" is used to mean one or
more of the listed items can be selected.
[0017] Notwithstanding that the numerical ranges and parameters
setting forth the broad scope of the invention are approximations,
the numerical values set forth in the specific examples are
reported as precisely as possible. Any numerical value, however,
inherently contains certain errors necessarily resulting from the
standard deviation found in their respective testing measurements.
Moreover, all ranges disclosed herein are to be understood to
encompass any and all sub-ranges subsumed therein. For example, a
range of "less than 10" can include any and all sub-ranges between
(and including) the minimum value of zero and the maximum value of
10, that is, any and all sub-ranges having a minimum value of equal
to or greater than zero and a maximum value of equal to or less
than 10, e.g., 1 to 5. In certain cases, the numerical values as
stated for the parameter can take on negative values. In this case,
the example value of range stated as "less than 10" can assume
negative values, e.g. -1, -2, -3, -10, -20, -30, etc.
[0018] The fuser or fixing member can include a substrate having
one or more functional intermediate layers formed thereon. The
substrate described herein includes a belt. The one or more
intermediate layers include cushioning layers and release layers.
Such fixing member can be used as an oil-less fusing member for
high speed, high quality electrophotographic printing to ensure and
maintain a good toner release from the fused toner image on an
image supporting material (e.g., a paper sheet), and further assist
paper stripping.
[0019] In various embodiments, the fixing member can include, for
example, a substrate, with one or more functional layers formed
thereon. The substrate can be formed in various shapes, such as a
belt, or a film, using suitable materials that are non-conductive
or conductive depending on a specific configuration, for example,
as shown in FIG. 1.
[0020] In FIG. 1, the exemplary fixing member 200 can include a
belt substrate 210 with one or more functional intermediate layers,
e.g., 220 and an outer surface layer 230 formed thereon. The outer
surface layer 230 is also referred to as a release layer. The belt
substrate 210 is described further and is made of a polyimide
polymer and a phosphate ester.
Intermediate Layer
[0021] Examples of materials used for the functional intermediate
layer 220 (also referred to as cushioning layer or intermediate
layer) include fluorosilicones, silicone rubbers such as room
temperature vulcanization (RTV) silicone rubbers, high temperature
vulcanization (HTV) silicone rubbers, and low temperature
vulcanization (LTV) silicone rubbers. These rubbers are known and
readily available commercially, such as SILASTIC.RTM. 735 black RTV
and SILASTIC.RTM. 732 RTV, both from Dow Corning; 106 RTV Silicone
Rubber and 90 RTV Silicone Rubber, both from General Electric; and
JCR6115CLEAR HTV and SE4705U HTV silicone rubbers from Dow Corning
Toray Silicones. Other suitable silicone materials include
siloxanes (such as polydimethylsiloxanes); fluorosilicones such as
Silicone Rubber 552, available from Sampson Coatings, Richmond,
Va.; liquid silicone rubbers such as vinyl crosslinked heat curable
rubbers or silanol room temperature crosslinked materials; and the
like. Another specific example is Dow Corning Sylgard 182.
Commercially available LSR rubbers include Dow Corning Q3-6395,
Q3-6396, SILASTIC.RTM. 590 LSR, SILASTIC.RTM. 591 LSR,
SILASTIC.RTM. 595 LSR, SILASTIC.RTM. 596 LSR, and SILASTIC.RTM. 598
LSR from Dow Corning. The functional intermediate layers provide
elasticity and can be mixed with inorganic particles, for example
SiC or Al.sub.2O.sub.3, as required.
[0022] Other examples of the materials suitable for use as
functional intermediate layer 220 also include fluoroelastomers.
Fluoroelastomers are from the class of 1) copolymers of two of
vinylidenefluoride, hexafluoropropylene, and tetrafluoroethylene;
2) terpolymers of vinylidenefluoride, hexafluoropropylene, and
tetrafluoroethylene; and 3) tetrapolymers of vinylidenefluoride,
hexafluoropropylene, tetrafluoroethylene, and cure site monomer.
These fluoroelastomers are known commercially under various
designations such as VITON A.RTM., VITON B.RTM., VITON E.RTM.,
VITON E 60C.RTM., VITON E430.RTM., VITON 910.RTM., VITON GH.RTM.;
VITON GF.RTM.; and VITON ETP.RTM.. The VITON.RTM. designation is a
Trademark of E.I. DuPont de Nemours, Inc. The cure site monomer can
be
4-bromoperfluorobutene-1,1,1-dihydro-4-bromoperfluorobutene-1,3-bromoperf-
luoropropene-1, 1,1-dihydro-3-bromoperfluoropropene-1, or any other
suitable, known cure site monomer, such as those commercially
available from DuPont. Other commercially available fluoropolymers
include FLUOREL 2170.RTM., FLUOREL 2174.RTM., FLUOREL 2176.RTM.,
FLUOREL 2177.RTM. and FLUOREL LVS 76.RTM., FLUOREL.RTM. being a
registered trademark of 3M Company. Additional commercially
available materials include AFLAS.TM. a
poly(propylene-tetrafluoroethylene) and FLUOREL II.RTM. (LII900) a
poly(propylene-tetrafluoroethylenevinylidenefluoride) both also
available from 3M Company, as well as the Tecnoflons identified as
FOR-60KIR.RTM., FOR-LHF.RTM., NM.RTM. FOR-THF.RTM., FOR-TFS.RTM.,
TH.RTM., NH.RTM., P757.RTM., TNS.RTM., T439.RTM., PL958.RTM.,
BR9151.RTM. and TN505 , available from Ausimont.
[0023] Examples of three known fluoroelastomers are (1) a class of
copolymers of two of vinylidenefluoride, hexafluoropropylene, and
tetrafluoroethylene, such as those known commercially as VITON
A.RTM.; (2) a class of terpolymers of vinylidenefluoride,
hexafluoropropylene, and tetrafluoroethylene known commercially as
VITON B.RTM.; and (3) a class of tetrapolymers of
vinylidenefluoride, hexafluoropropylene, tetrafluoroethylene, and
cure site monomer known commercially as VITON GH.RTM. or VITON
GF.RTM..
[0024] The fluoroelastomers VITON GH.RTM. and VITON GF.RTM. have
relatively low amounts of vinylidenefluoride. The VITON GF.RTM. and
VITON GH.RTM. have about 35 weight percent of vinylidenefluoride,
about 34 weight percent of hexafluoropropylene, and about 29 weight
percent of tetrafluoroethylene, with about 2 weight percent cure
site monomer.
[0025] The thickness of the functional intermediate 220 layer is
from about 30 microns to about 1,000 microns, or from about 100
microns to about 800 microns, or from about 150 to about 500
microns.
Release Layer
[0026] An exemplary embodiment of a release layer includes
fluoropolymer particles. Fluoropolymer particles suitable for use
in the formulation described herein include fluorine-containing
polymers. These polymers include fluoropolymers comprising a
monomeric repeat unit that is selected from the group consisting of
vinylidene fluoride, hexafluoropropylene, tetrafluoroethylene,
perfluoroalkylvinylether, and mixtures thereof. The fluoropolymers
may include linear or branched polymers, and cross-linked
fluoroelastomers. Examples of fluoropolymer include
polytetrafluoroethylene (PTFE); perfluoroalkoxy polymer resin
(PFA); copolymer of tetrafluoroethylene (TFE) and
hexafluoropropylene (HFP); copolymers of hexafluoropropylene (HFP)
and vinylidene fluoride (VDF or VF2); terpolymers of
tetrafluoroethylene (TFE), vinylidene fluoride (VDF), and
hexafluoropropylene (HFP); and tetrapolymers of tetrafluoroethylene
(TFE), vinylidene fluoride (VF2), and hexafluoropropylene (HFP),
and mixtures thereof. The fluoropolymer particles provide chemical
and thermal stability and have a low surface energy. The
fluoropolymer particles have a melting temperature of from about
255.degree. C. to about 360.degree. C. or from about 280.degree. C.
to about 330.degree. C. These particles are melted to form the
release layer 230.
[0027] For the fuser member 200, the outer surface layer or release
layer 230 can be from about 10 microns to about 100 microns, or
from about 20 microns to about 80 microns, or from about 40 microns
to about 60 microns.
Adhesive Layer
[0028] Optionally, any known and available suitable adhesive layer
may be positioned between the release layer 230, the functional
intermediate layer 220 and the substrate 210. Examples of suitable
adhesives include silanes such as amino silanes (such as, for
example, HV Primer 10 from Dow Corning), titanates, zirconates,
aluminates, and the like, and mixtures thereof. In an embodiment,
an adhesive in from about 0.001 percent to about 10 percent
solution can be wiped on the substrate. The adhesive layer can be
coated on the substrate, or on the outer layer, to a thickness of
from about 2 nanometers to about 2,000 nanometers, or from about 2
nanometers to about 500 nanometers. The adhesive can be coated by
any suitable known technique, including spray coating or
wiping.
Substrate Layer
[0029] The polyimide composition suitable for use as a substrate
layer 210 of FIG. 1 is described below. The polyimide composition
includes an internal release agent that self releases from a metal
substrate such as stainless steel. Most references report applying
an external release layer on the metal substrate before coating the
polyimide layer, and then releasing it. The composition is cost
effective since only one coating layer is needed.
[0030] The composition comprises a polyamic acid and an internal
release agent comprising a phosphate ester. Less than one weight
percent of the internal release agent is needed to fully release
the polyimide layer from the stainless steel. In embodiments, the
internal release agent is present in an amount of from less than
about 0.5 weight percent. In embodiments, the internal release
agent is present in an amount of from less than about 0.1 weight
percent. The polyimide and the phosphate ester of the substrate
composition are present in a weight ratio of about 99.9/0.1 to
about 95/5.
[0031] The composition comprises a polyamic acid and an internal
release agent comprising a phosphate ester. Less than 4 weight
percent of the internal release agent is needed to fully release
the polyimide layer from the stainless steel. In embodiments, the
internal release agent is present in an amount of from less than
about 1 weight percent. In embodiments, the internal release agent
is present in an amount of from less than about 0.1 weight
percent.
[0032] The disclosed polyamic acid includes one of a polyamic acid
of pyromellitic dianhydride/4,4'-oxydianiline, a polyamic acid of
pyromellitic dianhydride/phenylenediamine, a polyamic acid of
biphenyl tetracarboxylic dianhydride/4,4'-oxydianiline, a polyamic
acid of biphenyl tetracarboxylic dianhydride/phenylenediamine, a
polyamic acid of benzophenone tetracarboxylic
dianhydride/4,4'-oxydianiline, a polyamic acid of benzophenone
tetracarboxylic dianhydride/4,4'-oxydianiline/phenylenediamine, and
the like and mixtures thereof.
[0033] Commercial examples of polyamic acid of pyromellitic
dianhydride/4,4-oxydianiline include PYRE-ML RC5019 (about 15-16
weight percent in N-methyl-2-pyrrolidone, NMP), RC5057 (about
14.5-15.5 weight percent in NMP/aromatic hydrocarbon=80/20), and
RC5083 (about 18-19 weight percent in NMP/DMAc=15/85), all from
Industrial Summit technology Corp., Parlin, N.J.; DURIMIDE.RTM.
100, commercially available from FUJIFILM Electronic Materials
U.S.A., Inc.
[0034] Commercial examples of polyamic acid of biphenyl
tetracarboxylic dianhydride/4,4'-oxydianiline include U-VARNISH A,
and S (about 20 weight in NMP), both from UBE America Inc., New
York, N.Y.
[0035] Commercial examples of polyamic acid of biphenyl
tetracarboxylic dianhydride/phenylenediamine include PI-2610 (about
10.5 weight in NMP), and PI-2611 (about 13.5 weight in NMP), both
from HD MicroSystems, Parlin, N.J.
[0036] Commercial examples of polyamic acid of benzophenone
tetracarboxylic dianhydride/4,4'-oxydianiline include RP46, and
RP50 (about 18 weight percent in NMP), both from Unitech Corp.,
Hampton, Va.
[0037] Commercial examples of polyamic acid of benzophenone
tetracarboxylic dianhydride/4,4'-oxydianiline/phenylenediamine
include PI-2525 (about 25 weight percent in NMP), PI-2574 (about 25
weight percent in NMP), PI-2555 (about 19 weight percent in
NMP/aromatic hydrocarbon=80/20), and PI-2556 (about 15 weight
percent in NMP/aromatic hydrocarbon/propylene glycol methyl
ether=70/15/15), all from HD MicroSystems, Parlin, N.J.
[0038] Various amounts of polyamic acid can be selected for the
substrate, such as for example, from about 90 to about 99.9 weight
percent, from 95 to about 99.8 weight percent, or from 97 to about
99.5 weight percent.
[0039] Other polyamic acid or ester of polyamic acid examples that
can be included in the intermediate transfer member are from the
reaction of a dianhydride and a diamine. Suitable dianhydrides
include aromatic dianhydrides and aromatic tetracarboxylic acid
dianhydrides such as, for example,
9,9-bis(trifluoromethyl)xanthene-2,3,6,7-tetracarboxylic acid
dianhydride, 2,2-bis(3,4-dicarboxyphenyl)hexafluoropropane
dianhydride, 2,2-bis((3,4-dicarboxyphenoxy)
phenyl)hexafluoropropane dianhydride,
4,4'-bis(3,4-dicarboxy-2,5,6-trifluorophenoxy)octafluorobiphenyl
dianhydride, 3,3',4,4'-tetracarboxybiphenyl dianhydride,
3,3',4,4'-tetracarboxybenzophenone dianhydride,
di-(4-(3,4-dicarboxyphenoxy)phenyl)ether dianhydride,
di-(4-(3,4-dicarboxyphenoxy)phenyl) sulfide dianhydride,
di-(3,4-dicarboxyphenyl)methane dianhydride,
di-(3,4-dicarboxyphenyl)ether dianhydride,
1,2,4,5-tetracarboxybenzene dianhydride, 1,2,4-tricarboxybenzene
dianhydride, butanetetracarboxylic dianhydride,
cyclopentanetetracarboxylic dianhydride, pyromellitic dianhydride,
1,2,3,4-benzenetetracarboxylic dianhydride,
2,3,6,7-naphthalenetetracarboxylic dianhydride,
1,4,5,8-naphthalenetetracarboxylic dianhydride,
1,2,5,6-naphthalenetetracarboxylic dianhydride,
3,4,9,10-perylenetetracarboxylic dianhydride, 2,3,6,7-anthracene
tetracarboxylic dianhydride, 1,2,7,8-phenanthrenetetracarboxylic
dianhydride, 3,3',4,4'-biphenyltetracarboxylic dianhydride,
2,2',3,3'-biphenyltetracarboxylic dianhydride,
3,3',4-4'-benzophenonetetracarboxylic dianhydride,
2,2',3,3'-benzophenonetetracarboxylic dianhydride,
2,2-bis(3,4-dicarboxyphenyl)propane dianhydride,
2,2-bis(2,3-dicarboxyphenyl)propane dianhydride,
bis(3,4-dicarboxyphenyl)ether dianhydride,
bis(2,3-dicarboxyphenyl)ether dianhydride,
bis(3,4-dicarboxyphenyl)sulfone dianhydride,
bis(2,3-dicarboxyphenyl)sulfone
2,2-bis(3,4-dicarboxyphenyl)-1,1,1,3,3,3-hexafluoropropane
dianhydride,
2,2-bis(3,4-dicarboxyphenyl)-1,1,1,3,3,3-hexachloropropane
dianhydride, 1,1-bis(2,3-dicarboxyphenyl)ethane dianhydride,
1,1-bis(3,4-dicarboxyphenyl)ethane dianhydride,
bis(2,3-dicarboxyphenyl)methane dianhydride,
bis(3,4-dicarboxyphenyl)methane dianhydride,
4,4'-(p-phenylenedioxy) diphthalic dianhydride,
4,4'-(m-phenylenedioxy)diphthalic dianhydride,
4,4'-diphenylsulfidedioxybis(4-phthalic acid)dianhydride,
4,4'-diphenylsulfonedioxybis(4-phthalic acid)dianhydride,
methylenebis(4-phenyleneoxy-4-phthalic acid)dianhydride,
ethylidenebis(4-phenyleneoxy-4-phthalic acid)dianhydride,
isopropylidenebis-(4-phenyleneoxy-4-phthalic acid)dianhydride,
hexafluoroisopropylidenebis(4-phenyleneoxy-4-phthalic
acid)dianhydride, and the like. Exemplary diamines suitable for use
in the preparation of the polyamic acid include
4,4'-bis-(m-aminophenoxy)-biphenyl,
4,4'-bis-(m-aminophenoxy)-diphenyl sulfide,
4,4'-bis-(m-aminophenoxy)-diphenyl sulfone,
4,4'-bis-(p-aminophenoxy)-benzophenone,
4,4'-bis-(p-aminophenoxy)-diphenyl sulfide,
4,4'-bis-(p-aminophenoxy)-diphenyl sulfone,
4,4'-diamino-azobenzene, 4,4'-diaminobiphenyl,
4,4'-diaminodiphenylsulfone, 4,4'-diamino-p-terphenyl,
1,3-bis-(gamma-aminopropyl)-tetramethyl-disiloxane,
1,6-diaminohexane, 4,4'-diaminodiphenylmethane,
3,3'-diaminodiphenylmethane, 1,3-diaminobenzene,
4,4'-diaminodiphenyl ether, 2,4'-diaminodiphenylether,
3,3'-diaminodiphenylether, 3,4'-diaminodiphenylether,
1,4-diaminobenzene,
4,4'-diamino-2,2',3,3',5,5',6,6'-octafluoro-biphenyl,
4,4'-diamino-2,2',3,3',5,5',6,6'-octafluorodiphenyl ether,
bis[4-(3-aminophenoxy)-phenyl] sulfide,
bis[4-(3-aminophenoxy)phenyl] sulfone,
bis[4-(3-aminophenoxy)phenyl] ketone,
4,4'-bis(3-aminophenoxy)biphenyl,
2,2-bis[4-(3-aminophenoxy)phenyl]-propane,
2,2-bis[4-(3-aminophenoxy)phenyl]-1,1,1,3,3,3-hexafluoropropane,
4,4'-diaminodiphenyl sulfide, 4,4'-diaminodiphenyl ether,
4,4'-diaminodiphenyl sulfone, 4,4'-diaminodiphenylmethane,
1,1-di(p-aminophenyl)ethane, 2,2-di(p-aminophenyl)propane, and
2,2-di(p-aminophenyl)-1,1,1,3,3,3-hexafluoropropane, and the like
and mixtures thereof.
[0040] The dianhydrides and diamines are, for example, selected in
a weight ratio of dianhydride to diamine of from about 20:80 to
about 80:20, and more specifically, in an about 50:50 weight ratio.
The above aromatic dianhydride like aromatic tetracarboxylic acid
dianhydrides and diamines like aromatic diamines are used singly or
as a mixture, respectively.
[0041] Examples of phosphate esters selected as an internal release
agent with a polyamic acid, such as a polyamic acid of pyromellitic
dianhydride/4,4-oxydianiline, include a number of known phosphate
esters, and more specifically, where the phosphate ester is a
phosphate ester of alkyl alcohol alkoxylate such as alkyl alcohol
ethoxylate, alkyl phenol alkoxylate such as alkyl phenol
ethoxylate, alkyl polyethoxyethanol such as alkyl
polyalkoxyethanol, alkylphenoxy polyalkoxyethanol such as
alkylphenoxy polyethoxyethanol, mixtures thereof, and corresponding
alkoxy esters wherein alkyl and alkoxy contain, for example, from 1
to about 36 carbon atoms, from 1 to about 18 carbon atoms, from 1
to about 12 carbon atoms, from 1 to about 6 carbon atoms,
optionally mixtures thereof, and the like.
[0042] Examples of phosphate esters of alkyl alcohol ethoxylate
include POLYSTEP.RTM. P-11, P-12 and P-13 (tridecyl alcohol
ethoxylate phosphate, available from STEPAN Company, Northfield,
Ill.) with an average mole number of ethoxy (EO) of about 3, 6 and
12, respectively. Examples of phosphate esters of alkyl phenol
ethoxylates include POLYSTEP.RTM. P-31, P-32, P-33, P-34 and P-35
(nonylphenol ethoxylate phosphate, available from STEPAN Company,
Northfield, Ill.) with an average mole number of ethoxy (EO) of
about 4, 6, 8, 10 and 12, respectively. Examples of phosphate
esters of alkyl polyethoxyethanol include STEPFAC.TM. 8180, 8181
and 8182 (polyethylene glycol monotridecyl ether phosphate,
available from STEPAN Company, Northfield, IL) with an average mole
number of ethoxy (EO) of about 3, 6 and 12, respectively. Examples
of phosphate esters of alkylphenoxy polyethoxyethanol include
STEPFAC.TM. 8170, 8171, 8172, 8173, 8175 (nonylphenol ethoxylate
phosphate, available from STEPAN Company, Northfield, Ill.) with an
average mole number of ethoxy (EO) of about 10, 6, 4, 8 and 12,
respectively, and TSP-PE (tristyrylphenol ethoxylate phosphate,
available from STEPAN Company, Northfield, Ill.) with an average
mole number of ethoxy (EO) of about 16.
[0043] Various amounts of phosphate ester can be selected for the
substrate, such as for example, from about 0.1 to about 10 weight
percent, from 0.2 to about 5 weight percent, or from 0.5 to about 3
weight percent.
[0044] The polyimide substrate composition can optionally contain a
polysiloxane copolymer to enhance or smooth the coating. The
concentration of the polysiloxane copolymer is less than about 1
weight percent or less than about 0.2 weight percent. The optional
polysiloxane copolymer includes a polyester modified
polydimethylsiloxane, commercially available from BYK Chemical with
the trade name of BYK.RTM. 310 (about 25 weight percent in xylene)
and 370 (about 25 weight percent in
xylene/alkylbenzenes/cyclohexanone/monophenylglycol=75/11/7/7); a
polyether modified polydimethylsiloxane, commercially available
from BYK Chemical with the trade name of BYK.RTM. 330 (about 51
weight percent in methoxypropylacetate) and 344 (about 52.3 weight
percent in xylene/isobutanol=80/20), BYK.RTM.-SILCLEAN 3710 and
3720 (about 25 weight percent in methoxypropanol); a polyacrylate
modified polydimethylsiloxane, commercially available from BYK
Chemical with the trade name of BYK.RTM.-SILCLEAN 3700 (about 25
weight percent in methoxypropylacetate); or a polyester polyether
modified polydimethylsiloxane, commercially available from BYK
Chemical with the trade name of BYK.RTM. 375 (about 25 weight
percent in Di-propylene glycol monomethyl ether). The polyimide,
the phosphate ester and the polysiloxane polymer of the substrate
are present in a weight ratio of about 99.9/0.09/0.01 to about
95/4/1.
[0045] The polyimide substrate composition includes a solvent.
Examples of the solvent selected to form the composition include
toluene, hexane, cycloheaxne, heptane, tetrahydrofuran, methyl
ethyl ketone, methyl isobutyl ketone, N,N'-dimethylformamide,
N,N'-dimethylacetamide, N-methyl pyrrolidone (NMP), methylene
chloride and the like and mixtures thereof where the solvent is
selected, for example, in an amount of from about 70 weight percent
to about 95 weight percent, and from 80 weight percent to about 90
weight percent based on the amounts in the coating mixture.
[0046] The polyimide composition is flow coated on the outer
surface of a welded stainless steel belt at the desired product
circumference. The seam thickness and profile can be minimized, and
the surface finish and roughness of the substrate belt can be
specified, for example, a rough lathed or honed belt is better for
the polyimide layer release. Such a configuration easily allows the
production of belts of various lengths and widths. Using a rotating
mandrel limits the width and length of the belts able to be
produced as each belt requires a separate mandrel.
[0047] In one embodiment, the coating belt substrate is a rough
lathed belt substrate with a R.sub.a of from about 0.05 micron to
about 0.2 micron, or from about 0.1 to about 0.15 micron; and a
R.sub.max of from 0.75 micron to about 1 micron, or from about 0.8
micron to about 0.9 micron. The back of the polyimide fuser
substrate flow coated from this substrate is similarly rough
lathed, thus recognizable.
[0048] In another embodiment, the coating belt substrate is a honed
belt substrate with a R.sub.a of from about 0.15 micron to about
0.35 micron, or from about 0.2 to about 0.3 micron; and a R.sub.max
of from 2 micron to about 4 micron, or from about 2.5 micron to
about 3.5 micron. The back of the polyimide fuser substrate flow
coated from this substrate is similarly honed, thus
recognizable.
[0049] The polyimide layer thickness can be achieved by single pass
or multi pass coating. For single pass, the polyimide layer is
coated, and pre-cured at a temperature between about 125.degree. C.
and about 190.degree. C. for a time of about 30 to about 90
minutes, and then fully cured at a temperature between about
250.degree. C. and about 370.degree. C. for a time of about 30 to
about 90 minutes. For multi-pass, such as dual pass, the bottom
polyimide layer is coated on a substrate and pre-cured between
about 125.degree. C. and about 190.degree. C. for a time of about
30 to about 90 minutes, and the top polyimide layer is subsequently
coated and pre-cured between about 125.degree. C. and about
190.degree. C. for a time of about 30 to about 90 minutes, and
finally the dual layer is fully cured at a temperature between
about 250.degree. C. and about 370.degree. C. for a time of about
30 to about 90 minutes. In an embodiment a stainless steel belt is
used as the substrate. The substrate is rotated at a speed of from
about 20 rpm to about 100 rpm during the thermal curing of the
coating. The polyimide layer stays on the coating substrate all the
time during the curing process.
[0050] In the other embodiment, for single pass, the polyimide
layer is coated, and pre-cured at a temperature between about
125.degree. C. and about 190.degree. C. for a time of about 30 to
about 90 minutes. For multi-pass, such as dual pass, the bottom
polyimide layer is coated on a substrate and pre-cured between
about 125.degree. C. and about 190.degree. C. for a time of about
30 to about 90 minutes, and the top polyimide layer is subsequently
coated and pre-cured between about 125.degree. C. and about
190.degree. C. for a time of about 30 to about 90 minutes. In an
embodiment a stainless steel belt is used as the substrate. The
substrate is rotated at a speed of from about 20 rpm to about 100
rpm during the thermal curing of the coating.
[0051] The pre-cured polyimide belt self releases from the
stainless steel belt, and then is further completely cured at about
250.degree. C. to about 370.degree. C. for a time of about 30 to
about 90 minutes under tension in the configuration shown in FIG.
2. This final curing is at a tension of from about 1 kilogram to
about 10 kilograms. As shown in FIG. 2, the pre-cured belt 210 is
tensioned between two rollers 250 while rotating the direction of
arrow 20. The final curing produces a belt that exhibits a modulus
suitable for use as a fuser member.
[0052] Additives and additional conductive or non-conductive
fillers may be present in the above-described composition or the
various layers of the fuser belt. In various embodiments, other
filler materials or additives including, for example, inorganic
particles, can be used for the coating composition and the
subsequently formed surface layer. Conductive fillers used herein
include carbon blacks such as carbon black, graphite, fullerene,
acetylene black, fluorinated carbon black, and the like; carbon
nanotubes, metal oxides and doped metal oxides, such as tin oxide,
antimony dioxide, antimony-doped tin oxide, titanium dioxide,
indium oxide, zinc oxide, indium oxide, indium-doped tin trioxide,
and the like; and mixtures thereof. Certain polymers such as
polyanilines, polythiophenes, polyacetylene, poly(p-phenylene
vinylene), poly(p-phenylene sulfide), pyrroles, polyindole,
polypyrene, polycarbazole, polyazulene, polyazepine,
poly(fluorine), polynaphthalene, salts of organic sulfonic acid,
esters of phosphoric acid, esters of fatty acids, ammonium or
phosphonium salts and mixture thereof can be used as conductive
fillers. In various embodiments, other additives known to one of
ordinary skill in the art can also be included to form the
disclosed composite materials.
[0053] Specific embodiments will now be described in detail. These
examples are intended to be illustrative, and not limited to the
materials, conditions, or process parameters set forth in these
embodiments. All parts are percentages by solid weight unless
otherwise indicated.
EXAMPLES
[0054] Experimentally, a composition (Example 1) of polyamic acid
of pyromellitic dianhydride/4,4-oxydianiline/phosphate ester of
alkyl phenol ethoxylate/polyester-co-polysiloxane in a weight ratio
of 99.3/0.5/0.2 was prepared in NMP, at about 13 weight percent
solid, where the polyamic acid of pyromellitic
dianhydride/4,4-oxydianiline was commercially available from
Industrial Summit Technology Corp., Parlin, N.J. with the trade
name of PYRE-ML RC5019 (about 15-16 weight percent in
N-methyl-2-pyrrolidone, NMP). The phosphate ester of alkyl phenol
ethoxylate was commercially available from Stepan Company,
Northfield, Ill. with the trade name of POLYSTEP.RTM. P-34
(nonylphenol ethoxylate phosphate with an average mole number of
ethoxy of about 10). The polyester-co-polysiloxane was commercially
available from BYK Chemical with the trade name of BYK.RTM. 310
(about 25 weight percent in xylene). The clear coating solution was
flow coated on a stainless steel belt, and subsequently cured at
125.degree. C. for 30 minutes and then at 190.degree. C. for 30
minutes. A 40 .mu.m thick polyimide bottom layer was formed on the
stainless steel substrate belt. Subsequently, a second pass
polyimide layer was coated on top of the existing polyimide layer,
and cured at 125.degree. C. for 30 minutes and then at 190.degree.
C. for 30 minutes. The dual pass coating produced an 80 micron
polyimide belt.
[0055] The pre-cured polyimide belt self released from the
stainless steel substrate belt. The pre-cured polyimide belt was
further cured at 320.degree. C. for an additional hour under
tension of 1 kilogram. A seamless polyimide belt was obtained with
a smooth surface and a thickness of about 80 mirons.
[0056] The other composition (Example 2) of polyamic acid of
biphenyl tetracarboxylic dianhydride/4,4'-oxydianiline/phosphate
ester of alkylphenoxy polyethoxyethanol in a weight ratio of
99.1/0.9 was prepared in NMP, at about 18 weight percent solid,
where the polyamic acid of biphenyl tetracarboxylic
dianhydride/4,4'-oxydianiline was commercially available from UBE
America Inc., New York, N.Y. with the trade name of U-VARNISH S
(about 20 weight in NMP). The phosphate ester of alkylphenoxy
polyethoxyethanol was commercially available from Stepan Company,
Northfield, Ill. with the trade name of STEPFAC.TM. 8171
(nonylphenol ethoxylate phosphate with an average mole number of
ethoxy (EO) of about 6). The clear coating solution was coated on a
stainless steel belt, and subsequently cured at 125.degree. C. for
30 minutes, 190.degree. C. for 30 minutes and 320.degree. C. for 60
minutes. The resulting polyimide film self released from the
substrate, and an 80 .mu.m smooth polyimide film was obtained.
[0057] It will be appreciated that variants of the above-disclosed
and other features and functions or alternatives thereof, may be
combined into other different systems or applications. Various
presently unforeseen or unanticipated alternatives, modifications,
variations, or improvements therein may be subsequently made by
those skilled the in the art which are also encompassed by the
following claims.
* * * * *