FIELD OF THE INVENTION
[0001] This invention relates in general to imaging elements and in particular to thermally
processable imaging elements. More specifically, this invention relates to imaging
elements comprising a thermographic or photothermographic layer, an overcoat layer
and an adhesive interlayer interposed between the overcoat layer and the thermographic
or photothermographic layer.
BACKGROUND OF THE INVENTION
[0002] Thermally processable imaging elements, including films and papers, for producing
images by thermal processing are well known. These elements include photothermographic
elements in which an image is formed by imagewise exposure of the element to light
followed by development by uniformly heating the element. These elements also include
thermographic elements in which an image is formed by imagewise heating the element.
Such elements are described in, for example,
Research Disclosure, June 1978, Item No. 17029 and U.S. Patents 3,080,254, 3,457,075 and 3,933,508.
[0003] An important feature of the aforesaid thermally processable imaging elements is a
protective overcoat layer. To be fully acceptable, a protective overcoat layer for
such imaging elements should: (a) provide resistance to deformation of the layers
of the element during thermal processing, (b) prevent or reduce loss of volatile components
in the element during thermal processing, (c) reduce or prevent transfer of essential
imaging components from one or more of the layers of the element into the overcoat
layer during manufacture of the element or during storage of the element prior to
imaging and thermal processing, (d) enable satisfactory adhesion of the overcoat to
a contiguous layer of the element, and (e) be free from cracking and undesired marking,
such as abrasion marking, during manufacture, storage, and processing of the element.
[0004] A particularly preferred overcoat for thermally processable imaging elements is an
overcoat comprising poly(silicic acid) as described in U.S. Patent 4,741,992, issued
May 3, 1988. Advantageously, water-soluble hydroxyl-containing monomers or polymers
are incorporated in the overcoat layer together with the poly(silicic acid). The combination
of poly(silicic acid) and a water-soluble hydroxyl-containing monomer or polymer that
is compatible with the poly(silicic acid) is also useful in a backing layer on the
side of the support opposite to the imaging layer as described in U.S. Patent 4,828,971,
issued May 9, 1989.
[0005] One of the most difficult problems involved in the manufacture of thermally processable
imaging elements is that the protective overcoat layer typically does not exhibit
adequate adhesion to the imaging layer. The problem of achieving adequate adhesion
is particularly aggravated by the fact that the imaging layer is typically hydrophobic
while the overcoat layer is typically hydrophilic. One solution to this problem is
that described in U.S. Patent 4,886,739, issued December 12, 1989, in which a polyalkoxysilane
is added to the thermographic or photothermographic imaging composition and is hydrolyzed
in situ to form an Si(OH)₄ moiety which has the ability to crosslink with binders
present in the imaging layer and the overcoat layer. Another solution to the problem
is that described in U.S. Patent 4,942,115, issued July 17, 1990, in which an adhesion-promoting
layer composed of certain adhesion-promoting terpolymers is interposed between the
imaging layer and the overcoat layer.
[0006] The known solutions to the problem of providing adequate overcoat adhesion with thermally
processable elements exhibit certain disadvantages which have hindered their commercial
utilization. For example, while incorporation of a polyalkoxysilane in the imaging
composition brings about a gradual increase in adhesion on aging of the element, the
in situ hydrolysis of the polyalkoxysilane is slow and its rate is limited by the
availability of water in the coated layer. Moreover, the alcohol which is formed as
a by-product of the hydrolysis, for example, the ethyl alcohol that is formed by hydrolysis
of tetraethoxysilane, is unable to escape through the highly impermeable overcoat
layer and tends to migrate into the support. The support is typically a polyester,
most usually poly(ethylene terephthalate), and migration of the alcohol into such
a support causes a highly undesirable width-wise curl which makes the imaging element
very difficult to handle. A serious consequence of such width-wise curl, even though
it may be very slight in extent, is jamming of processing equipment.
[0007] The problem of unwanted curl can be reduced by use of the adhesion-promoting interlayer
of U.S. Patent 4,942,115, but use of this interlayer can result in adverse sensitometric
effects, requires an additional coating step which makes it economically less attractive,
and requires the use of terpolymers which are costly, difficult to handle and environmentally
disadvantageous.
[0008] Unwanted curl can be reduced by use of a barrier layer which is comprised of poly(silicic
acid) and a water-soluble hydroxyl-containing monomer or polymer that is compatible
therewith and which is interposed between the support and the image-forming layer,
as described in U.S. Patent 5,264,334, issued November 23, 1993. However, this method
also requires the use of an additional coating step.
[0009] Unwanted curl can also be reduced by incorporating a pre-hydrolyzed polyalkoxysilane
in the imaging composition as described in U.S. Patent No. 5,294,526, issued March
15, 1994. By utilizing a pre-hydrolyzed polyalkoxysilane, the by-products of hydrolysis,
such as the ethyl alcohol that is formed by hydrolysis of tetraethoxysilane, are not
present in the image-forming layer and thus the problems caused by their migrating
into the support are avoided. However, this method requires very exacting control
of all process parameters.
[0010] It is toward the objective of providing an improved thermally processable imaging
element having an adhesion-promoting-interlayer which overcomes the disadvantages
of the prior art that the present invention is directed.
SUMMARY OF THE INVENTION
[0011] In accordance with this invention, a thermally processable imaging element is comprised
of:
(1) a support;
(2) a thermographic or photothermographic imaging layer;
(3) an overcoat layer overlying the imaging layer; and
(4) an adhesive-interlayer bonding the overcoat layer to the imaging layer; and is
characterized in that the adhesive interlayer comprises at least one of (1) a polymer
having pyrrolidone functionality, (2) a polymer having epoxy functionality and (3)
a polyalkoxysilane.
[0012] An adhesive interlayer comprising a polymer having pyrrolidone functionality or a
polymer having epoxy functionality or a polyalkoxysilane has been found to serve as
an effective adhesion-promoting layer which overcomes the difficult problem of providing
good adhesion between an overcoat which is typically hydrophilic and an imaging layer
which is typically hydrophobic. Moreover, use of such polymers for this purpose not
only provides very effective adhesion but causes no adverse sensitometric effects
and involves the use of low cost, readily available materials which are easily handled
and coated and are environmentally advantageous.
[0013] The overcoat layer utilized in the thermally processable imaging elements of this
invention performs several important functions as hereinabove described. It can be
composed of hydrophilic colloids such as gelatin or poly(vinyl alcohol) but is preferably
composed of poly(silicic acid) and a water-soluble hydroxyl-containing monomer or
polymer as described in U.S. Patent 4,741,992, issued May 3, 1988.
[0014] In addition to the support, the imaging layer, the overcoat layer and the adhesive
interlayer, the thermally processable imaging element of this invention can optionally
include additional layers such as a backing layer. Particularly useful backing layers
are those comprising poly(silicic acid) and a water-soluble hydroxyl-containing monomer
or polymer that is compatible therewith as described in U.S. Patent 4,828,971, issued
May 9, 1989. Thus, the improved thermally processable imaging element of this invention
can contain three different layers each of which is comprised of poly(silicic acid),
namely, (1) an overcoat layer whose purpose is to protect the element as described
in U.S. Patent 4,741,992, (2) a backing layer whose purpose is to improve conveyance,
reduce static electricity and eliminate formation of Newton Rings as described in
U.S. Patent 4,828,971 and (3) a barrier layer whose purpose is to protect the support
against migration from the imaging layer of hydrolysis by-products and thereby prevent
width-wise curl as described in U.S. Patent 5,264,334.
[0015] In a preferred embodiment, the thermally processable imaging elements of this invention
also include an electroconductive layer to provide antistatic protection as described
in United States Patent No. 5,310,640, issued May 10, 1994.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] The thermally processable imaging element of this invention can be a black-and-white
imaging element or a dye-forming imaging element. It can be of widely varying construction
as long as it includes the aforesaid support, imaging layer, overcoat layer and adhesive
interlayer.
[0017] Typical imaging elements within the scope of this invention comprise at least one
imaging layer containing in reactive association in a binder, preferably a binder
comprising hydroxyl groups, (a) photographic silver halide prepared in situ and/or
ex situ, (b) an image-forming combination comprising (i) an organic silver salt oxidizing
agent, preferably a silver salt of a long chain fatty acid, such as silver behenate,
with (ii) a reducing agent for the organic silver salt oxidizing agent, preferably
a phenolic reducing agent, and (c) an optional toning agent. References describing
such imaging elements include, for example, U.S. Patents 3,457,075; 4,459,350; 4,264,725
and 4,741,992 and
Research Disclosure, June 1978, Item No. 17029.
[0018] Polymers having pyrrolidone functionality that are useful in this invention can vary
widely in structure and include homopolymers of N-vinyl-2-pyrrolidone, copolymers
formed by polymerizing two polymerizable monomers one of which provides pyrrolidone
functionality, and interpolymers formed by polymerizing three or more polymerizable
monomers at least one of which provides pyrrolidone functionality. Polymers having
epoxy functionality that are useful in this invention can vary widely in structure
and include homopolymers of epoxy monomers, copolymers formed by polymerizing two
polymerizable monomers one of which provides epoxy functionality and interpolymers
formed by polymerizing three or more polymerizable monomers at least one of which
provides epoxy functionality.
[0019] Polyalkoxysilanes useful in this invention to form the adhesive interlayer include
those represented by the formulae I or II as follows:
I Si(OR₁)₄
II R₂-Si(OR₃)₃
wherein R₁ and R₃ are individually unsubstituted or substituted alkyl containing 1
to 4 carbon atoms, such as methyl, ethyl, propyl and butyl, and R₂ is unsubstituted
or substituted alkyl, such as alkyl containing 1 to 22 carbon atoms, such as methyl,
ethyl, propyl, butyl, and n-octadecyl; or unsubstituted or substituted phenyl.
[0020] Specific examples of useful polyalkoxysilanes for the aforesaid purpose include:
Si(OC₂H₅)₄
Si(OCH₃)₄
CH₃Si(OC₂H₅)₃
CH₃Si(OCH₃)₃
C₆H₅Si(OC₂H₅)₃
C₆H₅Si(OCH₃)₃
NH₂CH₂CH₂CH₂Si(OC₂H₅)₃
NH₂CH₂CH₂CH₂Si(OCH₃)₃

and
CH₃(CH₂)₁₇Si(OC₂H₅)₃.
[0021] Polyalkoxysilanes can also be utilized in the thermally processable imaging elements
of this invention to form overcoat layers, backing layers or barrier layers or as
components of the imaging layer.
[0022] The optimum layer thickness of the imaging layer, the overcoat layer and the adhesive
interlayer depends upon various factors, such as the particular element, processing
conditions, thermal processing means, desired image and the particular components
of the layers. A particularly useful imaging layer thickness is typically within the
range of 1 to 10 microns, preferably 3 to 7 microns. A particularly useful overcoat
layer thickness is also typically within the range of 1 to 10 microns, preferably
1 to 3 microns. A particularly useful adhesive interlayer thickness for the polymers
having pyrrolidone or epoxy functionality is typically within the range of about 0.008
to about 0.05 microns, preferably 0.01 to 0.02 microns. A particularly useful adhesive
interlayer thickness for use of the polyalkoxysilane is typically within the range
of about 0.05 to about 1.0 microns, preferably 0.10 to 0.40 microns.
[0023] Useful overcoat compositions are typically transparent and colorless. If the overcoat
is not transparent and colorless, then it is necessary, if the element is a photothermographic
element, that it be at least transparent to the wavelength of radiation employed to
provide and view the image. The overcoat does not significantly adversely affect the
imaging properties of the element, such as the sensitometric properties in the case
of a photothermographic element, such as minimum density, maximum density, or photographic
speed.
[0024] The overcoat composition preferably comprises 50 to 90% by weight of the overcoat
of poly(silicic acid) and comprises a water-soluble hydroxyl-containing polymer or
monomer that is compatible with the poly(silicic acid). Such an overcoat composition
is described in, for example, U.S. Patent 4,741,992. Examples of water soluble hydroxyl-containing
polymers are acrylamide polymers, water-soluble cellulose derivatives, hydroxy ethyl
cellulose, water-soluble cellulose acetate, and poly(vinyl alcohol). Partially hydrolyzed
poly(vinyl alcohols) are preferred.
[0025] Thermally processable imaging elements as described can contain multiple polymer-containing
layers, such as multiple overcoat layers. For example, the thermally processable imaging
element can contain a first overcoat layer comprising a polymer other than poly(silicic
acid), such as a cellulose derivative, and a second overcoat layer comprising poly(silicic
acid) and poly(vinyl alcohol).
[0026] A preferred overcoat comprises 50 to 90% by weight of poly(silicic acid) represented
by the formula:

wherein x is an integer within the range of at least 3 to about 600 and wherein the
overcoat also comprises 10 to 50% poly(vinyl alcohol).
[0027] The photothermographic element comprises a photosensitive component that consists
essentially of photographic silver halide. In the photothermographic material it is
believed that the latent image silver from the silver halide acts as a catalyst for
the described image-forming combination upon processing. A preferred concentration
of photographic silver halide is within the range of 0.01 to 10 moles of photographic
silver halide per mole of silver behenate in the photothermographic material. Other
photosensitive silver salts are useful in combination with the photographic silver
halide if desired. Preferred photographic silver halides are silver chloride, silver
bromide, silver bromochloride, silver bromoiodide, silver chlorobromoiodide, and mixtures
of these silver halides. Very fine grain photographic silver halide is especially
useful. The photographic silver halide can be prepared by any of the known procedures
in the photographic art. Such procedures for forming photographic silver halides and
forms of photographic silver halides are described in, for example,
Research Disclosure, December 1978, Item No. 17029 and
Research Disclosure, June 1978, Item No. 17643. Tabular grain photosensitive silver halide is also useful,
as described in, for example, U.S. Patent No. 4,435,499. The photographic silver halide
can be unwashed or washed, chemically sensitized, protected against the formation
of fog, and stabilized against the loss of sensitivity during keeping as described
in the above Research Disclosure publications. The silver halides can be prepared
in situ as described in, for example, U.S. Patent No. 4,457,075, or prepared ex situ
by methods known in the photographic art.
[0028] The photothermographic element typically comprises an oxidation-reduction image forming
combination that contains an organic silver salt oxidizing agent, preferably a silver
salt of a long chain fatty acid. Such organic silver salts are resistant to darkening
upon illumination. Preferred organic silver salt oxidizing agents are silver salts
of long chain fatty acids containing 10 to 30 carbon atoms. Examples of useful organic
silver salt oxidizing agents are silver behenate, silver stearate, silver oleate,
silver laurate, silver hydroxystearate, silver caprate, silver myristate, and silver
palmitate. Combinations of organic silver salt oxidizing agents are also useful. Examples
of useful organic silver salt oxidizing agents that are not organic silver salts of
fatty acids are silver benzoate and silver benzotriazole.
[0029] The optimum concentration of organic silver salt oxidizing agent in the photothermographic
element will vary depending upon the desired image, particular organic silver salt
oxidizing agent, particular reducing agent and particular photothermographic element.
A preferred concentration of organic silver salt oxidizing agent is within the range
of 0.1 to 100 moles of organic silver salt oxidizing agent per mole of silver in the
element. When combinations of organic silver salt oxidizing agents are present, the
total concentration of organic silver salt oxidizing agents is preferably within the
described concentration range.
[0030] A variety of reducing agents are useful in the photothermographic element. Examples
of useful reducing agents in the image-forming combination include substituted phenols
and naphthols, such as bis-beta-naphthols; polyhydroxybenzenes, such as hydroquinones,
pyrogallols and catechols; aminophenols, such as 2,4-diaminophenols and methylaminophenols;
ascorbic acid reducing agents, such as ascorbic acid, ascorbic acid ketals and other
ascorbic acid derivatives; hydroxylamine reducing agents; 3-pyrazolidone reducing
agents, such as 1-phenyl-3-pyrazolidone and 4-methyl-4-hydroxymethyl-1-phenyl-3-pyrazolidone;
and sulfonamidophenols and other organic reducing agents known to be useful in photothermographic
elements, such as described in U.S. Patent 3,933,508, U.S. Patent 3,801,321 and
Research Disclosure, June 1978, Item No. 17029. Combinations of organic reducing agents are also useful
in the photothermographic element.
[0031] Preferred organic reducing agents in the photothermographic element are sulfonamidophenol
reducing agents, such as described in U.S. Patent 3,801,381. Examples of useful sulfonamidophenol
reducing agents are 2,6-dichloro-4-benzenesulfonamidophenol; benzenesulfonamidophenol;
and 2,6-dibromo-4-benzenesulfonamidophenol, and combinations thereof.
[0032] An optimum concentration of organic reducing agent in the photothermographic element
varies depending upon such factors as the particular photothermographic element, desired
image, processing conditions, the particular organic silver salt oxidizing agent,
and the particular polyalkoxysilane.
[0033] The photothermographic element preferably comprises a toning agent, also known as
an activator-toner or toner-accelerator. Combinations of toning agents are also useful
in the photothermographic element. Examples of useful toning agents and toning agent
combinations are described in, for example,
Research Disclosure, June 1978, Item No. 17029 and U.S. Patent No. 4,123,282. Examples of useful toning
agents include, for example, phthalimide, N-hydroxyphthalimide, N-potassium-phthalimide,
succinimide, N-hydroxy-1,8-naphthalimide, phthalazine, 1-(2H)-phthalazinone and 2-acetylphthalazinone.
[0034] Post-processing image stabilizers and latent image keeping stabilizers are useful
in the photothermographic element. Any of the stabilizers known in the photothermographic
art are useful for the described photothermographic element. Illustrative examples
of useful stabilizers include photolytically active stabilizers and stabilizer precursors
as described in, for example, U.S. Patent 4,459,350. Other examples of useful stabilizers
include azole thioethers and blocked azolinethione stabilizer precursors and carbamoyl
stabilizer precursors, such as described in U.S. Patent 3,877,940.
[0035] The thermally processable elements as described preferably contain various colloids
and polymers alone or in combination as vehicles and binders and in various layers.
Useful materials are hydrophilic or hydrophobic,. They are transparent or translucent
and include both naturally occurring substances, such as gelatin, gelatin derivatives,
cellulose derivatives, polysaccharides, such as dextran, gum arabic and the like;
and synthetic polymeric substances, such as water-soluble polyvinyl compounds like
poly(vinylpyrrolidone) and acrylamide polymers. Other synthetic polymeric compounds
that are useful include dispersed vinyl compounds such as in latex form and particularly
those that increase dimensional stability of photographic elements. Effective polymers
include water insoluble polymers of acrylates, such as alkylacrylates and methacrylates,
acrylic acid, sulfoacrylates, and those that have cross-linking sites. Preferred high
molecular weight materials and resins include poly(vinyl butyral), cellulose acetate
butyrate, poly(methylmethacrylate), poly(vinylpyrrolidone), ethyl cellulose, polystyrene,
poly(vinylchloride), chlorinated rubbers, polyisobutylene, butadiene-styrene copolymers,
copolymers of vinyl chloride and vinyl acetate, copolymers of vinylidene chloride
and vinyl acetate, poly(vinyl alcohol) and polycarbonates.
[0036] Photothermographic elements and thermographic elements as described can contain addenda
that are known to aid in formation of a useful image. The photothermographic element
can contain development modifiers that function as speed increasing compounds, sensitizing
dyes, hardeners, antistatic agents, plasticizers and lubricants, coating aids, brighteners,
absorbing and filter dyes, such as described in
Research Disclosure, December 1978, Item No. 17643 and
Research Disclosure, June 1978, Item No. 17029.
[0037] The thermally processable element can comprise a variety of supports. Examples of
useful supports are poly(vinylacetal) film, polystyrene film, poly(ethyleneterephthalate)
film, polycarbonate film, and related films and resinous materials, as well as paper,
glass, metal, and other supports that withstand the thermal processing temperatures.
[0038] The layers of the thermally processable element are coated on a support by coating
procedures known in the photographic art, including dip coating, air knife coating,
curtain coating or extrusion coating using hoppers. If desired, two or more layers
are coated simultaneously.
[0039] Spectral sensitizing dyes are useful in the photothermographic element to confer
added sensitivity to the element. Useful sensitizing dyes are described in, for example,
Research Disclosure, June 1978, Item No. 17029 and
Research Disclosure, December 1978, Item No. 17643.
[0040] A photothermographic element as described preferably comprises a thermal stabilizer
to help stabilize the photothermographic element prior to exposure and processing.
Such a thermal stabilizer provides improved stability of the photothermographic element
during storage. Preferred thermal stabilizers are 2-bromo-2-arylsulfonylacetamides,
such as 2-bromo-2-p-tolysulfonylacetamide; 2-(tribromomethyl sulfonyl)benzothiazole;
and 6-substituted-2,4-bis(tribromomethyl)-s-triazines, such as 6-methyl or 6-phenyl-2,4-bis(tribromomethyl)-s-triazine.
[0041] The thermally processable elements are exposed by means of various forms of energy.
In the case of the photothermographic element such forms of energy include those to
which the photographic silver halides are sensitive and include ultraviolet, visible
and infrared regions of the electromagnetic spectrum as well as electron beam and
beta radiation, gamma ray, x-ray, alpha particle, neutron radiation and other forms
of corpuscular wave-like radiant energy in either non-coherent (random phase) or coherent
(in phase) forms produced by lasers. Exposures are monochromatic, orthochromatic,
or panchromatic depending upon the spectral sensitization of the photographic silver
halide. Imagewise exposure is preferably for a time and intensity sufficient to produce
a developable latent image in the photothermographic element.
[0042] After imagewise exposure of the photothermographic element, the resulting latent
image is developed merely by overall heating the element to thermal processing temperature.
This overall heating merely involves heating the photothermographic element to a temperature
within the range of about 90°C. to 180°C. until a developed image is formed, such
as within about 0.5 to about 60 seconds. By increasing or decreasing the thermal processing
temperature a shorter or longer time of processing is useful. A preferred thermal
processing temperature is within the range of about 100°C. to about 130°C.
[0043] In the case of a thermographic element, the thermal energy source and means for imaging
can be any imagewise thermal exposure source and means that are known in the thermographic
imaging art. The thermographic imaging means can be, for example, an infrared heating
means, laser, microwave heating means or the like.
[0044] Heating means known in the photothermographic and thermographic imaging arts are
useful for providing the desired processing temperature for the exposed photothermographic
element. The heating means is, for example, a simple hot plate, iron, roller, heated
drum, microwave heating means, heated air or the like.
[0045] Thermal processing is preferably carried out under ambient conditions of pressure
and humidity. Conditions outside of normal atmospheric pressure and humidity are useful.
[0046] The components of the thermally processable element can be in any location in the
element that provides the desired image. If desired, one or more of the components
can be in more than one layer of the element. For example, in some cases, it is desirable
to include certain percentages of the reducing agent, toner, stabilizer and/or other
addenda in the overcoat layer over the photothermographic imaging layer of the element.
This, in some cases, reduces migration of certain addenda in the layers of the element.
[0047] It is necessary that the components of the imaging combination be "in association"
with each other in order to produce the desired image. The term "in association" herein
means that in the photothermographic element the photographic silver halide and the
image forming combination are in a location with respect to each other that enables
the desired processing and forms a useful image.
[0048] The thermally processable imaging element of this invention preferably includes a
backing layer. The backing layer utilized in this invention is an outermost layer
and is located on the side of the support opposite to the imaging layer. It is typically
comprised of a binder and a matting agent which is dispersed in the binder in an amount
sufficient to provide the desired surface roughness.
[0049] A wide variety of materials can be used to prepare a backing layer that is compatible
with the requirements of thermally processable imaging elements. The backing layer
should be transparent and colorless and should not adversely affect sensitometric
characteristics of the photothermographic element such as minimum density, maximum
density and photographic speed. Preferred backing layers are those comprised of poly(silicic
acid) and a water-soluble hydroxyl containing monomer or polymer that is compatible
with poly(silicic acid) as described in U.S. Patent 4,828,971. A combination of poly(silicic
acid) and poly(vinyl alcohol) is particularly useful. Other useful backing layers
include those formed from polymethylmethacrylate, cellulose acetate, crosslinked polyvinyl
alcohol, terpolymers of acrylonitrile, vinylidene chloride, and 2-(methacryloyloxy)ethyltrimethylammonium
methosulfate, crosslinked gelatin, polyesters and polyurethanes.
[0050] In the thermally processable imaging elements of this invention, either organic or
inorganic matting agents can be used. Examples of organic matting agents are particles,
often in the form of beads, of polymers such as polymeric esters of acrylic and methacrylic
acid, e.g., poly(methylmethacrylate), styrene polymers and copolymers, and the like.
Examples of inorganic matting agents are particles of glass, silicon dioxide, titanium
dioxide, magnesium oxide, aluminum oxide, barium sulfate, calcium carbonate, and the
like. Matting agents and the way they are used are further described in U.S. Patent
Nos. 3,411,907 and 3,754,924.
[0051] The backing layer preferably has a glass transition temperature (Tg) of greater than
50°C, more preferably greater than 100°C, and a surface roughness such that the Roughness
Average (Ra) value is greater than 0.8, more preferably greater than 1.2, and most
preferably greater than 1.5.
[0052] As described in U.S. Patent 4,828,971, the Roughness Average (Ra) is the arithmetic
average of all departures of the roughness profile from the mean line.
[0053] The concentration of matting agent required to give the desired roughness depends
on the mean diameter of the particles and the amount of binder. Preferred particles
are those with a mean diameter of from about 1 to about 15 micrometers, preferably
from 2 to 8 micrometers. The matte particles can be usefully employed at a concentration
of about 1 to about 100 milligrams per square meter.
[0054] In order to improve image tone, improve printout, provide better visual contrast
and enhance the appearance of the thermally processable imaging elements of this invention,
a small amount of a colorant can be added to the overcoat layer and/or adhesive interlayer.
Blue colorants, such as Victoria Pure Blue BO, Victoria Brilliant Blue G, Serva Blue
WS, Aniline Blue, Page Blue G-90 and Methylene Blue, are especially useful for this
purpose.
[0055] In a preferred embodiment of this invention, the thermally processable imaging element
also includes an electroconductive layer to serve as an antistatic layer. For this
purpose, the electroconductive layer should have an internal resistivity of less than
5 X 10¹⁰ ohms/square. Such electroconductive layers are described in United States
Patent No. 5,310,640, issued May 10, 1994.
[0056] The electroconductive layer utilized in this invention in accordance with the teachings
of the aforesaid United States Patent No. 5,310,640 is an "inner layer", i.e., a layer
located under one or more overlying layers. It can be disposed on either side of the
support. As indicated hereinabove, it has an internal resistivity of less than 5 X
10¹⁰ ohms/square. Preferably, the internal resistivity of the electroconductive layer
is less than 1 X 10¹⁰ ohms/square.
[0057] The electroconductive layer can be composed of any of a very wide variety of compositions
which are capable of forming a layer with suitable physical and electrical properties
to be compatible with the requirements of thermally processable imaging elements.
Included among the useful electroconductive layers are:
(1) Electroconductive layers comprised of electrically-conductive metal-containing
particles dispersed in a polymeric binder. Examples of useful electrically-conductive
metal-containing particles include donor-doped metal oxide, metal oxides containing
oxygen deficiencies and conductive nitrides, carbides or borides. Specfic examples
of particularly useful particles include conductive TiO₂, SnO₂, Al₂O₃, ZrO₂, In₂O₃,
ZnO, TiB₂, ZrB₂, NbB₂, TaB₂, CrB₂, MoB, WB, LaB₆, ZrN, TiN, TiC, WC, HfC, HfN and
ZrC.
Examples of the many patents describing electrically-conductive metal-containing particles
that are useful in this invention include:
(a) semiconductive metal salts such as cuprous iodide as described in U.S. Patents
3,245,833, 3,428,451 and 5,075,171;
(b) metal oxides, preferably antimony-doped tin oxide, aluminum-doped zinc oxide and
niobium-doped titanium oxide as described in U.S. Patents 4,275,103, 4,394,441, 4,416,963,
4,418,141, 4,431,764, 4,495,276, 4,571,361, 4,999,276 and 5,122,445;
(c) a colloidal gel of vanadium pentoxide as described in U.S. Patents 4,203,769 and
5,006,451;
(d) fibrous conductive powders comprising, for example, antimony-doped tin oxide coated
onto non-conductive potassium titanate whiskers as described in U.S. Patents 4,845,369
and 5,116,666;
(e) electroconductive ceramic particles, such as particles of TiN, NbB₂, TiC, LaB₆
or MoB dispersed in a binder as described in Japanese KOKAI NO. 4/55492, published
February 24, 1992;
(2) Electroconductive layers composed of a vapor-deposited metal such as silver, aluminum
or nickel;
(3) Electroconductive layers composed of binderless electrically-semiconductive metal
oxide thin films formed by oxidation of vapor-deposited metal films as described in
U.S. Patent 4,078,935.
(4) Electroconductive layers composed of conductive polymers such as, for example,
the cross-linked vinylbenzyl quaternary ammonium polymers of U.S. Patent 4,070,189
or the conductive polyanilines of U.S. Patent 4,237,194.
[0058] A colloidal gel of vanadium pentoxide is especially useful for forming the electroconductive
layer. When vanadium pentoxide is used for this purpose, it is desirable to interpose
a barrier layer between the electroconductive layer and the imaging layer so as to
inhibit migration of vanadium pentoxide from the electroconductive layer into the
imaging layer with resulting adverse sensitometric affects. Suitable barrier layers
include those having the same composition as the backing layer of U.S. Patent 4,828,971,
namely, a mixture of poly(silicic acid) and a water-soluble hydroxyl-containing monomer
or polymer.
[0059] Use in this invention of a colloidal gel of vanadium pentoxide, the preparation of
which is described in U.S. Patent 4,203,769, issued May 20, 1980, has many important
beneficial advantages. The colloidal vanadium pentoxide gel typically consists of
entangled, high aspect ratio, flat ribbons about 50-100 angstroms wide, about 10 angstroms
thick and about 1000-10000 angstroms long. The ribbons stack flat in the direction
parallel to the surface when the gel is coated to form a conductive layer. The result
is very high electrical conductivities which are typically about three orders of magnitude
greater than is observed for layers of similar thickness containing crystalline vanadium
pentoxide particles. Low surface resistivities can be obtained with very low vanadium
pentoxide coverages. This results in low optical absorption and scattering losses.
Also, the coating containing the colloidal vanadium pentoxide gel is highly adherent
to underlying support materials.
[0060] As hereinabove described, the improved thermally processable imaging element of this
invention includes an adhesive interlayer, interposed between the imaging layer and
the overcoat layer, which comprises at least one of (1) a polymer having pyrrolidone
functionality, (2) a polymer having epoxy functionality and (3) a polyalkoxysilane.
The purpose of the adhesive interlayer is to strongly bond the overcoat layer to the
imaging layer so that it cannot be easily removed. By the term "pyrrolidone functionality"
is meant the presence of one or more pendant pyrrolidone rings. Preferably the polymer
is comprised of recurring units of which at least 50 mole percent comprise a pendant
pyrrolidone ring. By the term "epoxy functionality" is meant the presence of one or
more pendant oxirane rings. Preferably, the polymer is comprised of recurring units
of which at least 50 mole percent comprise a pendant oxirane ring.
[0061] For use in this invention, the polymer having pyrrolidone functionality can be a
homopolymer of N-vinyl-2-pyrrolidone or a copolymer of N-vinyl-2-pyrrolidone with
one or more ethylenically-unsaturated copolymerizable monomers. Preferably, the copolymer
is one which contains at least 60 weight percent of N-vinyl-2-pyrrolidone.
[0062] The pendant pyrrolidone rings of the polymer can be substituted or unsubstituted.
For example, they can be substituted with alkyl groups.
[0063] The homopolymer of N-vinyl-2-pyrrolidone,i.e., poly(N-vinyl-2-pyrrolidone), is represented
by the formula:

wherein n represents a whole number, e.g., a number sufficiently high to provide a
molecular weight of from several hundred to several hundred thousand. These polymers
are well known and can be prepared, for example, by processes of polymerization of
N-vinyl-2-pyrrolidone, disclosed in U.S. Patent No. 2,265,540, issued December 9,
1941, and U.S. Patent 2,335,454, issued November 30, 1943.
[0064] Ethylenically unsaturated monomers that are copolymerizable with N-vinyl-2-pyrrolidone
include:
vinyl acetate
glycidyl acrylate
glycidyl methacrylate
vinyl propionate
vinyl chloride
styrene
methylacrylate
methylmethacrylate
ethylacrylate
n-propylacrylate
ethylmethacrylate
butylacrylate
butylmethacrylate
methylacrylamide
methylmethacrylamide
N-isopropylacrylamide
N,N-dimethylacrylamide
N-acryloylmorpholine
N-acryloylpiperidine
vinylpyridine
and the like.
[0065] Specific examples of polymers having pyrrolidone functionality that are preferred
for use in this invention include:
poly(N-vinyl-2-pyrrolidone)
poly(N-vinyl-2-pyrrolidone-co-vinyl acetate)
poly(N-vinyl-2-pyrrolidone-co-glycidyl acrylate)
poly(N-vinyl-2-pyrrolidone-co-glycidyl methacrylate)
poly(N-vinyl-2-pyrrolidone-co-N-acryloylmorpholine)
poly(N-vinyl-2-pyrrolidone-co-N-acryloylpiperidine)
poly(N-vinyl-2-pyrrolidone-co-methylacrylate)
poly(N-vinyl-2-pyrrolidone-co-ethyl methacrylate)
poly(N-vinyl-2-pyrrolidone-co-4-vinyl-pyridine)
poly(N-vinyl-2-pyrrolidone-co-N,N-dimethylacrylamide)
poly(N-vinyl-2-pyrrolidone-co-N-isopropylacrylamide)
and the like.
[0066] In a particularly preferred embodiment of the invention, the polymer having pyrrolidone
functionality is comprised of recurring units represented by the formula:

wherein
R₁ is hydrogen or methyl,
D is alkylene of 1 to 6 carbon atoms,
L is

x = 30-100 mole %
y = 0-70 mole %.
[0067] Polymers having epoxy functionality which are preferred for use in this invention
are comprised of recurring units represented by the formula:

wherein:
R₁ is hydrogen or methyl,
R₂ is alkyl of 1 to 8 carbon atoms or cycloalkyl of 3 to 8 carbon atoms,
D is alkylene of 1 to 6 carbon atoms,
L is

a = 30-70 mole %,
b = 0-10 mole %,
c = 20-70 mole %.
[0068] The above-described polymers having epoxy functionality are readily prepared by reacting
a polymerizable epoxy compound with one or more polymerizable acrylic monomers.
[0069] Examples of suitable polymerizable acrylic monomers include:
ethyl acrylate
ethyl methacrylate
butyl acrylate
butyl methacrylate
cyclohexyl acrylate
cyclohexyl methacrylate
styrene
methyl acrylate
lauryl acrylate
lauryl methacrylate
allyl methacrylate
and the like
[0070] Examples of suitable polymerizable epoxy monomers include:
glycidyl methacrylate
glycidyl acrylate
allyl glycidyl ether.
[0071] Specific examples of polymers having epoxy functionality that are preferred for use
in this invention include:
poly(butyl acrylate-co-allyl methacrylate-co-glycidyl methacrylate)
poly(butyl methacrylate-co-allyl methacrylate-co-glycidyl methacrylate)
poly(butyl acrylate-co-glycidyl methacrylate)
poly(lauryl methacrylate-co-allyl methacrylate-co-glycidyl methacrylate)
In a particularly preferred embodiment of the invention, the overcoat layer comprises
polysilicic acid and polyvinylalcohol, the imaging layer comprises polyvinylbutyral,
and the adhesive interlayer is comprised of poly(N-vinyl-2-pyrrolidone).
[0072] In a second particularly preferred embodiment of the invention, the overcoat layer
comprises polysilicic acid and polyvinylalcohol, the imaging layer comprisies polyvinylbutyral,
and the adhesive interlayer is comprised of poly(butyl acrylate-co-allyl methacrylate-co-glycidyl
methacrylate).
[0073] In a third particularly preferred embodiment of the invention, the overcoat layer
comprises polysilicic acid and polyvinylalcohol, the imaging layer comprises polyvinylbutyral,
and the adhesive interlayer is comprised of glycidoxypropyltrimethoxysilane.
[0074] The use of a polymer having pyrrolidone functionality, or a polymer having epoxy
functionality or a polyalkoxysilane in the adhesive interlayer is highly advantageous
in comparison with the prior art. Thus, for example, U.S. Patent 4,942,115 describes
the use of an adhesive interlayer comprising a terpolymer such as poly(2-propenenitrile-co-1,1-dichloroethene-co-2-propenoic
acid) or poly(2-propenoic acid methyl ester-co-1,1-dichloroethene-co-itaconic acid).
These terpolymers are very effective in providing good adhesion but are costly, difficult
to handle and environmentally disadvantageous and can cause adverse sensitometric
effects such as an undesirably high D
min.
[0075] The invention is further illustrated by the following examples of its practice.
Example 1
[0076] A thermally processable imaging element was prepared by coating a poly(ethylene terephthalate)
film support, having a thickness of 0.114 millimeters, with a photothermographic imaging
layer, an adhesive interlayer and a protective overcoat layer. The photothermographic
imaging composition was coated from a solvent mixture containing 90 parts by weight
methyl isobutyl ketone and 10 parts by weight acetone to form an imaging layer of
the following composition.
Component |
Coverage (g/m²) |
Silver behenate |
0.952 |
AgBr |
0.388 |
Succinimide |
0.428 |
*Surfactant |
0.018 |
2-Bromo-2-p-tolylsulfonyl acetamide |
0.070 |
2,4-Bis(trichloromethyl)-6-(1-naphtho)-S-triazine |
0.017 |
Sensitizing dye |
0.005 |
4-Benzenesulfonamidophenol |
1.132 |
**Binder |
3.020 |
* A polysiloxane fluid available under the trademark SF-96 from General Electric Company. |
** A poly(vinylbutyral) available under the trademark BUTVAR B-76 resin from Monsanto
Company. |
[0077] The adhesive interlayer consisted of poly(N-vinyl-2-pyrrolidone), having a molecular
weight of 360,000, coated at a coverage of 0.11 g/m².
[0078] To prepare the protective overcoat layer, polysilicic acid was prepared by mixing
29.4 weight % water, 1.2 weight % one normal p-toluene sulfonic acid, 34 weight %
methanol and 35.4 weight % tetraethoxysilane to form a 16.3 weight % polysilicic acid
solution. The polysilic acid was mixed with polyvinyl alcohol, a surfactant, matte
beads and water to form a protective overcoat layer of the following composition.
Component |
Coverage (g/m²) |
* Polyvinyl alcohol |
1.1 |
Polysilicic acid |
1.65 |
**Surfactant |
0.044 |
Polymethylmethacrylate beads |
0.055 |
* A high molecular weight polyvinyl alcohol available under the trademark Elvanol
52/22 from E. I. duPont deNemours and Company |
** A para-isononylphenoxy polyglycidol surfactant available under the trademark Surfactant
10G from Olin Corporation. |
[0079] A second thermally processable imaging element, identified as Control A, was prepared
in the same manner as the element described above except that the adhesive interlayer
was omitted.
[0080] A third thermally processable imaging element, identified as Control B, was prepared
in the same manner as the element described above except that the poly(N-vinyl-2-pyrrolidone)
in the adhesive interlayer was replaced with poly(butylacrylate-co-2-sulfo-1,1-dimethylethyl
acrylamide-co-methyl-2-acrylamido-2-methoxyacetate).
[0081] For each of the elements of Example 1 and Controls A and B, adhesion of the overcoat
layer to the imaging layer was evaluated using a tape adhesion test. In carrying out
the test, a 35-mm wide sample was prepared and laid flat on a table and a section
of SCOTCH Magic Tape #811, available from Minnesota Mining and Manufacturing Company,
was placed across the width of the sample and smoothed out by hand to assure uniform
adhesion. Upon manually removing the tape, the percent of the overcoat layer removed
was estimated and related to adhesion. Ideally, the extent of removal would be zero.
The test was performed up to ten times for each sample. Measurements were made for
fresh samples, for samples aged two weeks at ambient conditions, and for samples aged
two weeks at 49°C/15% relative humidity.
[0082] The effect of the adhesive interlayer on sensitometry was determined by measuring
the D
min of each sample after exposure (10⁻³ sec, EG & G, Wratten 29 filter) and heat processing
for 5 seconds at 119°C. The lower the D
min value the better the results. In each case, the D
min was determined for a sample that had been aged two weeks at 49°C/15 % relative humidity.
[0083] Results obtained in both the adhesion test and the sensitometry test are summarized
in Table I below.
Table I
Percent of Overcoat Removed |
Example |
Fresh |
2 Week Ambient |
2 Week 49°C/15%RH |
Dmin |
1 |
4 |
3.5 |
0 |
0.22 |
Control A |
60 |
76 |
16.5 |
0.23 |
Control B |
25 |
0 |
0 |
1.22 |
[0084] The data reported in Table I show that incorporation of an adhesive interlayer in
accordance with this invention in the thermally processable element substantially
improves the adhesion of the overcoat layer to the imaging layer and does so without
adverse effects on D
min. In marked contrast, use of the adhesive interlayer employed in Control B improved
adhesion but caused a highly undesirable increase in D
min.
Example 2
[0085] To evaluate the effect of the thickness of the adhesive interlayer, four samples
were prepared in which the coverage of poly(N-vinyl-2-pyrrolidone) was varied. In
this test, the proportions of the ingredients in the imaging layer varied slightly
from that of Example 1 and palmitic acid was incorporated in the imaging layer. As
disclosed in Dedio et al, U.S. Patent 4,857,439, issued August 15, 1989, palmitic
acid and similar carboxylic acids can be incorporated in photothermographic elements
for the purpose of improving latent image stability.
[0086] The composition of the imaging layer was as follows:
Component |
Coverage (g/m²) |
Silver behenate |
1.008 |
AgBr |
0.400 |
Succinimide |
0.352 |
*Surfactant |
0.019 |
2-Bromo-2-p-tolylsulfonyl acetamide |
0.072 |
2,4-Bis(trichloromethyl)-6-(1-naphtho)-S-triazine |
0.017 |
Sensitizing dye |
0.005 |
Palmitic acid |
0.110 |
4-Benzenesulfonamidophenol |
1.166 |
**Binder |
3.092 |
* A polysiloxane fluid available under the trademark SF-96 from General Electric Company |
** A poly(vinylbutyral) available under the trademark BUTVAR B-76 resin from Monsanto
Company. |
[0087] The results obtained in the tape adhesion test (carried out in each case on an element
aged for 2 weeks at 49°C/15% RH) with variation in the thickness of the poly(N-vinyl-2-pyrrolidone)
layer are summarized in Table II below.
Table II
Dry Coverage of Adhesive Interlayer (g/m²) |
Tape Adhesion (% removed) |
0.055 |
100 |
0.11 |
4 |
0.22 |
1 |
0.44 |
0 |
[0088] The results reported in Table II indicate that the coverage of poly(N-vinyl-2-pyrrolidone)
is important and sufficient coverage must be provided to get the desired good adhesion.
Generally speaking, the coverage of an adhesive interlayer employing a polymer having
pyrrolidone functionality should be ate least about 0.1 g/m².
Examples 3-6
[0089] Polymers having pyrrolidone functionality, coated at a dry coverage of 0.11 g/m²,
were evaluated as an adhesive interlayer using a modified adhesion test. In this example,
the imaging layer was of the same composition as described in Example 2. In the adhesion
test, a 1.25 X 4.0 cm piece of SCOTCH Magic Tape #811 was firmly pressed by hand onto
the overcoated sample and then manually removed. The test was conducted on a fresh
sample and on a sample that had been dried for one hour at 60°C. The amount of the
overcoat layer removed was determined and the sample was rated in accordance with
the following scale:
Good - no layer removal
Fair - partial layer removal
Poor - total layer removal
The results obtained in this test are summarized in Table III below.
Table III
Example No. |
Interlayer Material |
Tape Adhesion (Fresh) |
Tape Adhesion (1 hr 60°C) |
Control A |
None |
Poor |
Fair |
3 |
Poly(N-vinyl-2-pyrrolidone) |
Poor |
Good |
4 |
Poly(N-vinyl-2-pyrrolidone-co-glycidyl methacrylate) 70/30 wt% |
Good |
Good |
5 |
Poly(N-vinyl-2-pyrrolidone-co-glycidyl acrylate) 70/30 wt% |
Good |
Good |
6 |
Poly(N-vinyl-2-pyrrolidone-co-vinyl acetate) 70/30 wt% |
Poor |
Good |
[0090] As indicated by the data reported in Table III, both the homopolymer of N-vinyl-2-pyrrolidone
and copolymers of N-vinyl-2-pyrrolidone with ethylenically unsaturated copolymerizable
monomers are capable of providing good adhesion in the test performed after one hour
of drying at 60°C. In comparison, the use of a 50/50 wt% copolymer of N-vinyl-2-pyrrolidone
and vinyl acetate provided poor results in both tests. Similarly, the use of a 30/70
wt% copolymer of N-vinyl-2-pyrrolidone and vinyl acetate provided poor results in
both tests. These results indicate that the polymer must have a sufficient level of
pyrrolidone functionality to perform well. Typically, when N-vinyl-2-pyrrolidone is
copolymerized with one or more other monomers, the amount of N-vinyl-2-pyrrolidone
should be at least about 60 weight percent.
Examples 7-9
[0091] To evaluate the effect of variation in molecular weight, three samples were prepared
in which poly(N-vinyl-2-pyrrolidones) of different molecular weight were employed.
In these tests, the same support, photothermographic imaging layer and protective
overcoat layer as described in Example 1 were employed. The layers were coated simultaneously
using multiple-layer slide hopper coating techniques. In each of Examples 7 to 9,
the poly(N-vinyl-2-pyrrolidone) was coated at a coverage of 0.22 g/m². Tape adhesion
test measurements were made for fresh samples in the manner described in Example 1
and D
min values were determined in the manner described in Example 1.
[0092] The results obtained in both the adhesion test and sensitometry test are summarized
in Table IV below.
Table IV
Example |
Molecular Weight |
Percent of Overcoat Removed |
Dmin |
7 |
10,000 |
0.8 |
0.14 |
8 |
40,000 |
0 |
0.14 |
9 |
360,000 |
8.2 |
0.13 |
[0093] The data reported in Table IV indicate that good results are obtained with poly(N-vinyl-2-pyrrolidone)
over a wide range of molecular weights.
Example 10
[0094] In this example, the support, photothermographic imaging layer and protective overcoat
layer were the same as described in Example 1. The adhesive interlayer consisted of
poly(butyl acrylate-co-allyl methacrylate-co-glycidyl methacrylate) coated at a coverage
of 0.11 g/m².
[0095] For each of the elements of this example and Controls A and B, adhesion of the overcoat
layer to the imaging layer was evaluated using the tape adhesion test described in
Example 1 and the effect of the adhesive interlayer on sensitometry was determined
in the same manner as described in Example 1.
[0096] Results obtained in both the adhesion test and the sensitometry test are summarized
in Table V below.
Table V
Percent of Overcoat Removed |
|
Fresh |
2 Week Ambient |
2 Week 49°C/15%RH |
Dmin |
Example 10 |
0 |
1.5 |
0 |
0.22 |
Control A |
60 |
76 |
16.5 |
0.23 |
Control B |
25 |
0 |
0 |
1.22 |
[0097] The data reported in Table V show that incorporation of an adhesive interlayer in
accordance with this invention in the thermally processable element substantially
improves the adhesion of the overcoat layer to the imaging layer and does so without
adverse effects on D
min. In marked contrast, use of the adhesive interlayer employed in Control B improved
adhesion but caused a highly undesirable increase in D
min.
Example 11
[0098] In this example, the support, photothermographic imaging layer and protective overcoat
layer were the same as described in Example 1. The adhesive interlayer consisted of
glycidoxypropyltrimethoxysilane coated at a coverage of 0.11 g/m².
[0099] For each of the elements of this example and Controls A and B, adhesion of the overcoat
layer to the imaging layer was evaluated using the tape adhesion test described in
Example 1 and the effect of the adhesive interlayer on sensitometry was determined
in the same manner as described in Example 1.
[0100] Results obtained in both the adhesion test and the sensitometry test are summarized
in Table VI below.
Table VI
Percent of Overcoat Removed |
Example |
Fresh |
2 Week Ambient |
2 Week 49°C/15%RH |
Dmin |
11 |
1.5 |
0 |
0 |
0.22 |
Control A |
60 |
76 |
16.5 |
0.23 |
Control B |
25 |
0 |
0 |
1.22 |
[0101] The data reported in Table VI show that incorporation of an adhesive interlayer in
accordance with this invention in the thermally processable element substantially
improves the adhesion of the overcoat layer to the imaging layer and does so without
adverse effects on D
min. In marked contrast, use of the adhesive interlayer employed in Control B improved
adhesion but caused a highly undesirable increase in D
min.
Example 12
[0102] A thermally processable imaging element was prepared in the same manner as described
in Example 11 except that the glycidoxypropyltrimethoxysilane in the adhesive interlayer
was replaced with tetraethoxysilane. The results obtained were similar to Example
11 with the percentage removal being 10 percent for the fresh sample, zero for the
two-week ambient sample and zero for the 2-week 49°C/15% RH sample and the D
min being 0.21. Thus, tetraethoxysilane behaves in a similar manner to glycidoxypropyltrimethoxysilane
in providing effective improvement in adhesion without adverse effects on sensitometry.
Example 13
[0103] To evaluate the effect of the thickness of the adhesive interlayer, four samples
were prepared in which the coverage of glycidoxypropyltrimethoxysilane was varied.
In this test, the ingredients of the imaging layer were the same as described in Example
2.
[0104] The results obtained in the tape adhesion test (carried out in each case on an element
aged for 2 weeks at 49°C/15% RH) with variation in the thickness of the glycidoxypropyltrimethoxysilane
layer are summarized in Table VII below.
Table VII
Dry Coverage of Adhesive Interlayer (g/m²) |
Tape Adhesion (% removed) |
0.055 |
0 |
0.11 |
0 |
0.22 |
0 |
0.44 |
0 |
[0105] The results reported in Table VII indicate that the thickness of the glycidoxypropyltrimethoxysilane
interlayer did not affect its adhesive performance.
Example 14
[0106] Glycidoxypropyltrimethoxysilane coated at a dry coverage of 0.11 g/m² was evaluated
as an adhesive interlayer using a modified adhesion test. In this example, the imaging
layer was of the same composition as described in Example 2. In the adhesion test,
a 1.25 X 4.0 cm piece of SCOTCH Magic Tape #811 was firmly pressed by hand onto the
overcoated sample and then manually removed. The test was conducted on a fresh sample
and on a sample that had been dried for one hour at 60°C. The amount of the overcoat
layer removed was determined and the sample was rated in accordance with the following
scale:
Good - no layer removal
Fair - partial layer removal
Poor - total layer removal
For both the fresh test and the test after one hour of drying at 60°C the rating was
good, whereas the rating for Control A, in which the adhesive interlayer was omitted,
was poor in the fresh test and fair in the test after one hour of drying at 60°C.
[0107] The present invention provides an important improvement in thermally processable
imaging elements. A hydrophilic overcoat layer, such as a layer containing poly(silicic
acid) and poly(vinyl alcohol), provides excellent protection for such elements. However,
the degree of adhesion of such an overcoat layer to hydrophobic imaging layers, such
as those that contain poly(vinyl butyral), is inadequate as a consequence of the general
lack of compatability of hydrophiic and hydrophobic layers. The adhesive interlayer
of this invention overcomes the problem of inadequate adhesion and does so with low
cost readily-available materials which are easy to coat and handle, are environmentally
advantageous and do not cause adverse sensitometric effects.