JPH10232459A - Silver halide photographic sensitive material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide the silver halide photographic sensitive material capable of enhancing processing speed and reducing a replenishing rate and superior in sharpness. SOLUTION: The silver halide photographic sensitive material provided on a support with at least one photosensitive silver halide emulsion layer has a layer containing fine dispersed particles having an average particle diameter as a corresponding sphere diameter of <=0.5μm and having adsorbed a dye forming a J association product as a layer near to the support then the emulsion layer, and this emulsion layer contains flat silver halide grains occupying at least >=50% of the projection areas of the total silver halide grains and having an aspect ratio of 2-30.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silver halide photographic light-sensitive material, and more particularly to a light-sensitive material requiring an antihalation layer or a crossover cut layer to improve image quality (sharpness), especially when processed by an automatic developing machine. More particularly, the present invention relates to a technique for reducing a failure such as contamination of a processing solution and a resulting residual color in a rapid and low waste liquid processing system.

[0002]

2. Description of the Related Art In recent years, rapid processing, low waste liquid processing, and anti-halation and high image quality by improving sharpness by crossover cut have been achieved by rapid processing of dyes used in these antihalation layers and crossover cut layers. Various techniques have been devised to increase the outflow rate of ash out of the system.

[0003] In the old days, Japanese Patent Publication No. 49-8333 discloses a technique using a water-soluble dye for an antihalation layer. Further, JP-A-62-70830 and JP-A-1-26645,
There is disclosed a technique in which a layer in which a dye is mordanted is used as a crossover cut layer.

Further, Japanese Patent Publication No. 51-5574 and Japanese Patent Application Laid-Open No. 1-172828
Discloses a technique in which a solid-dispersed water-soluble dye is used as an antihalation layer or a crossover cut layer. Techniques for adsorbing a dye on a fine particle dispersion, particularly silver halide fine crystal, and using the dye in a crossover cut layer or an antihalation layer are also disclosed in, for example, JP-A-2-29641, JP-A-64-73336, and JP-A-64-73336. JP-A-63-194251, JP-A-63-46438,
It is disclosed in Japanese Patent Publication No. 8-20688.

[0005] The above-mentioned JP-A-1-172828 discloses a technique using a dye in a solid dispersion state. Also, JP-A-1-126645 describes a crossover cut layer formed by fixing a dye with a mordant. Further, a method of increasing the absorption rate of the spectral sensitizing dye is also a well-known technique in the art.

However, these techniques have the following disadvantages.

[0007] 1. Since mordanting or solid dispersion is required, the absorption wavelength of the dye cannot be freely selected. Further, since no J-aggregate was formed, the absorption coefficient at the maximum absorption was low, and a large amount of the dye had to be applied. 2. Although the residual color of the photographic material is basically prevented by elution into the processing solution, the problem of the coloring and the residual color of the processing solution became evident with low replenishment, low waste liquefaction, and rapid processing. 3. Since the emission wavelength of the phosphor is not one, the light of other wavelengths becomes crossover light even if it is simply cross-cut with a J-band forming type dye, so silver bromide having a particularly wide spectral sensitivity distribution In the case of the silver iodobromide emulsion system, the crossover light did not decrease.

[0008] From the above, it has been impossible in the prior art to advance high-quality images by accelerating processing, reducing replenishment and reducing waste liquid, and improving sharpness.

Further, considering the light-sensitive material, in order to achieve such high speed, low replenishment and high image quality, a large amount of dyes can be adsorbed, and the light absorption of each particle is large and the particles are hardly scattered. It has been considered as common sense in the art that the use of tabular grains having a higher particle size is preferable, but there are limits to this, and further advances have been made in speeding up, reducing replenishment, and improving image quality.

The following are known examples of tabular grains.

High aspect tabular grains and a thickness of 0.07 μm
With respect to ultrathin tabular grains having a particle size of less than m, see JP-A-62-997.
No. 51, JP-A-62-115435, JP-A-6-43
No. 605 and JP-A-6-43606.

High silver chloride-containing emulsions having a {111} plane as a main plane are described in JP-B-64-8326 and JP-B-64-8326.
No. 325, No. 64-8324, JP-A-1-25094
No. 3, Japanese Patent Publication No. 3-14328, Japanese Patent Publication No. 4-81782
JP-A-5-40298, JP-A-5-39459, JP-A-5-12696, and JP-A-63-213836, JP-A-6-213836.
These are described in detail in JP-A-3-218938, JP-A-63-281149 and JP-A-62-218959.

The prior art of high silver chloride-containing tabular grains having a {100} plane as a main plane is disclosed in JP-A-5-2040.
No. 73, JP-A-51-88017, JP-A-63-24
238 and Japanese Patent Application No. 5-264059.

[0014] Therefore, there is a demand for a technique for improving sharpness in the case of using such tabular grains to speed up processing and reduce replenishment.

[0015]

SUMMARY OF THE INVENTION An object of the present invention is to provide a silver halide photographic light-sensitive material which can be processed at a high speed and can be replenished at a low rate and has excellent sharpness.

[0016]

The above objects are achieved by the present invention described below. (1) In a silver halide photographic material having at least one photosensitive silver halide emulsion layer on a support, a dye which forms a J-aggregate as a layer closer to the support than the photosensitive silver halide emulsion layer And a layer using a dispersion of fine particles having an average size (equivalent sphere diameter) of 0.5 μm or less, wherein the photosensitive silver halide emulsion layer has an aspect ratio of at least 50% or more of the total projected area. More than 30
A silver halide photographic light-sensitive material comprising the following tabular grains, ie, photosensitive silver halide grains. (2) The silver halide photographic material as described in (1) above, wherein the tabular grains are tabular grains having a silver chloride content of 50 mol% or more. (3) The applied amount of the fine particles is 0.05 g or more per 1 m ^{2 on} one side.
The silver halide photographic light-sensitive material according to the above (1) or (2), which is not more than 5 g. (4) The silver halide photographic light-sensitive material according to any one of the above (1) to (3), wherein the dispersion of fine particles is a non-photosensitive silver halide fine particle emulsion having a silver iodide content of 20 mol% or less. (5) The crossover light when exposed from one side using a silver halide photographic light-sensitive material having a photosensitive silver halide emulsion layer on both sides of the support is 10% or less, and the total processing time is 60 seconds or less. After processing, the amount of fixer waste liquid is reduced to 4 1
The silver halide photographic light-sensitive material according to any one of the above (1) to (4), wherein the amount is 12 ml or less per sheet.

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail.
The silver halide photographic material of the present invention may be a single-sided photosensitive material having a photosensitive silver halide emulsion layer on one side of a support, or a double-sided photosensitive material having a photosensitive silver halide emulsion layer on both sides. And preferably those used with intensifying screens.

In such a light-sensitive material, the light-sensitive silver halide emulsion layer has an aspect ratio of 2 to 3 at least 50% or more of the total projected area of the light-sensitive silver halide grains.
0 or less tabular grains (preferably having a silver chloride content of 50 mol% or more) are used. Fine particles (equivalent sphere equivalent diameter) adsorbing a dye forming a J-aggregate between the emulsion layer and the support are used. A crossover cut layer using a dispersion having an average size of 0.5 μm or less represented by the following formula is provided.

By using an emulsion layer for tabular grains as described above, processing can be speeded up and replenishment can be reduced, and a crossover cut layer of fine particles adsorbing a dye forming a J aggregate is provided. Thereby, in a photosensitive material having an emulsion layer using tabular grains, crossover light which causes deterioration in sharpness (sharpness) can be efficiently absorbed, and sharpness can be improved. Further, since the color is erased by the fixing process, the problem of residual color does not occur.

Such dye-adsorbed fine particles are added as a dispersion, but it is preferable to add a non-photosensitive silver halide having a silver iodide content of 20 mol% or less as a fine particle emulsion. It is preferred in that respect. In order to obtain the effects of the present invention, such a dispersion of fine particles is expressed as a coating amount per one side of a light-sensitive material, and is expressed as fine particles of 0.05 to 0.5.
g / m ² is preferred. Even when silver halide fine particles are used as fine particles, the amount of the fixing solution used does not increase and there is no adverse effect on the fixing performance.

As an example of the dye which forms a J-aggregate by being adsorbed on the fine particles of the present invention, a dye which can be decolored with a fixing solution is preferable.

The dye capable of forming a J-aggregate on the surface of fine silver halide grains, which is characterized by decoloring with the fixing solution of the present invention, is not particularly limited as long as it has such characteristics. Without, for example, benzimidazolocarbocyanine dye, benzoxazolocarbocyanine dye,
And the like, and a benzimidazolocarbocyanine dye represented by the following general formula [I] is preferably used.

[0023]

Embedded image

In the general formula [I], R ¹¹ , R ¹² , R ¹³ and R ¹⁴
Represents a substituted or unsubstituted alkyl group, at least one of R ^11, R ¹² represents an alkoxyalkyl group, R ^13,
At least one of R ¹⁴ represents a sulfoalkyl group (including a sulfonatoalkyl group; the same applies hereinafter).

[0025] ^{X 11, X 12, X 13} , X 14 may be the same or different, represent a hydrogen atom, a cyano group, halogen-substituted alkyl group or a halogen atom, the X ^11, X ¹³ At least one represents a hydrogen atom.

Z represents an ion necessary for balancing the charges, n is 1 or 2, and n = 1 when an internal salt is formed.

The benzimidazolocarbocyanine dye of the general formula [I] will be described in more detail.

In the general formula [I], R ¹¹ and R ¹² represent a substituted or unsubstituted alkyl group. At least one of them is an alkoxyalkyl group (having 2 to 20, preferably 2 to 8, more preferably 2 to 5 carbon atoms. Specifically, a methoxymethyl group, a methoxypropyl group, an ethoxymethyl group, an ethoxy group Ethyl group or the like), and preferably at least one is an ethoxyethyl group. The remaining one of R ¹¹ and R ¹² is preferably a methyl group or an ethyl group.

R ¹³ and R ^{14 each} represent a substituted or unsubstituted alkyl group, at least one of which is substituted with an aromatic group having preferably 1 to 7 carbon atoms, more preferably 1 to 4 carbon atoms. There is no sulfoalkyl group. Also, R
^The remaining one of ¹³ and R ¹⁴ is a substituted or unsubstituted alkyl group having 1 to 18, preferably 1 to 7, and more preferably 1 to 4 carbon atoms (methyl, ethyl, propyl, butyl, isobutyl, hexyl, octyl , Dodecyl, octadecyl, etc.). Examples of the substituted alkyl group include a fluorine-substituted alkyl group (2,2-difluoroethyl group, 2,2,2-trifluoroethyl group, 2,2,3,
3-tetrafluoropropyl group, 2,2,3,3,3-
Pentafluoropropyl group, etc.), hydroxyalkyl group (hydroxymethyl group, hydroxyethyl group, hydroxypropyl group, etc.), aralkyl group (benzyl, 2-phenylethyl, etc.), carboxyalkyl group (carboxymethyl, 2-carboxyethyl, 3 -Carboxypropyl, 4-carboxybutyl, etc.), alkoxyalkyl group (2-methoxyethyl, 2- (2-methoxyethoxy)
Ethyl), a sulfoalkyl group (2-sulfoethyl, 3
-Sulfopropyl, 3-sulfobutyl, 4-sulfobutyl, 2- (3-sulfopropoxy) ethyl, 2-hydroxy-3-sulfopropyl, 3-sulfopropoxyethoxyethyl, etc.) sulfatoalkyl group (3-sulfatopropyl, 4-sulfatobutyl and the like, a hetero-substituted alkyl group ((2-pyrrolidin-2-one-1-yl) ethyl, tetrahydrofurfuryl, 2-morpholinoethyl and the like), 2-acetoxyethyl group, carboxymethoxymethyl group, Examples thereof include a 2-methanesulfonylaminoethyl group and an allyl group.

X ¹¹ , X ¹² , X ¹³ and X ¹⁴ may be the same or different, and each represents a hydrogen atom, a halogen atom (such as chlorine, bromine or fluorine), a cyano group, or a halogen-substituted alkyl group (trifluoromethyl). , 2,2-difluoroethyl, 2,2,2-trifluoroethyl, 2,2,3
3-tetrafluoropropyl, etc.), and X
^At least one of ¹¹ and X ¹³ is preferably a hydrogen atom, and X ¹² and X ¹⁴ are preferably any of a cyano group, a haloalkyl group and a halogen atom.

Z represents an ion necessary for neutralizing the charge, and n is 1 or 2. In addition, an inner salt is formed,
When the charge is neutralized, n is 1.

Specific examples of the substituent in the compound of the formula [I] are shown in Table 1, but the present invention is not limited to these compounds.

[0033]

[Table 1]

The benzimidazolocarbocyanine dye of the present invention represented by the general formula [I] is adsorbed on the surface of silver halide which is a fine particle to form a J-aggregate, and accordingly has a wavelength of 530 to 560 nm. A sharp J-band absorption is formed, which can efficiently absorb intensifying screen light emission. In addition, because of its high basicity, by treating at a low pH during fixing, protons are instantaneously added to discolor,
In addition, since the planarity of the dye molecule is lost due to the proton addition, the J-aggregate is destroyed and easily detached from the surface of the silver halide, so that the fixation of the silver halide fine particles on which the dye is adsorbed is not suppressed.

In particular, when the emulsion used for the photosensitive emulsion layer is a tabular emulsion, the spectral sensitivity in the specific region is relatively low,
In the case of a high silver chloride emulsion, it has no absorption in a wavelength region around 400 nm, and its spectral sensitivity rapidly attenuates as it deviates from the spectrally sensitized wavelength region. That is, of the crossover light at the time of exposing the photosensitive material, only the crossover light in the spectrally sensitized wavelength range contributes to the deterioration of the sharpness of the image, and the adverse effect that the crossover light in other wavelength ranges has on the sharpness is relatively. It will be small. Therefore, the crossover cut layer having J-band absorption having a sharp spectral absorption profile as in the present invention is:
It is possible to efficiently and effectively cut crossover light harmful to sharpness with a smaller amount of dye.

The coating amount of these dyes is 1 m ² per side of the photosensitive material.
A preferred range is 5 mg to 100 mg. More preferably 10
mg to 100 mg. The maximum absorption wavelength is preferably 500 nm or more and 600 nm or less, but is not particularly limited as long as the crossover light at the time of X-ray exposure can be absorbed.

The substantially light-insensitive silver halide fine grains preferably used as the fine grains of the present invention will be described in more detail.

The above-mentioned J-aggregate-forming / decolorizable dye may be added as an aqueous solution or dissolved in an organic solvent such as methanol, and added during or after the formation of the fine particles. In order to suppress Ostwald ripening and obtain small-sized fine particles, it is most preferable to add them during the formation of fine particles. In addition, when added after the formation of fine particles, immediately after the formation of the fine particles, it is preferable to add the dye without leaving time as much as possible, it is possible to more effectively suppress Ostwald ripening, more preferably, immediately after the preparation in the dye solution A fine grain emulsion is preferably added. More preferably, fine grains are formed in the first mixer, and the fine grains are immediately discharged from the mixer and introduced into the second mixer. And a method of mixing with. The dye to be added may be an aqueous solution or a solution obtained by dissolving the dye in an organic solvent, but in order to more efficiently form the dye into a J-aggregate, it is preferable to add the dye as a solution in a polar solvent.
More preferably, it is added as an aqueous solution.

Certain of these dyes have low hydrophilicity and are poorly soluble in water, and cannot be added as such as an aqueous solution. In the case of such a poorly water-soluble dye, the pH is adjusted to a value not higher than the pKa of the dye, the dye is converted to a water-soluble protonated product, and the aqueous solution of the dye-protonated product is adjusted to a concentration sufficient to adjust the pH to the pKa or higher of the dye. May be added at the same time as the aqueous alkali solution. By doing so, the proton is quickly released from the dye protonated product,
It becomes sparingly soluble in water again, and can be efficiently adsorbed to more hydrophobic and covalently bonded silver halide fine particles.

The dye functions as a growth inhibitor by adsorbing on silver halide fine particles, but has no protective colloid itself, and therefore is generally used in combination with a protective colloid polymer such as gelatin. Specifically, a protective colloid polymer such as gelatin is (1) contained in a water-soluble silver salt aqueous solution, (2) contained in a water-soluble halide aqueous solution, (3)
It may be contained in a dye solution, or may be contained in a plurality of these. The dye itself is also (1) a water-soluble silver salt aqueous solution, or (2) a water-soluble halide aqueous solution,
Or a protective colloid polymer such as gelatin may be contained in one or both of the above, and may be added as another aqueous solution.

The protective colloid polymer used in the present invention is gelatin and other natural polymers and synthetic polymers, and particularly, it inhibits physical ripening (coalescing ripening and Ostwald ripening) of fine silver halide particles. A polymer having a high degree is preferably used. The specific example is shown below.

(1) A gelatin inhibitor having a high degree of physical inhibition A gelatin rich in adenine and guanine. (2) Polyvinylpyrrolidone Homopolymer of vinylpyrrolidone, French Patent 203
1396. A copolymer of acrolein and pyrrolidone. (3) Polyvinyl alcohol Homopolymer of vinyl alcohol, US Patent 30007
An organic acid monoester of vinyl alcohol according to No. 14,
Maleic acid esters described in U.S. Pat. No. 3,236,653;
A copolymer of polyvinyl alcohol and polyvinyl pyrrolidone described in U.S. Pat. No. 3,479,189. (4) Polymer having a thioether group US Pat. Nos. 3,615,624, 3,860,428 and 3,
A polymer having a thioether group described in No. 706564. (5) Polyvinyl imidazole Homopolymer of polyvinyl imidazole, copolymer of polyvinyl imidazole and polyvinyl amide, Shoko 4
3-7561, German Patent No. 20120195, 20
No. 12970 terpolymer of acrylamide, acrylic acid and vinylimidazole.

(6) Polyethylene imine (7) Acetal polymer Water-soluble polyvinyl acetal described in US Pat. No. 2,358,836, polyvinyl acetal having a carboxyl group described in US Pat. No. 3,0038,879, British Patent 77115
5. The polymer according to item 5. (8) Amino polymer US Pat. Nos. 3,345,346, 3,706,504 and 4,
No. 350759, amino polymers described in German Patent 2,138,872, British Patent No. 1413125, U.S. Pat.
No. 4,258,836, polymers having an amino group and a carboxyl group described in US Pat. No. 3,511,818, and polymers described in US Pat. No. 3,832,185. (9) Polyacrylamide polymer Homopolymer of acrylic amide, US Pat. No. 25414
No. 74, copolymer of polyacrylamide and imidized polyacrylamide, German Patent No. 120213
No. 2, copolymer of acrylamide and methacrylamide, a partially aminated acrylamide polymer described in US Pat. No. 3,284,207, Japanese Patent Publication No. 45-1
No. 4031, U.S. Pat. Nos. 3,713,834 and 37,465.
No. 48, the substituted acrylamide polymer described in British Patent 788,343. (10) Polymer having hydroxyquinoline The polymer having hydroxyquinoline described in U.S. Pat. Nos. 4,030,929 and 4,152,161. (11) Others A vinyl polymer having an azaindene group described in JP-A-59-8604, a polyalkylene oxide derivative described in U.S. Pat. No. 2,976,150, a polyvinylamine imide polymer described in U.S. Pat.
No. 94920, No. 4089688, polyvinyl pyridine described in U.S. Pat. No. 2,484,456, vinyl polymer having imidazole group described in U.S. Pat. No. 3,520,857, vinyl polymer having triazole group described in JP-B-60-658, Zeitschrift Bisenshaftrich Photography 45, 43 (1
950) The water-soluble polyalkyleneaminotriazoles according to the above.

In the silver halide fine grain emulsion, excess water-soluble salts are removed by a known method. From the viewpoint of avoiding desorption of the dye adsorbed on the fine grains, ultrafiltration is particularly useful in the present invention. The specific device is described in, for example, JP-A-2-172816.

In the present invention, the fact that the fine particles are substantially non-photosensitive is less than 1 in ASA sensitivity, preferably 0 to 0.1.

The smaller the size of the fine particles, the larger the specific surface area, so that a larger amount of dye can be adsorbed with a smaller amount of silver. Although the lower limit of the particle size depends solely on manufacturing constraints, it is difficult for extremely small-sized fine particles to exist alone alone, and unless the dye adsorbed on the surface suppresses Ostwald ripening, the fine particles dissolve and recrystallize. And the size increases.

The size of the fine particles can be confirmed by placing the fine particles on a mesh and using a transmission electron microscope as it is.
The magnification is preferably 20 to 40,000 times. The average size of the fine particles of the present invention expressed in terms of the equivalent sphere diameter is 0.5 μm or less, and further 0.00
5 to 0.5 μm, preferably 0.005 to 0.3
5 μm, more preferably 0.01 to 0.30 μm
It is.

The halogen composition of the fine grains preferably has a silver iodide content of 20 mol% or less, more preferably 0 to 10 mol%.
Mol%. From the viewpoint of strong dye adsorption, silver iodide or a core-shell particle having a high surface iodine is preferable, but from the viewpoint of good decolorization in processing, silver bromide or silver chloride is preferable. This is because the dye in the adsorbed state is stabilized and has a lower pKa than in the case where the dye is freely present in the solution, which makes it more difficult to add a proton. The halogen composition of the fine particles of the present invention is silver chloride, silver bromide, silver iodide having a uniform composition, or silver chlorobromide having a high bromo surface and iodine bromide having a high iodine surface having a halogen composition mixed crystal structure or a core-shell structure. It may be silver, silver iodochlorobromide with a high surface iodine, or silver iodochloride with a high iodine surface, preferably silver chloride, silver bromide, silver chlorobromide with a high surface bromo, iodine salt with a high surface iodine Silver chloride, silver iodochloride having a high surface iodine, and more preferably silver chloride.

The amount of the dye adsorbed on the fine particles is generally preferably in excess of the saturated coating amount. However, if the Ostwald ripening of the fine particles is suppressed and a sufficient crossover cut can be obtained, a smaller amount of the dye may be added. Although the optimum dye addition amount may vary depending on the halogen composition of the fine particles, the dye addition amount is generally selected in the range of 0.001 to 0.5 mol per mol of silver of the fine particles. More preferably, it is selected in the range of 0.001 to 0.05 mol.

The substantially light-insensitive silver halide fine particles of the present invention can be produced by any of the well-known methods, but the following method is particularly preferred. That is, an aqueous solution of a water-soluble silver salt and an aqueous solution of a water-soluble halide are supplied to an airtight mixing vessel having an agitation function of several ml in internal volume, and mixed by mixing to form silver halide fine particles. Is discharged from such a mixer to prevent the fine grains from growing and increasing in size, and to obtain silver halide fine grains of extremely small size.

The size of the fine particles obtained by the above-mentioned method for producing fine silver halide particles strongly depends on the number of revolutions of stirring, and in order to obtain small-sized fine particles, generally, the higher the number of revolutions of stirring, the better.
If the stirring is insufficient, the particles become coarse due to coalescence aging (contact and adhesion of fine particles). The preferred stirring rotation speed is selected in the range of 500 to 10000 rpm, and more preferably in the range of 1000 to 10000 rpm.

The size of the fine grains obtained by the above-mentioned method for producing fine silver halide grains strongly depends on the residence time of the fine grain emulsion in the mixing vessel. In order to obtain small-sized fine grains, the shorter the residence time, the better. . Here, the residence time is defined below.

T = c / v t: retention time of fine grain emulsion / sec c: internal volume of mixing vessel / ml v: total amount of liquid added to mixing vessel per unit time / mls
ec ^-1

The preferred residence time t in the present invention is 60
Seconds or less, more preferably 10 seconds or less, and most preferably 2 seconds or less.
Seconds or less. The lower limit of t is not particularly limited, but is about 0.01 second due to the restriction of equipment.

The coating amount of the dye-adsorbed fine particle dispersion of the present invention is 0.05 g (as fine particles) per 1 m ^{2 on} one side of the photographic material.
It is preferably from 0.5 to 0.5 g, more preferably from 0.1 to 0.4 g. When the coating amount is small, the effect of the present invention is not effective. When the coating amount is too large, the haze of the photographic material increases, the film strength decreases, the residual color increases, and the like.

The crossover cut layer containing the dye-adsorbed fine particles of the present invention is provided between the support and the emulsion layer, and is preferably provided in combination with the emulsion layer using the tabular grains of the present invention. It is preferable to provide the layer on the side having such an emulsion layer. When such an emulsion layer is provided on both sides, it is preferable to provide such a crossover cut layer on both sides. Further, such a crossover cut layer may be provided as a single layer on one side, or may be provided as a plurality of layers. Further, another crossover cut layer as described later may be used in combination.

The thickness of one layer of the crossover cut layer of the present invention is preferably 0.05 to 5 μm.

According to the present invention, by providing such a crossover cut layer, the crossover light when exposed from one side of a double-sided photosensitive material is obtained by 10% according to the method described in JP-A-1-172828. Less than,
Preferably, the content is 9% or less and 3% or more, which is extremely excellent in sharpness.

The tabular emulsion containing a large amount of silver chloride which is preferably used in the photosensitive silver halide emulsion layer of the present invention will be described.

In a silver halide emulsion containing at least a dispersion medium and silver halide grains, 50% or more, preferably 60% to 100%, more preferably 70 to 100%, of the total projected area of the silver halide grains is a main plane. Are tabular grains having an aspect ratio of 2 to 30 having {100} or {111} planes. Here, the tabular grains are grains having an aspect ratio (diameter / thickness) larger than 1. The major plane refers to the largest outer surface of the tabular grains. The thickness of such tabular grains is 0.35 μm or less, and 0.05 to 0.3 μm.
Is more preferable, and 0.05 to 0.25 μm is further preferable. The preferred aspect ratio is 2 to 30, preferably 3 to
30, more preferably 5 to 20. Here, the diameter refers to the diameter of a circle having an area equal to the projected area of the tabular grains, and the thickness refers to the distance between two principal planes. Cl ^- content 20 mol% or more, preferably 30 to 100 mol%,
More preferably 40 to 100 mol%, even more preferably 5
0-100 mol% is preferred.

With respect to the nucleation of the emulsion of the present invention having a {111} plane as the main plane, see Japanese Patent Publication No. 64-8326.
Nos. 64-8325, 64-8324, JP-A-1-250943, JP-B-3-14328, JP-B-4-81782, JP-B-5-40298, and 5-3
No. 9459, No. 5-112696 and JP-A-63-213.
No. 836, No. 63-218938, No. 63-2811
No. 49, JP-A-62-218959, and the like, and as prior art of tabular grains having a {100} plane as a main plane, JP-A-5-204073,
JP-A-51-88017, JP-A-63-24238
And Japanese Patent Application No. 5-264059.

In the present invention, tabular grains having a high silver chloride content and having {100} in the main plane are most preferably used.

In the present invention, any of the nucleation methods described in these prior arts can be used.

The method of the present invention for crystal growth by physical ripening in the presence of silver halide fine grains (the fine grains dissolve and the substrate grains grow) will be described below.

In the fine grain emulsion addition method, the diameter is 0.15 μm or less, preferably 0.1 μm or less, more preferably 0.1 μm or less.
An AgX fine grain emulsion having a diameter of from 0.6 to 0.006 μm was added,
Tabular grains are grown by Ostwald ripening. Fine grain emulsions can be added either continuously or continuously. The fine grain emulsion can be continuously prepared by supplying the AgNO ₃ solution and the X ⁻ salt solution by a mixer provided near the reaction vessel, and can be immediately added continuously to the reaction vessel, or can be added to another vessel in advance. It can be added continuously or continuously after being prepared in a batch system. The fine grain emulsion can be added in a liquid form or as a dry powder. The dry powder can be mixed with water just before addition, liquefied and added. The added fine particles are preferably added in such a manner that they disappear within 20 minutes, more preferably 10 seconds to 10 minutes. If the elimination time is long, ripening occurs between the fine particles, and the particle size increases, which is not preferable. Therefore, it is preferable not to add the whole amount at once. Such fine particles preferably do not substantially contain a large amount of twin particles. Here, the multiple twin particles refer to particles having two or more twin planes per particle. "Substantially not contained" means that the ratio of the number of multiple twin grains is 5%.
Or less, preferably 1% or less, more preferably 0.1% or less. Further, it is preferable that substantially no single twin particles are contained. Further, it is preferable that the screw dislocation is not substantially contained. Here, "substantially not included" complies with the above-mentioned rules.

The halogen composition of the fine particles is AgCl, AgB
r, AgBrI (I ^- content is preferably at most 10 mol%, more preferably at most 5 mol%) and mixed crystals of two or more thereof. For other details, refer to Japanese Patent Application No. 4-2141.
09 can be referred to.

The total amount of the fine grains added must be at least 20% by weight of the total amount of silver halide, preferably 40% by weight.
More preferably, the content is 50% by weight or more and 98% by weight or less.

The Cl content of such fine particles is preferably at least 10 mol%, more preferably at least 50 mol%.
0 mol% or less is preferable.

As a dispersion medium for nucleation, ripening and growth, conventionally known dispersion mediums for AgX emulsions can be used. In particular, the methionine content is preferably from 0 to 80 μmol / g, and more preferably from 0 to 80 μmol / g. ５０50 μmol / g of gelatin can be preferably used. When such gelatin is used during ripening and growth, thinner tabular grains having a uniform diameter size distribution are formed, which is preferable. Also, Japanese Patent Publication No. 52-16365, Journal of the Photographic Society of Japan, 29 (1), 17, 22 (1966), 30 (1),
10, 19 (1967), Vol. 30 (2), 17 (1
967), 33 (3), 24 (1967) can be preferably used as a dispersion medium. The pH at the time of growth by adding fine particles needs to be 2.0 or more, but is preferably 3 or more and 10 or less. More preferably, the pH is 4 or more and 9 or less.

Further, pCl needs to be 1.0 or more, and preferably 1.0 or more. More preferably, it is 1.5 or more and 3.0 or less.

These growth conditions are particularly preferable for tabular grains having a {100} plane as a main plane.

Here, pCl is defined as pCl = -log [Cl-] with respect to the activity [Cl-] of Cl ions in the solution. Written by THJames THE THEORY OF THE RHOTO
This is described in detail in GRAPHIC PROCESS, 4th edition, Chapter 1.

When the pH is less than 2.0, for example, in the case of tabular grains having a {100} plane as a main plane, the lateral growth is suppressed, the aspect ratio is reduced, and the covering power of the emulsion is reduced. Tends to be low and the sensitivity is lowered. When the pH is 2.0 or more, an emulsion having a high lateral growth rate and a high aspect ratio and a high covering power can be obtained, but fog is high and sensitivity is easily reduced. On the other hand, when pCl is less than 1.0, the growth in the vertical direction is promoted, the aspect ratio is reduced, the covering power of the emulsion is low, and the sensitivity is lowered. pCl is 1.
If the ratio is 6 or more, the aspect ratio is increased to increase the covering power, but the fog is high and the sensitivity is easily reduced. At this time, when the substrate grains are grown with silver halide fine grains, the pH becomes 2.0 or more, furthermore, 6 or more and / or p
Even when Cl is 1.6 or more, fog is low, high sensitivity, high aspect ratio, and high covering power are obtained.

With respect to the monodispersity of the emulsion of the present invention, the monodispersity is preferably 30% or less, more preferably 5% or more, based on the coefficient of variation defined by the method described in JP-A-59-745481. It is preferably at most 25%. In particular, when used for a high-sensitivity photosensitive material, the content is preferably 5% or more and 15% or less.

Next, a particularly preferred embodiment of the present invention is a tabular emulsion having a {100} principal plane helical transition.

The nucleus of the grain of the present invention exists within a square of 0.001% or more and 10% or less, more preferably 0.001% or more and 7% or less of the total projected area including one corner. Is preferred. The corners of such tabular grains refer to the portions where the side surfaces of the {100} tabs intersect. Therefore, such tabular grains usually have four corners.

The nucleus portion of such tabular grains extends from the portion having no anisotropic growth to the portion where the anisotropy grows for the first time due to a halogen gap and / or impurities due to different types of halogen. Say. Anisotropic growth is often imparted due to the introduction of dislocations or the like into grains. The nucleus is a direct image low temperature transmission electron micrograph image
The lattice distortion is observed by “direct TEM image”, and the location can often be confirmed. In addition, the nucleus is I ^-
And / or Br ^- against added silver amount of different halide such as, preferably 5 mol% or more 0.01 mole% or less, more than preferably 0.05 mol% to 3 mol% or less, more preferably 0.1 mol % Or more and 1 mol% or less, by adding a growth history and directly observing a TEM image or, in the case of I ⁻ , low-temperature emission [for example, Journal of Imagi
ng Science, vol. 31, 15-26 (1987)] can be referred to indirectly to confirm the location of the nucleus, even if lattice distortion of the nucleus is not directly observed in the TEM image. good. In many cases, the core of the particles of the present invention has a different composition from a portion other than the core, but it is not always necessary that the composition be different. However, also in this case, it is necessary to confirm the location of the nucleus by putting the growth history into the nucleus.

Such a tabular grain preferably has two dislocation lines extending from the nucleus when observed from a direction perpendicular to the main plane in a direct TEM image. Such a dislocation line is preferably such that the projected area of the growing tabular grains is kept up to 20% of the projected area of the finished grains,
More preferably, it is held up to 50%, and 99%
It is particularly preferable that the temperature is maintained up to the maximum. In addition, dislocation lines often extend directly from the nucleus at the time of nucleation, but even if a part of the dislocation line is lost, if the extension of the dislocation line reaches the nucleus at the time of nucleation, the present invention It is a particle of a preferred embodiment.

The angle between such dislocation lines is
5 ° or more when observed from a direction perpendicular to the main plane 8
It is characterized by being at most 5%, preferably at least 30 ° and at most 75 °, more preferably at least 45 ° and at most 75 °. Dislocation lines are often introduced in the (31n) direction when the side surfaces of tabular grains are {100}.

In order to form particles having such a structure, it is preferable that dislocation lines introduced during nucleation do not disappear. For {100} tabular grains, it is observed that dislocation lines introduced during nucleation disappear during grain formation, for example, during physical ripening and grain growth, and the grains become thicker. For this reason, ripening is performed, for example, in the presence of fine particles, and dislocation lines due to dissolution of each corner of tabular grains must not be lost, and growth must be performed from the state where dislocation lines remain. No. Furthermore, in order for the dislocation lines to exist stably, the introduced dislocation lines need to be pinned. For this purpose, the growth is preferably carried out not by a single halogen composition but by a different halogen, preferably 0.1 mol% or more.
A method using a mixed halogen containing 5 mol% or less, more preferably 0.5 mol% or more and 10 mol% or less, particularly preferably 0.7 mol or more and 7 mol% or less, and impurities such as yellow blood salts are preferably 0.1 mol% or less. A method of growing with a halogen solution having a single halogen composition containing 1 mol% or more and 20 mol% or less, more preferably 0.2 mol% or more and 10 mol% or less, and lowering the growth temperature so that pinning of dislocation lines is hard to be removed. , Preferably 30 ° C or higher and 75 ° C or lower, more preferably 35 ° C
There is a method of growing at a temperature of 65 ° C. or less, and any one of the methods may be used or used in combination. by the way,
In order to grow while maintaining the anisotropic growth, low supersaturation addition of the Ag ⁺ salt solution and the X ^- salt solution may be performed.

An example of the direct TEM method is shown below.

1. Sample preparation The emulsion during and / or after grain formation was added to a methanol solution of phenylmercaptotetrazole (1 × 10 ⁻³ to 1 × 10 ⁻² mol / mol Ag) so as not to deform the grains. Thereafter, the particles were taken out by centrifugation, dropped onto a sample support for electron microscopy observation (mesh) to which a carbon support film had been previously attached, and dried to obtain a sample.

2. Observation of particles The prepared sample was subjected to an electron microscope JEM-20 manufactured by JEOL Ltd.
00FXII, acceleration voltage 200kV, magnification 5000x ~
50000 times, sample cooling holder gatan 626
Observation temperature using -300 Cryostation-
Observation was performed at 120 ° C. For particles for which dislocation lines could not be observed, the sample was tilted and observed to confirm the presence or absence of dislocations.

Most of the dislocation lines observed extend from the nucleus to the edge. However, some dislocation lines are observed only partially, which is also a preferred embodiment of the present invention.

The nucleation of the tabular grains of the present invention is caused by the introduction of dislocations into the grains due to halogen gaps or impurities, but is finally obtained when more than three dislocations are introduced into the grains. As the particles, thick particles having a low aspect ratio and promoted in the x, y, and z axes are generated. Here, the x and y axes are parallel to and orthogonal to the main plane, and the z axis is perpendicular to the main plane. Therefore, the amount of dislocation formation may be controlled so that the generation frequency of thick grains is low and the generation frequency of tabular grains increases. In order to control this, appropriate values can be selected by trial and error for the halogen species and the amount of addition for forming dislocations and the impurity species and the amount of addition. Further, the addition of the halogen used for aging and the stop of the introduction of the rearrangement of the present invention, the type of the halogen, and the amount of addition can be appropriately selected by trial and error.

An embodiment in which colloidal silica is contained in the photosensitive silver halide emulsion layer of the silver halide photographic light-sensitive material according to the present invention is preferred.

The colloidal silica preferably has an average particle size of 0.1 μm or less, and preferably has a mean particle size of 0.005 to 0.08 μm.
Is particularly preferred.

The main component of the colloidal silica is made of silicon dioxide, and may contain an aluminate as a minor component. Examples of the aluminate include sodium aluminate and potassium aluminate.

These colloidal silicas may contain, as a stabilizer, inorganic salts such as sodium hydroxide, potassium hydroxide, lithium hydroxide and ammonium hydroxide, and organic salts such as tetramethylammonium ion.

Specific examples of colloidal silica include, for example,
Ludox AM, from EIDu Pont de Nemouvs & Co (USA)
Ludox AS, Ludox LS, Ludox TM, Ludox HS, etc., Snowtex 20 and Snowtex 3 from Nissan Chemical Industries, Ltd.
Syton C-30, SytonZOO from Mons anto Co (USA) with trade names such as 0, Snowtex C and Snowtex O
Nalco Chem Co from Nalcoag-1060
, Nalcoag-ID 21-64 and the like, which are readily available.

[0091] The amount of the colloidal silica to be added to the emulsion according to the present invention may be a 0.05 to 1.5 g / m ^2, more preferably from 0.1 to 1.0 g / m ^2. At the time of addition, those appropriately diluted with water or a hydrophilic solvent may be added, and the timing of addition to the emulsion is not particularly limited, but it is preferable to add it to any step after completion of chemical ripening and before coating. .

In the silver halide photographic light-sensitive material, the amount of silver halide used is not particularly limited, but is preferably 5.0 g / m ² or less and 1.0 g / m ² or more per one side in terms of silver. Furthermore, 3.5 g / m ² or less 1.0 g /
It is preferably at least m ² .

Although the amount of silver relative to the gelatin binder is not particularly limited, it is preferable to use silver in a ratio of 0.01 to 5.0 in terms of silver amount (weight) / gelatin (weight) depending on the purpose. .

When the silver halide photographic light-sensitive material has a plurality of silver halide emulsion layers, the plurality of silver halide emulsion layers may be provided on one side of the support. It may be provided.

In the light-sensitive material of the present invention, for the purpose of further sharpening an image, in addition to the above-mentioned cross-over cut layer of the present invention, if necessary, another cross-over cut layer may be further provided with a light-sensitive emulsion layer and a support. May be provided between them. A dye corresponding to the photosensitive wavelength range is added to such a crossover cut layer. Any dye can be used as long as it does not leave harmful absorption after the development processing. A method of adding a dye in a state of solid fine particles is disclosed in
64936, JP-A-3-210553, JP-A-3-210
No. 210554, Japanese Unexamined Patent Application Publication No.
-14038, JP-A-4-14039, JP-A-4-14039
125635, JP-A-4-338747, JP-A-6
-27589 and the like. Dyes which can be used include, for example, dyes of the general formulas (I) to (VII) described in JP-A No. 4-212542, and examples of compounds I-1 to I-37 and I-37.
I-1 to II-6, III-1 to III-36, IV-1 to IV-1
6, V-1 to V-6, VI-1 to VI-13, VII-1 to VII
-5. Dyes of the general formula (1) described in JP-A-8-73767, Compound examples 1 to 6. Dyes of general formulas (VIII) to (XII) described in JP-A-8-87091, examples of compounds VIII-1 to VII
I-5, IX-1 to IX-10, X-1 to X-21, XI-1
XI-6, XII-1 to XII-7.

In addition to these, a method of adsorbing a known dye to a mordant, a method of dissolving a known dye in oil and emulsifying and dispersing it in oil droplets, and a method of adsorbing a dye described in JP-A-3-5748 on an inorganic material surface For example, a method described in JP-A-2-298939, in which a dye is adsorbed on a polymer, can be used.

The method for introducing the crossover cut layer into the photographic material, including that of the present invention, can be the one described in each specification.

The crossover cut layer is a dye layer,
It is also called an undercoat layer or the like.

The present invention relates to black-and-white silver halide photographic materials such as printing photographic materials, microfilm photographic materials, medical X-ray photographic materials, industrial X-ray photographic materials, general negative photographic materials, general reversal photographic materials and the like. It can be applied to general color negative photosensitive materials and general color reversal photosensitive materials. Preferably, it is a medical X-ray photosensitive material. There are no particular restrictions on the various additives and the like used in the photographic light-sensitive material of the present invention.

Item: This section 1) Silver halide emulsion and its production method from the lower right column on page 8 of JP-A-2-68539, from line 6 to the upper right column on page 10, page 12, upper right column, line 3 JP-A-24537, page 2, lower right column, line 10 to page 6, upper right column, line 1, page 10, upper left column, line 16 to page 11, lower left column, line 19, JP-A-4-10742. . 2) Chemical sensitization method JP-A-2-68539, page 10, upper right column, line 13 to upper left column, line 16, JP-A-5-313282. 3) Antifoggants, JP-A-2-68539, page 10, lower left column, 17 stabilizer, line 11 to page 11, upper left column, line 7 and page 3, lower left column, line 2, page 4 lower left column. . 4) Color tone improver JP-A-62-276439, page 2, lower left column, line 7 to page 10, lower left column, line 20; JP-A-3-94249, page 6, lower left column, line 15 to line 1 19th line, top right column on page 1. 5) Spectral sensitizing dyes JP-A-2-68539, page 4, lower right column, line 4 to page 8, lower right column. 6) Surfactant, JP-A-2-68539, page 11, upper left column, line 14 antistatic agent, line 12 to page 12, upper left column, line 9; 7) Matting agents, slip agents, JP-A-2-68539, page 12, upper left column, 10 plasticizers, from line 10 to line 10, right upper column, page 14, line 10, lower left column to line 1, lower right column, line 14 . 8) Hydrophilic colloid From page 11, upper right column, line 11 to lower left column, line 16 of JP-A-2-68539. 9) Hardener From page 17, lower left column, line 17 to page 13, upper right column, line 6 of JP-A-2-68539. 10) Support: JP-A-2-68539, page 13, upper right column, lines 7 to 20. 11) Crossover Japanese Patent Laid-Open No. 2-264944, page 4, upper right column, 20 cut method From the line, page 14 upper right column. 12) Dyes and mordants JP-A-2-68539, page 13, lower left column, line 1 to page 14, lower left column, line 9. No. 3-24537, page 14, lower left column to page 16, lower right column. 13) Polyhydroxyl JP-A-3-39948, from page 11, upper left column to benzenes, page 12, lower left column, EP Patent No. 452772A. 14) Layer structure JP-A-3-198041. 15) Developing method JP-A-2-103737, page 16, upper right column, line 7 to page 19, lower left column, line 15 and JP-A-2-15837, page 3, lower right column, line 5 10th line in the upper right column on page 6.

In the light-sensitive material of the present invention, it is preferable to use an intensifying screen at the time of exposure, but it is particularly preferable to use HGM and HGH orthoscreen manufactured by Fuji Photo Film Co., Ltd. Details of such an intensifying screen are described in JP-A-6-67365 and JP-A-6-67366.

The total processing time of the light-sensitive material of the present invention is preferably 90 seconds or less, more preferably 5 to 70 seconds.
In this case, the developing time is 4 to 30 seconds, and the fixing time is 4 to 30 seconds.
The second and the washing time are preferably 5 to 30 seconds.

The replenisher amount of the developing solution is 30 to 650 ml per 1 m ^{2 of the} light-sensitive material (2.3 to 50 ml per 4 pieces).
Replenisher amount of fixer sensitive material 1 m ² per 30~650ml (4
It is preferably 2.3 to 50 ml per cut, and the replenishing amount of the washing solution is 30 to 50 per m ^{2 of the} light-sensitive material.
It is preferably 000 ml (2.3-3900 ml per 4 slices). Further, the waste liquid of the washing liquid can be used as a diluting liquid of the fixing replenisher.

Although the amount of waste liquid corresponds to the amount of replenisher, in the present invention, the amount of waste fixer can be reduced to preferably 12 ml or less per four slices (10 inches × 12 inches). .

[0105]

Next, the present invention will be described in more detail by way of examples, but embodiments of the present invention are not limited thereto.

Example 1 Preparation of Ultrafine Particles Adsorbed with Dye of the Present Invention (1) Preparation of Fine Particle Emulsion Preparation of Fine Particle Emulsion (1-1) The mixing container used in this example is a cylindrical closed container having an inner volume of 8 ml. In addition, it has a stirring blade above and below it that can rotate at high speed in opposite directions.

A 0.5N aqueous solution of silver nitrate and a 0.5N aqueous solution of sodium chloride were respectively added to such a mixing vessel.
Added at 5 ml / min and 30 ml / min, and simultaneously the following benzimidazolocarbocyanine dyes (Exemplary Compound I-15)
Aqueous solution of a protonated product (0.002 mol / l, pH
5) and an aqueous solution of sodium hydroxide at a concentration sufficient to completely neutralize the mixture were added at 200 ml / min. A low molecular weight gelatin having an average molecular weight of 30,000 or less is used as a protective colloid in the aqueous solution of the dye protonated product.
It dissolves and contains 15 g per 0 ml.

[0108]

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The above solution was vigorously stirred in the mixing vessel at a stirring rotation speed of 2,000 rpm and rapidly and uniformly mixed to obtain an emulsion of silver halide fine particles having a dye adsorbed on the surface. After keeping such an emulsion in the mixing container for about 1 second, it is immediately discharged out of the container and introduced as it is into an ultrafiltration membrane to remove excess water-soluble salts and to prepare a coating solution. Concentration. By redispersing the concentrated emulsion in water, the resulting emulsion 100
A silver halide fine grain emulsion having a silver amount of 45 g per 0 g was obtained. The average size of the fine particles was 0.018 μm.

Preparation of Fine Grain Emulsion (1-2) In the same mixing vessel used for the preparation of the fine grain emulsion (1-1), the stirring speed was set to 2,000 rpm, and a 0.1N aqueous silver nitrate solution and a 0.1M aqueous solution were added. A 1N aqueous solution of sodium chloride was added at 125 ml / min and 150 ml / min, respectively. Such an aqueous sodium chloride solution contains, as a protective colloid, a low-molecular-weight gelatin having an average molecular weight of 30,000 or less dissolved at a rate of 25 g per 1,000 ml of the aqueous solution. The emulsion stays in the mixing container for about 2 seconds and is immediately discharged out of the container, and the following dye (Exemplified Compound I-
20) in a methanol solution. The concentration of such a dye in a methanol solution is 0.0015 mol / l,
The volume was 3000 ml and the emulsion was continued to be added thereto for 10 minutes.

[0111]

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In the methanol solution, the dye was adsorbed on the surface of the silver halide fine particles, and the emulsion precipitated due to the aggregation of gelatin. After allowing the emulsion to settle completely, the supernatant was decanted to remove excess water-soluble salts and concentrated. By re-dispersing the concentrated emulsion in water, a silver halide fine grain emulsion having a silver amount of 45 g per 1000 g of emulsion was obtained as a result. The average size of the fine particles was 0.020 μm.

Preparation of Fine Particle Emulsion (1-3) A stirring device similar to that used in the preparation of the fine particle emulsion (1-1), except that an internal volume of 2 ml was used, and the stirring rotation speed was set to 2000 rpm. . To this, a 0.5N silver nitrate aqueous solution and a 0.5N sodium chloride aqueous solution were added at 25 ml / min and 30 ml / min, respectively, and at the same time, a protective colloid aqueous solution was added at 50 ml / min. This aqueous sodium chloride solution contains 0.02 mol of a solution of the following benzimidazolocarbocyanine dye (exemplified compound I-21) in a ratio of 0.02 mol per 1000 ml. It contains 20,000 PVA (polyvinyl alcohol) having a saponification degree of 98% dissolved at a ratio of 50 g per 1000 ml of the solution.

[0114]

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After the emulsion has been retained in the mixing container for about 1 second, it is immediately discharged out of the container, and the second
Was introduced into the stirring device. A 0.1 N aqueous solution of potassium iodide was added thereto at a rate of 25 ml / min. After the emulsion was retained in the second mixing vessel for about 1 second, it was immediately discharged out of the vessel and introduced into an ultrafiltration membrane to remove excess water-soluble salts and concentrate the emulsion. By redispersing the emulsion in water, a silver halide fine grain emulsion having a silver amount of 45 g per 1000 g of emulsion was obtained as a result. The average size of the fine particles was 0.015 μm.

Preparation of fine grain emulsion (1-4) A fine grain emulsion was prepared in the same manner as in the fine grain emulsion (1-2). However, the aqueous halogen solution was a mixture of potassium bromide and potassium iodide, and the prepared fine particles had a halogen composition of silver iodobromide with a silver bromide / silver iodide molar ratio of 95/5. The dye methanol solution to which the emulsion was added after the preparation was a methanol solution of the following dye. The particle size was 0.160 μm.

[0117]

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Preparation of fine grain emulsion (1-5) A fine grain emulsion was prepared in the same manner as in the fine grain emulsion (1-4). However, the aqueous halogen solution is an aqueous potassium bromide solution, and the dye methanol solution to which the emulsion is added after preparation is
A methanol solution of the following dye was prepared. The average size of the fine particles was 0.100 μm.

[0119]

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Emulsion A of the Present Invention: Preparation of High Silver Chloride Tabular Grain Emulsion with {100} as the Main Plane (hereinafter simply referred to as {100}) In a reaction vessel, 1582 ml of an aqueous gelatin solution (gelatin-1) was added.
(19.5 g of deionized alkali-treated bone gelatin having a methionine content of about 40 μmol / g), HNO ₃ IN solution 7.
An aqueous solution containing 8 ml. pH 4.3), 13 ml of NaCl-1 solution (containing 10 g of NaCl in 100 ml of water)
While maintaining the temperature at 40 ° C., the Ag-1 solution (containing 20 g of AgNO _{3 in} 100 ml of water) and the X-1 solution (containing 7.05 g of NaCl in 100 ml of water) at a rate of 62.4 ml / min.
5.6 ml were added simultaneously. After stirring for 3 minutes, A
liquid g-2 (containing 2 g of AgNO _{3 in} 100 ml of water) and X
2 liquid (1.4 g of KBr in 100 ml of water)
28.2 ml were mixed simultaneously at 0.6 ml / min. After stirring for 3 minutes, Ag-1 solution and X-1 solution were added at 62.4 ml / min.
6.8 ml were added simultaneously. After stirring for 2 minutes, 203 ml of an aqueous gelatin solution (13 g of gelatin-1, 13 g of NaC
1.3 g, an aqueous solution containing 1N NaOH solution to adjust the pH to 6.5) to adjust the pCl to 1.75, raise the temperature to 63 ° C., and then add aqueous hydrogen peroxide to 1 g of gelatin. 6 × 10 ^-4 mol was added, the pCl was adjusted to 1.70, and the mixture was aged for 3 minutes. Thereafter, the AgCl fine particle emulsion (E-1) (average particle diameter: 0.1 μm) was
It was added at a rate of 2.68 × 10 ⁻² mol / min for 20 minutes. After aging for 40 minutes after completion of the addition, the following precipitant-1 was added, the temperature was lowered to 35 ° C, and the precipitate was washed by settling. An aqueous alkali-treated gelatin solution was added, and the pH was adjusted to 6.0 at 60 ° C. A TEM image of a replica of the obtained particles was observed. The resulting grains were silver chlorobromide {100} tabular grains containing 0.44 mol% of AgBr based on silver.

[0121]

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The shape characteristic value of the obtained grains was (the total projected area of {100} tabular grains having an aspect ratio of 2 to 30 / the sum of the projected areas of all silver halide grains) × 1.
00 = a1 = 95% (average aspect ratio (average diameter / average thickness) of {100} tabular grains having an aspect ratio of 2 or more and 30 or less) = a2 =
15.5 (Average projected area diameter of {100} tabular grains having an aspect ratio of 2 to 30) = a3 = 1.40 μm (principal edge length ratio of {100} tabular grains having an aspect ratio of 2 to 30) = A4 = 0.90 (average thickness of {100} tabular grains having an aspect ratio of 2 to 30) = a5 = 0.09 μm (average thickness of {100} tabular grains having an aspect ratio of 2 to 30) Coefficient of variation (standard deviation of thickness / average thickness) =
a6 = 0.11 (Two dislocation lines extending from the corners of the {100} tabular grains having an aspect ratio of 2 or more and 30 or less are the projected area sum of the grains / aspect ratio 2 that can be observed with a transmission electron microscope. (Projected area sum of {100} tabular grains of 30 or less) × 100 = a7 = 87% (average angle of angles formed by two dislocation lines) = a8 = 56 °

When the tabular grains were observed with a direct TEM image, the dislocation lines could be observed in grains having a projected area of 57% even in the emulsion after coating.

Emulsion B of the Invention: Preparation of {111} AgBr Tabular Grains 6.0 g of potassium bromide and 7.0 g of low molecular weight gelatin having a weight average molecular weight of 15,000 were added to 1 liter of water.
37 ml of silver nitrate aqueous solution while stirring into a container maintained at ℃
38 ml of an aqueous solution containing 4.00 g of silver nitrate and 5.9 g of potassium bromide was added over 37 seconds by the double jet method. Then, after adding 18.6 g of gelatin, the temperature was raised to 70 ° C., and 89 ml of an aqueous silver nitrate solution (9.80 g of silver nitrate) was added.
Added over 2 minutes. Here, 7 ml of a 25% aqueous ammonia solution was added, the mixture was physically aged at the same temperature for 10 minutes, and then 6.5 ml of a 100% aqueous acetic acid solution was added. Subsequently, 435 ml of an aqueous solution of 153 g of silver nitrate and 5 parts of potassium bromide were added.
73 g of an aqueous solution (677 ml) was added by a control double jet method over 35 minutes while maintaining the pAg at 8.5 until the entire amount of silver nitrate aqueous solution was added. Next, 15 ml of a 2N potassium thiocyanate solution was added. After physical ripening at the same temperature for 5 minutes, the temperature was lowered to 35 ° C. a1 =
95%, a2 = 12.0, a3 = 1.20 μm, a5 =
Monodispersed pure silver bromide {111} tabular grains having a diameter of 0.10 μm and a variation coefficient of projected area diameter of 15.5% were obtained.

Thereafter, soluble salts were removed by a sedimentation method. The temperature was raised again to 40 ° C. and 30 g of deionized and alkali-treated gelatin, 2.35 g of phenoxyethanol and 0.8 g of sodium polystyrene sulfonate as a thickener.
And pH 5.90 with caustic soda and silver nitrate solution, p
Ag was adjusted to 8.00.

Emulsion C of the present invention: high Br content {100} plate particles An aqueous gelatin solution [1.2 liters of H ₂ O,
Contains 25g of gelatin, 0.11g of NaCl, HNO
_The pH was adjusted to 3.9 with ₃ solutions], and while keeping the temperature at 40 ° C., stirring, 8.0 ml of AgNO ₃ -1 solution (AgNO ₃ 10 g / l) was added in 2 seconds. After 5 minutes, X-1 solution (KBr 140 g / liter solution) and Ag-2 solution (Ag
NO _{3 (} 200 g / liter solution) was added at about 50 ml / min for about 1 minute. However, the start of the addition of the X-1 solution was made to precede the start of the addition of the Ag-2 solution by one second.
One minute after the completion of the addition, a NaOH solution was added to adjust the pH to 5.5. Further, an aqueous polyvinyl alcohol solution [the average degree of polymerization of vinyl acetate is 500, and the average saponification rate to alcohol is 9
5 g of 8% polyvinyl alcohol, 50 ml of H ₂ O]
And the following polyvinyl imidazole copolymer (weight average molecular weight 1.5 × 10 ⁵ , x: y: z: w = 60: 7: 1)
3:30) aqueous solution (10 g of copolymer, 10 g of H ₂ O)
0 ml) was added to bring the silver potential to 50 mV and the temperature was raised to 75 ° C. After the temperature was raised, the silver potential was readjusted to 50 mV. 3
After aging for 0 minutes, the Ag-3 solution (AgNO ₃ 100 g /
Liter) and X-2 solution (KBr 71 g / liter) while maintaining the silver potential at 50 mV, Ag-3 solution was added for 30 minutes at an initial speed of 5 ml / min and a linear flow rate acceleration of 0.05 ml / min. After 3 minutes, a sedimentation agent was added, and the temperature was lowered to 30 ° C.
H.sub.4.0 and the emulsion was allowed to settle. Wash the sedimented emulsion with water,
The temperature was raised to 38 ° C., a gelatin solution was added, and the emulsion was redispersed. Observation of a TEM image (transmission electron micrograph image) of a replica of the obtained emulsion particles revealed the following. According to this, 92% of the total projected area of all AgX has a {100} principal plane, and the projected outline shape is a shape in which one or two of the four corners of a right-angled parallelogram are missing, and the average corner is missing. The rate was about 10% of the edge length. The edge face with no corner was a {110} face. The average diameter was 1.4 μm, the average aspect ratio was 10.0, and the variation coefficient of the diameter distribution (standard deviation of distribution / average diameter) was 0.21. The ratio of the projected area of tabular grains having an Aspex of 2 to 30 to the projected area of all silver halide grains is 9%.
5%.

[0127]

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Chemical sensitization Each particle prepared as described above was subjected to chemical sensitization while being kept at 56 ° C. while stirring. First, thiosulfonic acid compound-1 was added in an amount of 1 × 10 ⁻⁴ mol per mol of silver halide, and then AgBr fine particles having an average grain diameter of 0.10 μm were added in an amount of 1.0 mol% based on the total silver. After 1 minute, a 1% by weight KI solution was added to 1 × 10 ⁻³ per mole of silver halide.
After 3 minutes, thiourea dioxide was added to 1 × 10
^-6 mol / mol Ag was added, and the mixture was kept as it was for 22 minutes to perform reduction sensitization. Next, 4-hydroxy-6-methyl-
1,3,3a, 7-Tetraazaindene was added in an amount of 3 × 10 ⁻⁴ mol / mol Ag and the following sensitizing dyes 1, 2, and 3 in the following amounts. Further, 1 × 10 ⁻² mol / mol Ag was added to calcium chloride. Furthermore, chloroauric acid 1 × 10 ^-5 mol /
Mol Ag and potassium thiocyanate 3.0 × 10 ⁻³ mol / mol Ag were added, followed by sodium thiosulfate (6 × 10 ⁻⁶ mol / mol Ag) and selenium compound-1.
(4 × 10 ⁻⁶ mol / mol Ag) was added. After a further 3 minutes, the nucleic acid (0.5 g / mol Ag) was added. After 40 minutes, water-soluble mercapto compound-1 was added, and the mixture was cooled to 35 ° C.

Thus, the preparation of the emulsion (chemical ripening) was completed.

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(Preparation of Coating Solution for Emulsion Layer) The following chemicals were added to the above chemically sensitized emulsion per mole of silver halide to prepare an emulsion coating solution. Each emulsion was separately coated as shown in Table 2.

Gelatin (including gelatin in emulsion) 50.0 g Dextran (average molecular weight 39,000) 10.0 g Sodium polyacrylate (average molecular weight 400,000) 5.1 g Sodium polystyrene sulfonate ( 1.2 g-Potassium iodide 78 mg-Hardener 1,2-bis (vinylsulfonylacetamido) ethane (adjusted amount so that swelling ratio is 90%)-Compound A-1 42.1 mg Compound A-2 10.3 g Compound A-3 0.11 g Compound A-4 8.5 mg Compound A-5 0.43 g Compound A-6 0.04 g Compound A-7 70 g Dye emulsion a (as dye solids) 0.50 g Dye emulsion m (as dye solids) 30 mg Dye emulsion m (as dye solids) 30 mg Colloidal silica (average particle size) 0.02 μm) 2.5 g (adjusted to 6.1 with NaOH)

The compounds A-1 to A-
7 is as shown below, and the dye emulsions a and m were prepared as follows.

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(Preparation of Dye Emulsion a)
0 g and 62.8 g of 2,4-diamylphenol,
62.8 g of dicyclohexyl phthalate and 333 g of ethyl acetate were dissolved at 60 ° C. Next, 65 ml of a 5% by weight aqueous solution of sodium dodecylbenzenesulfonate, 94 g of gelatin and 581 ml of water were added and emulsified and dispersed at 60 ° C. for 30 minutes with a dissolver. Then, 2 g of methyl p-hydroxybenzoate and 6 liters of water were added, and 40
The temperature was lowered to ° C. Next, using an ultrafiltration laboratory module ACP1050 manufactured by Asahi Kasei, the mixture was concentrated until the total amount became 2 kg, and 1 g of methyl p-hydroxybenzoate was added to obtain a dye emulsion a.

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(Preparation of Dye Emulsion m)
0 g was weighed, dissolved in a solvent consisting of 10 ml of tricresyl phosphate and 20 ml of ethyl acetate, and then emulsified and dispersed in 100 ml of a 15% by weight aqueous gelatin solution containing 750 mg of anionic surfactant-1 to obtain a dye emulsion. m
Was prepared.

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(Preparation of Dye Layer Coating Solution) A coating solution was prepared so that each component of the dye layer had the following coating amount.

Gelatin 0.25 g / m ² Compound A-8 1.4 mg / m ² Sodium polystyrene sulfonate (average molecular weight 600,000) 5.9 mg / m ² Dye dispersion i (as dye solids) 20 mg / m ² · Dye-adsorbed fine particle emulsions (1-1) to (1-5) (added as shown in Table 2. However, the coating amount is as fine particles.)

The compound A-8 described above is as shown below, and the dye dispersion i is prepared as follows.

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(Preparation of Dye Dispersion i) The following Dye-3 was treated as a wet cake without drying, and weighed to a dry solid content of 6.3 g. The following dispersion aid V is
It was treated as a 25% by weight aqueous solution, and was added so that the dry solid content was 30% by weight based on the dye solid content. Water was added to make a total amount of 63.3 g, and mixed well to form a slurry.
100 ml of beads made of zirconia having an average diameter of 0.5 mm were prepared, placed in a vessel together with the slurry, and dispersed in a disperser (1/1).
6G sand grinder mill: manufactured by Imex Co., Ltd.)
For 6 hours, and water was added so that the dye concentration became 8% by weight to obtain a dye dispersion.

The resulting dispersion was mixed so that the solid content of the dye was 5% by weight and the photographic gelatin was equal to the weight of the solid content of the dye. Add distilled water to refrigerate,
Stored in jelly form.

In this way, a dye-like dye dispersion i was obtained as a non-elutable solid fine particle dispersion dye having a light absorption maximum at 915 nm.

The average particle diameter of the solid fine particles of the dye dispersion i was 0.4 μm.

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(Preparation of Coating Solution for Surface Protective Layer) A coating solution for surface protective layer was prepared such that each component had the following coating amount.

・ Gelatin 0.780 g / m ²・ Sodium polyacrylate (average molecular weight: 400,000) 0.025 g / m ²・ Sodium polystyrene sulfonate (average molecular weight: 600,000) 0.0012 g / m ²・ Mat agent-1 (average particle size) 3.7 μm in diameter) 0.072 g / m ² · Mat agent-2 (average particle size 0.7 μm) 0.010 g / m ² · Compound A-9 0.018 g / m ² · Compound A-10 0.037 g / m ² · Compound A-11 0.0068g / m ² · compound A-12 0.0032g / m ² · compound A-13 0.0012g / m ² · compound A-14 0.0022g / m ² · compound ^{A-15 0.030 g / m 2} · Proxel (Manufactured by ICI) 0.0010 g / m ² (adjusted to pH 6.8 with NaOH)

The above matting agents-1 and 2 and compounds A-9 to A-15 are as follows.

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(Preparation of Support) (1) Preparation of Dye Dispersion B for Undercoat Layer The following Dye-4 was ball-milled by the method described in JP-A-63-197943.

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434 ml of water and Triton X200
(Registered trademark) surfactant (TX-200 (registered trademark))
791 ml of a 6.7% aqueous solution was placed in a 2 liter ball mill. 20 g of Dye-4 were added to this solution. 400 ml of zirconium oxide (ZrO ₂ ) beads (2 m
m diameter) and the contents were ground for 4 days. After this, 1
160 g of 2.5% gelatin was added. After defoaming, the ZrO ₂ beads were removed by filtration. Observation of the obtained dye dispersion showed that the particle size of the pulverized dye was 0.05
It had a wide distribution from 1.15 μm, and the average particle size was 0.37 μm. Furthermore, dye particles having a size of 0.9 μm or more were removed by centrifugation. Thus, a dye dispersion B was obtained.

(2) Preparation of Support A corona discharge was carried out on a biaxially stretched polyethylene terephthalate film having a thickness of 175 μm, and the coating amount of the first undercoating solution having the following composition was 4.9 ml / m ^2. And then dried at 185 ° C. for 1 minute to provide a first undercoat layer.

Next, a first undercoat layer was similarly provided on the opposite surface. The polyethylene terephthalate used contained Dye-1 (described above) at 0.04% by weight.

(First undercoat liquid) • Butadiene-styrene copolymer latex solution (solid content: 40%; butadiene / styrene weight ratio = 31/69) 158 ml • 2,4-dichloro-6-hydroxy-s-triazine sodium Salt 4% by weight solution 41 ml ・ Distilled water 801 ml * Latex solution contains the following compound A-16 as an emulsifying dispersant in an amount of 0.4 wt% based on the latex solids.

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(3) Application of a second undercoat layer A second undercoat layer having the following composition was coated on the first undercoat layers on both surfaces so that the coating amount would be as described below.
Apply to both sides by wire bar coder method, 15
Dried at 5 ° C.

Gelatin 100 mg / m ² Dye dispersion B (as dye solids) 50 mg / m ² Compound A-17 1.8 g / m ² Compound A-18 0.27 g / m ² Matting agent Average 2.5 g / m ^{2 of} polymethyl methacrylate having a particle size of 2.5 μm Compounds A-17 and A-18 used above are shown below.

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(Preparation of photographic material) The above dye layer, emulsion layer and surface protective layer were combined on the support prepared as described above, coated on both sides by a simultaneous extrusion method, and dried. The coated silver amount per one side was 1.4 g / m ² , and the total coated gelatin amount per one side was 1.8 g / m ² .

(Measurement of swelling ratio)
It is aged for 7 days at 0 ° C. and 60% RH. Next, this photosensitive material is immersed in distilled water at 21 ° C. for 3 minutes, and this state is frozen and fixed with liquid nitrogen. This photosensitive material is cut by a microtome so as to be perpendicular to the surface of the photosensitive material, and then freeze-dried at -90 ° C. The swelled film thickness Tw is determined by observing the processed product under a scanning electron microscope. On the other hand, the film thickness Td in a dry state is also obtained by cross-sectional observation using a scanning electron microscope. The difference between Tw and Td thus obtained is divided by Td to obtain 100.
The multiplied value was defined as a swelling ratio (unit%).

{(Tw−Td) / Td} × 100 = Swelling rate (%) In this photographic material, Tw = 3.5 μm, Tw =
6.65 μm, and the swelling ratio was 90% as described above.

(Preparation of Developing Solution) A developing solution having the following formulation and using sodium erythorbate as a developing agent was prepared.

Diethylenetriaminepentaacetic acid 8.0 g Sodium sulfite 20.0 g Sodium carbonate monohydrate 52.0 g Potassium carbonate 55.0 g Sodium erythorbate 60.0 g 4-Hydroxymethyl-4-methyl-1-phenyl-3-pyrazolidone 13.2 g 3,3'-diphenyl-3,3'-dithiopropionic acid 1.44 g diethylene glycol 50.0 g

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Add water to make 2 liters. Adjust to pH 10.1 with sodium hydroxide.

(Preparation of developer replenisher) The above developer was used as it was as a developer replenisher.

(Preparation of developing mother liquor) Two liters of the above developing solution was taken, and a starter solution having the following composition was added in an amount of 55 ml per liter of the developing solution, and a developing solution having a pH of 9.5 was used as a developing mother liquor. (Preparation of starter solution) Potassium bromide 11.1 g Acetic acid 10.8 g Water was added to make up to 55 ml.

(Preparation of concentrated fixing solution) A concentrated fixing solution having the following formulation was prepared. Water 0.5 liter Ethylenediaminetetraacetic acid dihydrate 0.05 g sodium thiosulfate 200 g sodium bisulfite 98.0 g sodium hydroxide 2.9 g Adjust the pH to 5.2 with NaOH, and add water to make 1 liter.

(Preparation of Fixing Replenisher) The concentrated fixing solution was diluted 2-fold with the first washing water waste solution and used as a fixing replenisher.

(Preparation of fixing mother liquor) 2 liters of the above concentrated fixing solution was diluted with water to 4 liters. pH was 5.4.

(Washing water replenisher) Glutaraldehyde 0.3 g Diethylene-triamine-penta-acetic-acid 0.5 g Diluted with distilled water, and adjusted to pH 4.5 with NaOH to obtain 1 liter of a finished solution. Was.

(Processing of photographic material) A modified washing tank was used for CEPROS-S manufactured by Fuji Photo Film Co., Ltd.
As a stepwise countercurrent washing, the second washing layer was supplemented with washing water.
The opening ratios of the developing tank and the fixing tank were improved to 0.02 cm ^-1 . The capacity of each washing tank is 6 liters. Drying is performed by a heat roller method (roller surface temperature 8
5 ° C.).

Using the developing mother liquor, the fixing mother liquor, and the washing water replenisher, replenishing the developing replenisher, the fixing replenisher, and the washing water replenisher with 65 ml per 1 m ^{2 of the} photosensitive material (5 ml per 4 sheets). Processed.

Process temperature Processing time Current image 35 ° C. 8 seconds Fixed 35 ° C. 7 seconds Rinse 1st 30 ° C. 5 seconds Rinse 2nd 25 ° C. 5 seconds Dry 3 seconds Total 28 seconds

(Evaluation of Residual Color) The degree of residual color of the photographic material after processing was visually evaluated according to the following criteria. ◎ No residual color. ○ Almost no residual color. △ Slight residual color. × There is residual color.

(Evaluation of Crossover) JP-A-1-17
According to the method described in No. 2828, a screen is arranged on only one side of the light-sensitive material, and the difference between the sensitivity of the emulsion layer on the screen side and the sensitivity of the emulsion layer on the opposite side of the support when exposed to X-rays is The amount of light that leaked to the opposite side was determined as crossover light (%). Table 2 shows the evaluation results.

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[Table 2]

It can be seen that the light-sensitive material of the present invention is excellent in sharpness due to little crossover light and also excellent in residual color performance. Further, the photographic performance was satisfactory and the fixing performance was also good.

Example 2 In place of the emulsion of the present invention of Example 1, JP-A-8-101
No. 473, emulsions A, B, C, D, EP 06
Example of 99944A1 Emulsions A and B, JP-A-8-690
No. 69 emulsions EmA, B, D, I, J,
K, L, MW, X, Y, European Patent 0701164A
The emulsions Em L to Y of the examples described in Example 1 were used in the light-sensitive material configuration of Example 1. However, the same spectral sensitizing dye as in Example 1 was used.

As a result, it was found that the same tendency was exhibited according to the constitution of the light-sensitive material of Example 1, and it was found that the light-sensitive material of the present invention exhibited excellent performance.

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According to the present invention, the sharpness is excellent and the residual color is small even in the rapid and low replenishment processing.

──────────────────────────────────────────────────続 き Continued on front page (51) Int.Cl. ⁶ Identification code FI G03C 5/395 G03C 5/395

Claims (5)

[Claims] 1. A silver halide photographic material having at least one photosensitive silver halide emulsion layer on a support, wherein a J-aggregate is formed as a layer closer to the support than the photosensitive silver halide emulsion layer. A layer using a dispersion of fine particles having an average size (equivalent sphere diameter) of 0.5 μm or less adsorbing a dye to be formed, and the photosensitive silver halide emulsion layer has an aspect ratio of at least 50% or more of the total projected area. Ratio 2 or more 30
A silver halide photographic light-sensitive material comprising the following tabular grains, ie, photosensitive silver halide grains. 2. Tabular grains having a silver chloride content of 50 mol%
The silver halide photographic light-sensitive material according to claim 1, which is the above tabular grains. 3. A coating amount of the fine particles, one side 1 m ² per 0.05
3. The silver halide photographic light-sensitive material according to claim 1, wherein the photographic material is not less than 0.5 g and not more than 0.5 g. 4. A dispersion of fine particles having a silver iodide content of 20%.
The silver halide photographic material according to any one of claims 1 to 3, wherein the emulsion is a fine grain emulsion of a non-light-sensitive silver halide of not more than mol%. 5. A cross-over light of 10% or less when exposed from one side using a silver halide photographic material having a photosensitive silver halide emulsion layer on both sides of a support,
5. The silver halide photographic light-sensitive material according to claim 1, wherein the processing is performed in a total processing time of 60 seconds or less, and the amount of waste fixing solution is 12 ml or less per 4 slices.