JP2001242576A - Silver halide photographic emulsion and silver halide photographic sensitive material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a silver halide photographic emulsion excellent in sensitivity and shelf life and a silver halide photographic sensitive material using the emulsion. SOLUTION: In the silver halide photographic emulsion containing a dispersion medium and silver halide grains, when the average silver iodide content of the principal plane part and side part of the top layer is represented by I1 (mol%) and I2 (moil%), respectively, plate-like silver halide grains which satisfy I1>I2 are contained by >=50% by number and the emulsion is sensitized by reduction.

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 emulsion, and more particularly, to a silver halide photographic emulsion excellent in sensitivity and storage stability and a silver halide photographic material using the same.

[0002]

2. Description of the Related Art Photographic equipment such as cameras has become increasingly popular in recent years, and opportunities for taking photographs using silver halide photographic light-sensitive materials (hereinafter, also referred to as light-sensitive materials) have been increasing. Demands for higher sensitivity and higher image quality are increasing.

One of the dominant factors for increasing the sensitivity and image quality of photosensitive materials is silver halide grains. Development of silver halide grains aiming at higher sensitivity and higher image quality is required. It has traditionally been advanced in the industry.

However, as generally practiced, the sensitivity tends to decrease as the grain size of silver halide grains is reduced in order to improve the image quality, and both high sensitivity and high image quality can be achieved. Had limitations.

In order to achieve higher sensitivity and higher image quality, techniques for improving the sensitivity / grain size ratio per silver halide grain have been studied. As one of them,
A technique using tabular silver halide grains is disclosed in
No. 111935, No. 58-111936, No. 58-1
Nos. 11937, 58-113927, 59-99
No. 433, etc. These tabular silver halide grains are octahedral, tetrahedral, or hexahedral,
Compared to the so-called normal crystal silver halide grains, the surface area increases when the volume of the silver halide grains is the same,
Therefore, many sensitizing dyes can be adsorbed on the surface of the silver halide grains, and there is an advantage that the sensitivity can be further increased.
JP-A-6-230491, JP-A-6-235988, JP-A-6-258745, JP-A-6-289516, etc. disclose a tabular halide having a higher aspect ratio (diameter ratio to silver halide grain thickness) than before. The use of silver particles has also been studied.

JP-A-63-92942 discloses a technique of providing a core having a high silver iodide content in tabular silver halide grains, and JP-A-63-163541 discloses a technique for forming a core between twin planes. A technique using tabular silver halide grains having a ratio of grain thickness to long distance of 5 or more is disclosed.
The effects on sensitivity and granularity are shown, respectively.

JP-A-63-106746 discloses a tabular silver halide grain having a substantially layered structure in a direction parallel to two opposing main planes.
No. 279237 has a layered structure separated by a plane substantially parallel to two opposite main planes, and the average silver iodide content of the outermost layer is the average silver iodide of the entire silver halide grains. A technique is described in which tabular silver halide grains at least 1 mol% higher than the content are used.

Japanese Patent Application Laid-Open No. 3-121445 discloses a silver halide grain composed of an interface layer having parallel twin planes and regions having different iodine contents from each other.
No. 305343, tabular silver halide grains having a development start point in the vicinity of the vertex are disclosed in JP-A-2-34 (1).
Silver halide grains having a (00) plane and a (111) plane are disclosed, respectively.

In addition, Japanese Patent Application Laid-Open No. 1-183644 discloses that
A technique using tabular silver halide grains, characterized in that the silver iodide distribution of silver halide containing silver iodide is completely uniform is disclosed.

Further, there is disclosed a technique for controlling carriers by metal doping, that is, a technique for improving photographic characteristics by mainly including a polyvalent metal oxide in silver halide grains.

JP-A-3-196135 and JP-A-3-189
No. 641 and the like disclose a silver halide emulsion produced in the presence of an oxidizing agent for silver and the effect on sensitivity and fog when a photosensitive material using the same is used. Further, for example, JP-A-63-220238 discloses a technique using a silver halide emulsion containing tabular silver halide grains in which the position of a dislocation line is specified. A technique using a silver halide emulsion containing tabular silver halide grains in which dislocation lines are concentrated is disclosed. Japanese Patent Publication No. 3-18695 discloses a technique using silver halide grains having a clear core / shell structure. As for the technique, Japanese Patent Publication No. 3-31245 discloses a technique relating to a silver halide grain having a core / shell three-layer structure, and each of them has been studied as a technique for increasing the sensitivity.

JP-A-6-11781 and 6-1178
No. 2, No. 6-27564, No. 6-250309, No. 6-250310, No. 6-250311, No. 6-2
Nos. 50313, 6-242527, etc., use an iodide ion-releasing compound in forming silver halide grains.
High sensitivity and improved resistance to fog and pressure.

However, these conventional techniques have a limit in achieving both high sensitivity and high image quality, and are insufficient to satisfy recent demands on photosensitive materials. Was rare.

In order to improve the photographic performance described above, it is necessary to develop a technique for controlling a photosensitive nucleus site and a halogen composition more precisely than ever, and a chemical sensitization technique adapted to the silver halide grains. Previous considerations in the industry have not adequately responded to this need.

[0015]

SUMMARY OF THE INVENTION It is an object of the present invention to provide a silver halide photographic emulsion which achieves a balance between improved sensitivity and storage stability, which cannot be achieved by the prior art, and a silver halide photographic emulsion using the same. Provided is a photosensitive material.

[0016]

The above object of the present invention has been attained by the following means.

1. A silver halide photographic emulsion comprising a dispersion medium and silver halide grains, I ₁ (mol%) the average silver iodide content of the outermost layer at the main flat portion, when the I ₂ (mol%) in the side surface portion, 5 tabular silver halide grains satisfying I ₁ > I ₂
A silver halide photographic emulsion containing 0% or more (number) and being reduction sensitized.

2. A silver halide photographic emulsion containing a dispersion medium and silver halide grains, comprising tabular silver halide grains having at least three silver halide layers of the following internal phase, intermediate phase and external phase, and reduction sensitization: A silver halide photographic emulsion characterized in that:

Internal phase: average silver iodide content of 0.5 to 30
In mole%, the silver content ratio is 5 to 85%. Intermediate phase: the average silver iodide content is 以下 or less of the internal phase, and the silver content ratio is 2 to 85%. External phase: the average silver iodide content is intermediate. 2. higher than phase, silver content ratio 5-50% A silver halide photographic emulsion comprising a dispersion medium and silver halide grains, I ₃ (mol%) in the fringe portion of the silver iodide content, when I ₄ a (mol%) at the apex, 0 ≦ I ₄ / I
_A silver halide photographic emulsion containing 50% or more (number) of tabular silver halide grains satisfying ₃ ≦ 1.0 and being reduction sensitized.

4. Halo containing dispersion medium and silver halide grains
Projection of all silver halide grains in silver halide photographic emulsion
50% or more of the area is flat with fringe dislocation lines
Silver halide grains and shells in dislocation line forming regions
(V₁) Is from 10% to the volume of silver halide grains.
50%, and the shell (V₁Flat)
Silver iodide content (A₁) Is from 4 mol% to 20 mol%
The shell (V) of the dislocation line forming region₁Outermost in)
The outermost shell (V_Two), And the outermost shell (V _Two)of
The volume ratio is 1% to 15% of the silver halide grain volume.
The outermost shell (V_Two) Average silver iodide content (A_Two)But
0 mol% to 3 mol% and reduction sensitization
And a silver halide photographic emulsion.

5. In a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains is tabular silver halide grains having dislocation lines in fringe portions, and average silver iodide. A silver halide phase (V ₅ ) separated from the silver halide phase (V ₄ ) is provided inside the grain outside the silver halide phase (V ₃ ) having the highest content, and the silver halide phase (V Assuming that the average silver iodide content of ₄ ) is A ₄ mol% and the average silver iodide content of the silver halide phase (V ₅ ) is A ₅ mol%, 0 ≦ A ₄ / A ₅ ≦ 1.0. And a reduction sensitized silver halide photographic emulsion.

6. In a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains is tabular silver halide grains having dislocation lines in fringe portions, and average silver iodide. a ₆ mol% average silver iodide content inside the silver halide phase (V ₆₎ of the halogen content is up to Kaginsho (V _3), the outside of the silver halide phase (V ₃₎ When the average silver iodide content in the silver halide phase (V ₇ ) is A ₇ mol%, 0 ≦
A silver halide photographic emulsion characterized in that A ₆ / A ₇ ≦ 1.0 and that the emulsion is reduction sensitized.

7. 7. A silver halide photographic light-sensitive material comprising the silver halide photographic emulsion according to any one of the above items 1 to 6 in at least one silver halide photographic emulsion layer on a support.

Hereinafter, the present invention will be described in detail. The dispersion medium in the present invention is a substance that can form a protective colloid, and it is preferable to use gelatin for the protective colloid.

In the present invention, when gelatin is used as the dispersion medium, lime-treated gelatin, acid-treated gelatin, ion-exchanged gelatin and the like can be used. Gelatin having an adenine content of 0.2 ppm or less described in US Pat. For details on the gelatin production method, see Arthur Weiss, "The Macromolecular Chemistry of
Gelatin "(Academic Press, 1964)
And so on.

Examples of substances that can form protective colloids other than gelatin include gelatin derivatives, graft polymers of gelatin and other polymers, proteins such as albumin and casein, hydroxyethylcellulose, carboxymethylcellulose, and cellulose sulfate. Cellulose derivatives such as sodium alginate, starch derivatives, etc., polyvinyl alcohol, polyvinyl alcohol partial acetal, poly-n-vinylpyrrolidone, polyacrylic acid, polyacrylamide, polymethacrylic acid, polyvinylimidazole, polyvinylpyrazole, etc. Examples include various types of synthetic or semi-synthetic hydrophilic high-molecular substances such as mono- or copolymers.

In the invention according to claim 1 of the present invention,
In a silver halide photographic emulsion containing a dispersion medium and silver halide grains, the silver halide photographic emulsion has an average silver iodide content of the outermost layer of the silver halide grains in the main plane portion of I ₁ (mol%), When I ₂ (mol%) is defined as I ₂ (mol%) on the side surface portion, it is characterized by containing 50% or more (number) of tabular silver halide grains satisfying I ₁ > I ₂ and being reduction sensitized.

The average silver iodide content of the outermost layer of each of the main plane portion and side surface portion of the silver halide grain according to the first aspect of the invention can be measured by the following method.

The tabular silver halide grains in the silver halide photographic emulsion are decomposed by gelatin using a proteolytic enzyme, taken out, embedded in methacrylic resin, and continuously cut into pieces having a thickness of about 50 μm with a diamond cutter. Cutting out, of these sections, those having a tomographic plane perpendicular to the two parallel principal planes of the tabular silver halide grains, including the principal plane surface on the tomographic planes of the tabular silver halide grains,
The silver halide phase having a depth of 5 mμ from the surface parallel to the main plane surface is referred to as a main plane portion, and the portion of the outermost layer of the silver halide crystal other than the main plane portion is referred to as a side surface portion. The silver iodide content of the main plane portion and the side surface portion is measured by a point analysis using the EPMA method well known in the art to narrow the spot diameter to 5 mμ or less, preferably 2 mμ or less. As for the measured values of I ₁ and I ₂ of each silver halide grain, at the main plane portion and the side surface portion, 10 or more portions are measured at equal intervals by the above-mentioned method, and the average value is used.

In the silver halide photographic emulsion according to the first aspect of the present invention, the relation between I ₁ and I ₂ is preferably I ₁ / I ₂ > 1.3, and I ₁ / I ₂ > 2. 0 is more preferable, and I ₁ / I ₂ > 2.5 is particularly preferable.
Also, I ₁ is preferably less than 30 mol%,
More preferably, it is less than mol%.

As an embodiment of the production of the silver halide photographic emulsion according to the first aspect of the present invention, tabular silver halide grains serving as a base are first prepared, and the tabular silver halide grains are first prepared. A method in which a low iodide silver halide phase is preferentially grown in the lateral direction, and then a high iodide silver halide phase is grown in the main plane direction, or conversely,
First, a high iodide silver halide phase is preferentially grown in the main plane direction, and then a method of growing a low iodide silver halide phase in the lateral direction is appropriately used. A method of forming an extremely thin silver halide layer while precisely controlling the composition by combining the conditions is considered.

In order to grow tabular silver halide grains preferentially in the lateral direction or in the major plane direction, silver ions, halide ions, or halogens growing during the growth of the silver halide grains are dissolved. It is important to select the concentration of an additive solution containing silver halide fine particles for supplying silver ions and halide ions to silver halide grains, the growth temperature, pBr, pH, gelatin concentration, and the like. The shape of the tabular base particles, the halogen composition,
It can be controlled to some extent by the combination of the (100) face / (111) face ratio of the side face and the like.

For example, the preferred pBr for growing preferentially in the lateral direction is 1.0 to 2.5, the gelatin concentration is 0.5 to 2.0%, and almost no (100) plane is observed on the lateral surface. For the formation of high aspect ratio tabular silver halide grains, the pH is more preferably 2.0 to 5.0. On the other hand, the preferred pBr for growing preferentially in the main plane direction is 2.5 to 4.5.

In order to control the thickness of the outermost layer of the silver halide crystal and the composition of the silver halide precisely and uniformly, rather than dissolving the silver halide grains, silver ions and halides are added to the growing silver halide grains rather than by the ion supply method. A method of supplying silver halide fine particles for supplying ions is suitable. The method described below can be used for preparing the silver halide fine particles. The silver halide fine particles themselves are preferably subjected to washing with a sedimentation / coagulant or the like described below, desalting operation or operation of removing unnecessary substances such as salts and ions by membrane separation. It is preferable that an operation of removing unnecessary substances such as salts and ions is performed by a membrane separation technique without using a flocculant.

When silver halide phases having different halogen compositions are separately formed in the side direction and / or the main plane direction, washing and desalting operations or operations for removing unnecessary substances such as salts and ions by membrane separation are appropriately used. By removing the remaining, excessive or unnecessary halogen ions after being used for forming one silver halide phase, it is possible to prevent the occurrence of unintended conversion in the subsequent manufacturing process, and to use the other halogen halide. When the silver phase is formed, the control of the halogen composition can be facilitated. The operation of removing unnecessary substances such as salts and ions by the water washing, desalting method or membrane separation is performed after formation of the base particles and after growth in any one of the lateral direction and / or the main plane direction, or of any composition. It is preferably performed after the formation of the silver halide layer, and particularly preferably performed each time the respective silver halide formation process is completed.

Salt by the above-mentioned water washing, desalting method or membrane separation,
For the operation of removing unnecessary substances such as ions, the method described below can be applied, but it is particularly preferable to perform the operation of removing unnecessary substances such as salts and ions by a membrane separation method without using a precipitation / coagulant.

In the production of the silver halide photographic emulsion according to the first aspect of the present invention, in order to suppress the growth of tabular silver halide grains in the main plane direction or the side direction, the above-mentioned control of the growth conditions of the silver halide grains is carried out. In addition, it is also preferable to use additives called silver halide growth control agents, crystal habit control agents or inhibitors in the art. For example, on a tabular silver halide grain, a low silver iodide-containing surface phase is first grown in the lateral direction, and thereafter, U.S. Patent Nos. 5,147,771, 5,147,772, and 5,147. 773, JP-A-6-308644, and the like. Addition of a polyalkylene oxide-related compound used at the time of nucleation for the purpose of monodispersion of the particle size of tabular silver halide grains. The above growth is suppressed, and then the growth of the high silver iodide-containing surface phase in the main plane direction is facilitated, and the development of tabular silver halide grains according to the present invention can be promoted.

When silver halide phases having different halogen compositions in the lateral direction and / or the main plane direction are separately formed, for example, a conversion method by solely adding an iodide salt or a halide salt, or a method described in, for example, −108
No. 526, No. 59-133540, No. 59-1625
No. 40 etc. can also be used.

When a silver halide phase having a different halogen composition in each of the lateral direction and / or the principal plane direction is separately formed, the difference in the crystal surface between the principal plane and the side surface is used, and the plane selection known in the art is used. Dyes having specific adsorptivity, adsorbing substances such as inhibitors, are adsorbed on a specific crystal surface of silver halide grains, and a silver halide phase having an arbitrary halogen composition is formed on the non-adsorbing surface by the method described above or below. Forming is also a preferred method.

The operations for producing silver halide phases having different halogen compositions in the various lateral directions and / or main plane directions are performed from the start of silver halide grain formation to crystal growth of silver halide grains and physical ripening. Desalting, color sensitization, and chemical sensitization can be carried out in any one or more steps as necessary until the coating liquid preparation step is completed, if necessary. The formation is preferably carried out in a step after completion of 90% or more in terms of the amount of silver, particularly preferably after the formation of the tabular silver halide grains serving as the base and before the end of color sensitization and chemical sensitization. .

According to the first aspect of the present invention, Japanese Patent Application No.
It is also preferable to use a compound having a group capable of releasing a halide ion and a group capable of releasing a halogen ion in a molecule described in No. 95347 or the like.

In the invention according to claim 2, in a silver halide photographic emulsion containing a dispersion medium and silver halide grains, the silver halide photographic emulsion comprises the following internal phase, intermediate phase,
It is characterized by containing tabular silver halide grains having a silver halide layer of at least three external phases, and being reduction sensitized.

Internal phase: average silver iodide content of 0.5 to 30
In mole%, the silver content ratio is 5 to 85%. Intermediate phase: the average silver iodide content is 以下 or less of the internal phase, and the silver content ratio is 2 to 85%. External phase: the average silver iodide content is intermediate. In the invention according to claim 2, the average silver iodide content of the internal phase is 0.5 mol% or more and 30 mol% or less, but 1 mol% or more and 25 mol% or less. %, More preferably 3 mol% or more and 20 mol% or less. The ratio of the internal phase is 5% or more and 85% or less of the silver content, but is preferably 5% or more and 60% or less, more preferably 10% or more and 50% or less. The internal phase may have a uniform silver halide composition or may be composed of a plurality of regions having different silver halide compositions. Further, a region corresponding to a so-called nucleus or a seed may be provided in a portion corresponding to the center of the particle. When the internal phase is composed of a plurality of regions as described above, the average silver iodide content of the internal phase can be determined from the relationship between the silver iodide content and the silver content ratio in those regions.

The average silver iodide content of the intermediate phase is not more than の of the above-mentioned internal phase, and specifically, from 0 mol% to 5 mol%.
Or less, more preferably 0 mol% or more and 3 mol% or less. The ratio of the intermediate phase is 2% or more and 85% of the amount of silver particles.
But not more than 5% and not more than 60%, preferably 10%
More than 40% is more preferable. The intermediate phase preferably has a uniform silver halide composition in terms of formulation.

The average silver iodide content of the external phase may be higher than the value of the intermediate phase. Specifically, it is preferably 0.5 mol% or more and 20 mol% or less, more preferably 1 mol% or more and 10 mol% or less. preferable. The ratio of the external phase is 5% or more and 50% or less of the amount of silver particles, but is preferably 10% or more and 50% or less, more preferably 20% or more and 40% or less. The external phase may have a uniform silver halide composition or may be composed of a plurality of regions having different silver halide compositions. In particular, it is preferable to have a region having a high silver iodide content locally in the external phase, and it is particularly preferable that this region is adjacent to the intermediate phase.

The local high silver iodide content region can be obtained by a method of adding an aqueous solution of silver salt and an aqueous solution of iodide by a double jet method, a method of adding an aqueous solution of iodide by a single jet method, and JP-A-6-11781. And a method using an iodide ion releasing agent as described in (1). Further, a local high iodide phase can be formed by adding a silver iodide emulsion containing fine silver iodide fine grains. The silver iodide fine grain emulsion can be easily prepared by the method described in US Pat. No. 4,672,026. The average size of the silver iodide fine particles is preferably not more than 0.06 μm, more preferably not more than 0.03 μm in terms of sphere-converted diameter.

In the invention according to claim 2, a method of adding a silver salt aqueous solution and an iodide aqueous solution by a double jet, a method of adding a silver iodide fine grain emulsion, and a method of using an iodide ion releasing agent in the above method. It is preferable to form a local high iodine phase at the same time. In this case, the ratio of the local high iodine phase is preferably 0.5% or more and 5% or less of the grain silver amount.
1% or more and 3.5% or less are more preferable.

In the invention according to claim 2, 60% or more of the total projected area of the tabular silver halide grains is preferably tabular grains having an aspect ratio of 3 or more, and the aspect ratio is 60% or more. The number of tabular grains is preferably 5 or more.

In the invention according to claim 3, the dispersion medium
In silver halide photographic emulsion containing silver halide grains
The silver halide photographic emulsion is
The silver halide content is determined by the fringe portion._Three(Mol%), I at the top_Four
(Mol%), 0 ≦ I _Four/ I_Three≦ 1.0
Contains 50% or more (number) of tabular silver halide grains;
It is characterized by being reduced sensitized.

The apex of the tabular silver halide grains in the invention according to claim 3 means the shape of the projected image when the tabular silver halide grains are viewed from a direction perpendicular to the main plane.
In the case of a polygon, it is a corner of the polygon, and in the case where the tabular silver halide grains have a rounded shape, a tangent is drawn in contact with the outer periphery and the intersection point is defined as a vertex. The silver iodide content I ₄ at the apex of each silver halide grain is determined by measuring the silver iodide content at five or more places at equal intervals at the apex of each silver halide grain and calculating the average value. Is used.

According to the third aspect of the present invention, the vertex portion is
In the projected image when the tabular silver halide grains are viewed from the direction perpendicular to the main plane, 1/10 of the projected area circle equivalent particle diameter of the tabular silver halide grains with the vertex obtained above as the center. Means a region inside the circle when a circle is drawn with a radius corresponding to.

The fringe portions of the tabular silver halide grains in the inventions according to claims 3 to 6 refer to the sides of the projected image when the tabular silver halide grains are viewed from the direction perpendicular to the main plane. On the other hand, when a parallel straight line is drawn inside at a distance corresponding to 1/20 of the projected area circle-equivalent grain size of the tabular silver halide grains, a region surrounded by the side and the parallel straight line, and The area excluding the vicinity of the vertex is referred to. Silver iodide content I in the fringe portion of each silver halide grain
₃ is at the fringe portion of each silver halide grain,
The silver iodide content is measured at five or more locations at equal intervals, and the average value is used.

In the present invention, the silver iodide content ratio in the fringe portion and near the vertex can be determined by the following method.

The silver halide grains in the silver halide photographic emulsion are taken out by gelatin decomposition with a protease enzyme and dispersed in ultrapure water. This dispersion is dropped on a mesh with a carbon support film and dried. This was set in a sample holder, and an analytical transmission electron microscope (Ana)
lytical Electron Microsco
pe), acceleration voltage 200 kV, spot diameter 10 n
At m, in order to prevent damage to the sample due to electron beam irradiation, silver halide grains are observed while cooling with liquid nitrogen, and the silver halide composition in the fringe portion and near the apex is analyzed.

In the analysis, an EDS (Energy) that separates characteristic X-rays emitted from an electron beam irradiation region by energy is used.
y Dispersive Spectroscope
y) method is used. The quantitative calculation is performed by the Standardless method using the integrated intensity of the Br-K line and the k factor input to the EDS computer.

In the present invention, 0 ≦ I ₄ / I ₃ ≦ 1.0
Is preferably 70% or more (number).

In the present invention, 0 ≦ I ₄ / I ₃ ≦ 0.8
And more preferably 0 ≦ I ₄ / I ₃ ≦ 0.6.

In the invention according to claim 3, the silver halide photographic emulsion is prepared by the method described in Japanese Patent Application Nos. 11-95347 and 9-95347.
349421 and Japanese Patent Application No. 10-152852.

According to a fourth aspect of the present invention, in a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains has a tabular shape having dislocation lines in a fringe portion. The volume ratio of the shell (V ₁ ) of the dislocation line forming region is 10% to 50% of the volume of the silver halide grain, and the average iodine of the shell (V ₁ ) of the dislocation line forming region is silver halide grains. Silver halide content (A ₁ )
From 4 mol% to 20 mol%, the outermost shell (V ₂ ) in the shell (V ₁ ) of the dislocation line forming region, and the volume ratio of the outer shell (V ₂ ) is halogen. The outermost shell (V ₂ ) has an average silver iodide content (A ₂ ) of 0 mol% to 3 mol%, and is reduction sensitized. It is characterized by the following.

According to the fifth aspect of the present invention, in a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains has a tabular shape having dislocation lines in fringe portions. A silver halide phase (V ₅ ) separated by a silver halide phase (V ₄ ) is provided outside a silver halide phase (V ₃ ) which is a silver halide grain and has a maximum average silver iodide content. When the silver halide phase (V ₄ ) has an average silver iodide content of A ₄ mol% and the silver halide phase (V ₅ ) has an average silver iodide content of A ₅ mol% 0 ≦ A ₄ / A ₅ ≦ 1.0 and reduction sensitization.

In the invention according to claim 6, in a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains has a tabular shape having dislocation lines in the fringe portion. The average silver iodide content in the silver halide phase (V ₆ ) inside the silver halide phase (V ₃ ) which is a silver halide grain and has the maximum average silver iodide content is A ₆ mol%; When the average silver iodide content in the silver halide phase (V ₇ ) outside the silver halide phase (V ₃ ) is A ₇ mol%, 0 ≦ A ₆ / A ₇ ≦ 1.0. , And reduction sensitization.

In the silver halide photographic emulsion according to claims 4 to 6, 50% or more of the projected area of all silver halide grains are tabular silver halide grains having dislocation lines in fringe portions. The tabular silver halide grains having dislocation lines in the fringe portion are preferably at least 60% of the projected area of all silver halide grains, more preferably at least 80% of the projected area of all silver halide grains. .

In claims 4 to 6 of the present invention, it is essential that dislocation lines exist in the fringe portion of the tabular silver halide grains, but it is essential that the dislocation line be located in a portion other than the fringe portion, for example,
It may also be present at a main plane portion, a vertex portion, or the like.

In the present invention, the dislocation lines are preferably introduced at a position of at least 50%, more preferably at least 60% and less than 85%, based on the total silver content of the silver halide grains. . The number of dislocation lines is preferably 10 or more per particle, more preferably 20 or more, and even more preferably 30 or more.

In the present invention, the term "silver halide grain volume" means the volume of silver halide grains at the time point when all the growth of silver halide grains in the silver halide photographic emulsion of the present invention is completed.

In the present invention, when the silver halide phase is formed by a double jet method of an aqueous solution of silver nitrate and an aqueous solution of halogen containing iodide, the average silver iodide content of the silver halide phase is determined by adding Is expressed by the ratio (mol%) of iodine ions in the aqueous halogen solution to silver ions in the aqueous silver nitrate solution, and the volume of the formed silver halide phase is newly formed by the silver ions in the added aqueous silver nitrate solution. It is the volume of silver halide.

In the present invention, the average silver iodide content of the silver halide phase means the content of silver iodide in the fine silver halide grains when silver halide fine grains containing silver iodide are added. Mol%), and the volume of the formed silver halide phase is equal to the volume of the added silver halide fine particles.

In the present invention, the average silver iodide content of the silver halide phase refers to the case where an aqueous halide solution containing iodide is added alone or the case where an iodide ion releasing compound is added and the iodide ion releasing compound is added. When iodine ions are released, the halogenation formed immediately before the addition of the aqueous halogen solution or the iodide ion releasing compound is caused by the iodine ions in the aqueous halogen solution or the iodide ions released from the iodide ion releasing compound. Assuming that 100% of the halogen conversion occurs on the surface of the silver grains, the average silver iodide content is set to 100 mol%, and the volume of the formed silver halide phase is determined by the iodine ion or the iodine ion release in the aqueous halogen solution. Equal to the volume of silver iodide formed by 100% of the iodide ions released from the compound Formation of the silver halide phase in that case,
Halogen containing the surface of silver halide grains formed immediately before the addition of the aqueous halogen solution or the iodide ion releasing compound and occupying a volume equal to the volume of the silver iodide formed inside from the surface of the silver halide grains. Let it happen in the silver halide phase.

In the present invention, the shell (V ₁ ) of the dislocation line forming region is defined as the shell (V ₁ ) of the silver halide phase formed by the growth of silver halide grains from the dislocation line introduction operation described later to the end of silver halide grain formation. That means.

The volume ratio of the shell (V ₁ ) in the dislocation line forming region is preferably from 15% to 50%, more preferably from 20% to 50% of the silver halide grain volume.

The average silver iodide content (A ₁ ) of the shell (V ₁ ) in the dislocation line forming region is preferably from 5 mol% to 17 mol%, more preferably from 6 mol% to 15 mol%. .

In the present invention, the outermost shell (V ₂ ) is the outermost silver halide contained in the shell (V ₁ ) of the dislocation line forming region and the outermost silver halide in the shell (V ₁ ) of the dislocation line forming region. Refers to a phase.

The volume ratio of the outermost shell (V ₂ ) is preferably 2% to 12% of the silver halide grain volume,
More preferably, it is 3% to 10%.

The average silver iodide content (A ₂ ) of the outermost shell (V ₂ ) is preferably 0 mol% to 2 mol%.
More preferably, it is 0 mol% to 1 mol%.

In the present invention, the term "inside of the grains" means a silver halide phase excluding the outermost layer of the silver halide grains described later in the silver halide grains.

In the silver halide photographic emulsion according to the fifth and sixth aspects, the silver halide phase (V ₄ ) is separated from the silver halide phase (V ₃ ) having the highest average silver iodide content. Silver halide phase (V ₅ ) inside the grains, the average silver iodide content of the silver halide phase (V ₄ ) is A ₄ mol%, and the average silver iodide of the silver halide phase (V ₅ ) characterized in that the content is taken as a ₅ mol% is _{0 ≦ a 4 / a 5 ≦} 1.0.

The silver halide photographic milk according to claims 5 and 6.
Agent, the silver halide phase (V _Three) Average silver iodide content
A rate_Three(Mol%), 20 ≦ A_Three≦ 100
Preferably, 40 ≦ A_Three≦ 100
More preferred.

The silver halide photographic milk according to claim 5 or 6
Agent, the silver halide phase (V _Three) But halogenated
Exists outside 60% and inside 85% by silver particle volume
Is preferably present.

In the silver halide photographic emulsion according to the _{fifth aspect} , it is preferable that 0 ≦ A ₄ / A ₅ ≦ 0.5,
More preferably, 0 ≦ A ₄ / A ₅ ≦ 0.3.

A ₄ is preferably 0 to 7 mol%, more preferably 0 to 3 mol%. A ₅ is preferably 3 to 20 mol%, and 5 to 15 mol%
Is more preferable.

In the silver halide photographic emulsion according to the fifth aspect, the difference between A ₃ and A ₄ is preferably at least 5 mol%, more preferably at least 10 mol%.

The silver halide photographic emulsion according to claim 5, wherein the silver halide phase (V ₄ ) is separated from the silver halide phase (V ₃ ) having the highest average silver iodide content. and has silver phase (V ₅₎ inside the particles, the silver halide phase (V ₃₎ silver halide phases (V ₄₎ in the silver halide phase formed after the formation of and silver halide phase (V ₅ ) is present and the silver halide phase (V ₅ ) is formed after the formation of the silver halide phase (V ₄ );
In addition, it means that the silver halide phase (V ₅ ) exists inside the grains.

In the silver halide photographic emulsion according to claim 6, the average silver iodide in the silver halide phase (V ₆ ) inside the silver halide phase (V ₃ ) having the highest average silver iodide content. When the content is A ₆ mol% and the average silver iodide content in the silver halide phase (V ₇ ) outside the silver halide phase (V ₃ ) is A ₇ mol%, 0 ≦ A ₆ / A ₇ ≦ 1.0.

In the silver halide photographic emulsion according to claim 6, it is preferable that 0 ≦ A ₆ / A ₇ ≦ 0.7,
More preferably, 0 ≦ A ₆ / A ₇ ≦ 0.5.

In the silver halide photographic emulsion according to the _{sixth aspect} , A ₆ is preferably 0 to 12 mol%, more preferably 0 to 8 mol%.
₇ is preferably 3 to 20 mol%, and 5 to 15 mol%.
More preferably, it is mol%.

In the silver halide photographic emulsion according to claim 6, the silver halide phase (V ₆ ) inside the silver halide phase (V ₃ ) is different from the silver halide phase (V ₆ ) in the growth of silver halide grains. V ₃ ) means all silver halide phases formed before the formation of the silver halide phase (V 3)
_The silver halide phase (V ₇ ) outside of ₃ ) refers to all silver halide phases formed after the formation of the silver halide phase (V ₃ ).

For the reduction sensitization in the present invention, a reduction sensitization technique known in the art can be used. More specifically, as a method of reduction sensitization, it is called silver ripening in the industry,
Low pA by supplying silver ions to silver halide grains
A method of ripening and growing with g, a method of ripening and growing by increasing the pH using an alkaline compound or the like, an optional method or a combination thereof can be used since a reducing agent is added, but a reducing agent is used. The method is preferred.

When a reducing agent is used in the present invention, examples of the reducing agent include thiourea dioxide, ascorbic acid and its derivatives, stannous salts, borane compounds, hydrazine derivatives, formamidine sulfinic acid, silane compounds, and amines. And polyamines and sulfites can be used, and these can also be used in combination.Preferably, thiourea dioxide, ascorbic acid and its derivatives, stannous salts are used, and more preferably, thiourea dioxide is used. .

The amount of the reducing agent added is preferably 10 ^-2 to 10 ^-8 mol per mol of silver halide, but is preferably 10 ^-3 to 10 ^-7.
Molar is more preferred.

The reducing agent may be a solid or a method known in the art for adding a photographic additive to a silver halide photographic emulsion, such as being dissolved in a solvent such as water, alcohols, esters and glycols. Can be added alone during the formation of silver halide grains, for example, or together with an aqueous solution containing water-soluble silver ions or halide ions or silver halide fine particles.

The addition of the reducing agent may be carried out while growing the silver halide grains, or may be carried out by temporarily interrupting the growth of the silver halide grains.

In the production of the silver halide photographic emulsion of the present invention, reduction sensitization is carried out by reducing the protective colloid aqueous solution in which silver halide grains are grown, which is referred to in the art as silver ripening.
In the case of performing the reaction under Ag conditions, it is preferable to add a silver salt to the protective colloid aqueous solution to obtain an appropriate pAg, and then ripen the silver halide grains. The silver salt is preferably a water-soluble silver salt, and particularly preferably an aqueous solution of silver nitrate.
The above pAg is preferably 7.0 or less, more preferably 2.0 to 5.0.

In the preparation of the silver halide photographic emulsion of the present invention, when the reduction sensitization is carried out under a high pH condition of an aqueous solution of protective colloid in which silver halide grains grow, the aqueous solution of protective colloid is added to the aqueous solution of protective colloid. After adding an alkaline compound to a suitable pH, it is preferable to ripen the silver halide grains.

As the alkaline compound, for example, potassium hydroxide, sodium hydroxide, ammonia and ammonium compounds can be used, but it is preferable to use compounds other than ammonia and ammonium compounds.
The pH is 7.0 or more, preferably 7.5 or more and 1 or more.
1.0 or less, more preferably 8.0 or more and 10.0 or more
It is as follows.

In the preparation of the silver halide photographic emulsion of the present invention, reduction sensitization can be carried out by adding previously prepared reduction sensitized silver halide fine grains. It is preferred to ripen after addition of reduction sensitized silver halide fine grains.

In the present invention, the temperature at which reduction sensitization is performed is 5
The temperature is preferably from 0 ° C. to 95 ° C., more preferably 55 ° C.
The temperature is from 90 ° C to 90 ° C, more preferably from 60 ° C to 90 ° C.

In the production of the silver halide photographic emulsion of the present invention, the reduction sensitization is carried out by interrupting the growth of the silver halide grains during the formation of the silver halide grains and ripening them in the above reducing atmosphere. You can also. In the present invention, the reducing atmosphere refers to an environment in which the amount of silver nuclei in the silver halide grains increases in the protective colloid aqueous solution in which the silver halide grains contained in the silver halide photographic emulsion according to the present invention are formed. And more specifically, an environment in which silver ions are converted to metallic silver. In the present invention, by using the above-described reduction sensitization technique, a reducing atmosphere can be formed when silver halide grains are formed.

In the present invention, it is also possible to use a production method in which silver halide grain growth is resumed after reduction sensitization and then the atmosphere is changed to a silver nucleic acid atmosphere.

In the present invention, the term “silver nucleic acid conversion atmosphere” means that an aqueous protective colloid solution in which silver halide grains contained in the silver halide photographic emulsion according to the present invention are formed reduces silver nuclei in the silver halide grains. It means that it is in the environment, more specifically, it is in the environment that converts metallic silver to silver ions, and the silver nucleus is converted to silver sulfide, chalcogen silver such as silver selenide, or water such as silver halide. This includes the case of forming a silver salt that is hardly soluble in water and the case of forming a water-soluble silver salt such as silver nitrate.

In the present invention, the tabular silver halide grains are silver halide grains having an aspect ratio of 2 or more. Tabular silver halide grains have an aspect ratio of 3 to 10.
0 is preferable, 5 to 100 is more preferable, and 8 to 100
Is particularly preferred.

The average aspect ratio of the tabular silver halide grains can be adjusted to the above range by a production method known in the art.

The average aspect ratio of the tabular silver halide grains is determined by measuring the grain size and grain thickness of each silver halide grain by the method described below, and obtaining the aspect ratio by the following formula. The average can be obtained for 300 or more silver particles.

Aspect ratio = grain size / grain thickness In the present invention, the average grain size of the silver halide grains is 0.2 to 10 μm.
Is preferably 0.3 to 7.0 μm, more preferably 0.3 to 7.0 μm.
Most preferably, it is 4 to 5.0 μm.

In the present invention, the average particle size refers to the particle size ri.
The arithmetic mean of However, three significant figures and the least significant figure are rounded off, and the number of measured particles is indiscriminately 1,000 or more.

In the case of tabular silver halide grains, the grain size ri is a diameter obtained by converting a projected image viewed from a direction perpendicular to the main plane into a circular image having the same area. In the case of silver halide grains having a shape other than tabular silver halide grains, the diameter is obtained by converting a projected image of the silver halide grains into a circular image having the same area.

The particle diameter ri can be obtained by photographing a silver halide particle with an electron microscope at a magnification of 10,000 to 70,000 and actually measuring the particle diameter or the projected area of the print.

In the present invention, the projected area and thickness of each grain for calculating the grain size and the aspect ratio of the silver halide grain can be obtained by the following method. A sample is prepared by coating a latex ball with a known particle size as an internal standard on a support and silver halide particles so that the main plane is oriented parallel to the substrate, and the particles are shaded by carbon deposition from a certain angle. After that, a replica sample is prepared by a normal replica method. An electron micrograph of the sample is taken, and the projected area and thickness of each particle are determined using an image processing device or the like. In this case, the projected area of the particle can be calculated from the projected area of the internal standard, and the thickness of the particle can be calculated from the internal standard and the length of the shadow of the particle.

In the present invention, any silver halide photographic emulsion such as a polydisperse emulsion having a wide particle size distribution and a monodisperse emulsion having a narrow particle size distribution is used, but a monodisperse emulsion is preferable.

A monodisperse emulsion is one having a particle size distribution of less than 20%, more preferably less than 16%, when the particle size distribution is defined by the following formula.

Particle size distribution (%) = (standard deviation of particle size / average particle size) × 100 The average particle size and standard deviation are determined from the particle size ri defined above.

In the silver halide photographic emulsion of the present invention, any silver halide such as silver iodobromide, silver iodochlorobromide, silver iodochloride and the like can be used. Is preferably silver iodobromide or silver iodochlorobromide.

In the present invention, the average silver iodide content of the silver halide grains contained in the silver halide photographic emulsion is 0.5.
To 40 mol%, more preferably 1 to 40 mol%.
~ 20 mol%.

In the present invention, the average silver iodide content of silver halide grains is determined by the EPMA method (Electron Pr).
ob Micro Analyzer method).

As the silver halide grains contained in the silver halide photographic emulsion of the present invention, core / shell type grains can also be preferably used. The core / shell type particles are particles composed of a core and a shell covering the core, and the shell is formed by one or more layers. The silver iodide content of the core and the shell are preferably different from each other.

The dislocation lines of the silver halide grains are described, for example, in J. Am. F. Hamilton, Photo. Sci.
Eng. 11 (1967) 57 and T.I. Shiozaw
a. Soc. Photo. Sci. Japan35
(1972) 213 can be observed by a direct method using a transmission electron microscope at a low temperature.

In the present invention, the method for introducing dislocation lines into silver halide grains is not particularly limited.
Such as a method of adding an aqueous iodide ion solution such as potassium iodide and a water-soluble silver salt solution by double jet, a method of adding silver iodide fine particles, a method of adding only an iodide ion solution, and a method of using an iodide ion releasing compound. By a known method,
A desired position and amount of dislocation lines can be introduced into the silver halide grains, but a method using an iodide ion releasing compound is preferable, and a method using an iodide ion releasing compound described in Japanese Patent Application No. 11-50334 or the like. Is particularly preferred.

Various methods well-known in the art can be used for forming silver halide grains in the production of the silver halide photographic emulsion of the present invention. That is, a single jet method, a double jet method, a triple jet method, a method for supplying fine silver halide particles, or the like can be used in any combination. Further, a method of controlling the pH and pAg in the liquid phase in which silver halide is formed in accordance with the growth rate of silver halide can also be used. The formation of silver halide grains is preferably performed under conditions close to the critical growth rate.

For the production of the silver halide photographic emulsion of the present invention, a seed emulsion can also be used. When a seed emulsion is used, the silver halide grains in the seed emulsion may have a regular crystal structure such as cubic, octahedral, or tetradecahedral, or may have a spherical or plate-like shape. It may have an irregular crystal form. In these particles, the (100) plane and the (11) plane
1) Any ratio of planes can be used. The silver halide grains in the seed emulsion used may be a composite of these crystal forms, and grains of various crystal forms may be mixed. Twin silver halide grains having twin planes are used. And particularly preferred are twin silver halide grains having two opposing parallel twin planes.

In the present invention, either when a seed emulsion is used or when no seed emulsion is used, as a condition for silver halide nucleation and ripening, a method known in the art can be applied. it can.

For the production of the silver halide photographic emulsion of the present invention, a silver halide solvent known in the art can be used. Preferably, a silver halide solvent is used at the time of forming base tabular grains. Should be avoided except for ripening after nucleation.

For the production of the silver halide photographic emulsion of the present invention, any of an acidic method, a neutral method and an ammonia method can be used, but the acidic method or the neutral method is preferred.

In the production of the silver halide photographic emulsion of the present invention, a halide ion and a silver ion may be mixed simultaneously, or one of them may be mixed in the presence of the other. Also, considering the critical growth rate of silver halide crystals,
PAg and pH in a mixing vessel containing halide ions and silver ions
And can be added sequentially or simultaneously. The halogen composition of the silver halide grains may be changed by using a conversion method in any step of silver halide formation.

In the production of the silver halide photographic emulsion of the present invention, a cadmium salt, a zinc salt, a lead salt, a thallium salt, an iridium salt (including a complex salt) is formed in the step of forming and / or growing silver halide grains. ), Rhodium salts (including complex salts), salts of iron and other Group VIII metals (including complex salts)
Metal ions can be added using at least one selected from the above, and these metals can be contained inside silver halide grains and / or on the surface of the grains.

In the present invention, when silver halide fine grains are used, the silver halide fine grains may be prepared before the preparation of the silver halide grains according to the present invention, or may be prepared. May be prepared in parallel. When the latter is prepared in parallel, JP-A No. 1-18
As described in JP-A Nos. 3417, 2-44335 and the like, silver halide fine particles can be produced by using a mixer separately provided outside a reaction vessel in which silver halide grains according to the present invention are formed. Although it is possible to provide a preparation container separately from the mixer, the silver halide fine particles once prepared in the mixer can be arbitrarily selected so as to be suitable for a growth environment in a reaction container in which the preparation of the silver halide particles concerned is performed. It is preferable to supply the mixture to the reaction vessel after the preparation.

The method for preparing the silver halide fine particles is preferably an acidic to neutral environment (pH ≦ 7) when the preparation of reduction sensitized fine particles is not intended. When it is intended to prepare reduction sensitized fine grains, silver halide fine grains may be prepared by appropriately combining the above reduction sensitizing techniques.

In order to produce the silver halide fine particles, a water-soluble silver salt containing silver ions and an aqueous solution containing halide ions may be mixed while appropriately controlling a supersaturation factor.
Regarding control of the supersaturation factor, see JP-A-63-92942.
And JP-A-63-31244 can be referred to.

PAg for producing the silver halide fine particles
Is preferably at least 3.0, more preferably at least 5.0, even more preferably at least 8.0 in order to suppress the generation of reduced silver nuclei in the silver halide fine grains themselves. .

The temperature for producing the silver halide fine particles is as follows:
The temperature is preferably 50 ° C. or lower, more preferably 40 ° C. or lower, and most preferably 35 ° C. or lower.

Further, as the protective colloid used for producing the silver halide fine particles, the above-mentioned protective colloid-forming substance used for producing the silver halide particles according to the present invention can be used.

When the silver halide fine grains are formed at a low temperature, coarsening of the grain size due to Ostwald ripening after the formation of the silver halide fine grains can be suppressed, but at a low temperature, gelatin is easily coagulated. 2-16642
It is preferable to use low molecular weight gelatin described in No. 2, etc., a synthetic molecular compound having a protective colloidal action on silver halide grains, or a natural high molecular compound other than gelatin. The concentration of the protective colloid is preferably 1% by mass or more, more preferably 2% by mass or more, and further preferably 3% by mass or more.

The silver halide fine particles have a particle size of 0.1 μm.
Or less, more preferably 0.05 μm or less.

The silver halide fine grains can contain the above-described reduction sensitization and optionally metal ions, if necessary.

The silver halide photographic emulsion of the present invention is preferably subjected to ultrafiltration in at least a part of the process of forming silver halide grains. In the present invention, the step of forming silver halide grains refers to, in the production of a silver halide emulsion, after the nuclei of silver halide grains start to be formed,
It means a process until crystal growth and physical ripening of the silver halide grains are completed.

The ultrafiltration may be carried out by interrupting the growth of the silver halide grains at any time during the formation of the silver halide grains, or may be carried out over an arbitrary period while continuing the growth of the silver halide grains. May be carried out a plurality of times in the course of silver halide grain formation, preferably before the completion of silver halide grain formation, more preferably during growth of silver halide grains or during growth of silver halide grains. Is preferred.

By utilizing the ultrafiltration, unnecessary water-soluble salts can be removed and desalted in the process of forming silver halide grains. Further, a reducing agent, an oxidizing agent, a halogen ion releasing compound, a silver halide solvent, a polyvalent metal atom, a polyvalent metal atom ion, a polyvalent metal atom complex or a polyvalent metal atom complex ion added at the time of forming silver halide grains. And the like, and removal and deactivation of unreacted substances such as the unreacted substances, undoped residues and the like. Furthermore, control of the distance between silver halide grains, control of growth conditions of silver halide grains used for controlling silver halide grain growth pH and pBr, control of the volume of the reaction solution during silver halide grain formation, concentration, etc. Can be implemented.

Ultrafiltration using membrane separation is described in Chemical Engineering Handbook, Revised 5th Edition (Chemical Engineering Association, Maruzen) 924
954, RD 102, 10208 and 131, 13122, or JP-B-59-43727, 6
2-27008, JP-A-62-113137, 5
Nos. 7-209823, 59-43727, 62-
113137, 61-21948, 62-2
No. 3035, No. 63-40137, No. 63-4003
9, JP-A-3-140946 and JP-A-2-172816
And the methods described in JP-A Nos. 2-172817 and 4-22942 can also be referred to. In the present invention,
For the ultrafiltration, it is preferable to use an apparatus or a method described in JP-A-11-339923 or JP-A-11-231448.

In the production of the silver halide photographic emulsion of the present invention, desalting is preferably performed after formation. Desalination can be performed, for example, by the method described in Research Disclosure (hereinafter abbreviated as RD) No. 17643 No. II.

More specifically, in order to remove unnecessary soluble salts from a precipitate product or an emulsion after physical ripening,
A Nudel washing method in which gelatin is gelled may be used, and inorganic salts, anionic surfactants, anionic polymers (eg, polystyrenesulfonic acid), or gelatin derivatives (eg, acylated gelatin, carbamoylated gelatin) may be used. The precipitation method used can be used. Ultrafiltration utilizing the above-mentioned membrane separation can also be preferably used for desalination.

The silver halide grains contained in the silver halide photographic light-sensitive material of the present invention may have a regular crystal structure such as cubic, octahedral or tetradecahedral, or may have a spherical or plate-like shape. It may have such an irregular crystal form. In these particles, any ratio of the crystal habit (100) plane and the (111) plane can be used. Further, a composite of these crystal forms may be used, and particles of various crystal forms may be mixed. Twin silver halide grains having two opposing parallel twin planes can also be used.

The twins are silver halide crystals having one or more twin planes in one grain, and the classification of the twins is described in a report by Klein and Moiser, “Photographic. Correspondents (Photograph)
ishe Korrespondentz) ", Volume 99,
The details are described on page 99, volume 100, and page 57.

When tabular silver halide grains are used, 50% or more of the total projected area of the silver halide grains is preferably tabular silver halide grains, more preferably 60% or more, and still more preferably. 80% or more.

When tabular silver halide grains having a (111) main plane are used in the present invention, the ratio of tabular silver halide grains having two twin planes parallel to the main plane is determined by the number of silver halide grains. It is preferably at least 60%,
It is more preferably at least 70%, further preferably at least 80%.

In the production of a silver halide emulsion, conditions other than those described above are described in JP-A-61-6643 and JP-A-61-6643.
No. 1-1630, No. 61-112142, No. 62-
157024, 62-18556, 63-92
No. 942, No. 63-151618, No. 63-1634
No. 51, No. 63-220238, No. 63-31124
No. 4, RD38957, Sections I and III, RD4014
Appropriate conditions can be selected with reference to the XV section 5 and the like.

In constructing a color light-sensitive material using the silver halide emulsion of the present invention, a silver halide emulsion which has been subjected to physical ripening, chemical ripening and spectral sensitization is used.

The additive used in such a step is R
It is described in IV and V of D38957, XV of RD40145, and the like.

Known photographic additives that can be used in the present invention are also described in RD38957, Sections II to X, RD4014.
Those described in I to XIII of item 5 can be used.

In the silver halide photographic light-sensitive material of the present invention,
Red, green and blue-sensitive silver halide emulsion layers are provided, and each layer can contain a coupler. It is preferable that the coloring dye formed from the coupler contained in each of these layers has a spectral absorption maximum separated by at least 20 nm. As the coupler, it is preferable to use a cyan coupler, a magenta coupler, and a yellow coupler. As a combination of each emulsion layer and a coupler, usually, a combination of a yellow coupler and a blue photosensitive layer, a magenta coupler and a green photosensitive layer, a combination of a cyan coupler and a red photosensitive layer are used, but is not limited to these combinations. , And other combinations.

In the present invention, a DIR compound can be used. Specific examples of DIR compounds that can be used include, for example, D-1 to D-34 described in JP-A-4-114153, and these compounds can be preferably used in the present invention.

DIR that can be used in the present invention
Specific examples of the compounds other than those described above include, for example, U.S. Pat. Nos. 4,234,678, 3,227,554, 3,647,291, and 3,955.
8,993, 4,419,886,
No. 3,933,500, JP-A-57-5683
7, No. 51-13239, U.S. Pat.
72, 363, 2,070,266, and RD40145, section XIV.

Further, specific examples of the coupler which can be used in the present invention are described in RD40145, section II and the like.

The additive used in the present invention is RD4014
It can be added by the dispersion method described in section VIII of 5, etc.

In the present invention, the RD38957
Known supports described in Section XV and the like can be used.

The light-sensitive material of the present invention includes the aforementioned RD3895
Auxiliary layers such as a filter layer and an intermediate layer described in the section 7 XI can be provided.

The light-sensitive material can have various layer structures such as a normal layer, a reverse layer, and a unit structure described in RD38957, section XI.

The silver halide emulsion according to the present invention can be used for various color light-sensitive materials represented by general or movie color negative films, slide or television color reversal films, color papers, color positive films and color reversal papers. Can be preferably applied.

To develop the silver halide color light-sensitive material of the present invention, for example, T.I. H. James, Theory of the Photographic Process 4th Edition (The Theory of The Photog)
rafic ProcessForth Edition
n) Pages 291 to 334 and Journal of the
American Chemical Society (Journa1
of the American Chemical
Society, 73, 3,100 (195
The developer known per se described in 1) can be used, and the above-mentioned RD38957 XVII to XX can be used.
And development processing can be carried out by a usual method described in the section and RD40145, section XXIII.

[0157]

EXAMPLES Hereinafter, the present invention will be described specifically with reference to examples, but the present invention is not limited to these embodiments.

Example 1 << Preparation of silver halide emulsion >> (Preparation of emulsion Em-1) [Nucleation and ripening step] The following gelatin aqueous solution-1 in a reaction vessel was kept at 30 ° C. The following silver nitrate aqueous solution-1 and halide aqueous solution-1 were added at a constant flow rate for one minute by a double jet method while vigorously stirring using a mixing and stirring apparatus described in JP-A-160128 to form nuclei.

<Aqueous Gelatin Solution-1> Alkali-treated inert gelatin (average molecular weight 100,000) 32.4 g Potassium bromide 9.9 g H ₂ O 13.0 L <Silver nitrate aqueous solution-1> Silver nitrate 50.43 g H ₂ O 225. 9 ml <halide solution -1> potassium bromide 35.33g H ₂ O 224.7ml the addition finished, immediately following aqueous gelatin solution -2 addition, temperature was raised to take and 6 0 ° C. to 30 minutes, the pH It adjusted to 5.0 and aged for 20 minutes in that state.

<Aqueous Gelatin Solution-2> Alkali-treated inert gelatin (average molecular weight 100,000) 17.5 g Potassium bromide 3.18 g 10% by mass methanol solution of surfactant (EO-1) 0.20 ml H ₂ O 673 0.5 ml * EO-1: HO (CH ₂ CH ₂ O) _m [CH (CH ₃ ) CH ₂ O] _19.8 (CH ₂ CH ₂ O) _n H (m + n = 9.77) [Particle growth step-1 After the completion of the nucleus ripening step, an aqueous silver nitrate solution-2 and an aqueous halide solution-2 were added by double jet method while accelerating the flow rates. After the addition was completed, an aqueous solution of gelatin-3 was added, and subsequently, an aqueous solution of silver nitrate-3 and an aqueous solution of halide-3 were added at an increased flow rate. During this time, the silver potential in the reaction vessel (measured with a silver ion selective electrode using a saturated silver-silver chloride electrode as a reference electrode) was controlled at 6 mV using a 1 mol / L potassium bromide solution.

[0161] <nitrate aqueous -2> nitrate 639.8g H ₂ O 2866.2ml <halide solution -2> Potassium bromide 448.3g H ₂ O 2850.7ml <gelatin solution -3> alkali-treated inert gelatin (average (Molecular weight 100,000) 175.9 g 10% by mass methanol solution of surfactant (EO-1) 0.67 ml H ₂ O 4260.1 ml <aqueous silver nitrate-3> 989.8 g of silver nitrate H ₂ O 1437.2 ml <aqueous halide solution− 3> Potassium bromide 679.6 g Potassium iodide 19.35 g H ₂ O 1412.0 ml [Grain growth step-2] After the completion of the particle growth step-1, the following aqueous solution-A1 and then aqueous solution-B1 were added, and 1 mol /
The pH was adjusted to 9.3 using an aqueous L potassium hydroxide solution, and iodine ions were released while aging for 4 minutes. Thereafter, the pH was adjusted to 5.0 using a 1 mol / L nitric acid aqueous solution,
Next, the silver potential in the reaction vessel was adjusted to −19 mV using a 3.5 mol / L aqueous potassium bromide solution, and then a silver nitrate aqueous solution-4 and a halide aqueous solution-4 were added while accelerating the flow rates.

[0162] <aqueous -A1> p-iodoacetamide sodium benzenesulfonate 102.7g H ₂ O 770.1ml <aq -B1> sodium sulfite 35.6g H ₂ O 352.9ml <nitrate aqueous -4> nitrate 720. 0g H ₂ O 1045.6ml <halide solution -4> potassium bromide 494.4g potassium iodide 14.1g H ₂ O 1027.1ml Incidentally, through the particle growth step 1,2, addition rates of the aqueous silver nitrate solution and halide solution Was optimally controlled so that no new silver halide grains were formed and the grain size distribution did not deteriorate due to Ostwald ripening between the growing silver halide grains.

After the completion of the particle growth step, desalting and washing are performed, gelatin is added and dispersed well.
Was adjusted to 5.8 and pAg to 8.1 to prepare Emulsion Em-1. The silver halide emulsion thus obtained was a silver halide emulsion composed of hexagonal tabular grains having an average grain size of 1.5 μm, a grain size distribution of 18% and an average aspect ratio of 8. When observed with a transmission electron microscope, silver halide grains having five or more dislocation lines in the fringe portion occupy 90% of the projected area of all silver halide grains, and dislocation lines were formed in the fringe portion. The silver halide grains having 20 or more grains accounted for 70% of the projected area of all the silver halide grains.

(Preparation of Emulsion Em-2)
In the preparation of No. 1, the aqueous silver nitrate solution in the grain growth step-1
Emulsion Em-2 was prepared in the same manner except that the following solution I-4 was added at the end of the addition of No. 2, and the following solution J-4 was added at the end of the grain growth step-1 to perform reduction sensitization. .

<I-4 Solution> 100 ml of an aqueous solution containing 1 × 10 ⁻⁵ mol of thiourea dioxide per mol of silver halide <J-4 Solution> 2.5 × of sodium ethylthiosulfonate per mol of silver halide Aqueous solution containing 10 ^-4 mol 100 ml (Preparation of emulsion Em-3) The above-mentioned emulsion Em-2 was pAg at 50 ° C. by using a 3.5 mol / L aqueous solution of potassium bromide.
9.7, 0.5 mol of the following K-4 solution was added in 10 minutes, and after aging for 30 minutes, pAg was adjusted to 10 using 3.5 mol / L aqueous potassium bromide solution, 0.7 mol of the following L-4 solution was added in 10 minutes, aged for 30 minutes, desalted and washed again, and gelatin was added to disperse well.
The emulsion Em-3 was prepared by adjusting the pH to 5.8 and the pAg to 8.1 at 0 ° C.

<K-4 Solution> A method for preparing a fine grain emulsion comprising 3.0% by mass of gelatin and silver iodobromide fine grains (average particle size: 0.05 μm, silver iodide content: 10 mol%) is described below.

6.0 containing 0.06 mol of potassium bromide
5000 ml of a 1% by weight gelatin solution are added to the stirred reaction vessel, and then 2000 ml of an aqueous solution containing 7.06 mol of silver nitrate, 6.35 mol of potassium bromide and 0.70 mol of potassium bromide.
An aqueous solution containing 6 mol of potassium iodide was added at a constant speed over 10 minutes. The pH during the formation of the fine particles was adjusted to 3.0 using nitric acid.
And the temperature was controlled at 30 ° C. After the addition was completed, the pH was adjusted to 6.0 using an aqueous solution of sodium carbonate.

<Liquid L-4> 3.0% by mass of gelatin and silver bromide fine particles (average particle diameter: 0.3%).
The method for preparing a fine grain emulsion comprising the same (0.05 μm) is shown below.

6.0 containing 0.06 mol of potassium bromide
5000 ml of a mass% gelatin solution was added to the stirred reaction vessel, and then 2,000 ml of an aqueous solution containing 7.06 mol of silver nitrate and an aqueous solution containing 7.06 mol of potassium bromide were added at a constant rate over 10 minutes. During the formation of fine particles, the pH was controlled at 3.0 using nitric acid, and the temperature was controlled at 30 ° C. After the addition was completed, the pH was adjusted to 6.0 using an aqueous solution of sodium carbonate.

(Preparation of Emulsion Em-4) Emulsion Em-1
After the grain growth step-1 is completed, the silver halide emulsion is passed through an ultrafiltration module (manufactured by Asahi Kasei Kogyo Co., Ltd., type ALP-1010 using a polyacrylonitrile membrane having a molecular weight cut off of 13,000) to form a halogen. After circulating the silver halide emulsion until the volume becomes 1/5, the grain growth step-2 is performed, and the above solution I-4 is added immediately before the start of the addition of the aqueous silver nitrate solution-4 in the grain growth step-2. And, at the end of the grain growth step-2, the solution J-4 was added, subjected to reduction sensitization, and 3.5 mol / L after the completion of the desalting / washing treatment.
The pAg was adjusted to 9.7 at 50 ° C. using an aqueous potassium bromide solution, and 0.5 mol of the K-4 solution was added in 10 minutes.
After aging for 30 minutes, the pAg was adjusted to 10 using a 3.5 mol / L aqueous potassium bromide solution, and 0.7 g of the L-4 solution was used.
The mol was added in 10 minutes, the mixture was aged for 30 minutes, subjected to desalting and water washing again, dispersed well by adding gelatin, adjusted to pH 5.8 and pAg to 8.1 at 40 ° C. Em-4
Was prepared.

<< Preparation of Color Photosensitive Material >> On a 120 μm thick triacetyl cellulose film support provided with an undercoat layer, layers having the compositions shown in Tables 1 to 4 were sequentially formed from the support side to form a multilayer color photosensitive material. Material samples were prepared. In the table,
The amount of each material added is shown particularly in grams per 1 m ² unless otherwise indicated. Further, silver halide and colloidal silver are shown in terms of the amount of silver, and sensitizing dyes (shown by SD) are shown in moles per mole of silver.

[0172]

[Table 1]

[0173]

[Table 2]

[0174]

[Table 3]

[0175]

[Table 4]

Samples 1001 to 1004 were prepared using Emulsions Em-1 to Em-4 prepared above as Emulsions M described in the ninth layer in Table 3, respectively.

Table 5 shows the characteristics of the silver iodobromide emulsions a to j except for the emulsion M used in the sample preparation. In the table, the average particle size is represented by the length of one side of a cube having the same volume.

[0178]

[Table 5]

For the emulsions a to i and the emulsion M except for the emulsion j, the sensitizing dye described above was added, and then triphenylphosphine selenide, sodium thiosulfate,
Chloroauric acid and potassium thiocyanate were appropriately added, and a product subjected to chemical sensitization according to a conventional method so as to optimize fog and sensitivity was used.

Incidentally, in addition to the above components, a coating aid SU-
1, SU-2, SU-3, dispersing aid SU-4, viscosity modifier V-1, stabilizers ST-1, ST-2, antifoggant A
F-1, two kinds of polyvinylpyrrolidone (AF-2) having a weight average molecular weight of 10,000 and a weight average molecular weight of 100,000, inhibitors AF-3, AF-4, AF-5,
Hardeners H-1, H-2 and preservative Ase-1 were added. In addition, liquid paraffin is manufactured by Merck
ck Index 117139 was used.

The structure of each compound used in the preparation of the above sample is shown below.

[0182]

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[0183]

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[0184]

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[0185]

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[0186]

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[0187]

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[0188]

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[0189]

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[0190]

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[0191]

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[0192]

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<< Exposure, Development and Evaluation >> Two copies of each sample prepared as described above were prepared. One copy was left as it was, and the other copy was subjected to forced deterioration treatment at 65 ° C. and 20% relative humidity for one week. Then, both samples were exposed and developed.

Exposure was performed using a light source at 5400 ° K.
/ 200 seconds for wedge exposure
The color development processing was performed according to the development processing steps described in paragraphs [0220] to [0227] of No. 123652. Next, each of the obtained developed samples was measured for magenta density using a densitometer manufactured by X-rite, and the density D-exposure amount Lo was measured.
A characteristic curve composed of gE was prepared, and the sensitivity was measured. The sensitivity was defined as the reciprocal of the exposure amount giving the minimum density of magenta density + the optical density of 0.10, and was expressed as a relative value with the sensitivity of the sample 1001 not subjected to the forcible deterioration treatment as 100.

Table 6 shows the sensitivity values in the unprocessed and forcibly deteriorated processes obtained by the above evaluation.

[0196]

[Table 6]

As is clear from Table 6, Samples 1003 and 1004 according to the present invention are Comparative Samples 1001 and 1004.
No. 02 exhibited excellent performance in both improvement of sensitivity and storage stability.

Example 2 (Preparation of Emulsion Em-11) Emulsion Em- in Example 1
Emulsion Em-11 was prepared in the same manner as in Preparation 1, except that the following halide aqueous solution-14 was used in place of the halide aqueous solution-4 in the grain growth step-2.

[0199] (Preparation of Emulsion Em-12) <halide solution -14> Potassium bromide 499.3g Potassium iodide 7.0g H ₂ O 1027.1ml in the preparation of the emulsion Em-11, the particle growth process -1 At the end of the addition of the aqueous silver nitrate solution-2, the following liquid I-14 was added, and the particle growing step-1
Emulsion Em-12 was prepared in the same manner as above except that the following J-14 solution was added and reduction sensitization was performed.

<I-14 Solution> 100 ml of an aqueous solution containing 8 × 10 ⁻⁶ mol of thiourea dioxide per mol of silver halide <J-14 Solution> 3.0 × of sodium ethylthiosulfonate per mol of silver halide Aqueous solution containing 10 ^-4 mol 100 ml (Preparation of emulsion Em-13) In the preparation of the emulsion Em-11, the following halide aqueous solution-14a was used in place of the halide aqueous solution-2 in the grain growth step-1, and the grain growth step- 1-14 at the end of the addition of the aqueous silver nitrate solution-2.
A liquid is added, and at the end of the particle growing step-1, the above J-1
Emulsion Em-13 was prepared in the same manner except that four solutions were added and reduction sensitization was performed.

<Aqueous halide solution-14a> Potassium bromide 394.5 g Potassium iodide 75.0 g H ₂ O 2846.1 ml (Preparation of emulsion Em-14) In the preparation of the emulsion Em-11, in the grain growth step-1, The aqueous halide solution-14a was used in place of the aqueous halide solution-2, and after completion of the grain growth step-1, the silver halide emulsion was subjected to an ultrafiltration module (a polyacrylonitrile membrane having a molecular weight cut off of 13,000, manufactured by Asahi Kasei Corporation). Type ALP-101 using
0), the silver halide emulsion was circulated until the volume became 1/5, and then the grain growth step-2 was carried out. Emulsion Em-14 was prepared in the same manner except that Solution -14 was added, and the above-mentioned Solution J-14 was added at the end of the grain growth step-2 to perform reduction sensitization.

Each of the emulsions Em-13 and Em-14 contained silver halide grains having three silver halide layers of the internal phase, intermediate phase and external phase according to the present invention. Emulsion E
Table 7 shows the particle structures of m-11 to Em-14.

[0203]

[Table 7]

Next, the emulsions Em-11 to E prepared above were prepared.
Samples 1101 to 110 were prepared in the same manner as in Example 1 except that m-14 was used as the ninth layer emulsion M in Example 1.
No. 4 was prepared, subjected to development processing and evaluation in the same manner, and the obtained results are shown in Table 8.

[0205]

[Table 8]

As is clear from Table 8, Samples 1103 and 1104 according to the present invention are Comparative Samples 1101 and 1110.
No. 02 exhibited excellent performance in both improvement of sensitivity and storage stability.

Example 3 (Preparation of Emulsion Em-21) Emulsion Em-
Emulsion Em- was prepared in the same manner except that the following grain growth step-32 was used instead of grain growth step-2 in the preparation of emulsion Em-
21 was prepared.

[Particle Growth Step-32] After the completion of the particle growth step-1 in Example 1, the pH was adjusted to 5.0 using a 1 mol / L aqueous nitric acid solution, and then 3.5 mol / L bromide was added. The silver potential in the reaction vessel was set to -6 m using a potassium aqueous solution.
V, and the following silver nitrate aqueous solution-34 and halide aqueous solution-34 were added while accelerating the flow rate.

<Aqueous solution of silver nitrate-34> Silver nitrate 720.0 g H ₂ O 1045.6 ml <Aqueous solution of halide −34> Potassium bromide 479.2 g Potassium iodide 35.2 g H ₂ O 1025.0 ml (Preparation of emulsion Em-22 In the preparation of the emulsion Em-21, at the end of the addition of the aqueous silver nitrate solution-2 in the grain growth step-1, the above solution I-14 was added, and the grain growth step-1 was carried out.
Emulsion Em-22 was prepared in the same manner except that the solution J-14 was added at the end of the process, and reduction sensitization was performed.

Emulsions Em-21 and Em prepared above
The ratio (number) of tabular silver halide grains satisfying 0 ≦ I ₄ / I ₃ ≦ 1.0 in −22 was 20%.

(Preparation of Emulsion Em-23) In the preparation of Emulsion Em-1 of Example 1, the following grain growth step-32a was performed instead of the grain growth step-2, and the grain growth step-
Emulsion E was prepared in the same manner as above except that the solution I-14 was added at the end of the addition of the aqueous silver nitrate solution-2, and the solution J-14 was added at the end of the grain growth step-1 to perform reduction sensitization.
m-23 was prepared.

[Grain Growth Step-32a] After the completion of the particle growth step-1 described in Example 1, the pH was adjusted to 5.0 with a 1 mol / L aqueous nitric acid solution, and then the following silver nitrate aqueous solution-34a and halide Aqueous solution-34a was added by a double jet method in 2 minutes, and subsequently, an aqueous silver nitrate solution-34
b and an aqueous halide solution-34b were added while accelerating the flow rate. The silver nitrate aqueous solution-34b and the halide aqueous solution-3
The silver potential in the reaction vessel during the addition of 4b
Maintain at -19 mV until 30% of the addition of 34b is completed, and after that, at the end of the addition of the aqueous silver nitrate solution -34b,
It controlled so that it might be set to mV.

<Aqueous silver nitrate-34a> 72.0 g of silver nitrate 407.0 ml of H ₂ O <aqueous halide-34a> 70.3 g of potassium iodide 401.0 ml of H ₂ O <aqueous silver nitrate-34b> 720.0 g of silver nitrate H ₂ O 1045.6 ml <aqueous halide solution-34b> 504.4 g of potassium bromide 1027.0 ml of H ₂ O (Preparation of emulsion Em-24) In the preparation of emulsion Em-1 of Example 1, halogenation was carried out after completion of the grain growth step-1. The silver emulsion is passed through an ultrafiltration module (manufactured by Asahi Kasei Corporation, type ALP-1010 using a polyacrylonitrile membrane having a molecular weight cut off of 13,000) until the volume of the silver halide emulsion is reduced to one fifth. After the circulation, the particle growth step-2 is performed, and the particle growth step-32a is performed instead of the particle growth step-2. The same as above except that the liquid I-14 was added immediately before the start of the addition of the aqueous silver nitrate solution -34b in the grain growth step-2, and the liquid J-14 was added at the end of the grain growth step-2 to perform reduction sensitization. And the emulsion Em
-24 was prepared.

Emulsions Em-23 and Em prepared above
The ratio (number) of tabular silver halide grains satisfying 0 ≦ I ₄ / I ₃ ≦ 1.0 in −24 was 80%, and 0 ≦ I ₄ / I _3.
Ratio (number) of tabular silver halide grains satisfying ≦ 0.6
Was 50%.

Then, samples 1201 to 120-1 were prepared in the same manner as in Example 1 except that the above-prepared emulsions Em-21 to Em-24 were used as emulsion M of the ninth layer in Example 1.
No. 204 was produced, and similarly subjected to development processing and evaluation, and the obtained results are shown in Table 9.

[0216]

[Table 9]

As is clear from Table 9, the samples 1203 and 1204 according to the present invention are comparative samples 1201 and 1204.
In contrast, No. 2 exhibited excellent performance in both improvement of sensitivity and storage stability.

Example 4 (Preparation of Emulsion Em-101) Emulsion Em-101 was prepared according to the following method.

<A-101 solution> Ossein gelatin 36.4 g Potassium bromide 11.1 g 14.6 L with water <B-101 solution> 1.25 mol / L silver nitrate aqueous solution 3657 ml <C-101 solution> 1.25 Mol / L aqueous potassium bromide solution 3657 ml <D-101 solution> 1 mol / L sulfuric acid required amount <E-101 solution> Ossein gelatin 156.6 g 10% methanol aqueous solution of surfactant (EO-1) 5.2 ml water 3795 ml <F-101 solution> 28% aqueous ammonia solution required <G-101 solution> 56% acetic acid aqueous solution required <H-101 solution> Ossein gelatine 256.3 g 10% methanol surfactant (EO-1) Aqueous solution 7.0 ml with water 2127 ml <I-101 solution> 3.5 mol / L silver nitrate aqueous solution 3235 ml <J-101 solution> potassium bromide 1021 g Potassium iodide 29.1 g 2500 ml with water <K-101 solution> Potassium bromide 749.7 g 116.2 g Potassium iodide 2000 ml with water <L-101 solution> 1.75 mol / L aqueous solution of potassium bromide < M-101 solution> 0.1 mol / L potassium iodide aqueous solution 600 ml <O-101 solution> 10% potassium hydroxide aqueous solution required amount <P-101 solution> 3.5 mol / L potassium bromide aqueous solution required amount <R -101 solution> 1.0 mol / L silver nitrate aqueous solution required amount <S-101 solution> 1.0 mol / L potassium bromide aqueous solution required amount Add A-101 solution into the reaction vessel and use D-101 solution. And adjust the solution temperature in the reaction vessel to 30.
C, while stirring vigorously while maintaining at
268 ml of each of the 101 liquids was added at a constant speed for 1 minute by the simultaneous mixing method.

After the above addition was completed, E-101 solution was added, and 3
The temperature was raised to 60 ° C. over a period of 0 minutes. Then, F-101
The solution was added to adjust the pH to 9.3, and after aging for 7 minutes,
The pH was adjusted to 6.1 using G-101 solution.

During this time, the silver potential of the solution (measured with a silver ion selective electrode using a saturated silver-silver chloride electrode as a reference electrode) was L-1.
The solution was controlled at 6 mV using the 01 solution.

Then, while maintaining the potential at 6 mV and accelerating the flow rate by the simultaneous mixing method (the flow ratio between the start time and the end time is 1:12), the B-101 solution and the C-10
The remainder of Liquid 1 was added, and Liquid H-101 was added.

Subsequently, 1876 ml of each of the I-101 solution and the J-101 solution was acceleratedly added in 40 minutes (the flow ratio at the start and at the end was 1: 2), and the pH was adjusted using the G-101 solution.
Was adjusted to 5.0. Thereafter, the M-101 solution was added over 5 minutes, the pH was adjusted to 5.8 with the O-101 solution, and the remaining 1359 ml of the I-101 solution and 1 of the K-101 solution were subsequently added.
359 ml was acceleratedly added for 45 minutes (the flow ratio at the start and at the end was 1: 2). Thereafter, the silver potential was adjusted to -40 mV with the P-101 solution, and 300 ml of each of the R-101 solution and the S-101 solution was added at a constant rate for 6 minutes.

After grain formation, desalting treatment was performed according to the method described in JP-A-5-72658, and gelatin was added and dispersed to obtain an emulsion Em-101 having a pH of 5.8 at 70 mV at 40 ° C.

When the silver halide grains in this emulsion were observed with an electron microscope, 90% of the projected area of all the silver halide grains had an average grain size of 1.6 μm, a grain size distribution of 15%, and an average aspect ratio of 8. 0 hexagonal tabular monodispersed silver halide grains.

(Preparation of Emulsion Em-102) Emulsion Em
In the preparation of -101, the following solution I-44 was added at the end of the addition of the B-101 solution, and the following J-44 solution was added at the end of the addition of the I-101 solution.
Emulsion Em-102 was prepared.

<I-44 Solution> 100 ml of an aqueous solution containing 1 × 10 ⁻⁵ mol of thiourea dioxide per mol of silver halide <J-44 Solution> 3.0 × of sodium ethylthiosulfonate per mol of silver halide 100 ml of an aqueous solution containing 10 ^-4 mol (Preparation of Emulsion Em-103) In the preparation of Emulsion Em-102, at the end of addition of the B-101 solution, the I-44 was added.
After that, 1876 ml of each of the I-101 solution and the J-101 solution was acceleratedly added (flow ratio at the start and at the end was 1: 2), and the pH was adjusted to 5.0 using G-101. The same procedure was followed up to the step of adjusting the pH to 0.1, then the following M-101a solution and N-101a solution were added instead of the M-101 solution, and then the pH was adjusted to 9.3 with the O-101 solution and ripened for 4 minutes. Then, the pH was adjusted to 5.0 with G-101 solution. Subsequently, the remaining 1359 ml of the I-101 solution and 1359 ml of the K-101 solution were acceleratedly added in 45 minutes (the flow ratio at the start and at the end was 1: 2), and the J-44 solution was added.
Thereafter, the silver potential was adjusted to −40 mV with the P-101 solution, and the R-101 solution and the S-101 solution were each added to 1000 ml 1
Emulsion Em was prepared in the same manner except that the emulsion was added at a constant speed for 5 minutes.
-103 was prepared.

<M-101a solution> 600 ml of an aqueous solution containing 0.2 mol of sodium p-iodoacetamidobenzenesulfonate <N-101a solution> 300 ml of an aqueous solution containing 0.2 mol of sodium sulfite (Preparation of emulsion Em-104) In the preparation of the emulsion Em-102, the same procedure was carried out up to the addition of the H-101 solution. Thereafter, the silver halide emulsion was subjected to an ultrafiltration module (a polyacrylonitrile membrane having a molecular weight cut off of 13,000, manufactured by Asahi Kasei Corporation). The emulsion was circulated through the used type ALP-1010) until the volume of the silver halide emulsion became 1/5, and then 187 of each of the I-101 solution and the J-101 solution was used.
6 ml accelerated addition (flow ratio between start and end: 1: 2)
Then, the pH was adjusted to 5.0 using G-101. Thereafter, the above-mentioned I-44 solution was added, and 1359 ml of the remaining I-101 solution and 1359 ml of the K-101 solution were successively added for 4 hours.
Accelerated addition in 5 minutes (flow ratio between start and end: 1: 2)
did. Thereafter, the silver potential was adjusted to -40 mV with the P-101 solution, and the R-101b solution and the S-101b solution were added at a constant rate for 15 minutes in place of the R-101a solution and the S-101a solution, and the J-solution was added. Emulsion Em-104 was prepared in the same manner except that 44 solutions were added and ripened for 20 minutes.

Emulsions Em-101 to E prepared as described above
Table 10 shows the features of m-104.

[0230]

[Table 10]

The detailed contents of the items (1) to (6) in the table are as follows. (1) Dislocation line grain ratio (%): Represents the ratio (%) of tabular silver halide grains having dislocation lines in fringe portions to the projected area of all silver halide grains. (2) V ₁ (%): With respect to the volume of silver halide grains, V ₁
(3) A ₁ (mol%): average silver iodide content of V ₁ (mo)
(4) V ₂ (%): V _{2 with} respect to silver halide grain volume
(5) A ₂ (mol)
%): Represents the average silver iodide content (mol%) of V _2. (6) I ₁ > I ₂ Grain ratio (%): Number ratio of tabular silver halide grains satisfying I ₁ > I ₂ (%) Next, the above-prepared emulsions Em-101 to Em-1
Samples 1301 to 1304 were prepared in the same manner as in Example 1 except that Sample No. 04 was used as the emulsion M of the ninth layer in Example 1, and the same development and evaluation as in Example 1 were performed. Are shown in Table 11.

[0232]

[Table 11]

As is clear from Table 11, Samples 1303 and 1304 according to the present invention were Comparative Samples 1301 and 13
No. 02 exhibited excellent performance in both improvement of sensitivity and storage stability.

Example 5 (Preparation of Emulsion Em-311) A comparative emulsion Em-311 was prepared by the following method.

<A-303 solution> Ossein gelatin 36.4 g Potassium bromide 11.1 g 14.6 L with water <B-303 solution> 1.25 mol / L silver nitrate aqueous solution 3657 ml <C-303 solution> 1.25 Mol / L aqueous solution of potassium bromide 3657 ml <D-303 solution> 1 mol / L sulfuric acid required amount <E-303 solution> Ossein gelatin 156.6 g 10% by mass aqueous methanol solution of surfactant (EO-1) 5.2 ml 3795 ml with water <F-303 solution> 28% aqueous ammonia solution required <G-303 solution> 56% acetic acid aqueous solution required <H-303 solution> Ossein gelatin 256.3 g 10 mass of surfactant (EO-1) % Methanol aqueous solution 7.0 ml 2127 ml with water <I-303 solution> 3.5 mol / L silver nitrate aqueous solution 3235 ml <J-303 solution> Odor Potassium 1429 g Potassium iodide 40.7 g Water 3500 ml <K-303a solution> Potassium bromide 1041.3 g Water 2500 ml <K-303b solution> Potassium bromide 968.4 g Potassium iodide 101.7 g Water 2500 L <L- 303 solution> 1.75 mol / L potassium bromide aqueous solution required amount <M-303 solution> 0.1 mol / L potassium iodide aqueous solution 600 ml <O-303 solution> 10% potassium hydroxide aqueous solution required amount In reaction vessel A-303 solution was added, pH was adjusted to 1.9 with D-303 solution, and the solution temperature in the reaction vessel was adjusted to 30.
C-solution B-303 and C-
268 ml of each of the 303 liquids was added at a constant speed for 1 minute by the simultaneous mixing method.

After the completion of the addition, E-303 solution was added, and 3
The temperature was raised to 60 ° C. over a period of 0 minutes. Then, F-303
The solution was added to adjust the pH to 9.3, and after aging for 6 minutes,
The pH was adjusted to 5.8 using G-303 solution.

During this period, the silver potential of the solution (measured with a silver ion selective electrode using a saturated silver-silver chloride electrode as a reference electrode) was measured at L-3.
The solution was controlled at 6 mV using the 03 solution.

Then, while maintaining the potential at 6 mV and accelerating the flow rate by the simultaneous mixing method (the flow ratio between the end time and the start time is 1:12), the B-303 solution and the C-30 solution were taken for 38 minutes.
The remainder of Liquid 3 was added, and Liquid H-303 was added.

Subsequently, 1876 ml of each of the I-303 solution and the J-303 solution was acceleratedly added for 40 minutes (flow ratio at the start and at the end was 1: 2), and the pH was adjusted using the G-303 solution.
Was adjusted to 5.0. Thereafter, the M-303 solution was added for 5 minutes, the pH was adjusted to 5.8 with the O-303 solution, and then 454 ml of the I-303 solution and 454 ml of the K-303a solution.
ml was accelerated for 15 minutes (flow ratio between start and end: 1: 1.5). Subsequently, the remaining 9 of the I-303 solution
05 ml and 905 ml of the K-303b solution were acceleratedly added over 25 minutes (flow ratio at the start and at the end was 1: 1.5).

After grain formation, desalting was carried out according to the method described in JP-A-5-72658, and gelatin was added and dispersed to obtain an emulsion Em-311 having a pH of 5.8 at 70 mV at 40 ° C.

When the silver halide grains in this emulsion were observed with an electron microscope, 92% of the projected area of all the silver halide grains had an average grain size of 1.7 μm, a grain size distribution of 17%, and an average aspect ratio of 8.8. 0 hexagonal tabular monodispersed silver halide grains.

(Preparation of Emulsion Em-312) Emulsion Em
In the preparation of -311, the above-mentioned solution I-44 was added when the addition of the solution B-303 was completed, and the solution J-44 was added when the addition of the solution I-303 was completed.
Emulsion Em-312 was prepared.

(Preparation of Emulsion Em-313) Emulsion Em
In the preparation of -311, the above solution I-44 was added at the end of addition of solution B-303, and thereafter, solution I-303 and J were added.
The same process was performed until 1876 ml of each of the -303 solution was accelerated (the flow ratio at the start and end was 1: 2), and the pH was adjusted to 5.0 with G-303.
The following M-303a solution and N-303a solution were added in place of solution 03, then the pH was adjusted to 10.0 with O-303 solution and aged for 4 minutes, and then the pH was adjusted to 5.0 with G-303 solution.
Was adjusted. Subsequently, 453 ml of the I-303 solution and 454 ml of the K-303a solution were acceleratedly added in 15 minutes (flow ratio between the start time and the end time was 1: 1.5), and then the remaining 905 ml of the I-303 solution and the K-303b solution were added. Of 905 ml for 25 minutes (flow ratio between start and end: 1: 1.5)
Then, the J-44 solution was added. Then, the following P-303
The silver potential was adjusted to -40 mV with the liquid, and the L-
Emulsion Em-313 was prepared in the same manner except that the four liquids were added in an amount equivalent to 1.0 mol of silver halide and ripened for 20 minutes.

<M-303a solution> 600 ml of an aqueous solution containing 0.28 mol of sodium p-iodoacetamidobenzenesulfonate <N-303a solution> 300 ml of an aqueous solution containing 0.28 mol of sodium sulfite <P-303 solution> 3.5 Required amount of mol / L aqueous potassium bromide solution (Preparation of emulsion Em-314) In the preparation of emulsion Em-311, the same procedure as above was performed up to the addition of the H-303 solution, and then the silver halide emulsion was subjected to an ultrafiltration module ( Through a type ALP-1010 using a polyacrylonitrile membrane having a molecular weight cut off of 13,000, manufactured by Asahi Kasei Kogyo Co., Ltd., until the volume of the silver halide emulsion is reduced to 1/5. And 187 each of J-303 solution
6 ml accelerated addition (flow ratio between start and end: 1: 2)
Then, the pH was adjusted to 5.0 using G-303. Thereafter, the M-303a solution and N-3 were replaced with the M-303 solution.
03a solution was added, and then the pH was adjusted to 10.0 with O-303 solution.
Adjust to 0 and ripen for 4 minutes, then pH with G-303 solution
Was adjusted to 5.0. Thereafter, the above-mentioned I-44 solution was added, and then 454 m of I-303 solution and K-303a solution were added.
1 for 15 minutes (flow ratio at start and end: 1: 1.5), and then 905 m of remaining I-303 solution
1 and 905 ml of the K-303b solution were acceleratedly added over 25 minutes (the flow ratio at the start and at the end was 1: 1.5). Thereafter, the silver potential was adjusted to -40 mV with the P-303 solution,
The L-4 solution was added in an amount of 1.0 mol equivalent with silver halide, and after ripening for 30 minutes, the J-44 solution was added, and
Emulsion Em-314 was prepared in the same manner except that ripening was performed for 0 minutes.

Emulsions Em-311 to E prepared as described above
Table 12 shows the features of m-314.

[0246]

[Table 12]

The detailed contents of the items (1) to (6) described in the table are as follows. (1) Dislocation line grain ratio (%): Represents the ratio (%) of tabular silver halide grains having dislocation lines in fringe portions to the projected area of all silver halide grains. (2) V ₃ (%): With respect to the volume of silver halide grains, V ₃
(3) A ₃ (mol%): average silver iodide content of V ₃ (mo)
(4) A ₄ (mol%): average silver iodide content of V ₄ (mo)
represents a _{l%) (5) A 5} (mol%): Average iodide content of V ₅ (mo
It represents a l%) (6) I _1> I ₂ particles Ratio (%): I _1> incidentally representing the number of tabular silver halide grains is I ₂ ratio (%) Emulsion Em-311 to the above-mentioned prepared Emulsion Em-3
Samples 1401 to 1404 were prepared in the same manner as in Example 1 except that Sample No. 14 was used as the ninth layer emulsion M in Example 1, and the same development and evaluation were performed as in Example 1, and the obtained results were obtained. Are shown in Table 13.

[0248]

[Table 13]

As is clear from Table 13, the samples 1403 and 1404 according to the present invention are comparative samples 1401 and 1414.
No. 02 exhibited excellent performance in both improvement of sensitivity and storage stability.

Example 6 (Preparation of Emulsion Em-321) Emulsion Em-321 was prepared by the following method.

<A-304 solution> Ossein gelatin 36.4 g Potassium bromide 11.1 g 14.6 L with water <B-304 solution> 1.25 mol / L silver nitrate aqueous solution 3657 ml <C-304 solution> 1.25 Mol / L aqueous potassium bromide solution 3657 ml <D-304 liquid> 1 mol / L sulfuric acid required amount <E-304 liquid> Ossein gelatin 156.6 g 10% by mass aqueous methanol solution of surfactant (EO-1) 5.2 ml 3795 ml with water <F-304 solution> 28% aqueous ammonia solution required <G-304 solution> 56% acetic acid aqueous solution required <H-304 solution> Ossein gelatin 256.3 g 10 mass of surfactant (EO-1) % Methanol aqueous solution 7.0 ml 2127 ml with water <I-304 solution> 3.5 mol / L silver nitrate aqueous solution 3235 ml <J-304 solution> Odor Potassium 1212 g Potassium iodide 52.3 g Water 3000 ml <K-304 solution> Potassium bromide 1237 g Potassium iodide 17.4 g Water 3000 ml <L-304 solution> 1.75 mol / L Potassium bromide aqueous solution Required amount <M -304 solution> 0.1 mol / L aqueous solution of potassium iodide 600 ml <O-304 solution> 10% aqueous solution of potassium hydroxide Required amount A-304 solution is added into a reaction vessel, and pH 1.0 using solution D-304. 9 and adjust the solution temperature in the reaction vessel to 30.
C-solution B-304 and C-
268 ml of each of the 304 liquids was added at a constant speed by the simultaneous mixing method for 1 minute.

After the completion of the addition, E-304 solution was added, and 3
The temperature was raised to 60 ° C. over a period of 0 minutes. Then, F-304
The solution was added to adjust the pH to 9.3, and after aging for 7 minutes,
The pH was adjusted to 6.1 using G-304 solution.

During this period, the silver potential of the solution (measured with a silver ion selective electrode using a saturated silver-silver chloride electrode as a reference electrode) was L-3.
The solution was controlled at 6 mV using the solution 04.

Then, while maintaining the potential at 0 mV and accelerating the flow rate by the simultaneous mixing method (the flow ratio between the start time and the end time is 1:12), the B-304 solution and the C-30 solution were used for 38 minutes.
The remainder of Liquid 4 was added, and Liquid H-304 was added.

Subsequently, 1876 ml of each of the I-304 solution and the J-304 solution was acceleratedly added in 40 minutes (the flow ratio at the start and at the end was 1: 2), and the pH was adjusted to 5.0 using the G-304 solution. Adjusted to zero. Thereafter, the M-304 solution was added in 5 minutes, the pH was adjusted to 5.8 with the O-304 solution, and the remaining 1359 ml of the I-304 solution and 13 ml of the K-304 solution were subsequently added.
59 ml was acceleratedly added for 25 minutes (the flow ratio between the start time and the end time was 1: 2).

After grain formation, desalting was carried out according to the method described in JP-A-5-72658, and gelatin was added and dispersed to obtain an emulsion Em-321 having a pH of 5.8 at 70 mV at 40 ° C.

When the silver halide grains in this emulsion were observed with an electron microscope, 90% of the projected area of all the silver halide grains had an average grain size of 1.7 μm, a grain size distribution of 15%, and an average aspect ratio of 8.8. 0 hexagonal tabular monodispersed silver halide grains.

(Preparation of Emulsion Em-322) Emulsion Em
In the preparation of -321, the liquid I-44 was added at the end of the addition of the liquid B-304, and the liquid J-44 was added at the end of the addition of the liquid I-304.
Emulsion Em-322 was prepared.

(Preparation of Emulsion Em-323) Emulsion Em
In the preparation of -321, the above solution I-44 was added at the end of addition of solution B-304, and thereafter, solution I-304 and J were added.
1876 ml of the -304 solution was acceleratedly added (flow ratio between the start time and the end time was 1: 2), and the same procedure was performed until the pH was adjusted to 5.0 using G-304.
Solution M-101a and solution N-101a were added in place of solution 04, then the pH was adjusted to 10.0 with solution O-304, and the mixture was aged for 4 minutes, and then pH was adjusted to 5.0 with solution G-304.
Was adjusted. Continue with I-304 solution and the following K-304a
1362 ml of each of the solutions was acceleratedly added in 40 minutes (the flow ratio at the start and at the end was 1: 2), and the J-44 solution was added. Thereafter, the silver potential was adjusted to −40 mV with the P-304 solution, and the L-4 solution described in Example 1 was added in an amount of 1.0 mol equivalent with silver halide, followed by aging for 20 minutes.
Emulsion Em-323 was prepared.

<K-304a solution> Potassium bromide 1125 g Potassium iodide 174.3 g Water 3000 ml <P-304 solution> 3.5 mol / L aqueous solution of potassium bromide Required amount (Preparation of emulsion Em-324) In the preparation of Em-321, the same procedure was carried out up to the addition of the H-304 solution, and then the silver halide emulsion was filtered using an ultrafiltration module (a polyacrylonitrile membrane having a molecular weight cut off of 13,000, manufactured by Asahi Kasei Kogyo Co., Ltd.). The silver halide emulsion was circulated until the volume of the emulsion became 1/5, and then 187 of each of I-304 solution and J-304 solution was obtained.
6 ml accelerated addition (flow ratio between start and end: 1: 2)
Then, the pH was adjusted to 5.0 using G-304. Thereafter, the M-101a solution and the N-1 were replaced with the M-304 solution.
01a solution was added, and then the pH was adjusted to 10.0 with O-304 solution.
Adjusted to 0 and aged for 4 minutes.
Was adjusted to 5.0. Thereafter, the I-44 solution was added, and then 1362 ml of the I-304 solution and the K-304a solution were each added at an accelerated rate for 40 minutes (a flow ratio between the start time and the end time was 1: 2). The silver potential was adjusted to −40 mV with the P-303 solution, the L-4 solution was added in an amount of 1.0 mol equivalent with silver halide, and after ripening for 30 minutes, the J-44 solution was added, followed by 20 minutes. Emulsion Em-324 was prepared in the same manner except for ripening.

Emulsions Em-321 to E prepared as described above
Table 14 shows the features of m-324.

[0262]

[Table 14]

The details of the items (1) to (6) described in the table are as follows. (1) Dislocation line grain ratio (%): Represents the ratio (%) of tabular silver halide grains having dislocation lines in fringe portions to the projected area of all silver halide grains. (2) V ₃ (%): With respect to the volume of silver halide grains, V ₃
(3) A ₃ (mol%): average silver iodide content of V ₃ (mo)
(4) A ₆ (mol%): average silver iodide content (mo) of V ₆
(5) A ₇ (mol%): average silver iodide content of V ₇ (mo)
represents a l%) (6) I _1> I ₂ particles Ratio (%): I _1> incidentally representing the number of tabular silver halide grains is I ₂ ratio (%) Emulsion Em-321~ prepared above Emulsion Em-3
Samples 1501 to 1504 were produced in the same manner as in Example 1 except that 24 was used as the emulsion M of the ninth layer in Example 1, and the same development and evaluation as in Example 1 were performed. Are shown in Table 15.

[0264]

[Table 15]

As is clear from Table 15, Samples 1503 and 1504 according to the present invention were Comparative Samples 1501 and 1504.
No. 02 exhibited excellent performance in both improvement of sensitivity and storage stability.

[0266]

According to the present invention, a silver halide photographic emulsion having excellent sensitivity and storage stability and a silver halide photographic material using the same can be provided.

Claims (7)

[Claims] 1. A silver halide photographic emulsion comprising a dispersion medium and silver halide grains, I ₁ (mol%) the average silver iodide content of the outermost layer in the main planar portion, I the side portion ₂ (mol% ), 50% of tabular silver halide grains satisfying I ₁ > I _2.
% (Number) and reduction sensitized. 2. A silver halide photographic emulsion containing a dispersion medium and silver halide grains, comprising tabular silver halide grains having at least three silver halide layers of the following internal phase, intermediate phase and external phase. And a reduction sensitized silver halide photographic emulsion. Internal phase: average silver iodide content is 0.5 to 30 mol% and silver content ratio is 5 to 85%. Intermediate phase: average silver iodide content is 1/2 or less of the internal phase and silver content ratio is 2 to 85% External phase: average silver iodide content is higher than that of the intermediate phase, and silver ratio is 5 to 50% 3. A silver halide photographic emulsion comprising a dispersion medium and silver halide grains, I ₃ (mol%) in the fringe portion of the silver iodide content, when I ₄ a (mol%) at the apex portion, 0
Tabular silver halide grains satisfying ≦ I ₄ / I ₃ ≦ 1.0
A silver halide photographic emulsion containing 0% or more (number) and being reduction sensitized. 4. In a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains are tabular silver halide grains having dislocation lines in fringe portions, And the volume ratio of the shell (V ₁ ) in the dislocation line forming region is from 10% to 10% of the silver halide grain volume.
Is 50%, the average silver iodide content (A ₁₎ is 4 to 20 mol% of the dislocation line forming region of the shell (V _1), in the shell (V ₁₎ of the dislocation line forming region most have outermost shell (V ₂₎ on the outside, the volume ratio of the outermost shell (V ₂₎ is 1% to 15% of the silver halide grain volume, an average of outermost shell (V ₂₎ A silver halide photographic emulsion having a silver iodide content (A ₂ ) of 0 to 3 mol% and being reduction sensitized. 5. A halogen containing a dispersion medium and silver halide grains.
Projection surface of all silver halide grains in silver halide photographic emulsion
50% or more of the product has dislocation lines in the fringe portion.
Silver iodide grains and the average silver iodide content
Some silver halide phases (V_Three) Outside the silver halide phase
(V_Four) Separated silver halide phase (V _Five) Inside the particle
And the silver halide phase (V_Four) Average silver iodide content
A_FourMol%, silver halide phase (V_Five) Average silver iodide content
A_Five0 ≦ A when mol%_Four/ A_Five≦ 1.0
And halogen sensitized by reduction sensitization
Silver halide photographic emulsion. 6. In a silver halide photographic emulsion containing a dispersion medium and silver halide grains, 50% or more of the projected area of all silver halide grains are tabular silver halide grains having dislocation lines in fringe portions, The average silver iodide content in the silver halide phase (V ₆ ) inside the silver halide phase (V ₃ ) having the maximum average silver iodide content is A ₆ mol%, and the silver halide phase (V _{When the} average silver iodide content in the silver halide phase (V ₇ ) outside of ₃ ) is A ₇ mol%, 0 ≦
A silver halide photographic emulsion characterized in that A ₆ / A ₇ ≦ 1.0 and that the emulsion is reduction sensitized. 7. A silver halide photographic light-sensitive material comprising the silver halide photographic emulsion according to claim 1 in at least one silver halide photographic emulsion layer on a support. material.