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Патент USA US2126319

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Aug. 9, 1938.
v G. E. FALLESEN ET Al.
4
PRINT-OUT EMULSION
'
2,126,319‘ _
‘
Filed Feb. 9,1937
Prinl-out Emulsion ‘ formed of Silver Hydroxide
Organic Alkaliv Complex and a Halide, containing
a Hydrazine or Hydrozylamine Salt
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' ' Glass or cellulose
ester support
George E.Falle5en
Burl H.INVENTORS
Carroll
-
_ BY .
@JMM
ATTORNEYS
Patented Aug. 9, 1938
2,126,319
, UNITED STATES
PATENT. ' ‘OFFICE
2,126,319
PRINT-OUT EMULSION
George E. Fallesen and Burt H. Carroll, Roches
ter, N. Y., assignors to Eastman Kodak Com
pany, Rochester, N. Y., a corporation of New
Jersey
'
Application February 9, 1937, Serial No. 124,866 ‘
12 Claims.
This invenion relates to photographic material
and more particularly to a print-out photographic
emulsion having increased sensitivity to light.
Of the two types of commonly used photo
5
graphic emulsions, known respectively as develop
ing emulsions and print-out emulsions, the pres
ent invention relates primarily to‘ the latter type.
In these emulsions, a visible image is produced
directly by the action of light, as compared‘ with
10 developing emulsions in which the image is ren
dered visible, after exposure, by treatment with
a developing solution.
the prior patent, No. 2,030,860, consist of organic '
or inorganic salts othydrazine and hydroxyl
amine.
We prefer to use hydrazine sulfate and
hydroxyl amine hydrochloride, although other
organic or inorganic salts of these compounds
maybeused.
.
The following examples illustrate methods '01’
forming highly sensitive print-out emulsions suit-_
able for coating on glass or cellulose ester sup
ports according to our invention:
18, 1936, to C. J. Staud and ‘G. E. Fallesen, there
15 was disclosed a method for making a highly sensi
tive print-out emulsion. According to the inven
tion disclosed therein,‘ the print-out emulsion was
produced by precipitating silver hydroxide with
ammonia from a silver nitrate solution, dissolving
20 the precipitate in an organic base, mixing this
solution, with a carrier such as gelatin and adding
to it a halide such as potassium bromide. To the
emulsion thus formed, there could be added a fur
ther quantity of silver nitrate or an additional
25 amount of sodium nitrite, which results in an in
'
It was found that when the emulsions made ac-'
cording to our prior patent were coated on glass
or, cellulose ester supports, the sodium nitrite
'30 exhibited a tendency to crystallize out. A fur-,
ther disadvantage of ‘the sodium nitrite was that
it tended to weaken the gelatin in, the emulsion,
‘ thereby increasing the dii?culties of coating on
glass or cellulose ester supports. Although a
coating of the emulsion with excess silver nitrate
could be made on glass without crystallization en
suing, there was found to be an appreciable loss of
_ print-out sensitivity without the sodium nitrite.
“ It is, therefore, an object of the present inven
tion to provide a highly sensitive print-out emul
sion which may be coated on a cellulose ester or
glass support without objectionable crystallization
of the emulsion constituents. A further object is
to provide a print-out emulsion which may be
' 10
Example I
'
In U. S. Patent'No. 2,030,860, granted February
creased sensitivity. ‘
(Cl. 95—7)
Three solutions are made up as follows: _
Solution A is formed by dissolving‘ 100 grams of
silver nitratevin 300 cc. of water and adding to 15'
this solution 20 cc. of ammonium hydroxide (28%
concentration). A precipitate of silver hydroxide
is formed and this is redissolved in 140 cc. of
pyridine.
'
.
,
-
Solution B consists of 65 grams of sodium chlo
ride in 252 cc. of water.
‘
Solution C consists of 152 grams of gelatin in
3000 cc. 01' water.
'
To make up the emulsion from these solutions
one-half of Cris poured into A and the other hali.I 25
of C is poured into B. AC and BC are then poured
together at 40° C. The temperature of the mix
ture is gradually raised until it reaches 759C. at
the end of 15 minutes. The ‘mixture is then rap
idly chilled to 35° C., set andxshredded. The 30
emulsion is washed for one hour and allowed to
drain.
30 grams of gelatin are then added and ’
dissolved at 40° C. A solution of 4 grams of
hydrazine sulphate in 160 cc. of water is then
added and the emulsion chilled to coating tem 35
perature.
_
'
'
‘Example II
An emulsion is made up as in Example I. , After
adding the .30 grams .of gelatin at 40° C., a solu
tion of 4 grams of hydroxylamine hydrochloride 40
in 160 cc.-of water is added and the emulsion
chilled to coating temperature as before.
' In addition to pyridine, other organic bases or
easily coated on glass or cellulose ester supports. - alkalies may be used to dissolve the silver hydrox
These objects are accomplished by substituting
an organic or inorganic acid salt of hydrazine or
hydroxylamine for sodium nitrite and excess silver
nitrate in the emulsion of the prior patent of
Stand and Fallesen, No. 2,030,860.
In the accompanying drawing, the single ?gure
is a sectional view of a ?lm or plate formed ac
cording to our invention.
The materials which we .use instead of sodium
nitrite and excess silver nitrate in the emulsion of
20
- ,
ide precipitate. These include the amines, such
as methylamine, benzylamine, naphthylamine,
and triethanolamine; heterocyclic nitrogen bases
such as pyridine, piperidine, quinoline, (in methyl
alcohol), acridine (in methyl alcohol), and a-pic
oline; amides such as acetamide. As halides, we
have found that both potassium bromide and so
dium chloride, with or without further addition of
potassium iodide, are satisfactory.
_
As disclosed in the Stand and Fallesen Patent
2
2,126,819
_
No. 2,030,860, the gelatin used to disperse the ' then adding to the emulsion approximately 2.2%,
sensitive salt may be replaced by cellulose mixed based on the weight of gelatin, of a salt selected
esters such as cellulose acetate phthalate. In from the group consisting of hydroxylamine hy
the present case, the halide used to form the drochloride and hydrazine sulfate.
5. A process of producing a light-sensitive
sensitive salt may be replaced by bromacetic acid
or other halogenated aliphatic‘ acids or with emulsion which comprises precipitating silver
other bromide or halide substituted compounds, hydroxide in an aqueous solution,‘dissolving the
' such as bromo-esters, in the manner disclosed in
our prior patent.
In the single ?gure of the accompanying draw
10
ing, we have shown in sectional view a photo
graphic element formed according to our inven
tion. As shown therein, l is the‘ support of glass
or a cellulose ester and 2 is the sensitive emulsion
15 formed according to our process.
‘
The emulsions formed according to our inven
tion coat out as- pure white layers. When ex
posed to light, the emulsions produced with hy
drazine salts produce a deep violet density and
20 those formed with hydroxylamine salts produce
a deep lavender blue density. The colors formed
are much more intense than can be produced by
a print-out emulsion of the same formula with
out the hydrazine or hydroxylamine salts. The
sensitivity of the emulsions formed according to
our invention is about the same as that of the
emulsion of Fallesen and Stand U. S. Patent No.
2,030,860. In addition to being used as print
out emulsions, the emulsions formed according to
our invention may also be developed.
It- is to be understood that the examples in
cluded in the above speci?cations are illustrative
only and that our invention comprises all modi?-_
cations and equivalents coming within the scope
of the appended claims.
'
‘
We claim:
1. A process of producing a light-sensitive
emulsion which comprises precipitating silver
hydroxide in an aqueous solution, dissolving the
precipitate in an organic alkali, mixing the solu
tion with an inert carrier therefor and adding an
alkali metal halide to the mixture to form an
precipitate in a heterocyclic nitrogen base, mix
ing the solution with gelatin and adding an alkali
metal halide to the mixture to form an emulsion,
and then adding to the emulsion approximately
2.2%, based on the weight of gelatin, of a salt
selected from the group consisting of hydroxyl
amine hydrochloride and hydrazine sulfate.
6. A process of producing a light-sensitive
emulsion which comprises precipitating silver
hydroxide in an aqueous solution, dissolving the
precipitate in a heterocyclic nitrogen base, mix
ing the solution with gelatin and adding an al
kali metal halide to the mixture to form an 20
emulsion, and then adding approximately 2.2%,
based on the weight of gelatin, of hydroxylamine
hydrochloride to the emulsion.
7. A process of producing a light-sensitive
emulsion which comprises precipitating silver 25
hydroxide in an aqueous solution, dissolving the
precipitate in a heterocyclic hydrogen base, mix
ing the solution with gelatin and adding an al
kali metal halide to the mixture to form an emul
sion, and then adding approximately 2.2%, based
30
on the weight of gelatin, of hydrazine sulfate to
the emulsion.
8. A light-sensitive surface comprising the
product resulting from the reaction of a com
plex solution of silver hydroxide in an organic
alkali, on an alkali metal halide in the presence
of an inert carrier, and containing approximate
ly 2.2%, based on the weight of inert carrier, of
a salt selected from the group consisting of hy
droxylamine hydrochloride and hydrazine sul
fate.
40
'
9. A photographic element comprising a cellu
lost ester support coated with gelatin containing
based on the weight of inert carrier, of salt se
the product resulting from the reaction of a com
lected from the group consisting of hydroxyla
plex solution of silver hydroxide in an organic
mine and hydrazine salts.
2. A process of producing a light-sensitive . alkali on an alkali metal halide, and containing
emulsion which comprises precipitating silver approximately 2.2%, based on the weight of gel
hydroxide‘ in an aqueous solution, dissolving the atin, of hydroxylamine hydrochloride.
10. Aphotographic element comprising a cel
60 precipitate in an organic alkali, mixing the solu- ' lulose ester support coated with gelatin'contain
tion with an inert carrier therefor and adding
an alkali metal halide to the mixture to form an ing the product-‘resulting from ‘the reaction of a
emulsion, and then adding approximately 2.2%, complex solution‘bt silver hydroxide in an or
emulsion, and then adding approximately 2.2%,
based on the weight of inert carrier, of salt se
55 lected from the group consisting of hydroxyl
amine hydrochloride and hydrazine sulfate.
3. A process of producing a light-sensitive
ganic alkali on an alkali i'rie'tabhalide, and con
taining approximately 2.2%, based on the weight
of gelatin, of hydrazine sulfate.‘
11. A photographic element comprising a glass
emulsion which comprises precipitating silver
support coated withgelatin containing the procl
hydroxide in an aqueous solution, dissolving the
precipitate in an organic alkali, mixing the solu
tion with gelatin and adding an alkali metal hal
ide to the mixture to form an emulsion, and then
an alkali metal halide, and containing approxi
mately 2.2%, based on the weight of gelatin, of
adding to the emulsion approximately 2.2%,
based on the weight of gelatin, of a salt selected
65 from the group consisting of hydroxylamine and
hydrazine acid salts.
‘
.
4. A process of’ producing a light-sensitive
emulsion which vcomprises precipitating silver
hydroxide in an aqueous solution, dissolving the
precipitate in an organic alkali, mixing the solu
tion with gelatin and adding an alkali metal hal
ide to the mixture to form an emulsion, and
uct resulting from the reaction of a complex so
lution of silver hydroxide in an organic alkali on 60
hydroxylamine hydrochlorida.
12. A photographic element comprising a glass
support coated with gelatin containing the prod
uct resulting from the reaction of a complex so
lution of silver hydroxide in an organic alkali on
an alkali metal halide, and containing approxi
mately 2.2%, based on the weight of gelatin, of
hydrazine sulfate.
>
GEORGE E. FALLESEN.
BURT H. CARROLL.
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