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Патент USA US3077461

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Sates Patent "
3,077,456
” 1C6
Patented Feb. 12, 1953
1
2
‘ EXAMPLE III
3,077,456
The procedure of Example I was repeated with the
PHOSPHORESCENT GLASSES AND METHOD
OF MAKING SAME
Carroll J. Biliian, Perrys’ourg, Ohio, assignor to Owens
Illinois Glass Company, a corporation of Ohio
same results except that 8 parts of ZnS were used and a
proportionate lesser amount (92 parts) of B203, ZnO, ,
No Drawing. Filed Aug. 10, 1959, Ser. No. 832,423
9 Claims. (Cl. 252—301.6)
This invention relates to phosphorescent glasses and
EXAMPLE IV
Phosphorescent Solder Glass (Conducting)
the method of making the same. More particularly this 10
invention relates to conducting and non-conducting solder
glasses which exhibit phosphorescence and to the method
Ingredients:
Parts I
B203
___
___ __ __
_ _ . __
ZnO
_________________________________ _._
7.7
11.7 '
PbO _________________________________ __ 70.0
of preparing such solder glasses.
Si02 ._
The use of zinc sul?de and cadmium sul?de including
complexes thereof as phosphorescent material is well
F
known. Moreover, methods for the incorporation of these 10‘
phosphors in porcelain enamels are also well known;
ZnS
___
1.8
_________________________________ __
Ag
____
3.8
__
5.0
However, the use of a phosphor such as zinc sul?de in
Patties, which were formed as in Example I above and
?red at_380° C. for 20 minutes, had an electrical resistance
ground solder glass, whether conductive or non-conductive
of about 1/2 ohm using silver paint for contact spots.
and then ?ring the same at such a low temperature as to 20 Using three different current sources for excitation, name4
ly, a DC. source (20 ampere limit), a 60 cycle A.C. source leave the zinc sul?de unreacted is believed to be new. The
resulting ?red solder glass containing zinc sul?de exhibits
(6 ampere limit), and 60-6000 cycle A.C. source (2
phosphorescence and can be used as a sealing material or
ampere limit), it was noted that a visible glow occurred
a decorative medium for illuminating clock dials and in
strument panels.
I
at 2 amperes. Higher current intensities gave brighter,
25 glows providing the amperage did not exceed 8-10 amperes,
when melting of the patties or samples occurred.
Accordingly it is an object of this invention to provide
a novel solder glass which exhibits luminescent properties
when under the in?uence of radiant and electrical energy
and‘ to provide a method of making the same.
'
EXAMPLE V
Phosphorescent Solder Glass (Conducting)
,
_It is. a further object of this invention to provide phos 30 The procedure of Example IV was repeated with the '
phorescent solder glasses as sealing and decorating media;
same results of phosphorescence but the following com
‘It is a further object of this invention to provide con-‘
position was used.
ducting and non-conducting solder glasses having phos
phorescent properties.
It is a still further object of this invention to conduct
the ?ring at low temperatures so as to prevent disintegra
Ingredients:
35
,
Parts
B203 _________________________________ __
,
7.4
ZnO
_________________________________ __
11.2
tion of the phosphor. Additional objects will be apparent
PbO
_
67.1 '
from the description which follows.
SiOz
ZnS
.
The novel process of this invention comprises ?ring a
mixture of ground solder glass and a phosphor such as
zinc sul?de at temperatures under 400° C. whereby the
40
1.7
7.6 ‘I
,
_____________ -;- ------------------- _.-.>
5-0
EXAMPLE VI
glass resulting therefrom possesses phosphorescent prop
erties.
_____
Phosphorescent Solder Glass (Conducting)
'
The present invention will be more completely underl
.The procedure of Example IV was repeated with‘the
stood by reference to the following examples in which all 45 same results of conductive phosphorescence but the fol-p
parts and percentages are by weight unless otherwise
’
speci?ed.
.
‘50
‘
____ __
_
_
___
12.31
PbO
_______________ __-_____-_ _________ __
73.67
SiOz _______________________ __>___.._e____.
1.92
ZnS
4.0
>
-'
_____
'
Parts _
PbO
_
_‘
~
_
'
66.4
1.7
ZnS
________________________________ _V__
' Ag
55
'
7.3 _
__, 11.0v
‘ S102
8.10
ZnO
__
'
‘
ZnO,
Parts
B203 ________________________________ __
’
a
B203 ____________ _‘___,________________ _.__..
Phosphorescent Solder Glass
.
_
Ingredients:
EXAMPLE I
Ingredients:
lowing was used.
‘
_..__
'
.
___
3.6v I
110.0, ,
EXAMPLE VII
,
Phosphorescent Solder Gloss (Conducting)
1A ‘glass in powder‘ form consisting of the above ingredie "
'The' procedure 'o'f'Example IV' was‘ repeated withthe'~
ents, namely, B203, ZnO, PhD and SiOz in the proportions
same results of phosphorescence but the following compo
by weight set forth, was mixed with the aforementioned 60 sition was used.
weight of the phosphor, 2115, and shaped into patties of
Ingredients:
Parts
1 mm. thick and 1 inch in diameter using a binder of
1.5% nitrocellulose in amyl acetate and fired at 380° C.
for 20 minutes. The resulting solder glass exhibited
phosphorescence and was suitable for clock dials, instru
65
ment panels, and the like.
EXAMPLE II
The procedure of Example I was repeated with the
B203 _
7.0
ZnO
PbO
10.6
____
63.5
sio2 _-__
1.7
ZnS
7.2
Ag
_____ __ 10.0
The above examples are merely by way of illustration
same results except that 1 part of ZnS was used and a 70 and variations apparent to one skilled in the art may
proportionate larger amount (99 parts) of B203, ZnO,
PhD, and SiOZ.
be made without departing from the spirit of the inven
tion disclosed. For example, other phospors such as
‘3,077,456
3
4
CdS may be employed. In addition other solder-glass
selected from the class consisting of zinc sul?de and cad
compositions may be employed such as the following.
mium sul?de.
Ingredients:
3. A method of preparing phosphorescent solder
glasses comprising ?ring at a temperature of about 380
400" C. and for a period of about 4 to 20 minutes, a
Parts
ZnO
B203 ________________________________
-’
.._
__
12.83
PbO
76.22
SiO'z
"
'
_-_
"
-._
-
-
.'__' __________ __'____‘ ____ __'___’____ __
powdered glass mixture of the following composition:
75 to 80% PbO; 7 to 10% B203; 7 to 14% ZnO; and
1.5 to 3% SiO2 and which has added to said mixture
(a) from 1 to 10% of a phosphor selected from the class
2.0
In general it has been found that ground glass composi—
consisting of ,zinc sul?de and cadmium sul?de and ,(b)
tions which consist of about 75-80% PbO; of about
7-14% ZnO; of about 7-1'0% B203; and of about 1.5-3%
SiOz to which has been added from 1-10% of a phospor
such as ZnS provide not only the properties of a low
from 5 to 10% of a conducting material selected from
the class consisting of silver, gold and platinum. ,
4. A method of preparing phosphorescent solder
glasses comprising ?ring at a temperature of about 380°
and contraction but phosphorescence. However, the
and for a period of about 20 minutes, a powdered glass
preferred range of phospor in the above composition
mixture 'of the following composition; 75 to 80% PbO;
is from v4--8,%. Where conductance is also desired, the
7 to 10% B203; 7 to 14% ZnO; and 1.5 to 3% SiO,,,
further addition of 5—10% of a conductor such as silver
and which has added to said mixture (11) from 1 to 10%
may be employed with excellent results. Although the
of a phosphor selected from the class consisting of zinc
above ground glass and phosphor-silver mixture may be 20 sul?de and cadmium sul?de .and (b) from 5 to 10%
heated from 4 to 40 minutes and ‘from 360-440° C., the
of a conducting material selected from the class con
preferred ‘heating period is 4 to '20 minutes and the pre
sisting of silver, gold and platinum.
ferred temperature range is 380-400° C. Care must
5. The method of claim 4 in which the phosphor is
zinc sul?de and the conducting material is silver.
be taken not to heatthe glass mixture for an unduly
softening temperature and satisfactory thermal expansion
long ‘period of time even at the lower temperatures since 25
6.I A method of preparing phosphorescent solder
the phosphor willlose its phosphorescent properties.
glasses comprising ?ring at a temperature of about 360
However, the duration of the heating period for a given
temperature ‘can be readily determined for each glass
to 440° C. and for a period of about 4 to '40 minutes,
a ‘powdered glass mixture of the following ‘composition:
75 to 80% PbO; 7 1O 14% ZnO; 7 to 10% B203; and
It is obvious that various modi?cations may be made 30 1.5 to 3% SIiO2 to which has been added from I to, 10%
in the above formulations which would still come within
of a phosphor selected from the class consisting of zinc
the scope of the present invention. For example other
sul?de and cadmium sul?de.
conducting materials ‘such as ‘gold and platinum may be
7. A Imethod of preparing phosphorescent solder
composition by routine testing.
I
I
I
employed with equally good results. Morever, organic
glasses comprising ?ring at a temperature of about 360
binders other than nitrocellulose in amyl acetate may
to 440° C. and for a period of about '4 to 40 minutes, -
be used without departing from the spirit vof the invention
a powdered glass mixture of the, following composition:
herein disclosed.
75 to 80% PbO; 7 to 14% Zn(); 7 to 10% B203; and
1.5 to 3% sio2 10 which has been added from 1 ‘to 10%
of a phosphor selected from the class consisting of ‘zinc
sul?de and cadmium sul?de and from 5 to 10% of a’con
Organic binders which I have found
satisfactory include gelatin dissolved in water, camphor
with cellulose nitrate, 'dibutyl phthalate with cellulose
acetate, a'myl and butyl alcohols, paraffin, biphenyl, etc.
ducting material.
As indicated by the modi?cations given above, it is
to be understood that within the scope of the appended
claims, ‘the invention may be practiced otherwise than as
speci?cally described.
8. The product produced by the method of claim 6.
9. The product produced by ‘the method of claim 7.
I
The term ?ring as employed herein means heating the 45
composition until it is sintered or fused.
I claim:
I
I
I
References Cited in the ?le of this patent
UNITED STATES PATENTS
:
III.II A method of preparing phosphorescent ‘solder
2,130,215
2,643,020
glasses comprising ?ring at a temperature of about 380
Young ‘..; _____ _-_ _____ “Sept. 13, 1938
Dalton c___>__-_ _______ __ June 23, 1953
4009 C. and for a period of about 4-20 minutes, a pow 60
2,837,487
Huttar~ ____ __'..__' ______ __ June a, 1958
deIredIglass mixture of the following range in composi
tion: 75I_Ito 80% _Pb_O; 7 to,14% ZnO; 7 to_,10% B203;
2,866,117
2,924,540
Walker et a1. ________ __ Dec. 23, 1958
D’Andrea ____________ __ Feb. 9, 1960
and 1.5 to 3I%I§iQ2IIto which has been added from 1 to
2,945,128
Kuan-Han Sun et al. ..___ July 12, 1960
10% or; phosphorselected from the class consisting of
zinc sul?de and cadmium sul?de._
Aminethod of preparing phosphorescent solder
glasses I_coIrnIpIrIi_svinI'g_ firing at a temperature of about 380"
CI. for a period of about 20 minutes, a powdered glass
mixture of the following composition: 75 to 80% PbO;
7 to 14%_ ZnO; 7 to 10% B203; and-1.5 to 3% Slog
to which has been added from 1 to 10% of a phosphor
FOREIGN PATENTS
55
625,466
Great Britain ________ __ June 28, 1949
OTHER ‘REFERENCES
Egelstaff: “Glass ‘Scintillators for Prompt Detection of
Intermediate Energy Neutrons,” Nuclear Instruments 1
(1957), 197-199; North Holland Publ. Co., Amsterdam.
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