U.S. patent number 3,869,614 [Application Number 05/342,263] was granted by the patent office on 1975-03-04 for phosphor assembly for ultraviolet light absorption detector.
This patent grant is currently assigned to Varian Associates. Invention is credited to Miner N. Munk.
United States Patent |
3,869,614 |
Munk |
March 4, 1975 |
**Please see images for:
( Certificate of Correction ) ** |
PHOSPHOR ASSEMBLY FOR ULTRAVIOLET LIGHT ABSORPTION DETECTOR
Abstract
An inert phosphor package or enclosure assembly, especially for
use with an ultraviolet light absorption detector in liquid
chromatography, and a process for manufacture. A wave length
converting phosphor for location in a lamp housing is protected
from the surrounding environment and abrasion by an encapsulating
container comprised of a rigid base with a phosphor receptacle or
pocket, a protective cover or window over the pocket transparent to
ultraviolet radiation, and a heat-fused seal between the window and
base. The package is fabricated by filling the pocket with a
phosphor powder, covering the powder with the window, applying a
fusible sealing strip, heating the assembly to a first temperature
to dry the phosphor without fusing the sealing strip, and heating
to a higher temperature without intermediate cooling to seal the
window to the base.
Inventors: |
Munk; Miner N. (Walnut Creek,
CA) |
Assignee: |
Varian Associates (Palo Alto,
CA)
|
Family
ID: |
23341066 |
Appl.
No.: |
05/342,263 |
Filed: |
March 16, 1973 |
Current U.S.
Class: |
250/365;
250/483.1; 250/461.1 |
Current CPC
Class: |
G01J
1/58 (20130101); F21K 2/00 (20130101); F02D
41/1456 (20130101) |
Current International
Class: |
F21K
2/00 (20060101); G01J 1/00 (20060101); G01J
1/58 (20060101); G01t 001/10 () |
Field of
Search: |
;350/1,318 ;313/112
;356/204 ;73/23.1,61.1C
;250/364,365,503,504,458-461,483,485,486,487 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Dixon; Harold A.
Attorney, Agent or Firm: Cole; Stanley Z. Fisher; Gerald M.
Morrissey; John J.
Claims
1. In a method of making a sealed phosphor assembly, the steps
comprising:
placing loose particulate phosphor in a cavity of a base in an
amount sufficient to fill the cavity,
covering the cavity with a material substantially transparent to
electromagnetic radiation of at least certain transparent to
electromagnetic radiation of at least certain wave lengths,
heating the assembled base, phosphor and covering material to dry
the phosphor, and
2. A method as set forth in claim 1, wherein the covering material
is a quartz window, and the phosphor is dried and the covering
material is sealed to the base by placing a heat-fusible sealant
about the cavity between the base and window and heating the base,
phosphor, window and sealant first to a drying temperature below
the fusion temperature of the sealant and then subsequently to a
temperature at which the sealant fuses.
3. A method as set forth in claim 2, wherein the temperature is
raised to fuse the sealant without lowering the temperature below
the drying
4. A sealed wave length-converting phosphor assembly for use in an
ultraviolet radiation detector, comprised of a base for attachment
of the assembly to a support, a phosphor receptacle formed in said
base, a phosphor in particulate form in said receptacle, a cover
over said receptacle and phosphor, retaining the phosphor in the
receptacle, protecting the phosphor from moisture and abrasion, and
substantially transparent to ultraviolet radiation, said base
includes a ledge about said receptacle forming a seat for the
cover, and a rim about the ledge for locating the cover, the area
circumscribed by said rim being greater than the area of said
cover, and means surrounding said receptacle forming
5. A sealed wave length-converting phosphor assembly for use in an
ultraviolet radiation detector, comprising a metal base for
attachment of said phosphor assembly to a support, a phosphor
receptacle formed in said base, a phosphor in particulate form in
said receptacle, a fused silica cover over said receptacle and
phosphor, said cover serving to retain the phosphor in the
receptacle and to protect the phosphor from moisture and abrasion,
said cover being substantially transparent to ultraviolet
radiation, and fluorinated ethylene propylene sealing means
disposed along a continuous path surrounding said receptacle to
form an hermetic seal
6. The assembly of claim 5 wherein said base comprises a ledge
about said receptacle forming a seat for the cover, and a rim about
the ledge for locating the cover, the area circumscribed by said
rim being greater than
7. In an ultraviolet radiation detector for use in chromatography,
an ultraviolet wave length-converting phosphor powder enclosed
within and filling a dry closed hermetically-sealed chamber, said
chamber being formed by a base member having a cavity and by a
cover member over said cavity, said base member comprising a ledge
about the perimeter of said cavity, said ledge forming a seat for
said cover member, said base member and said cover member defining
the chamber filled by said phosphor powder, said cover member being
transparent to ultraviolet radiation.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a phosphor package or assembly,
particularly for use with an ultraviolet radiation absorption
detector in liquid chromatography, and to a method for making the
assembly.
2. Prior Art
Ultraviolet radiation absorption detectors are used with flow cells
in liquid chromatography to monitor effluent that contains
components to be detected or analyzed. A typical wave length of
ultraviolet radiation used in detectors by life scientists is 254
nm (nanometers), which is emitted by a low pressure mercury
discharge lamp. However, certain biologically interesting compounds
are more absorbing and certain useful solvents less absorbing at
wave lengths of 280 nm than they are at 254 nm, and a phosphor can
be used to convert the 254 nm radiation to 280 nm radiation where
the latter wave length is desired. The phosphor is located within a
lamp housing of the detector, along with the mercury lamp. A flow
cell assembly, including a light sensing detector, is secured to
the lamp housing. Radiation from the lamp causes the phosphor to
emit ultraviolet radiation at the different or "converted" wave
length, which is then directed through the effluent in the flow
cell for the detection and analysis of certain compounds.
Phosphors are susceptible to serious degradation when irradiated
with ultraviolet light in a moist atmosphere, which is common in
the ultraviolet lamp housing of a detector. In addition, an exposed
phosphor surface is subjected to abrasion, contamination, as by
solvent leakage from the flow cell, and film build up on the
phosphor surface, which degrades the phosphor and reduces
efficiency.
SUMMARY OF THE INVENTION
The present invention provides a phosphor package or assembly that
seals the phosphor against moisture and other elements of the
surrounding environment, facilitates the use of a phosphor in
particulate form, provides a viewed or emitting phosphor surface
that can be cleaned in the event of cell leakage of film build up,
and that physically protects the phosphor from abrasion. Further,
the assembly can be conveniently fabricated, facilitates the
provision and maintenance of a viewed surface that is uniform and
smooth, and facilitates the drying of the particulate phosphor and
sealing of the assembly in an efficient manner during
fabrication.
Briefly, the phosphor assembly, which because of its form is
referred to as a "button," is in the nature of a package that seals
and protects the phosphor and maintains the phosphor in a desired
location, arrangement and configuration without the need for
binders, adhesives, or the like in the phosphor. The assembly is
comprised of a backing and a protective cover, between which the
phosphor is sealed. The protective cover is transparent to
ultraviolet radiation and protects the phosphor against moisture or
other surrounding atmosphere, and against abrasion. It also
provides a surface to be viewed in use, which is smooth and
cleanable. Preferably, the protective cover is of fused silica,
i.e., quartz.
In its preferred form, the backing is a receptacle for containing a
quantity of phosphor in particulate, i.e., powdered form.
Preferably the backing is metal, suitably aluminum with an inner
ledge and outer flange surrounding the receptable to form a step
for receiving, locating and providing a seat and seal for the
protective cover. Preferably, the receptacle or cavity is of
uniform shallow depth to provide a phosphor layer of uniform
thickness and emissivity with a minimum of phosphor material.
The seal between the backing and protective cover must be resistent
to degradation from ultraviolet radiation and, for convenience in
fabrication of the assembly, is advantageously of a material that
is heat fusible above a temperature suitable for drying the
phosphor. Fluorinated ethylene propylene (Teflon) is especially
suitable.
Manufacture or fabrication is best accomplished by placing the
powder within the receptacle or cavity of the backing, using enough
powder to fully fill the cavity. The protective covering is applied
to flatten the phosphor powder and is then removed for cleaning.
The cover is replaced and the sealant applied between the cover and
flange of the backing. The assembly is then heated to a first
temperature suitable for drying the phosphor but below the fusion
temperature of the sealant, for a sufficient time to dry the
phosphor. Subsequently, the assembly is heated to a temperature at
which the sealant will fuse. Advantageously, the heating to the
higher temperature immediately follows the drying without
intermediate cooling, to avoid moisture pick-up and to shorten the
fabrication time.
It is an object of the present invention to provide a phosphor
assembly that is in part transparent to ultraviolet radiation and
in which the phosphor material is supported, protected, and sealed
from the surrounding atmosphere.
A more specific object is to provide a phosphor assembly that
provides a uniform, smooth, viewable, surface of phosphor powder,
that seals the powder from the surrounding atmosphere and protects
the surface of the powder against abrasion, that can be cleaned
after use, and that is economical convenient to fabricate.
A further object is to provide a method of fabrication of the
phosphor assembly that facilitates drying the phosphor material and
sealing the assembly against moisture.
The above and other objects, features and advantages of the
invention will become more apparent from the detailed description
that follows, when considered in connection with the accompanying
drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic sectional view, with parts in elevation,
of an ultraviolet radiation detector assembly for use in liquid
chromatography;
FIG. 2 is a top plan view of a phosphor assembly or button
embodying the present invention;
FIG. 3 is a sectional view of the assembly or button of FIG. 2,
taken along the line 3--3; and
FIG. 4 is a diagrammatic exploded view of the assembly or button of
FIGS. 2 and 3 on an assembly fixture, diagramatically illustrating
a preferred manner of fabrication.
DETAILED DESCRIPTION OF A PREFERRED EMBODIMENT
With reference to FIG. 1 of the drawings, an ultraviolet radiation
detector assembly 10 for use in liquid chromatography is shown
diagramatically. The detector assembly 10 includes a lamp housing
12, a low pressure mercury lamp 14 having two lobes in the
configuration shown, a phosphor assembly or button 16, a flow cell
assembly 18 carried by the lamp housing, and an ultraviolet
radiation detector 20 carried by the flow cell assembly.
The lamp housing 12 has an opening 22 in one wall 24 on which the
flow cell assembly 18 is mounted. The phosphor assembly or button
16 is secured inside the lamp housing on a wall 26, generally
opposite the opening 22, so that the surface of the button is
within the view of the flow cell assembly 18, including the
ultraviolet detector 20. The lamp 14 is offset from the opening 22
so that the detector is shielded from direct rays. Ultraviolet
radiation of a wave length of 254 nm is produced by the mercury
lamp 14, strikes the phosphor assembly 16, and causes the phosphor
to emit radiation having a wave length of 280 nm, some of which is
directed to the flow cell assembly. The ultraviolet radiation from
the phosphor is collimated by a quartz lens 29, passes through two
parallel fluid cells, one containing a liquid sample and the other
a reference liquid, and passes through a second quartz lens or
window 30 to the ultraviolet detector 20.
The construction of the phosphor assembly 16 is best shown in FIGS.
2 and 3 of the drawings. As shown, the phosphor assembly includes a
base 36, phosphor 38 in particulate form, a cover 40, and a seal 42
between the cover and base.
The base 36 serves as a receptacle for the phosphor powder,
facilitates securing the assembly 16 within the lamp housing, as by
a screw 43. The base is of rigid material, preferably metal, and
advantageously aluminum, which is light and readily fabricated. In
the preferred embodiment shown, the base is generally cylindrical
in shape, having a front or top surface 44 and a base or back
surface 46 at an angle to the top surface, 15.degree. in the
embodiment shown, to orient the top or front surface 44 in a proper
relationship to both the mercury lamp and the flow cell of the
apparatus with which the phosphor assembly is used. A threaded hole
48 in the base surface 46 receives the screw 43 and is located
directly under the center of the interface between the cover 40 and
the phosphor 38. By way of example, the base shown is, in a
preferred embodiment approximately 1 inch in diameter and 0.3 inch
in height, at the shortest portion of the periphery. The top or
front surface 44 has a recess 50 surrounded by a narrow ledge 52
and has a narrow rim 54 extending above the ledge for a short
distance, for example one-sixteenth of an inch. The recess 50 is
shallow, for example about 0.05 inch and is filled to the top with
powdered phosphor 38. The recess 50 is of uniform depth so that the
phosphor is of uniform thickness. The recess holds approximately
one gram of General Electric Type X--401 lanthanum fluoride
phosphor powder.
The cover 40 is a disc of a thickness essentially equal to the
height of the rim 54 and is shaped and sized to rest on the ledge
52 with a small peripheral clearance, for example, 0.025 inch,
between the disc and the rim. This surrounding clearance permits
relative sliding between the disc and base during assembly, and
provides space for the seal 42. In the preferred embodiment shown,
the cover is of quartz, i.e., fused silica, which is substantially
transparent to ultraviolet radiation. Such a cover disc can be
procured commercially and a suitable product is manufactured by
General Electric, identified as Type 125 polished quartz disc.
The seal 42 is a fused strip of material that wets the surfaces of
the quartz cover and the rim 54 of the base, that is chemically
resistant, and which further resists deterioration in an
ultraviolet environment. The fused material of the preferred
embodiment is fluorinated ethylene propylene, marketed under the
trademark Teflon. The seal extends completely around the cover disc
to a height approximately one-half that of the rim 54, to provide a
continuous hermetic seal between the quartz disc and the metal
base. The seal is achieved with a 5 millimeter strip (0.005 inch)
of fluorinated ethylene propylene film 42' (shown in FIG. 4)
approximately 1/8 inch in height and 3 1/4 inches long, so that it
completely surrounds the perimeter of the cover.
The manner in which the phosphor assembly is fabricated is best
shown in FIG. 4 of the drawings. The base 36 is placed on a jig or
fixture 60 that has a top surface 62 that slopes at the same angle
as the base surface 46 of the base 36, so that the top surface 44
of the base 36 can be held horizontal. A pin 63 extending from the
surface 62 of the fixture 60 is received in the threaded aperture
48, with a slight clearance fit, to retain the base on the fixture.
Approximately 1 gram of phosphor powder 38 is heaped into the
recess or pocket 50, as illustrated. The fused silica window 40 is
pushed down on the phosphor powder while being rotated slowly and
at the same time slid back and forth within the tolerance provided
in the window step to uniformly distribute the phosphor powder
within the recess. After the powder is uniformly distributed and
there are no gaps or vacancies at the interface between the powder
and the fused silica surface, the cover or window is removed,
excess powder removed from the ledge 52, and the window is cleaned
and then replaced in the ledge, within the surrounding rim 54. The
strip of fluorinated ethylene propylene film 42' is inserted
edgewise in the gap between the perimeter of the cover and the rim
of the base. The assembly is placed in an oven on the fixture 60
and is heated to dry the phosphor powder. This initial drying is
accomplished at a temperature below that at which the fluorinated
ethylene propylene film will fuse. By way of example, in the
preferred embodiment, the assembly is heated to a temperature
between 225.degree. centigrade and 250.degree. centigrade for 3 to
4 hours to dry the phosphor powder. At the end of the drying
operation, the temperature is elevated and held at the elevated
level for sufficient time to fuse the strip 42'. In the present
instance, the assembly is heated to a temperature of 350.degree.
centigrade and held at this temperature for 1/2 hour, to fuse the
strip 42' to form the seal 42. Most advantageously, the assembly is
not cooled between the drying and fusing operations, to avoid heat
loss and to eliminate the change of moisture condensation prior to
sealing.
The resulting assembly is durable and completely seals the phosphor
from any surrounding environment. The durability of the assembly
has been tested by submerging an assembly in an aqueous dye
solution for 72 hours. At the end of this period the assembly was
boiled in the dye solution for ten minutes and cooled to room
temperature. The assembly exhibited no penetration of the dye into
the phosphor material. Decay of the phosphor material was checked
by comparing the light emitted from an assembly exposed to
ultraviolet radiation in a lamp housing for approximately 2 weeks,
with the light emitted from a newly fabricated assembly. Relative
photocell light intensities for the two phosphor assemblies were
measured in the same lamp housing with the same photocell sensor or
detector, within 20 minutes of each other. The results of this
experiment show a meter reading from the photocell detector for the
phosphor button irradiated for 2 weeks of 0.359, and a meter
reading of the freshly prepared assembly of 0.360. Accordingly, the
irradiated assembly showed no decrease in emission intensity,
within experimental error.
While a preferred embodiment of this invention has been described
with particularity, it will be appreciated that various
modifications or alterations may be made without departing from the
spirit and scope of the invention set forth in the apended
claims.
* * * * *