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| United States Patent | 4582520 |
| Link to this page | http://www.wikipatents.com/4582520.html |
| Inventor(s) | Sturm; Steven P. (Columbus, OH) |
| Abstract | The degree of cure of a traveling carbonaceous polymeric material (on 48),
formed (at 34) from a plurality of chemical reactants (32) and subjected
to a curing process (at 42 and 44) is determined by directing (with 86 and
88) into the traveling material radiations including a first infrared
radiation (A1) from the group thereof adapted to selectively interact with
molecular resonance vibrations at frequencies that are characteristic of
respective terminal functional groups of atoms involved in reactions that
take place in the material during the curing process. Also directed into
the material is a second infrared radiation that is either of the kind (R)
that does not exhibit substantial selective interaction with molecular
resonance vibrations in the material or of the kind (A2) that is adapted
to selectively interact with molecular resonance vibrations at a frequency
that is characteristic of groups of atoms forming the backbones of the
polymeric molecules in the material. Received (at 102) from the traveling
material are radiations (148) that have interacted with the material.
Produced (at 116, 118 and 122) from the received radiations are first and
second responses to the first and second radiations. Produced (at 122) is
a third response that is a function of the mass of the polymeric material
interacting with the radiations. Produced (at 122) from the first, second
and third responses is an output response (140, 82) that is correlated
with the degree of cure effected by the curing process. |
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Title Information  |
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| Publication Date |
April 15, 1986 |
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| Filing Date |
September 10, 1984 |
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| Parent Case |
This application is a continuation of application Ser. No. 06/431,179 filed
Sept. 30, 1982, now abandoned. |
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Title Information  |
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References  |
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| Market Size |
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Market Review  |
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Technical Review  |
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Claims  |
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What is claimed is:
1. A method for determining the degree of cure of a traveling carbonaceous
polymeric material that has been formed from a plurality of chemical
reactants and subjected to a curing process, the method comprising
directing into the traveling material a first infrared radiation from the
group thereof adapted to selectively interact with molecular resonance
vibrations at frequencies that are characteristic of respective terminal
functional groups of atoms involved in reactions that take place in the
material during the curing process, so that the material exhibits an
absorptivity for the first infrared radiation that varies with the degree
of cure of the polymeric material,
also directing into the traveling material a second infrared radiation that
is either of the kind that does not exhibit substantial selective
interaction with molecular resonance vibrations in the material or of the
kind that is adapted to selectively interact with molecular resonance
vibrations at a frequency that is characteristic of groups of atoms
forming the backbones of the polymeric molecules in the material, so that
the material exhibits a relatively constant absorptivity for the second
infrared radiation as the curing process progresses,
receiving from the traveling material radiations that have interacted with
the material,
producing from the received radiations first and second responses to the
first and second radiations,
producing a third response that is indicative of the mass of the polymeric
material interacting with the radiations and substantially independent of
the variations in the absorptivity of the material for the first infrared
radiation which occur as the curing process progresses, and
producing from the first, second and third responses an output response
that is a function of the changes in the absorptivity of the material for
the first infrared radiation, substantially independent of the amount of
the polymeric material interacting with the radiations, and correlated
with the degree of cure effected by the curing process.
2. A method as in claim 1 wherein the first infrared radiation is selected
from the group adapted to selectively interact with molecular resonance
vibrations at respective O--H, N--H and C.dbd.O vibration frequencies.
3. A method as in claim 1 or claim 2 which comprises directing into the
traveling material a third infrared radiation of the other kind,
producing from the received radiations a further response to the third
infrared radiation, and
producing the third response from the further response and the second
response.
4. A method as in claim 3 wherein the third radiation is adapted to
selectively interact with molecular resonance vibrations at a C--H stretch
vibration frequency.
5. A method as in claim 3 wherein the first, second and third infrared
radiations comprise near-infrared overtone bands, the first radiation
having wavelengths in the vicinity of 1.50.mu., with either of the second
and third radiations having wavelengths in the vicinity of either 1.35.mu.
or 1.75.mu..
6. A method as in claim 3 which comprises forming a first mathematical
function of the ratio of the first and third responses,
forming a second mathematical function of the ratio of the second and third
responses, and
combining the first and second functions to produce the output response.
7. A method as in claim 6 wherein the first and second functions are
substantially linear functions.
8. A method as in claim 7 wherein the ratio of the first and second
functions is formed in order to produce the output response.
9. A method as in claim 6 wherein the first function is indicative of the
number of terminal functional groups present in relation to the number of
groups forming the backbones of the molecules, and
wherein the second function is indicative of the number of groups forming
the backbones of the molecules that have interacted with the radiations.
10. A method as in claim 1 wherein the carbonaceous polymeric material is
used to form a binder coating for the fibers in a mat of glass fibers,
wherein the curing process includes exposing the mat to elevated
temperatures, and
wherein the exposed mat is passed through a measuring zone in which the
radiations are directed into and received from the mat.
11. A method as in claim 10 which comprises controlling the exposure of the
mat to the elevated temperatures in accordance with the output response.
12. A method as in claim 10 wherein the first infrared radiation comprises
a near-infrared overtone band adapted to selectively interact with
molecular resonance vibrations at one or both of the O--H and N--H
vibration frequencies.
13. A method as in claim 12 wherein the first infrared radiation has
wavelengths in the vicinity of 1.50.mu., and the second infrared radiation
has wavelengths in the vicinity of 1.35.mu. or 1.75.mu..
14. A method as in claim 12 or claim 13 which comprises directing into the
mat a third infrared radiation which is different from the second
radiation and which lies in a band of wavelengths in the vicinity of
1.35.mu. or 1.75.mu.,
producing from the received radiations a further response to the third
infrared radiation, and
producing the third response from the further response and the second
response.
15. A method as in claim 14 which comprises forming a first mathematical
function of the ratio of the first and third responses,
forming a second mathematical function of the ratio of the second and third
responses, and
combining the first and second functions to produce the output response.
16. A method as in claim 15 wherein the first and second functions are
substantially linear functions.
17. A method as in claim 16 wherein the ratio of the first and second
functions is formed in order to produce the output response.
18. A method as in claim 15 which comprises
measuring the weight per unit area of the mat passing through the measuring
zone, and controlling the rate of travel of the mat in accordance with the
weight per unit area measurement,
controlling the rate of application of the binder coating in accordance
with the second mathematical function, and
controlling the temperature of the mat during at least a portion of the
curing process in accordance with the output response.
19. Apparatus for determining the degree of cure of a traveling
carbonaceous polymeric material that has been formed from a plurality of
chemical reactants and subjected to a curing process, comprising
means for directing into the traveling material a first infrared radiation
from the group thereof adapted to selectively interact with molecular
resonance vibrations at frequencies that are characteristic of respective
terminal functional groups of atoms involved in reactions that take place
in the material during the curing process, so that the material exhibits
an absorptivity for the first infrared radiation that varies with the
degree of cure of the polymeric material,
means for directing into the traveling material a second infrared radiation
that is either of the kind that does not exhibit substantial selective
interaction with molecular resonance vibrations in the material or of the
kind that is adapted to selectively interact with molecular resonance
vibrations at a frequency that is characteristic of groups of atoms
forming the backbones of the polymeric molecules in the material, so that
the material exhibits a relatively constant absorptivity for the second
infrared radiation as the curing process progresses,
means for receiving from the traveling material radiations that have
interacted with the material,
means for producing from the received radiations first and second responses
to the first and second radiations,
means for producing a third response that is indicative of the mass of the
polymeric material interacting with the radiations and substantially
independent of the variations in the absorptivity of the material for the
first infrared radiation which occur as the curing process progresses, and
means for producing from the first, second and third responses an output
response that is a function of the changes in the absorptivity of the
material for the first infrared radiation, substantially independent of
the amount of the polymeric material interacting with the radiations, and
correlated with the degree of cure effected by the curing process.
20. Apparatus as in claim 19 wherein the first infrared radiais selected
from the group adapted to selectively interact with molecular resonance
vibrations at respective O--H, N--H and C.dbd.O vibration frequencies.
21. Apparatus as in claim 19 or claim 20 which comprises means for
directing into the traveling material a third infrared radiation of the
other kind,
means for producing from the received radiations a further response to the
third infrared radiation, and
means for producing the third response from the further response and the
second response.
22. Apparatus as in claim 21 wherein the third radiation is adapted to
selectively interact with molecular resonance vibrations at a C--H stretch
vibration frequency.
23. Apparatus as in claim 21 wherein the first, second and third infrared
radiations comprise near-infrared overtone bands, the first radiation
having wavelengths in the vicinity of 1.50.mu., with either of the second
and third radiations having wavelengths in the vicinity of either 1.35.mu.
or 1.75.mu..
24. Apparatus as in claim 21 which comprises means for forming a first
mathematical function of the ratio of the first and third responses,
means for forming a second mathematical function of the ratio of the second
and third responses, and
means for combining the first and second functions to produce the output
response.
25. Apparatus as in claim 24 wherein the first and second functions are
substantially linear functions.
26. Apparatus as in claim 25 wherein the ratio of the first and second
functions is formed in order to produce the output response.
27. Apparatus as in claim 24 wherein the first function is indicative of
the number of terminal functional groups present in relation to the number
of groups forming the backbones of the molecules, and
wherein the second function is indicative of the number of groups forming
the backbones of the molecules that have interacted with the radiations.
28. Apparatus as in claim 19 wherein the carbonaceous polymeric material is
used to form a binder coating for the fibers in a mat of glass fibers,
wherein the curing process includes exposing the mat to elevated
temperatures, and
wherein the exposed mat is passed through a measuring zone in which the
radiations are directed into and received from the mat.
29. Apparatus as in claim 28 which comprises means for controlling the
exposure of the mat to the elevated temperatures in accordance with the
output response.
30. Apparatus as in claim 28 wherein the first infrared radiation comprises
a near-infrared overtone band adapted to selectively interact with
molecular resonance vibrations at one or both of the O--H and N--H
vibration frequencies.
31. Apparatus as in claim 30 wherein the first infrared radiation has
wavelengths in the vicinity of 1.50.mu., and the second infrared radiation
has wavelengths in the vicinity of 1.35.mu. or 1.75.mu..
32. Apparatus as in claim 30 or claim 31 which comprises means for
directing into the mat a third infrared radiation which is different from
the second radiation and which lies in a band of wavelengths in the
vicinity of 1.35.mu. or 1.75.mu.,
means for producing from the received radiations a further response to the
third infrared radiation, and
means for producing the third response from the further response and the
second response.
33. Apparatus as in claim 32 which comprises means for forming a first
mathematical function of the ratio of the first and third responses,
means for forming a second mathematical function of the ratio of the second
and third responses, and
means for combining the first and second functions to produce the output
response.
34. Apparatus as in claim 33 wherein the first and second functions are
substantially linear functions.
35. Apparatus as in claim 34 comprising means for forming the ratio of the
first and second functions in order to produce the output response.
36. Apparatus as in claim 33 which comprises
means for measuring the weight per unit area of the mat passing through the
measuring zone, and means for controlling the rate of travel of the mat in
accordance with the weight per unit area measurement,
means for controlling the rate of application of the binder coating in
accordance with the second mathematical function,
and
means for controlling the temperature of the mat during at least a portion
of the curing process in accordance with the output response.
37. A method as in claim 1 which comprises producing from the first and
second responses a fourth response that is indicative of the mass of the
polymeric material interacting with the radiations but which is dependent
on the variations in the absorptivity of the material for the first
infrared radiation that occur as the curing process progresses, and
utilizing the fourth response and the third response to produce the output
response.
38. A method as in claim 37 wherein the fourth response is compensated for
the radiation path length extension effects of radiation scattering.
39. A method as in claim 38 wherein the third response is similarly
compensated for the effects of scattering.
40. A method as in claim 38 which comprises directing into the material
further radiations having a mode of interaction with the material which is
different from that of the infrared radiations,
detecting the further radiations that have interacted with the material to
produce an additional response, and
using the additional response to effect the scattering compensation.
41. A method as in claim 40 wherein the further radiations are x rays or
gamma rays.
42. A method as in claim 39 which comprises directing into the material
further radiations having a mode of interaction with the material which is
different from that of the infrared radiations,
detecting the further radiations that have interacted with the material to
produce an additional response, and
using the additional response to effect scattering compensation of both the
third and fourth responses.
43. A method as in claim 42 wherein the further radiations are x rays or
gamma rays, and
the third and fourth responses are similarly compensated.
44. A method as in claim 10 which comprises producing from the first and
second responses a fourth response that is indicative of the mass of the
polymeric binder material interacting with the radiations but which is
dependent on the variations in the absorptivity of the binder material for
the first infrared radiation that occur as the curing proces progresses,
and
utilizing the fourth response and the third response to produce the output
response.
45. A method as in claim 44 wherein the fourth response is compensated for
the radiation path length extension effects of radiation scattering by the
binder-coated glass fibers.
46. A method as in claim 45 wherein the third response is similarly
compensated for the effects of the scattering.
47. A method as in claim 46 which comprises directing x rays or gamma rays
into the mat of glass fibers,
detecting the x rays or gamma rays that have interacted with the mat of
glass fibers to produce an additional response, and
using the additional response to effect scattering compensation of both the
third and fourth responses.
48. A method as in claim 47 wherein the additional response is additionally
used to compensate the third and fourth responses for the infrared
spectral effects of the glass in the fibers of the mat.
49. Apparatus as in claim 19 which comprises means for producing from the
first and second responses a fourth response that is indicative of the
mass of the polymeric material interacting with the radiations but which
is dependent on the variations in the absorptivity of the material for the
first infrared radiation that occur as the curing process progresses, and
means for utilizing the fourth response and the third response to produce
the output response.
50. Apparatus as in claim 49 comprising means for compensating the fourth
response for the radiation path length extension effects of radiation
scattering.
51. Apparatus as in claim 50 comprising means for similarly compensating
the third response for the effects of scattering.
52. Apparatus as in claim 50 which comprises means for directing into the
material further radiations having a mode of interaction with the material
which is different from that of the infrared radiations,
means for detecting the further radiations that have interacted with the
material to produce an additional response, and
means for using the additional response to effect the scattering
compensation.
53. Apparatus as in claim 52 wherein the further radiations are x rays or
gamma rays.
54. Apparatus as in claim 51 which comprises means for directing into the
material further radiations having a mode of interaction with the material
which is different from that of the infrared radiations,
means for detecting the further radiations that have interacted with the
material to produce an additional response, and
means for using the additional response to effect scattering compensation
of both the third and fourth responses.
55. Apparatus as in claim 54 wherein the further radiations are x rays or
gamma rays, and
the third and fourth responses are similarly compensated.
56. Apparatus as in claim 28 which comprises means for producing from the
first and second responses a fourth response that is indicative of the
mass of the polymeric binder material interacting with the radiations but
which is dependent on the variations in the absorptivity of the binder
material for the first infrared radiation that occur as the curing process
progresses, and
means for utilizing the fourth response and the third response to produce
the output response.
57. Apparatus as in claim 56 comprising means for compensating the fourth
response for the radiation path length extension effects of radiation
scattering.
58. Apparatus as in claim 57 comprising means for similarly compensating
the third response for the effects of the scattering.
59. Apparatus as in claim 58 which comprises means for directing x rays or
gamma rays into the mat of glass fibers,
means for detecting the x rays or gamma rays that have interacted with the
mat of glass fibers to produce an additional response, and
means for using the additional response to effect scattering compensation
of both the third and fourth responses.
60. Apparatus as in claim 59 comprising means for utilizing the additional
response to compensate the third and fourth responses for the infrared
spectral effects of the glass in the fibers of the mat. |
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Claims  |
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Description  |
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TECHNICAL FIELD
This invention relates to methods and apparatus for measuring and
controlling the degree of cure of carbonaceous polymeric materials that
are formed from a plurality of chemical reactants and passed through a
curing process, from which they issue as a traveling product or
intermediate in a continuous or semi-continuous form. More particularly
the invention relates to methods and apparatus for performing the
measurements by directing into the traveling material infrared radiations
at multiple wavelengths, detecting radiations that have been transmitted
or reflected by the material, and computing the degree of cure in a
substantially instantaneous, continuous and non-destructive manner from
instrument responses to the detected radiations.
The availability of instrumentation which functions or is constructed in
accordance with the invention permits immediate manual or automatic
feedback control of one or more of the process parameters that affect the
degree of cure, thus enabling the manufacture of a product or intermediate
in an optimized state of polymerization and with the probability of
substantial raw material savings and/or energy savings.
While the methods and apparatus of the invention are applicable to the
manufacture of many different polymeric material products, the invention
is herein described and illustrated in an embodiment for measuring and/or
controlling the degree of cure of the binder resin applied to a mat of
glass fibers, to be used, for example, in building insulation products.
BACKGROUND ART
Synthetic resins and natural polymeric compounds are used in the production
of a great many materials and discrete items whose manufacture includes a
curing stage. The manufactured material or item may consist of the
polymerized material itself, or the polymerized material may be used as a
binder to hold together various layers or aggregates of other materials
which in combination with the binder can impart to the finished product
its desired properties.
The desired properties are often significantly affected by the degree of
polymerization of the resin compound. The affected properties typically
include the flexibility and toughness of plastics, or the stiffness,
abrasion and impact resistance of laminated sheets.
In various manufacturing processes, the degree of polymerization has been
controlled by regulating one or more process parameters such as
concentration, residence time, temperature and catalysis. Various
instruments have been used to determine heat liberation, viscosity,
density and electrical conductivity. Spectroscopic instruments of the gas
chromatographic and nuclear magnetic resonance type have been very useful.
Laboratory determinations of molecular weights are commonly performed as a
quality control measure.
An article by Crandall, E. W. and Jagtap, A. N., entitled "The
Near-Infrared Spectra of Polymers", Journal of Applied Polymer Science,
Vol. 21, pp. 449-454 (1977) and its bibliography have indicated that
near-infrared spectroscopy can be useful in the identification of resins
and polymers and in following the course of polymerization and giving some
indication of the state of cure. Polymers were melted and pressed between
glass plates to give a transparent film, or they were dissolved and their
spectra in solution were run against the spectrum of the pure solvent. It
was observed that in various polymers the process of curing (with heat)
affected the relative intensities of the overtone bands of carbonyl
(C.dbd.O), amino and amide N--H and alcoholic O--H. The overtone bands of
alkyl and aryl C--H were also observed along with certain C--H combination
bands. The intensities of various bands were set forth by way of
comparison with that of the C--H stretch band whose fundamental vibration
lies at 3.3-3.5 .mu.m in the middle-infrared and whose first overtone
appears at 1.7 .mu.m in the near-infrared.
Two of the carbonaceous polymeric materials discussed by Crandall et al are
phenol-formaldehyde and urea-formaldehyde resins, which are commonly
utilized, inter alia, as binders in glass fiber mats, say, for building
insulation. In the manufacture of these mats, typically glass fiber is
spun from molten glass and is sprayed with uncured binder compound as the
fiber is being showered onto a moving chain conveyor. The conveyor carries
the resulting glass fiber blanket through curing ovens wherein the
polymeric binder material is exposed to elevated temperatures for an
appropriate time period to complete the curing of the binder. After its
exit from the ovens, the mat or blanket is cooled by a stream of air from
a fan, and certain of its properties may be measured, typically with
radiation gauges.
The mass per unit area of the traveling mat has been measured, with various
degrees of success, using beta ray gauges, gamma ray or x-ray gauges, or
infrared radiation gauges using combinations of wavelengths. The resulting
measurements have been used to automatically control the speed of the
chain conveyor, thereby determining the amount of coated glass fibers
deposited while a section of the conveyor moves through the felting
chamber, with the objective of maintaining the weight per unit area of the
mat constant along its length.
Various attempts have been made to measure the mass of the binder material
per se, for example by taking advantage of the fact that glass is
substantially transparent to certain optical (e.g., infrared) and x-ray
wavelengths that are significantly attenuated by the binder materials. The
objective of this measurement is to be able to control the mass of the
binder by regulating the amount or the dilution of the spray material
applied.
The degree of cure has been measured in laboratories, for example, by free
phenol determination or molecular weight determination. On the basis of
their experience with laboratory-analyzed samples, line operators
typically make a visual estimate of the degree of cure by inspection of
the "color" of the mat, and adjust the oven temperature accordingly.
However, as an indicator of cure, color has been shown objectively to be
misleading in many cases, as well as subjective. Moreover, color changes
do not exhibit high sensitivity except when the mat is already over-cured
(burnt).
The degree of cure of the binder is believed to have considerable economic
significance, since it affects the property of the glass fiber mat which
is termed "recovery". The manufactured mat is usually compressed into
rolls or bales for shipment and storage, and "recovery" is the extent to
which the mat is able to spring back to its original thickness when the
compression is relieved. Recovery is also related to the ability of the
mat to maintain its shape and thickness for long periods of time in use as
insulation and for other purposes. Hence, if the binder has an optimum
degree of cure, a mat with a desired thickness and insulation value in
service can be manufactured from a smaller amount of glass fiber and
binder. The avoidance of overcuring can also result in lower energy costs
during manufacture.
The properties of recovery and resistance to sag and deterioration in
service seem to be dependent on an adequate degree of polymerization.
There is evidence, on the other hand, that overcuring results in
depolymerization as well as other deleterious effects.
It follows that there has been a need for a method and apparatus which
provides an instantaneous, substantially continuous and non-destructive
indication of the degree of cure of certain traveling polymeric materials.
DISCLOSURE OF INVENTION
In accordance with this invention, there are provided methods and apparatus
for determining the degree of cure of a traveling carbonaceous polymeric
material that has been formed from a plurality of chemical reactants and
subjected to a curing process, comprising combinations of method steps and
apparatus elements for directing into the traveling material a first
infrared radiation from the group thereof adapted to selectively interact
with molecular resonance vibrations at frequencies that are characteristic
of respective terminal functional groups of atoms involved in reactions
that take place in the material during the curing process, so that the
material exhibits an absorptivity for the first infrared radiation that
varies with the degree of cure of the polymeric material, also directing
into the traveling material a second infrared radiation that is either of
the kind that does not exhibit substantial selective interaction with
molecular resonance vibrations in the material or of the kind that is
adapted to selectively interact with molecular resonance vibrations at a
frequency that is characteristic of groups of atoms forming the backbones
of the polymeric molecules in the material, receiving from the traveling
material radiations that have interacted with the material; producing from
the received radiations first and second responses to the first and second
radiations; producing a third response that is indicative of the mass of
the polymeric material interacting with the radiations, and substantially
independent of the variations in the absorptivity of the material for the
first infrared radiation which occur as the curing process progresses, and
producing from the first, second and third responses an output response
that is correlated with the degree of cure effected by the curing process.
Typically the first infrared radiation is selected from the group adapted
to selectively interact with molecular resonance vibrations at respective
O--H, N--H and C.dbd.O vibration frequencies.
Method steps and apparatus elements may be provided for directing into the
traveling material a third infrared radiation of the other kind, producing
from the received radiations a further response to the third infrared
radiation, and producing the third response from the further response and
the second response.
The third radiation may be adapted to selectively interact with molecular
resonance vibrations at a C--H stretch vibration frequency.
The first infrared radiation may comprise the near-infrared overtone band
having wavelengths in the vicinity of 1.50.mu., whereas either of the
second and third infrared radiations may have wavelengths in the vicinity
of either 1.35.mu. or 1.75.mu..
A first mathematical function of the ratio of the first and third responses
may be formed, together with a second mathematical function of the ratio
of the second and third responses, and the first and second functions may
be combined to produce the output response.
The first and second functions may be substantially linear functions. The
ratio of the first and second functions may be formed in order to produce
the output response.
The first function may be indicative of the number of terminal functional
groups present in relation to the number of groups forming the backbones
of the molecules, and the second function may be indicative of the number
of groups forming the backbones of the molecules that have interacted with
the radiations.
The first and second responses may be used to produce a fourth response
that is indicative of the mass of the polymeric material interacting with
the radiations but which is dependent on the variations in the
absorptivity of the material for the first infrared radiation that occur
as the curing process progresses, and the fourth response and the third
response may be utilized to produce the output response.
The fourth response may be compensated for the radiation path length
extension effects of scattering. The third response may be similarly
compensated.
Method steps and apparatus elements may be provided for directing into the
material further radiations having a mode of interaction that is different
from that of the infrared radiations; these further radiations that have
interacted with the material may be detected to produce an additional
response, and the additional response may be used to effect the scattering
compensation. The further radiations may be x rays or gamma rays.
The carbonaceous polymeric material may be used to form a binder coating
for the fibers in a mat of glass fibers; the curing process may include
exposing the mat to elevated temperatures, and the exposed mat may be
passed through a measuring zone in which the radiations are directed into
and received from the mat.
The exposure of the mat to the elevated temperatures may be controlled in
accordance with the output responses.
The first infrared radiation may comprise a near-infrared overtone band
adapted to selectively interact with molecular resonance vibrations at one
or both of the O--H and N--H vibration frequencies.
Method steps and apparatus elements may be provided for measuring the
weight per unit area of the mat passing through the measuring zone, and
controlling the rate of travel of the mat in accordance with the weight
per unit area measurement; controlling the rate of application of the
binder coating in accordance with the second mathematical function, and
controlling the temperature of the mat during at least a portion of the
curing process in accordance with the output response.
The objects of this invention are to provide methods and apparatus for
accurately and reliably measuring the degree of cure of traveling
carbonaceous polymeric materials in a substantially instantaneous,
continuous and non-destructive manner; to provide such methods and
apparatus which make possible automatic feedback control of curing
processes so as to maintain constant a desired degree of polymerization of
the material; to provide such methods and apparatus that are useable when
the polymeric material has been applied as a binder or coating for other
materials, and to provide an improved measuring and controlling system for
a glass fiber manufacturing process including binder cure control.
Other objects and advantages of the invention will become apparent in the
following detailed description of some best modes for carrying out the
invention, taken in conjunction with the appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic showing of a process for producing a mat of glass
fibers that are coated with a controlled amount of a carbonaceous
polymeric binder material and cured to an optimum degree of polymerization
of the binder by a method and apparatus according to the invention.
FIG. 2 is a schematic showing, including a quasi-section on the line 2--2
of FIG. 1, of an apparatus for automatically determining the degree of
cure and binder weight of the polymeric coating material.
FIG. 3 is an enlarged and more detailed schematic showing of a portion of
FIG. 2.
FIG. 4 is a graph depicting near-infrared absorption spectra of a
particular carbonaceous polymeric material in four different stages of
cure.
FIG. 5 is a graph depicting near-infrared reflection spectra of a
particular carbonaceous polymeric material in four different stages of
cure.
BEST MODES FOR CARRYING OUT THE INVENTION
Referring to FIG. 1, molten glass from a melter 10 flows into a forehearth
12 that supplies a stream 14 of melted glass to a centrifugal spinner 16.
Filaments 18 of glass ejected from the spinner 16 are directed downwardly
and partially solidified by air streams from jets as at 20. The filaments
18 descend through a felting chamber 22 and are collected on a traveling
conveyor chain 24. Air suction through the conveyor 24, depicted by arrows
26, aids the formation of a fiber blanket 28 on the conveyor.
The filaments 18 are sprayed, during their descent through the felting
chamber 22, with a binder spray ejected through a plurality of spray
nozzles as at 30. The binder spray comprises a carbonaceous polymeric
material that has been formed from a plurality of chemical reactants 32.
Typically the reactants 32 comprise the components of phenol-formaldehyde
and urea-formaldehyde that are mixed in a suitable material former 34 and
supplied to an injection pump 36. Pump 36 pressure-feeds the spray nozzle
30 through a header 38 and distributor pipes as at 40. As a result of the
foregoing process, the blanket 28 comprises a mat of glass fibers that
have a binder coating of uncured carbonaceous polymeric material.
The polymeric binder material is subjected to a curing process which is
completed by transporting the blanket 28 through ovens as at 42 and 44 on
the conveyor 24. The conveyor moves to the right in FIG. 1, as indicated
by the arrow 46. In the ovens 42 and 44, the mat of glass fibers is
exposed to elevated temperatures for a time period appropriate to effect
the cure of the polymeric material that forms the binder coating on the
fibers.
In due time the cured glass fiber mat 48 emerges from the last oven 44 and
is cooled by a current of air (indicated by arrows at 50 and 52) from a
fan (not shown). The mat 48 is picked up by other conveyors indicated
generally at 54 whose movement is synchronized with the operation of a
shear 56 and a windup 58 that forms somewhat compressed rolls of the glass
fiber mat for shipment or storage.
The filamentary glass 18 is commonly ejected from the spinner 16 at a
substantially constant rate (mass per unit time) and hence the weight
(mass per unit area) of the cured mat 48 depends on the rate of travel of
the chain conveyor 24 as set by a conveyor speed control 60. The cured and
cooled mat is commonly measured in a measuring zone 62 wherein there is
located a gamma-ray or x-ray gauge having a radiation source unit 64 and a
radiation detector unit 66. Radiations emitted from the source unit 64
pass through the mat 48 and are attenuated by absorption in the mat in
accordance with its mass per unit area. The unabsorbed radiation is
detected in the detector unit 66 to produce a detector signal that is
processed by conventional means not shown to produce a response,
represented by a line 68, that is utilized by the speed control unit 60 to
control the speed of conveyor 24. The objective of this feedback control
is to maintain the weight of the mat 48 nominally constant along its
length at a desired value.
The weight (mass per unit area) of the polymeric binder material contained
in the cured mat 48 is controlled by a sprayer control device 70. Device
70 may regulate the volume per unit time of the spray material fed by the
pump 36 to the spray nozzles 30, or it may control the dilution of the
spray material.
The degree of polymerization, or degree of cure, of the carbonaceous
polymeric binder material is determined by the temperature in the ovens as
at 42 and 44. The temperature of one or more of the ovens may be
controlled by a temperature control unit 72. As previously noted above,
the line operator commonly observes the "color" of the mat 48 issuing from
the last oven 44 and manually adjusts the set-point of the temperature
control unit 72 accordingly.
The apparatus so far described | | |