CN117470793B - High-efficiency comprehensive detection method for photosensitive resin composition - Google Patents
High-efficiency comprehensive detection method for photosensitive resin composition Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 153
- 239000011342 resin composition Substances 0.000 title claims abstract description 79
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 28
- 238000002835 absorbance Methods 0.000 claims abstract description 27
- 238000004364 calculation method Methods 0.000 claims abstract description 16
- 238000011156 evaluation Methods 0.000 claims abstract description 6
- 238000005452 bending Methods 0.000 claims description 24
- 238000000926 separation method Methods 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001228 spectrum Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 238000009864 tensile test Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 230000036962 time dependent Effects 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000001419 dependent effect Effects 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000005011 phenolic resin Substances 0.000 description 4
- 229920001568 phenolic resin Polymers 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002781 deodorant agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/20—Investigating strength properties of solid materials by application of mechanical stress by applying steady bending forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0001—Type of application of the stress
- G01N2203/0003—Steady
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0023—Bending
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
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- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
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Abstract
The invention relates to the field of resin quality detection, in particular to a high-efficiency comprehensive detection method of a photosensitive resin composition, which comprises the following steps: s1, acquiring a first sample to be detected, a second sample to be detected and a third sample to be detected from a photosensitive resin composition; s2, obtaining absorbance indexes of a first sample to be detected on light sources with different wavelengths through detection; s3, obtaining the decomposition temperature of a second sample to be detected through detection; s4, acquiring a curing rate index of a third sample to be detected through detection and calculation; s5, after the third sample to be detected is completely solidified, detecting and calculating the mechanical strength of the solidified third sample to be detected; s6, generating a detection report of the photosensitive resin composition. According to the scheme, different properties of the sample are detected through the plurality of modules, so that the absorbance, the decomposition temperature, the curing rate index and the mechanical strength of the photosensitive resin composition are obtained, and the comprehensive evaluation of the properties of the photosensitive resin composition is facilitated.
Description
Technical Field
The invention relates to the field of resin quality detection, in particular to a high-efficiency comprehensive detection method of a photosensitive resin composition.
Background
The photosensitive resin composition is a material which can be subjected to chemical reaction or physical change under the illumination condition, and is widely applied to the fields of 3D printing, photoetching manufacturing, microelectronic manufacturing and the like. In the preparation and application of photosensitive resin compositions, efficient integrated detection methods are critical to ensure product quality and performance.
In response to this demand, new detection techniques and methods such as optical spectroscopy, surface analysis, electron microscopy, etc. have emerged in recent years. The novel technology has the advantages of high sensitivity, real-time performance, non-destructive performance and the like, and can provide more possibility for comprehensive detection of the photosensitive resin composition.
The prior art of CN103235485A discloses a photosensitive dry film and a detection method thereof, which sequentially comprise a PET supporting film layer, a photosensitive resin layer and a PE protecting film layer, wherein the photosensitive resin layer mainly comprises alkali-soluble resin, a photopolymerizable compound with at least one ethylenically unsaturated group, a photopolymerization initiator and a deodorant, and the weight parts of the components of the photosensitive resin layer are 60-70 parts of the alkali-soluble resin, 15-25 parts of the photopolymerizable compound, 1-2 parts of the photopolymerization initiator and 0.01-0.1 part of the deodorant.
Another typical test method disclosed in the prior art of CN109374426a is a test method for high temperature resistance of phenolic resin used for precoated sand binder, which uses sand grains, phenolic resin and curing agent as raw materials, and prepares a standard test block, then the standard test block is loaded at constant temperature and constant pressure or continuously pressurized at constant temperature, the time or pressure required for crushing the standard test block is tested, and the time and pressure for high temperature resistance of phenolic resin are determined, so that the unused phenolic resin is selected according to different casting materials.
Looking at a laser curing rapid prototyping photosensitive resin luminousness detector as disclosed in the prior art of CN205719973U, the detector comprises a universal wheel, a detector, a resin container, a rotating support and an upper cover plate, wherein the detector is arranged above the universal wheel, the resin container is arranged inside the detector, the rotating support is arranged above the side of the resin container, the upper cover plate is arranged above the rotating support, a prototyping analyzer is arranged on one side of the upper cover plate, a data display is arranged above the prototyping analyzer, a signal lamp is arranged on one side of the data display, a starting button is arranged on the other side of the signal lamp, an input keyboard is arranged below the starting button, a storage box is arranged below the input keyboard, and a closing plate is arranged on one side of the storage box.
At present, the detection method of the photosensitive resin composition is mostly single, various detection indexes of the photosensitive resin composition are difficult to obtain through a single system, and the invention is made in order to solve the common problems in the field.
Disclosure of Invention
The invention aims to provide a high-efficiency comprehensive detection method of a photosensitive resin composition aiming at the defects existing at present.
In order to overcome the defects in the prior art, the invention adopts the following technical scheme:
a high-efficiency comprehensive detection method of a photosensitive resin composition comprises the following steps:
s1, acquiring a first sample to be detected, a second sample to be detected and a third sample to be detected from a photosensitive resin composition;
s2, obtaining absorbance indexes of a first sample to be detected on light sources with different wavelengths through detection;
s3, obtaining the decomposition temperature of a second sample to be detected through detection;
s4, acquiring a curing rate index of a third sample to be detected through detection and calculation;
s5, after the third sample to be detected is completely solidified, detecting and calculating the mechanical strength of the solidified third sample to be detected;
s6, generating a detection report of the photosensitive resin composition.
Further, in S1, obtaining the first sample to be detected, the second sample to be detected, and the third sample to be detected includes the following steps:
s11, fully stirring the photosensitive resin composition to uniformly mix the photosensitive resin composition;
s12, extracting a specified amount of a zeroth sample to be detected from the photosensitive resin composition through a separation funnel;
s13, measuring the mass of a zeroth sample to be detected;
s14, separating the zeroth sample to be detected into a first sample to be detected, a second sample to be detected and a third sample to be detected which are identical in mass through a separating funnel.
Further, in S2, obtaining the absorbance index of the first sample to be detected includes the following steps:
s21, equally dividing the first detection sample into a plurality of fourth detection samples with the same mass;
s22, respectively placing a plurality of fourth detection samples in light paths of light sources with different wavelengths at normal temperature;
s23, recording the light intensity of the light after passing through a plurality of fourth detection samples;
s24, calculating absorbance indexes of a plurality of fourth detection samples by the following formula:
A=;
wherein A is an absorbance index,for the light intensity of the light source>An initial value of the light intensity after the light passes through the fourth detection sample;
s25, selecting the wavelength of the light source corresponding to the fourth detection sample with the maximum absorbance as the optimal working wavelength of the photosensitive resin composition.
Further, in S3, obtaining the decomposition temperature of the second sample to be detected includes the following steps:
s31, heating a second sample to be detected;
s32, recording the condition that the mass of the second detection sample changes along with the temperature in the heating process;
s33, generating a mass-to-temperature change curve of the second detection sample, wherein the abscissa is temperature and the ordinate is mass;
s34, starting from the starting point of the mass-to-temperature curve, searching from left to right along the x-axis for the value x of the first x satisfying the following formula 1 As the value of the decomposition temperature:
;
wherein,values of the abscissa, which are the starting points of the mass versus temperature curve, +.>Values of the ordinate of the origin of the mass-versus-temperature curve, +.>For the value of the temperature of the decomposition process, +.>The value of the ordinate of the x-1 position in the mass versus temperature curve is +.>Is the value of the ordinate of the x+1 position in the mass versus temperature curve.
Further, in S4, obtaining the cure rate indicator of the third sample to be detected includes the following steps:
s41, placing a third sample to be detected in a light path at normal temperature;
s42, selecting the light source with the optimal working wavelength obtained in the S25 to irradiate a third sample to be detected;
s43, recording the condition that the light intensity of the light source changes along with time after passing through a third sample to be detected;
s44, calculating a curing rate index of the third sample to be detected according to the following formula:
;
wherein P is a curing rate index,is the light intensity of the light after the light passes through the third sample to be detected for a period of t, t being the period used for the detection,/-for>Is the initial value of the light intensity of the light after passing through the third sample to be detected.
S45, generating a time-dependent curve of the curing rate index according to the calculation result in S44.
Further, in S5, detecting and calculating the mechanical strength of the cured third sample to be detected includes the following steps:
s51, extracting the third sample to be detected after solidification in the S4;
s52, cutting the solidified third sample to be detected into three parts with approximately equal mass to obtain a fifth sample to be detected, a sixth sample to be detected and a seventh sample to be detected;
s53, carrying out a tensile test on a fifth sample to be detected to obtain tensile strength TS, elongation at break EB and elastic modulus YM of the fifth sample to be detected;
s54, performing bending test on the sixth sample to be detected to obtain bending strength FS and bending modulus FM of the fifth sample to be detected;
it is noted that the above tests all employ ASTM standards;
and S55, performing a Babbitt stiffness test on the seventh sample to be detected to obtain the Babbitt stiffness H of the seventh sample to be detected.
Further, in S6, generating a detection report of the photosensitive resin composition includes the steps of:
s61, calculating a mechanical strength index of the photosensitive resin composition according to the following formula:
JXZB=*/>*/>+/>*/>+H;
wherein JXZB is a mechanical strength index, and e is a natural constant;
s62, calculating the comprehensive performance index of the photosensitive resin composition according to the following formula:
ZB=*A*/>*/>;
wherein ZB is a comprehensive performance index, T is a temperature value in a normal temperature state, T is a detection duration of a third sample to be detected, and x 1 A value of x which is the first;
s63, comparing the comprehensive performance index with a specified threshold value, and evaluating the performance of the photosensitive resin composition;
s65, inputting each calculation result and each evaluation result into a specified template, and thus obtaining a detection report.
Still further, the system comprises a sampling module, an absorbance detection module, a decomposition temperature detection module, a photosensitive detection module, a mechanical strength detection module and a control module; the sampling module comprises a container, a stirrer, a separating funnel and a first quality detection unit, wherein the container is used for loading the photosensitive resin composition, the stirrer is used for stirring the photosensitive resin composition in the container, the separating funnel is used for separating the stirred photosensitive resin composition into a plurality of samples to be detected, and the first quality detection unit is used for detecting the quality of the separated samples to be detected;
the decomposition temperature detection module comprises a temperature control unit, a second quality detection unit and a curve generation unit, wherein the temperature control unit is used for heating the second sample to be detected, the second quality detection unit is used for detecting the quality of the second sample to be detected in the heating process, and the curve generation unit is used for generating a temperature and quality curve of the second sample to be detected according to the set temperature of the temperature control unit and the detection result of the second quality detection unit;
the photosensitive detection module comprises a first separation unit, a light source and a spectrum detection unit, wherein the first separation unit is used for separating the first sample to be detected into a plurality of fourth samples to be detected, the light source is used for providing light with different wavelengths, and the spectrum detection unit is used for detecting the spectrum of the light source after passing through the samples;
the mechanical strength detection module comprises a second separation unit, a tensile property detection unit, a bending property detection unit and a hardness detection unit, wherein the second separation unit is used for separating the third sample to be detected into fifth, sixth and seventh samples to be detected, the tensile property detection unit is used for detecting the tensile property of the fifth sample to be detected, the bending property detection unit is used for detecting the bending property of the sixth sample to be detected, and the hardness detection unit is used for detecting the hardness of the seventh sample to be detected;
the control module is used for controlling the opening and closing of each module.
The beneficial effects obtained by the invention are as follows: 1. the sampling module is used for acquiring a plurality of samples, and the plurality of modules are used for detecting different performances of the samples, so that the absorbance, the decomposition temperature, the curing rate index and the mechanical strength of the photosensitive resin composition are acquired, and the comprehensive evaluation of the performances of the photosensitive resin composition is facilitated;
2. the absorbance of the photosensitive resin composition to light with different wavelengths can be obtained through the photosensitive detection module, and the curing rate index of the photosensitive resin composition under the fixed wavelength can be known, so that the functional diversity of the photosensitive detection module is improved, and the cost of detection equipment required to be used is reduced;
3. and the mechanical strength of the cured third sample to be detected is detected through the mechanical strength detection module, the third sample to be detected is separated into a fifth sample to be detected, a sixth sample to be detected and a seventh sample to be detected, and then the mechanical strength of different types is detected, so that the resource utilization rate is improved, the consumption of the photosensitive resin composition is reduced, and the cost is reduced.
Drawings
The invention will be further understood from the following description taken in conjunction with the accompanying drawings. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the embodiments. Like reference numerals designate like parts in the different views.
FIG. 1 is a schematic of the workflow of the present invention.
FIG. 2 is a schematic diagram showing the structure of a high-efficiency comprehensive detection system for photosensitive resin compositions according to the present invention.
Fig. 3 is a flowchart of the operation of the present invention for obtaining the absorbance index of the first sample to be detected.
FIG. 4 is a flowchart illustrating the operation of obtaining the decomposition temperature of the second sample to be tested according to the present invention.
FIG. 5 is a flowchart illustrating the operation of obtaining the cure rate indicator of the third sample to be tested according to the present invention.
FIG. 6 is a flow chart showing the operation of the present invention for detecting and calculating the mechanical strength of the third sample to be detected after curing.
Detailed Description
The following embodiments of the present invention are described in terms of specific examples, and those skilled in the art will appreciate the advantages and effects of the present invention from the disclosure herein. The invention is capable of other and different embodiments and its several details are capable of modification and variation in various respects, all without departing from the spirit of the present invention. The drawings of the present invention are merely schematic illustrations, and are not intended to be drawn to actual dimensions. The following embodiments will further illustrate the related art content of the present invention in detail, but the disclosure is not intended to limit the scope of the present invention.
Embodiment one: according to fig. 1, 2, 3 and 4, the present embodiment provides a method for high-efficiency comprehensive detection of a photosensitive resin composition, comprising the steps of:
s1, acquiring a first sample to be detected, a second sample to be detected and a third sample to be detected from a photosensitive resin composition;
s2, obtaining absorbance indexes of a first sample to be detected on light sources with different wavelengths through detection;
specifically, absorbance refers to the degree to which light is absorbed as it passes through a substance;
s3, obtaining the decomposition temperature of a second sample to be detected through detection;
specifically, the decomposition temperature refers to a temperature at a moment when the second detection sample starts to undergo severe decomposition under the condition that the temperature is increased, and the quality of the sample rapidly decreases during the severe decomposition, that is, a temperature corresponding to a case when the decreasing quality of the second detection sample in unit time reaches a preset threshold, or a decomposition temperature when the formula set forth in S34 is satisfied;
s4, acquiring a curing rate index of a third sample to be detected through detection and calculation;
specifically, the normal state of the third sample to be detected is liquid, and the solidification rate index reflects the rate of the third sample to be detected that the third sample is changed from liquid to solid after being irradiated by the wavelength light source corresponding to the maximum absorbance index in the S2;
s5, after the third sample to be detected is completely solidified, detecting and calculating the mechanical strength of the solidified third sample to be detected;
s6, generating a detection report of the photosensitive resin composition.
Further, in S1, obtaining the first sample to be detected, the second sample to be detected, and the third sample to be detected includes the following steps:
s11, fully stirring the photosensitive resin composition to uniformly mix the photosensitive resin composition;
s12, extracting a specified amount of a zeroth sample to be detected from the photosensitive resin composition through a separation funnel;
specifically, the specified amount is set by one skilled in the art;
s13, measuring the mass of a zeroth sample to be detected;
s14, separating the zeroth sample to be detected into a first sample to be detected, a second sample to be detected and a third sample to be detected which are identical in mass through a separating funnel.
Further, in S2, obtaining the absorbance index of the first sample to be detected includes the following steps:
s21, equally dividing the first detection sample into a plurality of fourth detection samples with the same mass;
s22, respectively placing a plurality of fourth detection samples in light paths of light sources with different wavelengths at normal temperature;
specifically, the normal temperature state is set to 26 degrees celsius in this scheme;
s23, recording the light intensity of the light after passing through a plurality of fourth detection samples;
s24, calculating absorbance indexes of a plurality of fourth detection samples by the following formula:
A=;
wherein A is an absorbance index,for the light intensity of the light source>An initial value of the light intensity after the light passes through the fourth detection sample;
s25, selecting the wavelength of the light source corresponding to the fourth detection sample with the maximum absorbance as the optimal working wavelength of the photosensitive resin composition.
Specifically, the greater the absorbance of the fourth test sample to light of a certain wavelength, the better the photosensitivity of the photosensitive resin composition to that wavelength.
Further, in S3, obtaining the decomposition temperature of the second sample to be detected includes the following steps:
s31, heating a second sample to be detected;
s32, recording the condition that the mass of the second detection sample changes along with the temperature in the heating process;
s33, generating a mass-to-temperature change curve of the second detection sample, wherein the abscissa is temperature and the ordinate is mass;
s34, starting from the start point of the mass-to-temperature curve, i.e. from the first measured value of mass and temperature, searching from left to right along the x-axis for the value x of the first x satisfying the following formula 1 As the value of the decomposition temperature:
;
wherein,the abscissa value for the start of the mass versus temperature curve, +.>Ordinate value of the origin of the temperature-dependent mass curve,/->For the temperature value of the decomposition process, < >>The value of the ordinate of the x-1 position in the mass versus temperature curve is +.>Is the squat of the x+1 position in the mass-to-temperature curveTarget value.
Specifically, the higher the decomposition temperature, the better the thermal stability of the photosensitive resin composition.
Further, in S4, obtaining the cure rate indicator of the third sample to be detected includes the following steps:
s41, placing a third sample to be detected in a light path at normal temperature;
s42, selecting the light source with the optimal working wavelength obtained in the S25 to irradiate a third sample to be detected;
s43, recording the condition that the light intensity of the light source changes along with time after passing through a third sample to be detected;
s44, calculating a curing rate index of the third sample to be detected according to the following formula:
;
wherein P is a curing rate index,is the light intensity of the light after the light passes through the third sample to be detected for a period of t, t being the period used for the detection,/-for>Is the initial value of the light intensity of the light after passing through the third sample to be detected.
S45, generating a time-dependent curve of the curing rate index according to the calculation result in S44.
Specifically, as the curing proceeds, the curing rate index is correspondingly slowed down, and in the time-dependent curve of the curing rate index, the smaller the slope of the curve, that is, the negative value of the slope corresponds to, the larger the absolute value of the negative value corresponds to, the faster the decay rate of the curing rate index, and the better the curing effect of the photosensitive resin composition.
Further, in S5, detecting and calculating the mechanical strength of the cured third sample to be detected includes the following steps:
s51, extracting the third sample to be detected after solidification in the S4;
s52, cutting the solidified third sample to be detected into three parts with approximately equal mass to obtain a fifth sample to be detected, a sixth sample to be detected and a seventh sample to be detected;
s53, carrying out a tensile test on a fifth sample to be detected to obtain tensile strength TS, elongation at break EB and elastic modulus YM of the fifth sample to be detected;
specifically, the tensile test is performed by stretching the fifth sample to be detected and recording the maximum force that the fifth sample to be detected can bear, the stretching length and the cross-sectional area at break to obtain the result of the tensile test, and the tensile strength TS, the elongation at break EB and the elastic modulus YM can be obtained by calculating the result of the tensile test, and the calculation belongs to the prior art and will not be repeated herein;
s54, performing bending test on the sixth sample to be detected to obtain bending strength FS and bending modulus FM of the fifth sample to be detected;
specifically, the bending test is performed on the sixth sample to be detected, and the maximum bending moment, the distance between the force application points and the cross-sectional area of the sixth sample to be detected are recorded, so that a bending test result is obtained, the bending strength FS and the bending modulus FM can be obtained by calculating the bending test result, and the calculation belongs to the prior art and is not repeated herein;
and S55, performing a Babbitt stiffness test on the seventh sample to be detected to obtain the Babbitt stiffness H of the seventh sample to be detected.
Specifically, the Babbitt stiffness test belongs to the prior art and will not be described in detail herein.
Further, in S6, generating a detection report of the photosensitive resin composition includes the steps of:
s61, calculating a mechanical strength index of the photosensitive resin composition according to the following formula:
JXZB=*/>*/>+/>*/>+H;
wherein JXZB is a mechanical strength index, and e is a natural constant;
s62, calculating the comprehensive performance index of the photosensitive resin composition according to the following formula:
ZB=*A*/>*/>;
wherein ZB is a comprehensive performance index, T is a temperature value in a normal temperature state, T is a detection duration of a third sample to be detected, and x 1 A value of x which is the first;
s63, comparing the comprehensive performance index with a specified threshold value, and evaluating the performance of the photosensitive resin composition;
specifically, the specified threshold includes a first threshold and a second threshold, the first threshold being greater than the second threshold, the first threshold and the second threshold being empirically set by one skilled in the art, the photosensitive resin composition having excellent performance when the overall performance index is greater than the first threshold, the photosensitive resin composition having good performance when the overall performance index is less than the first threshold and greater than the second threshold, and the photosensitive resin composition having unacceptable performance when the overall performance index is less than the second threshold.
S65, inputting each calculation result and each evaluation result into a specified template, and thus obtaining a detection report.
In particular, the templates are designed by the skilled worker.
The beneficial effect of this scheme: and a plurality of samples are obtained through the sampling module, and the different properties of the samples are detected through the plurality of modules, so that the absorbance, the decomposition temperature, the curing rate index and the mechanical strength of the photosensitive resin composition are obtained, and the comprehensive evaluation of the properties of the photosensitive resin composition is facilitated.
Embodiment two: this embodiment should be understood to include all the features of any one of the foregoing embodiments, and further improvements thereto, and further include a high-efficiency integrated detection system for a photosensitive resin composition, the system including a sampling module, an absorbance detection module, a decomposition temperature detection module, a photosensitive detection module, a mechanical strength detection module, and a control module; the sampling module comprises a container, a stirrer, a separating funnel and a first quality detection unit, wherein the container is used for loading the photosensitive resin composition, the stirrer is used for stirring the photosensitive resin composition in the container, the separating funnel is used for separating the stirred photosensitive resin composition into a plurality of samples to be detected, and the first quality detection unit is used for detecting the quality of the separated samples to be detected;
the decomposition temperature detection module comprises a temperature control unit, a second quality detection unit and a curve generation unit, wherein the temperature control unit is used for heating the second sample to be detected, the second quality detection unit is used for detecting the quality of the second sample to be detected in the heating process, and the curve generation unit is used for generating a temperature and quality curve of the second sample to be detected according to the set temperature of the temperature control unit and the detection result of the second quality detection unit;
the photosensitive detection module comprises a first separation unit, a light source, a light path and a spectrum detection unit, wherein the first separation unit is used for separating the first sample to be detected into a plurality of fourth samples to be detected, the light source is used for providing light with different wavelengths for the light path, and the spectrum detection unit is used for detecting the spectrum of the light after passing through the samples placed in the light path;
the mechanical strength detection module comprises a second separation unit, a tensile property detection unit, a bending property detection unit and a hardness detection unit, wherein the second separation unit is used for separating the third sample to be detected into fifth, sixth and seventh samples to be detected, the tensile property detection unit is used for detecting the tensile property of the fifth sample to be detected, the bending property detection unit is used for detecting the bending property of the sixth sample to be detected, and the hardness detection unit is used for detecting the hardness of the seventh sample to be detected; the control module is used for controlling the opening and closing of each module.
Specifically, the spectrum detected by the spectrum detection unit can obtain corresponding light intensity information.
The beneficial effect of this scheme:
1. the absorbance of the photosensitive resin composition to light with different wavelengths can be obtained through the photosensitive detection module, and the curing rate index of the photosensitive resin composition under the fixed wavelength can be known, so that the functional diversity of the photosensitive detection module is improved, and the cost of detection equipment required to be used is reduced;
2. and the mechanical strength of the cured third sample to be detected is detected through the mechanical strength detection module, the third sample to be detected is separated into a fifth sample to be detected, a sixth sample to be detected and a seventh sample to be detected, and then the mechanical strength of different types is detected, so that the resource utilization rate is improved, the consumption of the photosensitive resin composition is reduced, and the cost is reduced.
Embodiment III: this embodiment should be understood to include all the features of any one of the foregoing embodiments, and further improve on the basis thereof, and further characterized in that the control module includes a control unit for controlling on and off of each module, a data acquisition unit for acquiring detection data of each module, a calculation unit for calculating various relevant indexes of the photosensitive resin composition based on the data acquired by the data acquisition unit, and a detection report generation unit for generating a detection report based on the detection data of the data acquisition unit and the calculation result of the calculation unit.
The beneficial effects of this embodiment are: all modules are controlled simultaneously through a single control module, so that the operation of workers is facilitated, various related indexes of the photosensitive resin composition can be calculated through a calculation unit, and the performance of the photosensitive resin composition can be judged through the indexes by the workers.
The foregoing disclosure is only a preferred embodiment of the present invention and is not intended to limit the scope of the invention, so that all equivalent technical changes made by applying the description of the present invention and the accompanying drawings are included in the scope of the present invention, and in addition, elements in the present invention can be updated as the technology develops. The above units are only examples, and those skilled in the art can implement the present embodiment according to actual requirements to implement different designs to adopt corresponding units.
Claims (2)
1. A high-efficiency comprehensive detection method of a photosensitive resin composition is characterized by comprising the following steps:
s1, acquiring a first sample to be detected, a second sample to be detected and a third sample to be detected from a photosensitive resin composition;
s2, obtaining absorbance indexes of a first sample to be detected on light sources with different wavelengths through detection;
s3, obtaining the decomposition temperature of a second sample to be detected through detection;
s4, acquiring a curing rate index of a third sample to be detected through detection and calculation;
s5, after the third sample to be detected is completely solidified, detecting and calculating the mechanical strength of the solidified third sample to be detected;
s6, generating a detection report of the photosensitive resin composition;
in S1, obtaining a first sample to be detected, a second sample to be detected, and a third sample to be detected includes the following steps:
s11, fully stirring the photosensitive resin composition to uniformly mix the photosensitive resin composition;
s12, extracting a specified amount of a zeroth sample to be detected from the photosensitive resin composition through a separation funnel;
s13, measuring the mass of a zeroth sample to be detected;
s14, separating the zeroth sample to be detected into a first sample to be detected, a second sample to be detected and a third sample to be detected which have the same mass through a separating funnel;
in S2, obtaining the absorbance index of the first sample to be detected includes the following steps:
s21, equally dividing the first detection sample into a plurality of fourth detection samples with the same mass;
s22, respectively placing a plurality of fourth detection samples in light paths of light sources with different wavelengths at normal temperature;
s23, recording the light intensity of the light after passing through a plurality of fourth detection samples;
s24, calculating absorbance indexes of a plurality of fourth detection samples by the following formula:
wherein A is absorbance index, I 0 For the light intensity of the light source, I 1 An initial value of the light intensity after the light passes through the fourth detection sample;
s25, selecting the wavelength of a light source corresponding to the fourth detection sample with the maximum absorbance as the optimal working wavelength of the photosensitive resin composition;
in S3, obtaining the decomposition temperature of the second sample to be detected includes the following steps:
s31, heating a second sample to be detected;
s32, recording the condition that the mass of the second detection sample changes along with the temperature in the heating process;
s33, generating a mass-to-temperature change curve of the second detection sample, wherein the abscissa is temperature and the ordinate is mass;
s34, starting from the starting point of the mass-to-temperature curve, searching from left to right along the x-axis for the value x of the first x satisfying the following formula 1 As the value of the decomposition temperature:
wherein x is 0 Values y are the abscissa of the origin of the mass-to-temperature curve 0 The value of the ordinate of the start point of the temperature-dependent mass curve, x is the value of the temperature of the decomposition process, y x-1 Y is the value of the ordinate of the x-1 position in the mass versus temperature curve x+1 Values are the ordinate of the x+1 position in the mass versus temperature curve;
in S4, obtaining the cure rate indicator of the third sample to be detected includes the following steps:
s41, placing a third sample to be detected in a light path at normal temperature;
s42, selecting the light source with the optimal working wavelength obtained in the S25 to irradiate a third sample to be detected;
s43, recording the condition that the light intensity of the light source changes along with time after passing through a third sample to be detected;
s44, calculating a curing rate index of the third sample to be detected according to the following formula:
wherein P is a cure rate indicator, I 3 Is the light intensity of the light after the light passes through the third sample to be detected for a period of t, t is the time used for detection, I 4 Is the initial value of the light intensity of the light after passing through the third sample to be detected;
s45, generating a time-dependent curve of the curing rate index according to the calculation result in S44;
in S5, detecting and calculating the mechanical strength of the cured third sample to be detected includes the following steps:
s51, extracting the third sample to be detected after solidification in the S4;
s52, cutting the solidified third sample to be detected into three parts with approximately equal mass to obtain a fifth sample to be detected, a sixth sample to be detected and a seventh sample to be detected;
s53, carrying out a tensile test on a fifth sample to be detected to obtain tensile strength TS, elongation at break EB and elastic modulus YM of the fifth sample to be detected;
s54, performing bending test on the sixth sample to be detected to obtain bending strength FS and bending modulus FM of the fifth sample to be detected;
s55, performing a Babbitt stiffness test on the seventh sample to be detected to obtain the Babbitt stiffness H of the seventh sample to be detected;
in S6, generating a detection report of the photosensitive resin composition includes the steps of:
s61, calculating a mechanical strength index of the photosensitive resin composition according to the following formula:
wherein JXZB is a mechanical strength index, and e is a natural constant;
s62, calculating the comprehensive performance index of the photosensitive resin composition according to the following formula:
wherein ZB is a comprehensive performance index, T is a temperature value in a normal temperature state, T is a detection duration of a third sample to be detected, and x 1 A value of x which is the first;
s63, comparing the comprehensive performance index with a specified threshold value, and evaluating the performance of the photosensitive resin composition;
s65, inputting each calculation result and each evaluation result into a specified template, and thus obtaining a detection report.
2. The method for the efficient and comprehensive detection of a photosensitive resin composition according to claim 1, further comprising an efficient and comprehensive detection system of the photosensitive resin composition, wherein the system comprises a sampling module, a decomposition temperature detection module, a photosensitive detection module, a mechanical strength detection module and a control module; the sampling module comprises a container, a stirrer, a separating funnel and a first quality detection unit, wherein the container is used for loading the photosensitive resin composition, the stirrer is used for stirring the photosensitive resin composition in the container, the separating funnel is used for separating the stirred photosensitive resin composition into a plurality of samples to be detected, and the first quality detection unit is used for detecting the quality of the separated samples to be detected;
the decomposition temperature detection module comprises a temperature control unit, a second quality detection unit and a curve generation unit, wherein the temperature control unit is used for heating the second sample to be detected, the second quality detection unit is used for detecting the quality of the second sample to be detected in the heating process, and the curve generation unit is used for generating a temperature and quality curve of the second sample to be detected according to the set temperature of the temperature control unit and the detection result of the second quality detection unit;
the photosensitive detection module comprises a first separation unit, a light source and a spectrum detection unit, wherein the first separation unit is used for separating the first sample to be detected into a plurality of fourth samples to be detected, the light source is used for providing light with different wavelengths, and the spectrum detection unit is used for detecting the spectrum of the light source after passing through the samples;
the mechanical strength detection module comprises a second separation unit, a tensile property detection unit, a bending property detection unit and a hardness detection unit, wherein the second separation unit is used for separating the third sample to be detected into fifth, sixth and seventh samples to be detected, the tensile property detection unit is used for detecting the tensile property of the fifth sample to be detected, the bending property detection unit is used for detecting the bending property of the sixth sample to be detected, and the hardness detection unit is used for detecting the hardness of the seventh sample to be detected;
the control module is used for controlling the opening and closing of each module.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5289990A (en) * | 1976-01-22 | 1977-07-28 | Toshiba Corp | Ultraviolet curing testing apparatus for photo sensitive resins |
CN102260382A (en) * | 2010-05-28 | 2011-11-30 | 住友化学株式会社 | Resin composition |
CN103319692A (en) * | 2012-03-22 | 2013-09-25 | 中科院广州化学有限公司 | High performance organosilicon epoxy material, preparation method and applications thereof |
JP5488752B1 (en) * | 2013-09-03 | 2014-05-14 | 住友ベークライト株式会社 | Photosensitive resin material and resin film |
CN103912154A (en) * | 2014-04-12 | 2014-07-09 | 北京大唐恒通机械输送技术有限公司 | Material of chimney with flame-retardant and corrosion-prevention glass fiber reinforced plastic structure |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6063367B2 (en) * | 2012-12-04 | 2017-01-18 | 本田技研工業株式会社 | Evaluation method of kneading dispersibility of epoxy resin |
US20230104391A1 (en) * | 2020-02-26 | 2023-04-06 | Showa Denko Materials Co., Ltd. | Photosensitive resin composition, method for selecting photosensitive resin composition, method for producing patterned cured film, and method for producing semiconductor device |
-
2023
- 2023-12-25 CN CN202311785557.6A patent/CN117470793B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5289990A (en) * | 1976-01-22 | 1977-07-28 | Toshiba Corp | Ultraviolet curing testing apparatus for photo sensitive resins |
CN102260382A (en) * | 2010-05-28 | 2011-11-30 | 住友化学株式会社 | Resin composition |
CN103319692A (en) * | 2012-03-22 | 2013-09-25 | 中科院广州化学有限公司 | High performance organosilicon epoxy material, preparation method and applications thereof |
JP5488752B1 (en) * | 2013-09-03 | 2014-05-14 | 住友ベークライト株式会社 | Photosensitive resin material and resin film |
CN103912154A (en) * | 2014-04-12 | 2014-07-09 | 北京大唐恒通机械输送技术有限公司 | Material of chimney with flame-retardant and corrosion-prevention glass fiber reinforced plastic structure |
Non-Patent Citations (4)
Title |
---|
POE-g-MAH 和EPDM 增韧改性回收聚丙烯/ 玻璃纤维复合材料性能的研究;陈荣源等;《塑料科技》;20230831;22-26 * |
光交联型聚苯醚的合成与表征;李香丹;向芹;何思威;李立忠;申凤善;;中南民族大学学报(自然科学版);20190615(第02期);161-164 * |
聚氨酯丙烯酸酯作为预聚体的光敏树脂的制备及性能;韩文娟;黄笔武;雍涛;谢王付;万时策;;南昌大学学报(理科版);20150825(第04期);363-367 * |
高分子材料的老化表征方法;王小军;文庆珍;朱金华;李志生;余超;;弹性体;20100625(第03期);58-61 * |
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