CN112557310B - Method for detecting carbon black in polymer material for selective laser sintering - Google Patents
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Abstract
A method for detecting carbon black in a polymer material for selective laser sintering, comprising: adding white powder into a material to be detected, and stirring at a high speed to obtain a sample to be detected, wherein the weight ratio of the material to be detected to the white powder is 1-19; measuring the hue value and the chromaticity parameter of a sample to be measured, firstly substituting the hue value into a pre-stored hue value database, and judging the carbon black type of the sample to be measured according to the affiliated range of the hue value; then substituting the chromaticity parameters into a pre-stored standard function model corresponding to the type of the carbon black to which the sample to be tested belongs to obtain the content value of the carbon black in the sample to be tested, wherein the detection method of the carbon black in the polymer material for selective laser sintering does not relate to the combustion of the carbon black, so that the environment pollution is avoided, namely the environment is protected; the detection method is simple and easy to implement, the use difficulty of testers is reduced, and the test speed is high; in addition, the invention can evaluate the type of the carbon black and synchronously detect the content of the carbon black.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to a method for detecting carbon black in a polymer material for selective laser sintering.
Background
Additive manufacturing is a technology for manufacturing objects by using three-dimensional model data in a layer-by-layer stacking mode, and has the unique advantages of short production period in small batch, no redundant tailings in production, high production flexibility and the like, so the additive manufacturing has more and more attention in the manufacturing industry in recent years. The Selective Laser Sintering (SLS) technology has the unique advantages of simple manufacturing process, no need of a supporting structure, extremely high material utilization rate and the like, and becomes one of additive manufacturing technologies which are developed fastest and have industrial production capacity.
As is well known, polymers are common materials for SLS, which achieve sinter molding by absorbing energy from a CO2 laser. However, the CO2 laser is expensive and has low energy density, so that the processing cost and speed of the polymer are greatly limited. To break through this bottleneck, the Flight technology based on the fiber laser with lower cost and extremely high upper limit of released energy is considered as a new generation technology for implementing the scale industrialization of the SLS technology. At present, the wavelength of an optical fiber laser is usually between 500 to 2000nm, almost all polymers cannot absorb the energy of the optical fiber, so the polymers for Flight in the market need to add carbon black into a polymer material as a 'heat medium' to realize sintering and molding of the polymer, such as patent numbers: CN109517377B, CN109575323A. However, carbon black is recognized as a 2B carcinogen by the world health organization, and is strictly controlled when sold at home and abroad. Therefore, whether the polymer for Flight is used for marketing behavior or product quality control, the detection of the carbon black auxiliary agent is an important ring in the production and sale of the material.
Currently, in the traditional technical field, there are three main methods for detecting carbon black in polymer: 1. a combustion method for measuring the content of carbon black by utilizing the difference of combustion characteristics of the material in oxygen and nitrogen atmosphere; 2. thermogravimetric analysis for determining carbon black content by using different decomposition characteristics of the material in oxygen and nitrogen atmosphere; 3. the content of the carbon black is calculated by utilizing the content of tail gas generated after the material is decomposed and calcined, such as the following patent numbers: CN103645116B. However, the above methods utilize the basic principle that the thermal characteristics of the polymer material and the carbon black are different to calculate the content of the carbon black, and have the following inherent defects. First, these methods inevitably involve material consumption and burning of carbon black, are environmentally unfriendly, and increase the cost of test consumables. Secondly, the methods all need professional equipment and professional testers to complete the content of the carbon black in the material, so that the fixed asset investment of material detection is increased. Thirdly, the method for detecting carbon black by utilizing thermal characteristics requires secondary air charging in equipment and slow gradient temperature rise, and the material test period is long. Fourth, these methods only quantitatively measure the content of the material, while other specialized equipment is required for qualitative measurement. From the above, these techniques are not conducive to industrial large-scale detection of carbon black in polymer materials for selective laser sintering.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides the method for detecting the carbon black in the polymer material for selective laser sintering, which does not pollute the environment, is simple and feasible and can synchronously realize the detection of the content and the type of the carbon black.
In order to solve the technical problem, the invention provides a preparation method of a method for detecting carbon black in a polymer material for selective laser sintering, which comprises the following steps:
step one, adding white powder into a material to be detected, and stirring at a high speed to obtain a sample to be detected, wherein the weight ratio of the material to be detected to the white powder is 1-19;
measuring the hue value and the chromaticity parameter of the sample to be measured, firstly substituting the hue value into a pre-stored hue value database, and judging the type of the carbon black of the sample to be measured according to the affiliated range of the hue value; then substituting the chromaticity parameters into a pre-stored standard function model corresponding to the type of the carbon black to which the sample to be tested belongs to obtain the content value of the carbon black in the sample to be tested; wherein the content of the first and second substances,
the pre-stored hue value database is obtained by the following method:
preparing a plurality of calibration group samples according to the method of the first step, wherein the carbon black type in each calibration group sample is different, and each calibration group sample comprises a plurality of samples with different carbon black contents;
respectively measuring the hue value of each sample in a plurality of calibration group samples, recording the fluctuation range of the hue value of different types of carbon black under different contents, and establishing a database for judging the type of the carbon black to which the sample to be tested belongs according to the fluctuation range in which the hue value of the sample to be tested is located;
the pre-stored standard function model is obtained by the following method:
respectively measuring the chromaticity parameters of each sample in each calibration group of samples in a pre-stored hue value database;
and establishing a standard function model of the calibration group of samples by a regression analysis method according to the known carbon black content parameter and the measured chromaticity parameter of each sample.
As a further preferable aspect of the present invention, the carbon black content covered by the several calibration group samples form a data set, and when the content of the carbon black in the material to be measured is i, the range of the data set is included in i ± 2%.
As a further preferable scheme of the invention, when the content of the carbon black in the material to be tested is 2%, the range of the data set is 0-4%.
In a further preferred embodiment of the present invention, the calibration material contains carbon black species to which the sample to be measured belongs, and the total number of species contained is at least 3.
In a further preferred embodiment of the present invention, the number of the calibration set samples is 5 to 10, and the parts of the white powder is 1 to 19.
As a further preferable aspect of the present invention, the material to be measured is nylon powder, thermoplastic polyurethane powder, polypropylene powder, polyethylene powder, ethylene-vinyl acetate copolymer powder, polyether sulfone powder, polyphenylene sulfide powder, or polyether ether ketone powder.
As a further preferable embodiment of the present invention, the white powder is mica, titanium dioxide, glass beads, talc, montmorillonite, silica or a polymer base material powder same as the material to be measured.
As a further preferable aspect of the present invention, the white powder has a white chroma value of 90% or more.
In a further preferable embodiment of the invention, the rotation speed of the high-speed stirring is 150 to 2000 r/min, and the time is 2 to 30min.
The invention relates to a method for detecting carbon black in a polymer material for selective laser sintering, which comprises the following steps: adding white powder into a material to be detected, and stirring at a high speed to obtain a sample to be detected, wherein the weight ratio of the material to be detected to the white powder is 1-19; measuring the hue value and the chromaticity parameter of a sample to be measured, firstly substituting the hue value into a pre-stored hue value database, and judging the carbon black type of the sample to be measured according to the affiliated range of the hue value; then substituting the chromaticity parameters into a pre-stored standard function model corresponding to the type of the carbon black to which the sample to be detected belongs to obtain the content value of the carbon black in the sample to be detected, so that the detection method does not relate to the combustion of the carbon black, avoids the environmental pollution, and protects the environment; the detection method is simple and easy to implement, the use difficulty of testers is reduced, and the test speed is high; in addition, the invention can evaluate the type of the carbon black and synchronously detect the content of the carbon black.
Drawings
FIG. 1 is a functional expression of the relationship between the carbon black content and the change in brightness.
Detailed Description
At present, most of substrates of SLS materials are white, and the added carbon black has three main characteristics. Firstly, in the existing form, the carbon black in the SLS polymer is usually added in a dry mixing and stirring manner, so that the carbon black is uniformly covered on the surface of the material, and the chromaticity of the carbon black determines the chromaticity characteristics of the material; secondly, different types of carbon black are usually subjected to different types of surface treatment, and hue values expressed in a visible spectrum region are different, for example, carbon black subjected to surface modification by an amine auxiliary agent has strong absorption in a range of 570 to 610nm, the chromaticity b value of the material is high, and the a value is low. Therefore, the color value of the material can be used for identifying the type of the carbon black; thirdly, carbon black is a black dye, and has a very strong dyeing ability. It is clear that the higher the content of carbon black in the material, the higher the coverage of carbon black, the darker the colour of the material and the lower the lightness value (L value). Therefore, the L value (or X, Y, Z, T, R, etc. parameters reflecting the brightness characteristics of the material) of the material can be used to obtain the carbon black content in the SLS polymer. The derivation process is detailed as follows:
according to the lambert beer's law, the absorbance of a material is directly proportional to the content (or concentration) and thickness of the substance, and for SLS materials containing carbon black, visible light is mainly absorbed by the carbon black. Therefore, in a spectroscopic apparatus in which the thickness of a sample is fixed, a, T are respectively absorbance and transmittance, k is a constant, and C is the carbon black content.
For the tristimulus value function CIE-XYZ, the light transmittance (or diffuse reflection factor) of the green primary color in the photopic function where the wavelength of 555nm is an extreme value is Y, and the lightness L value and Y value in the spatial chromaticity have the following relationship:
therefore, the relationship between the color value and the carbon black content is a logarithmic function with a base 10:
as shown in fig. 1, for a typical base 10 logarithmic function, when the argument is large, the function can be approximately regarded as a linear function in the interval. Therefore, only when the brightness of the material is high, i.e. the content of carbon black is low, the content is linear with the brightness L, which is described as the following model, where m and n correspond to two constants, namely the slope and the intercept, respectively, in a linear function.
In summary, the commonly used white powder is added into the selective laser sintering material containing carbon black, and when the content of the carbon black is diluted to a certain degree, a linear function can be established by a regression analysis method, so that the rapid detection of the content of the carbon black by spectral equipment such as a spectrophotometer and a colorimeter is realized.
The inventor of the present application provides a preparation method of a detection method of carbon black in a polymer material for selective laser sintering by the above inventive work, the method comprising the steps of:
step one, adding white powder into a material to be detected, and stirring at a high speed to obtain a sample to be detected, wherein the weight ratio of the material to be detected to the white powder is 1-19;
step two, measuring the hue value and the chromaticity parameter of the sample to be measured, firstly substituting the hue value into a pre-stored hue value database, and judging the carbon black type of the sample to be measured according to the range of the hue value; then substituting the chromaticity parameters into a pre-stored standard function model corresponding to the type of the carbon black to which the sample to be tested belongs to obtain the content value of the carbon black in the sample to be tested; wherein the content of the first and second substances,
the pre-stored hue value database is obtained by the following method:
preparing a plurality of calibration group samples according to the method of the first step, wherein the carbon black type in each calibration group sample is different, and each calibration group sample comprises a plurality of samples with different carbon black contents;
respectively measuring the hue value of each sample in a plurality of calibration group samples, recording the fluctuation range of the hue value of different types of carbon black under different contents, and establishing a database for judging the type of the carbon black to which the sample to be tested belongs according to the fluctuation range in which the hue value of the sample to be tested is located;
the pre-stored standard function model is obtained by the following method:
respectively measuring the chromaticity parameters of each sample in each calibration group of samples in a pre-stored hue value data base;
and establishing a standard function model of the calibration group of samples by a regression analysis method according to the known carbon black content parameters of each sample and the measured chromaticity parameters, namely establishing the standard function model corresponding to the carbon black type of the calibration group of samples.
In order to further improve the detection accuracy, preferably, the material to be detected can be detected in multiple batches, and the average value of the material to be detected is finally detected.
Preferably, for the sake of simple calculation, the standard function model is a linear equation C = m × S + n, where C is the weight content of carbon black, S is a chromaticity parameter, and m and n are constant values, which can be obtained by regression analysis method and parameters of several calibration group samples.
It should be noted here that the carbon black is subjected to different surface treatments, so that different types are presented, and preferably, in order to ensure the accuracy of the test, the calibration material includes the type of the carbon black to which the sample to be tested belongs, and the total number of the types of the carbon black is at least 3, that is, a designer first pre-judges the type of the material to be tested, then selects the calibration material including the same type of material as the material to be tested, and then selects several types of materials similar to the material to be tested.
The calibration set of samples selected comprised materials (containing the material to be tested and the white powder) that differed from the material of step 1 only in carbon black content, but of course could be the same, with the other materials being identical.
Specifically, the chromaticity parameter of the sample to be measured or the calibration group sample can be measured through a spectrometer; measuring hue parameters of the sample to be measured or the calibration group sample by a colorimeter; preferably, the colorimetric parameter is a hunter spatial lightness L value; the hue values are a and b values in the CIE1976 chromaticity space, and the L value can more quickly approach to the first-order function when being brought into the first-order function relative to other chromaticity parameters, namely, the effect of high test precision is achieved.
It should be noted here that, for each kind of material to be detected, a pre-stored standard function model can be obtained through a test, and then, the chromaticity parameters detected for the material to be detected for measuring the kind of carbon black are directly substituted into the standard function model, so that the content of the carbon black can be detected; however, if other types of materials to be detected need to be detected, the pre-stored standard function model needs to be obtained through experiments again according to the steps, and similarly, the content of the carbon black can be detected by directly substituting the chromaticity parameters detected by measuring the materials to be detected into the standard function model.
Preferably, the carbon black content covered by the several calibration group samples forms a data set, and when the content of carbon black in the material to be tested is i, the range of the data set is included in i ± 2%. For example, when the content of carbon black in the material to be measured is 2%, the range of the data set is 0 to 4%. Further preferably, the data set is distributed with more and less sides in the middle, and the detection result is faster and more accurate.
The number of the calibration group samples can be 3-20, preferably 5-10, and the appropriate number of the calibration groups can reduce the error of material testing and simultaneously reduce the workload; the number of parts of the white powder is preferably 1 to 19 parts because when the number of parts of the filler is too low, the error of regression analysis is large and the coefficient of determination is insufficient. And when the number of copies is too high, the precision of the test equipment is reduced, so that the test error is large.
The material to be detected is nylon powder, thermoplastic polyurethane powder, polypropylene powder, polyethylene powder, ethylene-vinyl acetate copolymer powder, polyether sulfone powder, polyphenylene sulfide powder or polyether ether ketone powder.
Preferably, the white powder is micaceite, titanium dioxide, glass microbeads, talcum powder, montmorillonite, silicon dioxide or the same polymer base material powder as the material to be tested. The materials are common materials of SLS technology, so that the samples can be recycled after being tested, the material waste is avoided, and the cost is saved.
Preferably, the white powder has a white chroma value greater than or equal to 90%, which can effectively reduce the test error caused by the filling material.
In a further preferable embodiment of the invention, the rotation speed of the high-speed stirring is 150 to 2000 r/min, and the time is 2 to 30min.
In order to make the technical solutions of the present invention better understood and realized by those skilled in the art, the technical solutions of the present invention are described in detail below by way of examples.
Example 1:
1 part of each of nylon 12 materials having carbon black contents of 1%, 1.5%, 2%, 2.5% and 3% in CB1, CB2 and CB3 (three different carbon black types represented by CB1, CB2 and CB 3) was taken, 1 part of each of glass beads having a whiteness of 92% was added, and the mixture was stirred at 200r/min for 5min. Measuring various chromaticity parameter L values of the polymer composite material by a colorimeter, and simultaneously recording the hue parameters a and b; obtaining the hue value fluctuation range of the composite material with different carbon black contents, and establishing a database, referring to table 1; meanwhile, a standard linear function model CB1= m1 xL 1+ n1, CB2= m2 xL 2+ n2 and CB3= m3 xL 3+ n3 is established by a regression analysis method, and the correlation between the L value and the carbon black content is obtained and is shown in a table 2;
test set 1
Taking 1 part of finished nylon 12 powder containing carbon black (for verifying the test accuracy, the known type of the carbon black is that the content of CB1 is 1.8 percent) and 1 part of glass beads, and stirring for 5min under the condition of 200r/min to obtain a sample to be tested; and respectively testing the L values and the a and b values of the three batches of samples, substituting the a and b values into the database in the table 1 to obtain the carbon black types of the test samples, referring to the table 5, and substituting the L values into the corresponding standard function models in the table 3 to obtain the content of the carbon black in the selective laser sintering material, referring to the table 6.
Example 2:
1 part of nylon 6 material with the carbon black contents of CB4, CB5 and CB6 of 1 percent, 2 percent and 3 percent respectively is taken, 2 parts of nylon 6 base material powder is added respectively, and the mixture is stirred for 5min under the condition of 200 r/min. Measuring various chromaticity parameter Y values of the polymer composite material by a colorimeter, and simultaneously recording the hue parameters a and b; obtaining the hue value fluctuation range of the composite material with different carbon black contents, and establishing a database, referring to table 3; meanwhile, a standard linear function model CB4= m4 × Y4+ n4, CB5= m5 × Y5+ n5 and CB6= m6 × Y6+ n6 is established by a regression analysis method, and the correlation between the Y value and the carbon black content is obtained and is shown in a table 4;
Taking 1 part of finished nylon 6 powder containing carbon black (for verifying the test accuracy, the known type of the carbon black is that the content of CB6 is 1.8 percent) and 2 parts of nylon 6 base material powder, and stirring for 5min under the condition of 200r/min to obtain a sample to be tested; and respectively testing the Y values and the a and b values of the three batches of samples, substituting the a and b values into the database in the table 3 to obtain the carbon black types of the test samples, and substituting the Y values into the corresponding standard function models in the table 4 to obtain the content of the carbon black in the selective laser sintering material.
Table 1: hue test value of each calibration set of samples in example 1
Table 2: calibration set of colorimetric parameter test values and corresponding regression analysis models in example 1
Table 3: hue test value of each calibration set of samples in example 2
Table 4: example 2 test values of colorimetric parameters of calibration group samples and corresponding regression analysis model
Table 5: discrimination of hue value and type of each sample to be measured
Table 6: error in testing carbon black content of each sample to be tested
According to the embodiment, the method is simple and easy to implement, and the test data is accurate. Not only the test for the carbon black content has a small error, but also the kind of carbon black can be evaluated. In addition, referring to table 6, it can be seen from comparison between example 1 and example 2 that when the number of test sets in the calibration set is high, the determination coefficient of the fitting function is relatively large, the test accuracy is increased, and the final test error is small. And because the tested L value can more quickly approach to a linear function relative to Y, the L value can more quickly approach to a target fitting function under the same mixing condition, the corresponding determination coefficient of the function is increased, the testing precision is higher, and the detection error of the carbon black content in the finished product is smaller.
The above-mentioned embodiments only express various embodiments of the present invention, and the description thereof is more specific and detailed, but does not represent a limitation to the scope of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention, and the scope of the invention is to be determined by the appended claims.
Claims (8)
1. A method for detecting carbon black in a polymer material for selective laser sintering is characterized by comprising the following steps:
step one, adding white powder into a material to be detected, and stirring at a high speed to obtain a sample to be detected, wherein the weight ratio of the material to be detected to the white powder is 1-19;
step two, measuring the hue value and the chromaticity parameter of the sample to be measured, firstly substituting the hue value into a pre-stored hue value database, and judging the carbon black type of the sample to be measured according to the range of the hue value; then substituting the chromaticity parameters into a pre-stored standard function model corresponding to the type of the carbon black to which the sample to be tested belongs to obtain the content value of the carbon black in the sample to be tested; wherein, the first and the second end of the pipe are connected with each other,
the pre-stored hue value database is obtained by the following method:
preparing a plurality of calibration group samples according to the method of the first step, wherein the carbon black type in each calibration group sample is different, and each calibration group sample comprises a plurality of samples with different carbon black contents;
respectively measuring the hue value of each sample in a plurality of calibration group samples, recording the fluctuation range of the hue value of different types of carbon black under different contents, and establishing a database for judging the type of the carbon black to which the sample to be tested belongs according to the fluctuation range in which the hue value of the sample to be tested is located;
the pre-stored standard function model is obtained by the following method:
respectively measuring the chromaticity parameters of each sample in each calibration group of samples in a pre-stored hue value data base;
establishing a standard function model of the calibration group of samples by a regression analysis method according to the known carbon black content parameter of each sample and the measured chromaticity parameter; wherein the content of the first and second substances,
the material to be detected is nylon powder, thermoplastic polyurethane powder, polypropylene powder, polyethylene powder, ethylene-vinyl acetate copolymer powder, polyether sulfone powder, polyphenylene sulfide powder or polyether ether ketone powder;
the white powder is mica stone, titanium dioxide, glass beads, talcum powder, montmorillonite, silicon dioxide or polymer base material powder which is the same as the material to be detected.
2. The method according to claim 1, wherein the carbon black content covered by the plurality of calibration group samples form a data set, and the range of the data set is i ± 2% when the content of carbon black in the material to be tested is i.
3. The detection method according to claim 2, wherein when the content of carbon black in the material to be detected is 2%, the range of the data set is 0 to 4%.
4. The detection method according to claim 3, wherein the calibration-group sample comprises the carbon black species to which the sample to be detected belongs, and the total number of the species contained is at least three.
5. The detection method according to claim 1, wherein the standard function model is a linear equation of one degree C = m × S + n, where C is a weight content of carbon black, S is a chromaticity parameter, and m and n are constant values.
6. The detection method according to claim 1, wherein the number of the calibration group samples is 5 to 10, and the parts of the white powder are 1 to 19.
7. The detection method according to claim 6, wherein the white powder has a white colorimetric value of 90% or more.
8. The detection method according to any one of claims 1 to 7, wherein the rotation speed of the high-speed stirring is 150 to 2000 r/min, and the time is 2 to 30min.
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