CN115236022B - Method and system for characterizing and predicting flame synthesis characteristics of precursor - Google Patents
Method and system for characterizing and predicting flame synthesis characteristics of precursor Download PDFInfo
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- 239000002243 precursor Substances 0.000 title claims abstract description 173
- 238000000034 method Methods 0.000 title claims abstract description 61
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 52
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 51
- 239000000654 additive Substances 0.000 claims abstract description 144
- 238000001757 thermogravimetry curve Methods 0.000 claims abstract description 108
- 239000011259 mixed solution Substances 0.000 claims abstract description 105
- 230000000996 additive effect Effects 0.000 claims abstract description 94
- 239000000243 solution Substances 0.000 claims abstract description 83
- 239000000843 powder Substances 0.000 claims abstract description 61
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- 239000007787 solid Substances 0.000 claims abstract description 41
- 230000008859 change Effects 0.000 claims abstract description 28
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- 150000001768 cations Chemical class 0.000 claims abstract description 27
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- 238000005259 measurement Methods 0.000 claims description 24
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- 238000004458 analytical method Methods 0.000 claims description 3
- 238000012795 verification Methods 0.000 claims description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 abstract description 7
- 238000005102 attenuated total reflection Methods 0.000 abstract description 4
- 238000001157 Fourier transform infrared spectrum Methods 0.000 abstract 3
- 150000001875 compounds Chemical class 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 72
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 35
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 32
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 30
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 28
- 239000002245 particle Substances 0.000 description 19
- 239000000047 product Substances 0.000 description 19
- AGOMHFKGCMKLDA-UHFFFAOYSA-K 2-ethylhexanoate;yttrium(3+) Chemical compound [Y+3].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O AGOMHFKGCMKLDA-UHFFFAOYSA-K 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000004580 weight loss Effects 0.000 description 7
- -1 yttrium isobutyrate Chemical compound 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
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- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- SHZIWNPUGXLXDT-UHFFFAOYSA-N caproic acid ethyl ester Natural products CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000002405 diagnostic procedure Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000004433 infrared transmission spectrum Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910001960 metal nitrate Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 239000011877 solvent mixture Substances 0.000 description 2
- 238000010200 validation analysis Methods 0.000 description 2
- BKHUGLYOPGMVDT-UHFFFAOYSA-N C(C)O.[N+](=O)([O-])[O-].[Y+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound C(C)O.[N+](=O)([O-])[O-].[Y+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] BKHUGLYOPGMVDT-UHFFFAOYSA-N 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000007416 differential thermogravimetric analysis Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention provides a method and a system for characterizing and predicting flame synthesis characteristics of a precursor by FTIR and TGA measurement means, wherein the method comprises the following steps: measuring a TGA curve and a DTG curve of a conventional precursor solid powder and a solid powder with a compound as a precursor cation and an additive anion; measuring a TGA and DTG curve of the precursor-solvent mixed solution; measuring ATG-FTIR spectra of the pure solvent solution and the precursor-solvent; measuring TGA curves of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution; the ATG-FTIR spectra of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution were measured. The method combines attenuated total reflection Fourier transform infrared spectrum and thermogravimetric analysis, measures the component change before and after the solvent and the additive are mixed, and can predict the conversion degree of the precursor in the solution when different additive-precursor solution formulas are adopted, so that the morphology of the synthesized product can be simply, conveniently and rapidly estimated.
Description
Technical Field
The invention relates to the technical field of nano material synthesis, in particular to a method for characterizing and predicting flame synthesis characteristics of a precursor by FTIR and TGA measurement means.
Background
The nano oxide particle material has excellent physical and chemical properties, shows excellent application value in the fields of optics, catalysis and the like, and flame synthesis is widely applied in the field of nano materials as a method for generating nano composite particle materials with uniform particle size, high purity and uniform mixing of atomic scale and having natural performance advantages. The composition and the morphology of the nano particles are required to be more complicated and various by different application backgrounds and functional requirements, inorganic salts (such as metal nitrate) with low price are often selected as precursors in flame synthesis, ethanol is used as a solvent, the synthesized particles are characterized by being hollow and large in particle size, and if carboxylic acid is used as an additive, volatile metal carboxylate is formed in the solution due to the existence of the carboxylic acid, so that the precursors are converted into particles through a vapor-particle phase path of evaporation-nucleation-collision-coalescence. This conclusion shows that in the case of inexpensive metal nitrates as precursors, the choice of suitable solvents can be considered to achieve the preparation of homogeneous nano-oxide particles without the need to purchase expensive organometallic precursors. However, the specific action mechanism of different additives and the improvement degree of the morphology of the product are still unknown.
Therefore, how to simply and quickly characterize and predict the morphology of precursor flame synthesized nanoparticles has become an important research problem, and it is necessary to establish a set of simple and easy-to-implement testing methods for precursor-solvent-additive systems that can measure the properties of precursor solutions at room temperature and high temperature, respectively.
Disclosure of Invention
In view of the above problems, the present invention provides a method for characterizing and predicting flame synthesis characteristics of a precursor by FTIR and TGA measurement means, which measures the component changes before and after mixing a solvent and an additive by combining attenuated total reflection fourier transform infrared (ATR-FTIR) and thermogravimetric analysis (TGA) methods, and can predict the conversion degree of the precursor in solution when different additive-precursor solution formulations are adopted, thereby having the advantage of simple and rapid estimation of morphology of a synthesized product.
The method for characterizing and predicting the flame synthesis characteristics of the precursor provided by the invention measures the characteristics of the precursor in the flame synthesis process through a thermogravimetric analyzer and an infrared spectrometer, and comprises the following steps:
S110: respectively measuring a first TGA curve of conventional precursor powder and solid powder with a chemical formula of combination of additive anions and precursor cations, and performing first-order differential treatment on the first TGA curve to obtain a first DTG curve; wherein the first TGA profile is used to characterize a decomposition process of the precursor powder from solid to target product, and the first DTG profile is used to characterize a change process of a sample mass change rate with temperature during the decomposition process;
S120: measuring a mixed solution TGA curve of a precursor-solvent of the precursor powder, and performing first-order differential treatment on the mixed solution TGA curve to obtain a mixed solution DTG curve;
s130: measuring a first infrared absorption spectrum of the pure solvent solution and the precursor-solvent mixed solution, respectively;
S140: measuring a third TGA curve of the pure additive solution, the solvent-additive mixed solution and the precursor-solvent-additive mixed solution respectively, and performing first-order differential treatment on the third TGA curve to obtain a third DTG curve;
S150: the second infrared absorption spectra of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution were measured, respectively.
Further alternatively, in S110, the method further includes, by comparing the result of the conventional precursor powder and the solid powder having the chemical formula of combining the additive anion and the precursor cation, obtaining a modification of a path of a product formed by decomposing the precursor after the additive is combined with the precursor.
Further, in the optional scheme, in S120, further including, according to the mixed solution TGA curve and the mixed solution DTG curve, obtaining mass loss of each stage reflecting mass change of the sample by analyzing information of heat absorption and heat release in a temperature rising process when the mixed solution TGA curve is measured, comparing the mixed solution TGA curve with the first TGA curve of the precursor powder in S110, so as to obtain a change of a decomposition path after the precursor is added into the solvent.
Further, in the alternative, in S130, the method further includes comparing the first infrared absorption spectrum of the pure solvent solution with the characteristic absorption peak in the first infrared absorption spectrum of the mixed solution to obtain whether the precursor is dissolved in the solvent and then a chemical reaction occurs to generate a new substance.
Further optionally, in S140, determining whether the additive is fully bound to the precursor by comparing the third TGA profile and the third DTG profile with characteristic peaks of the first TGA profile and the first DTG profile in S110; wherein,
And if the third TGA curve of the precursor-solvent-additive mixed solution is similar to the weightless step shape of the first TGA curve of the solid powder with the chemical formula of combining the additive anions and the precursor cations, and the peak point in the maximum mass loss interval corresponding to the first DTG curve and the third DTG curve is consistent, the additive is considered to be completely combined with the precursor.
Further alternatively, the additive is fully bound to the precursor, indicating that all precursor cations are bound to the additive anions, and the product formation route will be converted from a conventional precursor decomposition route to a decomposition route of a species of the formula where the additive anions are bound to the precursor cations.
Further, optionally, in S150, it is further determined whether the additive chemically reacts with the solvent to form a new substance and the precursor chemically reacts with the additive to form a new substance by comparing peak information of the three second infrared absorption spectrums.
The invention also provides a system for characterizing and predicting flame synthesis characteristics of a precursor, characterized by measuring characteristics of the precursor during flame synthesis by a thermogravimetric analyzer and an infrared spectrometer, comprising:
The solid powder thermogravimetry unit is used for respectively measuring a first TGA curve of conventional precursor powder and solid powder with a chemical formula of combination of additive anions and precursor cations, and performing first-order differential treatment on the first TGA curve to obtain a first DTG curve; wherein the first TGA profile is used to characterize a decomposition process of the precursor powder from solid to target product, and the first DTG profile is used to characterize a change process of a sample mass change rate with temperature during the decomposition process;
the mixed solution thermogravimetry unit is used for measuring a mixed solution TGA curve of a precursor-solvent of the precursor powder and performing first-order differential processing on the mixed solution TGA curve to obtain a mixed solution DTG curve;
A first infrared measurement unit for measuring first infrared absorption spectra of the pure solvent solution and the precursor-solvent mixed solution, respectively;
The additive thermogravimetry unit is used for respectively measuring a third TGA curve of the pure additive solution, the solvent-additive mixed solution and the precursor-solvent-additive mixed solution, and performing first-order differential treatment on the third TGA curve to obtain a third DTG curve;
And a second infrared measurement unit for measuring a second infrared absorption spectrum of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution, respectively.
The method and the system for characterizing and predicting the flame synthesis characteristics of the precursor have the following beneficial effects:
(1) The method and the system for characterizing and predicting the flame synthesis characteristics of the precursor, constructed by the invention, realize the prediction of the morphology of the final flame synthesis product in the precursor preparation stage of the liquid-phase feed flame synthesis, avoid developing the liquid-phase feed flame synthesis at high temperature, collect the product and characterize the product to obtain the method with long time consumption and higher cost of the influence of the precursor formula on the morphology of the product particles;
(2) The thermogravimetric analyzer and the infrared spectrometer adopted in the invention test the characteristics of the precursor in flame synthesis, and can respectively measure the conversion degree of the additive to the precursor at high temperature and low temperature by changing the temperature of a test sample, and can measure the properties of the precursor-solvent-additive system characterized at different temperatures, thus having wide adaptability;
(3) The present invention is applicable to a variety of precursor-solvent-additive systems, and similar predictions can be made for precursor solution systems other than the yttria precursor solution systems given in the examples of the present invention, for example, titania, silica, and the like.
Drawings
FIG. 1 is a flow diagram of a method of characterizing and predicting a precursor flame synthesis characteristic in accordance with an embodiment of the invention.
FIG. 2 is a TGA and DTG plot of (a, b) yttrium nitrate and (c, d) yttrium 2-ethylhexanoate solid powder in accordance with an embodiment of the invention;
FIG. 3 is a TGA curve of (a) an ethanol solution of yttrium nitrate and (b) an infrared absorption spectrum of an ethanol solution of ethanol, yttrium nitrate, according to an embodiment of the present invention;
FIG. 4 is (a) TGA and (b) DTG curves for EHA, a mixed solution of EHA and ethanol, and a precursor solution of yttrium nitrate dissolved in EHA and ethanol according to an embodiment of the present invention;
Fig. 5 is an infrared absorption spectrum of a precursor solution obtained by dissolving EHA, a mixed solution of EHA and ethanol, yttrium nitrate in the mixed solution according to an embodiment of the present invention;
FIG. 6 is (a, b) TGA and DTG curves and (c) infrared transmission spectra of a precursor solution of isobutyric acid, a mixed solution of isobutyric acid and ethanol, yttrium nitrate dissolved in the mixed solution, according to an embodiment of the invention;
FIG. 7 is a graph of particle morphology of final flame synthesis with the addition of EHA or iBA additives to a precursor solution according to an embodiment of the present invention.
Detailed Description
In view of the foregoing problems with the prior art, the present invention is directed to a method and system for characterizing and predicting flame synthesis characteristics of a precursor by FTIR and TGA measurement, by combining attenuated total reflection fourier transform infrared (ATR-FTIR) and thermogravimetric analysis (TGA) methods, to measure the composition changes before and after mixing a solvent with an additive, and to predict the degree of conversion of the precursor in solution using different additive-precursor solution formulations, thereby establishing a set of simple and easy-to-implement test schemes for precursor-solvent-additive systems that can measure the properties of precursor solutions at room temperature and at high temperature, respectively.
The technical scheme of the invention will be described in more detail with reference to the accompanying drawings and the following examples. However, the protective scope of the invention is not limited to the examples below.
FIG. 1 is a flow diagram of a method of characterizing and predicting a precursor flame synthesis characteristic in accordance with an embodiment of the invention. As shown in fig. 1, the method for characterizing and predicting flame synthesis characteristics of a precursor provided by the invention measures characteristics of the precursor in the flame synthesis process through a thermogravimetric analyzer and an infrared spectrometer, and comprises the following steps:
S110: respectively measuring a first TGA curve of conventional precursor powder and solid powder with a chemical formula of combination of additive anions and precursor cations, and performing first-order differential treatment on the first TGA curve to obtain a first DTG curve; wherein the first TGA profile is used to characterize a decomposition process of the precursor powder from solid to target product, and the first DTG (differential thermal gravimetric analysis) profile is used to characterize a change in sample mass rate of change with temperature during the decomposition process;
the TGA (thermogravimetric analysis) method adopted in the present invention is simply a method of heating a sample all the time, observing the change of the mass of the sample with temperature, forming a TGA curve according to the change data, and then analyzing the TGA curve.
S120: measuring a mixed solution TGA curve of a precursor-solvent of the precursor powder, and performing first-order differential treatment on the mixed solution TGA curve to obtain a mixed solution DTG curve;
s130: measuring a first infrared absorption spectrum of the pure solvent solution and the precursor-solvent mixed solution, respectively;
S140: measuring a third TGA curve of the pure additive solution, the solvent-additive mixed solution and the precursor-solvent-additive mixed solution respectively, and performing first-order differential treatment on the third TGA curve to obtain a third DTG curve;
S150: the second infrared absorption spectra of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution were measured, respectively.
Specifically, in step S110, a thermogravimetric analyzer is used to measure a Thermogravimetric (TGA) curve (referred to herein as a first TGA curve) of a conventional precursor powder and a solid powder having a chemical formula in which an additive anion is combined with a precursor cation, and the TGA curve is subjected to a first-order differential processing to obtain a differential thermogravimetric analysis curve (referred to herein as a first DTG curve).
It is apparent that the first TGA profile includes two types, namely a conventional precursor powder first TGA profile and a solid powder first TGA profile having a chemical formula of an additive anion and a precursor cation combined, and two types of corresponding first DTG profiles after first-order differential treatment.
The two first TGA curves can reflect the decomposition process of the solid precursor powder into the target product, and the two first DTG curves can represent the change process of the mass change rate of the sample along with the temperature.
Wherein, by comparing the conventional precursor powder with the solid powder having the chemical formula of combining the additive anion and the precursor cation, i.e. comparing the two first TGA curves and comparing the two first DTG curves, the change of the product path formed by decomposing the precursor after combining the additive and the precursor can be reflected.
In step S120, a thermogravimetric analyzer is used to measure the TGA curve of the precursor-solvent mixture of the precursor powder as a second TGA curve, and a first-order differential process is performed on the TGA curve of the mixture to obtain a DTG curve of the precursor-solvent mixture as a second DTG curve.
Then, according to the mixed solution TGA curve and the mixed solution DTG curve, the heat absorption and heat release information in the heating process when the mixed solution TGA curve is measured can be analyzed to obtain the mass loss of each stage reflecting the mass change of the sample, and the mass loss is compared with the TGA test result (i.e. the first TGA curve) of the solid powder of the pure precursor in the step S110, so that the change of the decomposition path after the precursor is added into the solvent is obtained.
In step S130, infrared absorption spectra of the pure solvent solution and the precursor-solvent mixed solution are measured as first infrared absorption spectra, respectively, using an infrared spectrometer.
Then, by comparing the characteristic absorption peaks in the absorption spectra of the two test results, that is, by comparing the characteristic absorption peaks in the first infrared absorption spectrum of the pure solvent solution and the first infrared absorption spectrum of the mixed solution, it is possible to obtain whether or not a chemical reaction occurs to generate a new substance after the precursor is dissolved in the solvent.
In step S140, a thermogravimetric analyzer is used to measure a third TGA (thermogravimetric analysis) curve of the pure additive solution, the solvent-additive mixture solution, and the precursor-solvent-additive mixture solution, and a first-order differential process is performed on the third thermogravimetric analysis curve to obtain a third DTG curve.
Obviously, the third TGA profile includes three types, namely, a third TGA profile of a pure additive solution, a third TGA profile of a solvent-additive mixed solution, and a third TGA profile of a precursor-solvent-additive mixed solution, and the corresponding third DTG profile after first-order differential treatment is also three types.
By comparing the third TGA profile of the precursor-solvent-additive mixed solution with the characteristic peaks of the TGA profile and DTG profile (i.e., the first TGA profile and the first DTG profile) of the two solid powders in step S110, it can be determined whether the additive is fully bound to the precursor.
If the third TGA curve of the precursor-solvent-additive mixed solution is similar to the weightless step shape of the first TGA curve of the solid powder with the chemical formula of combining the additive anions and the precursor cations, and the peak points in the maximum mass loss interval corresponding to the first DTG curve and the third DTG curve are identical, the additive is considered to be completely combined with the precursor, i.e. all the precursor cations are combined with the additive anions, and the product generation route is converted from a conventional precursor decomposition route to a decomposition route of a substance with the chemical formula of combining the additive anions and the precursor cations.
In step S150, infrared absorption spectra of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution are measured as second infrared absorption spectra, respectively, using an infrared spectrometer.
Also, the second infrared absorption spectrum includes a second infrared absorption spectrum of a pure additive solution, a second infrared absorption spectrum of a solvent-additive mixed solution, and a second infrared absorption spectrum of a precursor-solvent-additive mixed solution.
By comparing the peak information of the three second infrared absorption spectra, it can be known whether the additive chemically reacts with the solvent to form a new substance in newcastle and whether the precursor chemically reacts with the additive to form a new substance.
The above results are mutually verified with the results of TGA, and by supplementing information providing other components generated in the solution, the reaction mechanism of the additive in the solution can be revealed.
Specifically, after comparing the peak information of the three second infrared absorption spectrums, the result of comparing the peak information of the three second infrared absorption spectrums and the analysis result of the third TGA curve may be further used to perform mutual verification; wherein, if the third TGA profile indicates that the additive is fully bound to the precursor and the peak of the second infrared absorption spectrum also indicates that the precursor chemically reacts with the additive to form a new species, then the two diagnostic methods achieve mutual validation; by supplementing information providing other components generated in the solution, such as hydrolysis of precursor cations, the generated H + forms a new acid (e.g., HNO 3) component with precursor anions, and determining whether the additive is bound to precursor cations in the solution, thereby determining whether the additive can increase the volatility of the precursor and is more advantageous for flame synthesis.
Methods for characterizing and predicting flame synthesis characteristics of precursors using a combination of ATR-FTIR and thermogravimetric analysis are described in more detail below in conjunction with more specific examples.
Example 1
Predicting the process of synthesizing yttrium oxide (Y2O 3) product morphology by flame of 2-ethylhexanoic acid (EHA) and isobutyric acid (iBA) as additives, wherein the specific flame synthesis parameters are as follows:
When yttrium oxide is synthesized by flame, the conventional precursor is yttrium nitrate, and the solvent is ethanol (EtOH);
The thermal gravimetric analysis test conditions are uniformly selected to be in a temperature rising range of 35-900 ℃, the temperature rising rate is preferably 10K/min, the carrier gas of the thermal gravimetric analyzer is nitrogen, the carrier gas flow rate is 100ml/min, and the sample mass is 10mg;
in all the solutions containing the precursor, the molar concentration of Y3+ is 0.3mol/L;
in all solutions with the additive and the solvent, the ratio of the liquid additive to the solvent is 1:1;
after the parameters are determined, the flow for characterization and prediction of specific flame synthesis characteristics is as follows:
first, TGA curves of solid powders of yttrium nitrate and yttrium 2-ethylhexanoate were measured and subjected to first-order differentiation to obtain DTG curves.
FIG. 2 is a TGA and DTG plot of solid powders of yttrium (a, b) nitrate and yttrium (c, d) 2-ethylhexanoate in accordance with an embodiment of the invention. As shown in fig. 2 (a) and (b), the thermogravimetric analysis of the solid yttrium nitrate powder was stepped down and the DTG curve reflected a maximum sample mass loss rate of about 375 ℃. As shown in fig. 2 (c) and (d), the TGA profile of the yttrium 2-ethylhexanoate solid sample, which is distinct from the decomposition profile of yttrium nitrate, contains only one major weight loss region, and the DTG profile reflects a maximum sample mass loss rate of about 469.2 ℃.
Next, the TGA curve of the ethanol solution of yttrium nitrate is measured and subjected to first-order differentiation to obtain a DTG curve. FIG. 3 is a TGA curve of an ethanol solution of yttrium nitrate and an infrared absorption spectrum of an ethanol, yttrium nitrate ethanol solution according to an embodiment of the present invention.
Wherein (a) in fig. 3 is a schematic diagram of TGA curve of an ethanol solution of yttrium nitrate, and (b) in fig. 3 is a schematic diagram of infrared absorption spectrum of an ethanol solution of yttrium nitrate. As shown in fig. 3 (a), there is a significant difference between the TGA profile of the ethanol solution of yttrium nitrate and the TGA profile of the solid yttrium nitrate powder. In the DTG curve, the maximum weight loss rate corresponding temperatures in the two weight loss intervals are 323.7 ℃ and 394.7 ℃ respectively.
Then, the infrared absorption spectra of the pure ethanol solution and the yttrium nitrate-added ethanol solution were measured, and as shown in fig. 3 (b), the infrared absorption peak of the ethanol solution after adding yttrium nitrate was found in the infrared absorption spectra of the pure ethanol solution and the solid yttrium nitrate powder, indicating that no chemical reaction between ethanol and yttrium nitrate occurred to generate new substances.
Further, TGA curves of 2-ethylhexanoic acid, a mixed solution of 2-ethylhexanoic acid and ethanol in equal proportion, and a precursor solution of yttrium nitrate dissolved in 2-ethylhexanoic acid and ethanol were measured, and subjected to first-order differentiation to obtain DTG curves, and the results are shown in fig. 4.
Fig. 4 shows (a) TGA and (b) DTG curves of EHA, EHA-ethanol mixed solution, and yttrium nitrate in EHA-ethanol precursor solution according to an embodiment of the present invention. As shown in fig. 4, there are no more multiple weight loss steps of the ethanol and yttrium nitrate solutions of fig. 3 (a) for the TGA profile of the precursor solution of yttrium nitrate dissolved in 2-ethylhexanoate and ethanol, and the peak point in the maximum mass loss zone reflected by the DTG profile is 464.8 ℃ which coincides with the temperature 469.2 ℃ at which the maximum mass loss rate and the weight loss zone of the yttrium 2-ethylhexanoate solid sample are located. This result is sufficient to demonstrate that the addition of 2-ethylhexanoic acid converts all of the yttrium nitrate in the solution to yttrium 2-ethylhexanoate.
Finally, infrared absorption spectra of 2-ethylhexanoic acid, a mixed solution of 2-ethylhexanoic acid and ethanol in equal proportion, and a precursor solution of yttrium nitrate dissolved in 2-ethylhexanoic acid and ethanol were measured, and the results are shown in fig. 5.
Fig. 5 shows an infrared absorption spectrum of a precursor solution obtained by dissolving EHA, a mixed solution of EHA and ethanol, and yttrium nitrate in the mixed solution according to an embodiment of the present invention. As shown in FIG. 5, the infrared absorption spectrum of the mixed solution of 2-ethylhexanoic acid and ethanol contained characteristic absorption peaks from each of 2-ethylhexanoic acid and ethanol, indicating that the additive did not react with the solvent. For a precursor solution of yttrium nitrate dissolved in ethanol and 2-ethylhexanoic acid, the position of most of the absorption peaks remains unchanged compared to a mixed solution without yttrium nitrate. The peak appearing at 1520cm-1 corresponds to the R-COO-group of yttrium 2-ethylhexanoate, indicating the conversion of yttrium nitrate to yttrium 2-ethylhexanoate, which results are mutually verified with the results of TGA, and the reaction mechanism of 2-ethylhexanoic acid in solution is revealed by supplementing information providing other components generated in solution.
Example two
For the isobutyric acid additive, the same procedure was followed for the 2-ethylhexanoic acid additive. The main results are shown in fig. 6. FIG. 6 shows (a, b) TGA and DTG curves and (c) infrared transmission spectra of a precursor solution of isobutyric acid, a mixed solution of isobutyric acid and ethanol, and yttrium nitrate dissolved in the mixed solution according to an embodiment of the present invention. As shown in fig. 6 (a) and (b), the decomposition temperature of yttrium isobutyrate ranges from 260 ℃ to 360 ℃, and for precursor solutions in which yttrium nitrate is dissolved in ethanol and isobutyric acid, the weight loss range partially coincides with the weight loss range of yttrium isobutyrate, indicating the presence of a portion of yttrium nitrate converted to yttrium isobutyrate. As shown in the infrared spectrum of FIG. 6 (c), the position of most of the absorption peaks remained unchanged for the precursor solution of yttrium nitrate dissolved in isobutyric acid and ethanol, compared with the mixed solution of isobutyric acid and ethanol, and the peak appearing at 1520cm-1 corresponds to the R-COO-group of yttrium isobutyrate, which is consistent with the thermogravimetric measurement result. ;
by combining attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) with thermogravimetric analysis (TGA), it is found that when 2-ethylhexanoic acid is used as an additive, yttrium nitrate is completely converted into yttrium 2-ethylhexanoate, and when isobutyric acid is used as an additive, yttrium nitrate is partially converted into yttrium isobutyrate, according to the flame synthesis principle, when 2-ethylhexanoic acid is used as an additive, it can be predicted that the precursor forms nano particles through a typical gas phase-particle phase transition path, and when isobutyric acid is used as an additive, solvent evaporation and combustion firstly occur, the precursor precipitates on the surface of liquid drops to form a shell wrapping residual solvent, and finally heterogeneous particles such as hollow, shell and the like are formed through a relatively complex liquid phase-particle phase path;
FIG. 7 is a graph of particle morphology of final flame synthesis with EHA or iBA additives added to a precursor solution according to an embodiment of the present invention. As shown in fig. 7, 2-ethylhexanoic acid and isobutyric acid are respectively used as additives to prepare corresponding precursor solutions, a synthesis experiment is carried out in a high-temperature 1500K flame field, and irregular large particles and small particles with uniform particle size in the obtained product coexist in a TEM image of the product when isobutyric acid is added. The particle size was small and uniform when 2-ethylhexanoic acid was added, and the presence of large particles was not observed. This synthesis result is substantially consistent with the degree of conversion of nitrate to carboxylate in the precursor solution.
In response to the above method of characterizing and predicting a flame synthesis characteristic of a precursor, the present invention also provides a system for characterizing and predicting a flame synthesis characteristic of a precursor for measuring a characteristic of a precursor during flame synthesis by a thermogravimetric analyzer and an infrared spectrometer, the system comprising:
The solid powder thermogravimetry unit is used for respectively measuring a first TGA curve of conventional precursor powder and solid powder with a chemical formula of combination of additive anions and precursor cations, and performing first-order differential treatment on the first TGA curve to obtain a first DTG curve; wherein the first TGA profile is used to characterize a decomposition process of the precursor powder from solid to target product, and the first DTG profile is used to characterize a change process of a sample mass change rate with temperature during the decomposition process;
the mixed solution thermogravimetry unit is used for measuring a mixed solution TGA curve of a precursor-solvent of the precursor powder and performing first-order differential processing on the mixed solution TGA curve to obtain a mixed solution DTG curve;
A first infrared measurement unit for measuring first infrared absorption spectra of the pure solvent solution and the precursor-solvent mixed solution, respectively;
The additive thermogravimetry unit is used for respectively measuring a third TGA curve of the pure additive solution, the solvent-additive mixed solution and the precursor-solvent-additive mixed solution, and performing first-order differential treatment on the third TGA curve to obtain a third DTG curve;
And a second infrared measurement unit for measuring a second infrared absorption spectrum of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution, respectively.
In addition, the system for characterizing and predicting the flame synthesis characteristics of the precursor may further comprise a data analysis unit for analyzing the measurements of the solid powder thermogravimetry unit, the mixed solution thermogravimetry unit, the first infrared measurement unit, the additive thermogravimetry unit, and the additive thermogravimetry unit.
Specifically, as an example, the data analysis unit analyzes the measurement result of the solid powder thermogravimetry unit, and obtains a change in the path of the product formed by decomposing the precursor after the combination of the additive with the precursor by comparing the result of the conventional precursor powder with the solid powder having the chemical formula of the combination of the additive anion with the precursor cation.
The data analysis unit analyzes the measurement result of the mixed solution thermogravimetric measurement unit, obtains mass loss of each stage reflecting the mass change of the sample by analyzing the heat absorption and heat release information in the temperature rising process when the mixed solution TGA curve is measured according to the mixed solution TGA curve and the mixed solution DTG curve, and compares the mixed solution TGA curve with the first TGA curve of the precursor powder in S110 to obtain the change of the decomposition path after the precursor is added into the solvent.
The data analysis unit analyzes the measurement result of the first infrared measurement unit, and compares the first infrared absorption spectrum of the pure solvent solution with the characteristic absorption peak in the first infrared absorption spectrum of the mixed solution to obtain whether a chemical reaction occurs to generate a new substance after the precursor is dissolved in the solvent.
A data analysis unit analyzes the measurement result of the additive thermogravimetric measurement unit and determines whether the additive is completely combined with the precursor by comparing the third TGA curve and the third DTG curve with the characteristic peak values of the first TGA curve and the first DTG curve in S110; wherein the additive is considered to be fully bonded to the precursor if the third TGA profile of the precursor-solvent-additive mixed solution is similar to the weightless step shape of the first TGA profile of the solid powder having the formula of additive anions bonded to precursor cations, and the peak point in the maximum mass loss interval corresponding to the first DTG profile coincides with the peak point in the maximum mass loss interval corresponding to the third DTG profile.
The data analysis unit analyzes the measurement results of the second infrared measurement unit, and determines whether the additive chemically reacts with the solvent to form a new substance and whether the precursor chemically reacts with the additive to form a new substance by comparing peak information of the three second infrared absorption spectra.
In addition, the data analysis unit performs mutual verification by comparing the results of the peak information of the three second infrared absorption spectra with the analysis results of the third TGA profile after comparing the peak information of the three second infrared absorption spectra. Wherein, if the third TGA profile indicates that the additive is fully bound to the precursor and the peak of the second infrared absorption spectrum also indicates that the precursor chemically reacts with the additive to form a new species, then the two diagnostic methods achieve mutual validation; by supplementing information providing other components generated in the solution, such as hydrolysis of precursor cations, the generated H + forms a new acid (e.g., HNO 3) component with precursor anions, and determining whether the additive is bound to precursor cations in the solution, thereby determining whether the additive can increase the volatility of the precursor and is more advantageous for flame synthesis.
Specific implementations of the system for characterizing and predicting a precursor flame synthesis property described above may refer to the foregoing description of the method for characterizing and predicting a precursor flame synthesis property, which is not specifically recited herein.
Among the various experimental articles (including but not limited to chemical reagents, instruments, etc.) involved in the implementation process of the invention, the experimental articles are not specifically described, but are all conventional experimental articles, and can be conveniently obtained in various modes (such as purchase, self-preparation, etc.).
While the invention has been described in detail in the foregoing general description, specific embodiments, and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. Accordingly, such modifications and improvements can be made without departing from the spirit of the invention, and are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method of characterizing and predicting flame synthesis characteristics of a precursor, wherein the characteristics of the precursor during flame synthesis are measured by a thermogravimetric analyzer and an infrared spectrometer, comprising the steps of:
S110: respectively measuring a first TGA curve of conventional precursor powder and solid powder with a chemical formula of combination of additive anions and precursor cations, and performing first-order differential treatment on the first TGA curve to obtain a first DTG curve; wherein the first TGA profile is used to characterize a decomposition process of the precursor powder from solid to target product, and the first DTG profile is used to characterize a change process of a sample mass change rate with temperature during the decomposition process;
S120: measuring a mixed solution TGA curve of a precursor-solvent of the precursor powder, and performing first-order differential treatment on the mixed solution TGA curve to obtain a mixed solution DTG curve;
s130: measuring a first infrared absorption spectrum of the pure solvent solution and the precursor-solvent mixed solution, respectively;
S140: measuring a third TGA curve of the pure additive solution, the solvent-additive mixed solution and the precursor-solvent-additive mixed solution respectively, and performing first-order differential treatment on the third TGA curve to obtain a third DTG curve;
S150: the second infrared absorption spectra of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution were measured, respectively.
2. The method of characterizing and predicting the flame synthesis characteristics of a precursor according to claim 1, further comprising, in S110, obtaining a change in the precursor decomposition forming product path after the additive is combined with the precursor by comparing the conventional precursor powder with the solid powder having the chemical formula of additive anions combined with precursor cations.
3. The method of characterizing and predicting flame synthesis characteristics of a precursor according to claim 1, further comprising, in S120, obtaining mass loss at each stage reflecting mass change of a sample by analyzing information of heat absorption and heat release during temperature rise when measuring the mixed solution TGA curve based on the mixed solution TGA curve and the mixed solution DTG curve, comparing the mixed solution TGA curve with the first TGA curve of the precursor powder in S110 to obtain change of decomposition path after the precursor is added to the solvent.
4. The method of characterizing and predicting flame synthesis characteristics of a precursor according to claim 1, further comprising, in S130, comparing the characteristic absorption peaks in the first infrared absorption spectrum of the pure solvent solution and the first infrared absorption spectrum of the mixed solution to obtain whether a chemical reaction occurs to generate a new substance after the precursor is dissolved in the solvent.
5. The method of characterizing and predicting the flame synthesis characteristics of a precursor according to claim 1, further comprising, in S140, determining whether the additive is fully bound to the precursor by comparing the third TGA profile and the third DTG profile to the characteristic peaks of the first TGA profile and the first DTG profile in S110; wherein,
And if the third TGA curve of the precursor-solvent-additive mixed solution is similar to the weightless step shape of the first TGA curve of the solid powder with the chemical formula of combining the additive anions and the precursor cations, and the peak point in the maximum mass loss interval corresponding to the first DTG curve and the third DTG curve is consistent, the additive is considered to be completely combined with the precursor.
6. The method of characterizing and predicting the flame synthesis characteristics of a precursor of claim 5, wherein the additive is fully bound to the precursor, indicating that all precursor cations are bound to the additive anions, and wherein the product generation route is to be converted from a conventional precursor decomposition route to a decomposition route of a species having the chemical formula of the combination of additive anions and precursor cations.
7. The method of characterizing and predicting flame synthesis characteristics of a precursor according to claim 1, further comprising, in S150, determining whether the additive chemically reacts with the solvent to form a new species and whether the precursor chemically reacts with the additive to form a new species by comparing peak information of the three second infrared absorption spectra.
8. The method of characterizing and predicting a flame synthesis characteristic of a precursor as recited in claim 7, further comprising, after comparing peak information of three of said second infrared absorption spectra: mutual verification is performed by comparing the results of the peak information of the three second infrared absorption spectra with the analysis results of the third TGA profile.
9. A system for characterizing and predicting flame synthesis characteristics of a precursor, wherein characteristics of the precursor during flame synthesis are measured by a thermogravimetric analyzer and an infrared spectrometer, comprising:
The solid powder thermogravimetry unit is used for respectively measuring a first TGA curve of conventional precursor powder and solid powder with a chemical formula of combination of additive anions and precursor cations, and performing first-order differential treatment on the first TGA curve to obtain a first DTG curve; wherein the first TGA profile is used to characterize a decomposition process of the precursor powder from solid to target product, and the first DTG profile is used to characterize a change process of a sample mass change rate with temperature during the decomposition process;
the mixed solution thermogravimetry unit is used for measuring a mixed solution TGA curve of a precursor-solvent of the precursor powder and performing first-order differential processing on the mixed solution TGA curve to obtain a mixed solution DTG curve;
A first infrared measurement unit for measuring first infrared absorption spectra of the pure solvent solution and the precursor-solvent mixed solution, respectively;
The additive thermogravimetry unit is used for respectively measuring a third TGA curve of the pure additive solution, the solvent-additive mixed solution and the precursor-solvent-additive mixed solution, and performing first-order differential treatment on the third TGA curve to obtain a third DTG curve;
And a second infrared measurement unit for measuring a second infrared absorption spectrum of the pure additive solution, the solvent-additive mixed solution, and the precursor-solvent-additive mixed solution, respectively.
10. The system for characterizing and predicting a flame synthesis characteristic of a precursor of claim 9, further comprising:
And the data analysis unit is used for analyzing the measurement results of the solid powder thermogravimetric measurement unit, the mixed solution thermogravimetric measurement unit, the first infrared measurement unit, the additive thermogravimetric measurement unit and the additive thermogravimetric measurement unit.
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