CN111238992A - Quasi-magnetocaloric reanalysis method for researching thermal stability of magnetic material in composite material - Google Patents
Quasi-magnetocaloric reanalysis method for researching thermal stability of magnetic material in composite material Download PDFInfo
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- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
A quasi-magnetocaloric reanalysis method for researching the thermal stability of a magnetic material in a composite material comprises the following steps: respectively carrying out a TGA test of reference, a TGA test of a sample and an MTGA test of a magnet added at the periphery of the sample under the same test condition, and collecting and storing data; making the data into curves, normalizing the ordinate, and respectively naming the obtained curves as C0, C1 and C2; subtracting the difference between C2 and C1 to obtain C3; c0 and C3 are regressed to obtain an AMTGA curve C4; deriving the C4 to obtain C5, wherein the corresponding temperature of the extreme value of C5 is the temperature value with the maximum magnetic change rate of the magnetic material; and C4, taking a point on the base line before the mass change, which is flat, and a temperature point corresponding to the point with the maximum change rate, and respectively obtaining tangent lines through the two points to obtain an intersection point which is the extrapolation initial change temperature of the magnetic material. The method can accurately judge the thermal decomposition or oxidation temperature of the magnetic material in the composite material, and has simple operation and visual result.
Description
Technical Field
The invention belongs to the field of analysis and test methods, and particularly relates to a similar magnetothermal reanalysis method for researching the thermal stability of a composite material with changed magnetism in a heat treatment process.
Background
The magnetic composite material is an important functional material and is used in the fields of catalysis, biomedicine, electromagnetic interference shielding, microwave absorption and the likeDomains have a wide range of applications. Lu is a magnetic composite material for obtaining water treatment, and a coordination polymer is used as a precursor to synthesize a nickel-based composite material (Ni @ NC) taking nitrogen-doped mesoporous carbon as a matrix. In Ni @ NC, Ni nanoparticles, approximately 3-5nm in size, are uniformly dispersed in a nitrogen-doped mesoporous carbon matrix. In the presence of sodium borohydride, the Ni @ NC has remarkable catalytic activity for reducing and converting 4-resorcinol into 4-aminophenol, the conversion efficiency in 160s almost reaches 100% when the content is as low as 5mg, and the effect is still kept above 99% after 8 times of continuous reduction. The Carbon Nano Tube (CNT) is modified by ferromagnetic material and has important application in shielding electromagnetic interference, Mei deposits magnetic Fe nano wires with different concentrations on the CNT by chemical deposition method, and the highest SETThe average value can reach 70.01 dB. After the outer layer is sealed by SiC, the average absorption rate is reduced a little, but within the range of 25-600 ℃, the SE is only 1.20TThe decrease in the value proves that SiC is effective in preventing oxidation of Fe. Recently, Metal Organic Framework (MOF), a special mixed porous material constructed by metal ions and organic ligands, has been widely used in biomedicine due to its huge surface area, high porosity and adjustable structure and composition, diversity of functions, biocompatibility and biodegradability. Chen is in Fe3O4ZIF-90 grows on the MOF framework coated with polydopamine to prepare Fe3O4The @ PDA @ ZIF-90 nano ferromagnetic compound and adriamycin serving as a medicine carrier are used for researching the behaviors of carrying the medicine and triggering the medicine release by pH, wherein Fe3O4As a hyperthermia source, PDA was used as an inducer to grow ZIF-90, and ZIF-90 was used to carry drugs. The compound can be used for treating tumors, and has the efficacy of magnetothermal treatment and chemotherapy at the same time.
In the process of synthesizing or applying magnetic composite materials, the research on the performance, especially the thermal stability performance, of the composite materials is very important. By analyzing the thermal stability of the material, the proper temperature in the heat treatment process can be obtained, the preparation efficiency of the composite material is improved, the application temperature range of the composite material is determined, and the like. Thermal analysis is a more classical method for studying the thermal stability of materials, and thermogravimetric analysis (TGA) is a technique for measuring the relationship between the weight of a substance and temperature under the control of a programmed temperature; differential thermal analysis (DTA or DSC) is a technique that measures the heat of a substance as a function of temperature under programmed temperature control. However, for some composites, it is common to include an inorganic component and an organic component, and during the heat treatment, the organic component undergoes polycondensation or decomposition, and the inorganic component may also undergo decomposition or oxidation. When the decomposition or oxidation change of the inorganic material in the composite is judged, the weight change of the inorganic material is overlapped with the decomposition of the organic material, and the TGA method cannot be used for accurately judging the weight change; the change of the heat absorption and release is also influenced by the thermal effect of the decomposition of the organic matter, and cannot be distinguished by DTA or DSC method. The magnetothermal gravimetric analysis (MTGA) is a thermal analysis method for detecting the relationship between the magnetism and the temperature of a sample. The difference between the MTGA experiment and the ordinary TGA experiment is that magnets are arranged around an instrument furnace, when original magnetic substances in the composite material are changed into non-magnetic substances or new magnetic substances are generated, the balance collects the total weight change caused by the decomposition of the composite material and the action of magnetic force due to the influence of magnetic field attraction, and similarly, the change of weight reading caused by the magnetic change is still influenced by the decomposition of other components.
Therefore, the present invention needs to provide a new analysis method to better analyze the exact temperature of the formation or disappearance of the magnetic material in the composite material and understand the thermal stability of the magnetic composite material.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides a similar-magnetism thermal reanalysis method for researching the thermal stability of a composite material, the method can accurately judge the thermal decomposition or oxidation temperature of the magnetic material in the composite material, is simple to operate, has intuitive result, and is an effective method for researching the thermal stability of the composite material.
The technical scheme is as follows: a quasi-magnetocaloric reanalysis method for researching the thermal stability of a magnetic material in a composite material comprises the following steps:
(1) collecting data: respectively carrying out a TGA test for reference, a TGA test for a sample and an MTGA test for adding a magnet at the periphery of the sample under the same test condition, and collecting and storing corresponding weight and temperature data;
(2) normalizing: preparing weight-temperature curves according to data obtained in the TGA experiment, the TGA experiment of the sample and the MTGA experiment of the sample with magnets on the periphery in the reference in the step (1), and normalizing the weight of the ordinate to be weight 100%, wherein the obtained curves are respectively named as C0, C1 and C2;
(3) difference subtraction: carrying out difference subtraction on the curves C2 and C1 to obtain a curve C3;
(4) and (3) regression: c0 and C3 curves are regressed, the abscissa of the C3 curve is unchanged, and the ordinate is added with the ordinate of the C0 curve to obtain an AMTGA data curve C4;
(5) derivation: obtaining a first derivative curve C5 of the curve C4 by derivation of the curve C4, wherein the temperature corresponding to the extreme value of the curve C5 is the temperature value with the maximum magnetic change rate of the magnetic material;
(6) extrapolated onset temperature: and taking a point on the flat base line before the mass change on the curve C4 and a temperature point corresponding to the point with the maximum change rate on the curve C4, and respectively obtaining tangents through the two points to obtain an intersection point which is the extrapolation initial change temperature of the magnetic material.
Preferably, in the step (1), the reference and the sample are both taken in an amount of 5-10 mg.
Preferably, the same experimental conditions in step (1) are as follows: inert gas is used as protective atmosphere, the gas flow is 50-100 mL/min, and the programmed heating rate is set to be 5 or 10 ℃/min.
Preferably, the reference material in the step (1) is α -Al2O3。
Preferably, the steps (2) - (6) are all completed by TGA software.
Has the advantages that: the method cancels the change of the self weight of the composite material along with the temperature by subtracting the MTGA and TGA data, eliminates the influence of the weight change caused by the polycondensation or the decomposition of the organic component in the composite material on the weight change caused by the oxidation or the decomposition of the inorganic component, and singly highlights the magnetic change characteristic of the material along with the temperature, thereby more accurately judging the thermal decomposition or the oxidation temperature of the magnetic material in the composite material.
The invention can accurately analyze the proper temperature in the heat treatment process of the magnetic composite material, improve the preparation efficiency of the composite material and simultaneously determine the application temperature range of the magnetic composite material.
All experimental operations of the method can be completed only by a conventional thermogravimetric analysis instrument, the data processing process can be completed by using a corresponding menu on instrument operation software, and can also be completed by other data processing software, the operation is simple, the result is visual, and the method is an effective method for researching the thermal stability of the composite material.
Drawings
FIG. 1 shows Ni (OH)2The preparative flow sheet of @ RF;
FIG. 2 is a graph of a thermal analysis experiment in example 1;
fig. 3 is an XRD pattern before and after heat treatment of the sample.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the specific contents of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The Ni magnetic nano composite material can be prepared by Ni (OH)2@ RF. Ni (OH)2The process of @ RF preparation is shown in the attached figure 1 of the specification, and the specific steps are as follows: 2.91g of Ni (NO)3)2·6H2O、4g Glyine、4g NaSO4Dissolving in 50ml deionized water, magnetically stirring for 30min, dropwise adding 20ml of 5M NaOH solution, magnetically stirring for 1h, pouring into a reaction kettle, and placing in an oven at 100 ℃ for 3 h. Then washing with anhydrous alcohol for 3 timesWashing with ionized water for 1 time to obtain Ni (OH)2. Reacting Ni (OH)2Dissolving in 120ml deionized water, adding 5ml CTAB with concentration of 0.01M and 0.5ml ammonia water with concentration of 28% v/v, magnetically stirring for 1h, adding 25mg resorcinol (dissolved in 2ml deionized water) and 35 μ l formaldehyde, heating at 50 deg.C and magnetically stirring for 12h, centrifuging, washing and oven drying to obtain β -Ni (OH)2@ RF powder.
During the heat treatment, the RF resin will condense to carbon material C on the one hand and Ni (OH) on the other hand2Decomposed into NiO and H by heating2The O, C material can reduce part or all NiO into Ni, and finally prepare the composite material containing Ni @ C. To optimize the heat treatment process, a suitable temperature for the carbonization reduction is determined, which may be for Ni (OH)2@ RF thermal stability studies were performed.
The thermal analysis experiments were carried out on a Pyris 1 TGA (Perkin-Elmer, USA) under conditions such that the sample was 5mg, the temperature was raised from 30 ℃ to 400 ℃ at a rate of 10 ℃/min, the heating was carried out under a nitrogen atmosphere (purity 99.99%) and the flow rate was 50mL/min, the experimental contents included a reference α -Al2O3TGA of (1), sample Ni (OH)2The TGA @ RF and MTGA experiments with magnets in the periphery. And operating a temperature control program according to the experimental conditions, carrying out thermal analysis on the sample, acquiring data in real time, and respectively drawing corresponding weight-temperature relation curves according to the acquired weight and temperature data.
The experimental results are shown in figure 2, wherein C0, C1 and C2 are references α -Al, respectively2O3TGA of (1), sample Ni (OH)2The TGA and MTGA curves of @ RF were normalized by Weight 100% in the onboard menu of Pyris 1 TGA software, and C2 and C1 were subtracted from each other by the Substraction function in Math menu to obtain the C3 curve. As can be seen from the C3 curve, before 250 ℃, the two experiments almost coincide, and the value after the difference is reduced is about 0; between 250 ℃ and 300 ℃, there are some small deviations due to the randomness of the decomposition process of the two experiments; between 300 ℃ and 350 ℃, the magnetic Ni is generated, the two are obviously distinguished, and the C3 curve after the difference is reduced has an upward step. In order to be able to accurately perform the calculation of the thermal analysis extrapolated onset change temperature,the addition of C3 and C0 by using the Add function under Math menu returns the data to near 100%, and the C4 curve, i.e. AMTGA curve in the graph is obtained. And (4) utilizing a Derivation function under a Math menu to conduct Derivation on the C4 curve to obtain a C5 curve in the graph. The extreme value of the curve C5 corresponds to a temperature value at which the magnetic change rate is maximum at 332 ℃. And (3) calculating extrapolated Onset temperature, selecting a curve C4, selecting 'Onset' under a calibration menu, taking a point at the flat part on a baseline before mass change and a point at the maximum change rate of C4 on C4, and respectively calculating tangent lines of the two points to obtain intersection point Onset temperature, wherein 329 ℃ in the graph is the extrapolated initial change temperature of the NiO reduced into Ni detected by a thermal analysis method. Therefore, it passes through Ni (OH)2A suitable temperature for the carbonisation reduction of @ RF for the preparation of Ni magnetic nanocomposites is 329 ℃.
To confirm that the AMTGA method detects the generation of Ni as the magnetic material, XRD experiments were performed on samples before and after heat treatment, and the results are shown in figure 3, and the original sample Ni (OH)2@ RF with Ni (OH)2The sample after the heat treatment had characteristic peaks of Ni and NiO.
In the embodiment, the magnetic change characteristics of the magnetic composite material are highlighted by a similar-magnetocaloric re-analysis method, the preparation and application of the magnetic composite material are guided, the operation is simple, and the result is clear.
The invention overcomes the interference caused by polycondensation or decomposition of organic components which are difficult to eliminate through thermogravimetric-differential thermal analysis in the prior art, effectively reflects the magnetic change characteristic of the magnetic composite material, and provides reliable basis for the preparation and application of the magnetic composite material.
The above examples are only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (5)
1. A quasi-magnetocaloric reanalysis method for researching the thermal stability of a magnetic material in a composite material is characterized by comprising the following steps:
(1) collecting data: respectively carrying out a TGA test for reference, a TGA test for a sample and an MTGA test for adding a magnet at the periphery of the sample under the same test condition, and collecting and storing corresponding weight and temperature data;
(2) normalizing: preparing weight-temperature curves according to data obtained in the TGA experiment, the TGA experiment of the sample and the MTGA experiment of the sample with magnets on the periphery in the reference in the step (1), and normalizing the weight of the ordinate to be weight 100%, wherein the obtained curves are respectively named as C0, C1 and C2;
(3) difference subtraction: carrying out difference subtraction on the curves C2 and C1 to obtain a curve C3;
(4) and (3) regression: c0 and C3 curves are regressed, the abscissa of the C3 curve is unchanged, and the ordinate is added with the ordinate of the C0 curve to obtain an AMTGA data curve C4;
(5) derivation: obtaining a first derivative curve C5 of the curve C4 by derivation of the curve C4, wherein the temperature corresponding to the extreme value of the curve C5 is the temperature value with the maximum magnetic change rate of the magnetic material;
(6) extrapolated onset temperature: and taking a point on the flat base line before the mass change on the curve C4 and a temperature point corresponding to the point with the maximum change rate on the curve C4, and respectively obtaining tangents through the two points to obtain an intersection point which is the extrapolation initial change temperature of the magnetic material.
2. The method for researching thermal stability of the magnetic material in the composite material according to claim 1, wherein the reference and the sample are used in an amount of 5-10 mg in step (1).
3. The magnetocaloric reanalysis method for studying the thermal stability of magnetic materials in composite materials according to claim 1, wherein the same experimental conditions in step (1) are as follows: inert gas is used as protective atmosphere, the gas flow is 50-100 mL/min, and the programmed temperature rise is set to be 5 or 10 ℃/min.
4. According toThe method for researching thermal stability of magnetic material in composite material according to claim 1, wherein the reference material in step (1) is α -Al2O3。
5. The magnetocaloric thermogravimetry method for studying the thermal stability of a magnetic material in a composite material according to claim 1, wherein the steps (2) - (6) are all completed by TGA software.
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| CN112710577A (en) * | 2020-12-02 | 2021-04-27 | 国家能源集团宁夏煤业有限责任公司 | Rapid detection method for thermal stability of polyformaldehyde |
| CN113324868A (en) * | 2021-05-18 | 2021-08-31 | 北京科技大学 | Method for evaluating oxidizing property of magnetite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111849463A (en) * | 2020-07-21 | 2020-10-30 | 湘潭大学 | Preparation and application of near-infrared fluorescent probe based on MOF material |
| CN112710577A (en) * | 2020-12-02 | 2021-04-27 | 国家能源集团宁夏煤业有限责任公司 | Rapid detection method for thermal stability of polyformaldehyde |
| CN113324868A (en) * | 2021-05-18 | 2021-08-31 | 北京科技大学 | Method for evaluating oxidizing property of magnetite |
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