CN116297617B - Method for detecting hydrogen content in titanium hydrogen compound powder - Google Patents
Method for detecting hydrogen content in titanium hydrogen compound powder Download PDFInfo
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- CN116297617B CN116297617B CN202310176459.6A CN202310176459A CN116297617B CN 116297617 B CN116297617 B CN 116297617B CN 202310176459 A CN202310176459 A CN 202310176459A CN 116297617 B CN116297617 B CN 116297617B
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 124
- 239000001257 hydrogen Substances 0.000 title claims abstract description 124
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 106
- -1 titanium hydrogen compound Chemical class 0.000 title claims abstract description 55
- 239000000843 powder Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 20
- 239000010936 titanium Substances 0.000 title claims abstract description 19
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 38
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 38
- 238000001228 spectrum Methods 0.000 claims abstract description 26
- 238000006073 displacement reaction Methods 0.000 claims abstract description 24
- 238000010586 diagram Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 7
- 230000003993 interaction Effects 0.000 claims description 6
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 claims description 4
- 238000000425 proton nuclear magnetic resonance spectrum Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 10
- 230000008859 change Effects 0.000 abstract description 3
- 239000002772 conduction electron Substances 0.000 abstract description 2
- 230000005364 hyperfine coupling Effects 0.000 abstract 1
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 239000011232 storage material Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000009461 vacuum packaging Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241001212279 Neisseriales Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 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
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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- High Energy & Nuclear Physics (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to the field of hydrogen content detection, and particularly discloses a method for detecting the hydrogen content in titanium hydride powder, which comprises the following steps: s1, measuring nuclear magnetic resonance hydrogen spectrums of a plurality of titanium hydrogen compound sample powders with different hydrogen contents, and analyzing the nuclear magnetic resonance hydrogen spectrums to obtain Nett displacement; s2, drawing a scatter diagram corresponding to the Nett displacement and the hydrogen content, and fitting a standard curve; s3, measuring nuclear magnetic resonance hydrogen spectrum of the titanium hydride powder to be measured, and analyzing to obtain corresponding Netty displacement; and combining the standard curve to obtain the hydrogen content of the titanium hydride powder. For the titanium hydrogen compound, the Nett displacement reflects the hyperfine coupling field of the conduction electrons near the hydrogen atomic nucleus and is extremely sensitive to the change of the hydrogen content, and the characteristic is skillfully applied to quantitatively determine the hydrogen content of the titanium hydrogen compound, so that the hydrogen content detection precision can be greatly improved, and the method has the characteristics of simplicity in operation, accurate quantitative analysis, good reproducibility, nondestructive detection and the like.
Description
Technical Field
The invention belongs to the field of hydrogen content detection, and in particular relates to a method for detecting the hydrogen content in titanium hydride powder.
Background
The hydrogen energy is used as a clean energy source, pollution is not generated in the combustion process, the source is wide, the hydrogen energy belongs to renewable energy sources, and the hydrogen energy is a new focus of research in various countries. In the development and utilization of hydrogen energy, a hydrogen energy storage technology is the basis for the practical and large-scale development of hydrogen energy. The solid hydrogen storage technology has better safety and high hydrogen storage density. Titanium is the metal found to date to have the highest hydrogen absorption density, about 570ml/g, with a maximum hydrogen absorption of about 4wt.%, and a large hydrogen absorption. The titanium hydrogen compound has stable property in air, does not spontaneously ignite at room temperature, has rich titanium hydrogen compound resources and is a potential solid hydrogen storage material. Because of the recycling property of the hydrogen storage material, the accurate measurement of the hydrogen content can more effectively guide the use of the titanium hydrogen compound. However, no accurate and simple method for quantitatively characterizing the hydrogen content in materials exists at present.
The traditional hydrogen content detection means of the hydrogen storage material mainly comprise an X-ray diffraction analysis method, a volume method, a thermogravimetric method, a thermal desorption spectrum method and the like. X-ray diffraction analysis is widely used for phase identification of materials, belongs to a nondestructive detection means, and can detect the crystal structure of a sample, but cannot quantitatively and accurately distinguish the sample under high hydrogen content due to the lack of a standard PDF card. The volumetric method calculates the hydrogen content of the sample by measuring the volume of the sucked hydrogen, and the hydrogen content is easily influenced by temperature and equipment, so that the result deviation is larger. The thermogravimetry calculates the hydrogen content of the sample by calculating the mass change of the sample before and after heating under the protective atmosphere condition, and the measurement error is larger because the sample still suffers oxidation. The thermal desorption spectrometry test process also easily causes oxidation of the sample, and is not a good detection means because of too long time consumption. The problem of detecting the hydrogen content of the hydrogen storage material has a great impediment to the use of the hydrogen storage material. Therefore, how to accurately and rapidly detect the hydrogen content in the titanium hydride powder is a problem to be solved.
Disclosure of Invention
In order to meet the above defects or improvement demands of the prior art, the invention provides a method for detecting the hydrogen content in titanium hydride powder, which aims to accurately and rapidly detect the hydrogen content in the titanium hydride powder.
In order to achieve the above object, the present invention provides a method for detecting hydrogen content in titanium hydride powder, comprising the steps of:
s1, measuring nuclear magnetic resonance hydrogen spectrums of a plurality of titanium hydrogen compound sample powders with different hydrogen contents, and analyzing the nuclear magnetic resonance hydrogen spectrums to obtain Nett displacement;
s2, drawing a scatter diagram corresponding to the Nett displacement and the hydrogen content, and fitting a standard curve;
s3, measuring nuclear magnetic resonance hydrogen spectrum of the titanium hydride powder to be measured, and analyzing to obtain corresponding Netty displacement; and combining the standard curve to obtain the hydrogen content of the titanium hydride powder.
As a further preferable aspect, when the titanium hydride sample powder or the titanium hydride powder to be measured is measured, the powder is packed in a quartz glass tube, and then the nuclear magnetic resonance hydrogen spectrum is measured by a solid nuclear magnetic resonance spectrometer.
More preferably, the probe temperature of the solid-state nuclear magnetic resonance spectrometer used in the measurement of the nuclear magnetic resonance hydrogen spectrum is 50 to 300 ℃.
Further preferably, the probe temperature of the solid state nuclear magnetic resonance spectrometer used in the measurement of the nuclear magnetic resonance hydrogen spectrum is 150 ℃.
As a further preference, the fitting results in a standard curve of formula K s = -212+58.7/(x-1.2), where K s For Nett displacement, x is the hydrogen content in the titanium hydride, and x is more than or equal to 1.5 and less than or equal to 2.
As a further preferable aspect, the vacuum degree of the encapsulated quartz glass tube is not less than 10 -6 mbar。
Further preferably, the solid state nuclear magnetic resonance spectrometer uses a hahnecho pulse sequence of 1H spectrum.
As a further preferable mode, when the titanium hydrogen compound sample powder or the titanium hydrogen compound powder to be measured is measured, 20 to 50mg of the powder is taken and packed in a quartz glass tube.
As a further preferable example, in step S1, the number of kinds of the titanium hydride sample powders having different hydrogen contents is 4 or more.
Further preferably, in step S1, the number of the titanium hydride sample powders having different hydrogen contents is 4 to 8.
In general, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. the nett shift results from the interaction of the net electron magnetic moment generated by the berlite paramagnetic effect with the nuclear magnetic moment, also known as fermi contact interaction; for the titanium hydrogen compound, the Nett displacement reflects the ultra-fine coupling field of the conduction electrons near the hydrogen atomic nucleus and is extremely sensitive to the change of the hydrogen content.
2. For the titanium hydrogen compound, as two different phases exist at room temperature, the function relation fitting of the Nett displacement and the hydrogen content can be influenced.
3. The invention has high measuring speed, only needs to put the sample tube into nuclear magnetic equipment, runs the hahnecho pulse sequence, can obtain nuclear magnetic resonance spectrogram within one minute, and completes detection. Meanwhile, the detection method provided by the invention has no damage to the sample, and is a nondestructive detection means.
Drawings
FIG. 1 is a hydrogen nuclear magnetic resonance spectrum of a sample of titanium hydride of four known compositions at 150℃according to an embodiment of the present invention;
FIG. 2 is a graph of the normalized curve after the Nett's displacement is fitted to the hydrogen content in accordance with an embodiment of the present invention;
FIG. 3 is a chart showing the hydrogen nuclear magnetic resonance spectrum of a titanium hydride compound to be tested at 150 ℃.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The nett shift of the nmr hydrogen spectrum is caused by a shift in the resonance frequency due to electron cloud polarization. Depending on the source of the frequency offset, the Nett shift can be divided into three parts, namely K s ＝K+K d +K o The spin interactions of s-conduction band electrons, the d-band electron spin interactions, and the d-band electron orbital interactions, respectively.
K satisfies the following relationship:
where x is the atomic ratio of hydrogen to titanium and the other parameters are constant.
K d And K o The contribution of d energy charge in the titanium atom to the Netzt shift is not influenced by the hydrogen content in the compound. Thus Nett displacement K s Is a parameter directly related to the hydrogen content in the sample, and the Netty shift of the nuclear magnetic resonance hydrogen spectrum is different under different hydrogen contents.
Accordingly, the embodiment of the invention provides a method for detecting the hydrogen content in titanium hydride powder, which comprises the following steps:
s1, measuring nuclear magnetic resonance hydrogen spectrums of a plurality of titanium hydrogen compound sample powders with different hydrogen contents, and analyzing the nuclear magnetic resonance hydrogen spectrums to obtain Nett displacement;
s2, drawing a scatter diagram corresponding to the Nett displacement and the hydrogen content, and fitting a standard curve by using an analytical formula of the Nett displacement; specifically, fitting can be performed in the origin by using a simplified analytical formula, wherein Ks=K+C is a constant, and K is only related to the hydrogen content according to analysis of the Netty displacement;
s3, measuring nuclear magnetic resonance hydrogen spectrum of the titanium hydride powder to be measured, and analyzing to obtain corresponding Netty displacement; and combining the standard curve to obtain the hydrogen content of the titanium hydride powder.
Further, when the titanium hydride sample powder or the titanium hydride powder to be measured is measured, 20-50 mg of the powder is specifically taken and packaged in a quartz glass tube, and the vacuum degree of the packaged quartz glass tube is not lower than 10 -6 mbar and then determining the nuclear magnetic resonance hydrogen spectrum by means of a solid nuclear magnetic resonance spectrometer.
Further, during measurement, a solid nuclear magnetic resonance spectrometer adopts a hahnecho pulse sequence with a 1H spectrum.
Further, in order to achieve the subsequent fitting, the number of the titanium hydride sample powders having different hydrogen contents is 4 or more, and in consideration of the complexity and cost of the measurement, it is preferably 4 to 8.
The process of the invention may also be applied to some other metal hydrides, for example, those of Al, zr, V, hf, nb, ta and the like.
The following are specific examples:
(1) Weighing known component TiH 1.97 ，TiH 1.85 ，TiH 1.65 ，TiH 1.5 40mg of each sample powder was packed in a quartz glass tube having a diameter of 5mm and a length of about 2cm by a high vacuum packing apparatus, and the vacuum degree of the packed quartz glass tube was 10 -6 mbar；
(2) Respectively placing the quartz glass tubes in the step (1) into a solid nuclear magnetic resonance spectrometer, and measuring at 150 ℃ to obtain nuclear magnetic resonance hydrogen spectrograms, as shown in figure 1; the obtained nuclear magnetic resonance hydrogen spectrum was analyzed to obtain Neisserial shifts of-139.9 ppm, -122.3ppm, -87.5ppm and-29 ppm, respectively.
(3) Drawing a scatter diagram corresponding to the Nett displacement and the hydrogen content, fitting a standard curve by using an analytical formula of the Nett displacement, and obtaining an empirical formula of the Nett displacement and the hydrogen content as K, wherein the result is shown in figure 2 s = -212+58.7/(x-1.2), x is 1.5.ltoreq.x.ltoreq.2, where K s For the nuclear magnetic resonance hydrogen spectrum Nett shift, x is the ratio of hydrogen atoms to titanium atoms in the sample.
(4) Weighing 40mg of titanium hydride sample powder to be measured, respectively packaging in quartz glass tubes with the length of about 2cm and the diameter of 5mm by using high vacuum packaging equipment, wherein the vacuum degree of the packaged quartz glass tubes is 10 -6 mbar。
(5) Placing the quartz glass tube in the step (4) into a solid nuclear magnetic resonance spectrometer, and measuring at 150 ℃ to obtain a nuclear magnetic resonance hydrogen spectrum, as shown in figure 3; analyzing the obtained nuclear magnetic resonance hydrogen spectrum to obtain a Nettky shift K s -130.5ppm, the hydrogen content x=1.92 in the sample being calculated according to an empirical formula.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (7)
1. The method for detecting the hydrogen content in the titanium hydride powder is characterized by comprising the following steps of:
s1, measuring nuclear magnetic resonance hydrogen spectrums of a plurality of titanium hydrogen compound sample powders with different hydrogen contents, and analyzing the nuclear magnetic resonance hydrogen spectrums to obtain Nett displacement;
s2, drawing a scatter diagram corresponding to the Nett displacement and the hydrogen content, and fitting a standard curve by using an analytical formula of the Nett displacement; the analytical formula is K s ＝K+C，K s For the nett shift, C is a constant, K is the spin interaction of s conduction band electrons, which is related only to the hydrogen content; fitting to obtain a standard curve with the formula K s -212+58.7/(x-1.2), where x is the hydrogen content in the titanium hydride, x is 1.5.ltoreq.x.ltoreq.2;
s3, measuring nuclear magnetic resonance hydrogen spectrum of the titanium hydride powder to be measured, and analyzing to obtain corresponding Netty displacement; and then combining the standard curve to obtain the hydrogen content of the titanium hydride powder;
when the titanium hydrogen compound sample powder or the titanium hydrogen compound powder to be measured is measured, the powder is packaged in a quartz glass tube, and then the nuclear magnetic resonance hydrogen spectrum is measured through a solid nuclear magnetic resonance spectrometer; when the nuclear magnetic resonance hydrogen spectrum is measured, the probe temperature of the adopted solid nuclear magnetic resonance spectrometer is 50-300 ℃.
2. The method for detecting the hydrogen content in the titanium hydride powder according to claim 1, wherein the probe temperature of the solid state nuclear magnetic resonance spectrometer used in the measurement of the nuclear magnetic resonance hydrogen spectrum is 150 ℃.
3. The method for detecting hydrogen content in a titanium hydride compound powder as claimed in claim 1, wherein the vacuum degree of the encapsulated quartz glass tube is not less than 10 -6 mbar。
4. The method for detecting the hydrogen content in the titanium hydride powder according to claim 1, wherein the solid-state nuclear magnetic resonance spectrometer uses a hahnecho pulse sequence of 1H spectrum.
5. The method for detecting the hydrogen content in the titanium hydride compound powder according to claim 1, wherein 20 to 50mg of the powder is packed in a quartz glass tube when the titanium hydride sample powder or the titanium hydride powder to be measured is measured.
6. The method for detecting the hydrogen content of the titanium hydride powder according to any one of claims 1 to 5, wherein in step S1, the number of the titanium hydride sample powders having different hydrogen contents is 4 or more.
7. The method for detecting the hydrogen content of titanium hydride powder according to claim 6, wherein in step S1, the number of titanium hydride sample powders having different hydrogen contents is 4 to 8.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5886525A (en) * | 1997-03-17 | 1999-03-23 | The United States Of America As Represented By The Secretary Of The Navy | Apparatus and method for performing NMR spectroscopy on solid sample by rotation |
| EA201700578A1 (en) * | 2017-12-12 | 2019-06-28 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) | METHOD FOR DETERMINING A DIAMETER OF POROUS POROUS OBJECTS |
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| US9465089B2 (en) * | 2011-12-01 | 2016-10-11 | Neovision Llc | NMR spectroscopy device based on resonance type impedance (IR) sensor and method of NMR spectra acquisition |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5886525A (en) * | 1997-03-17 | 1999-03-23 | The United States Of America As Represented By The Secretary Of The Navy | Apparatus and method for performing NMR spectroscopy on solid sample by rotation |
| EA201700578A1 (en) * | 2017-12-12 | 2019-06-28 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) | METHOD FOR DETERMINING A DIAMETER OF POROUS POROUS OBJECTS |
Non-Patent Citations (2)
| Title |
|---|
| Negative Knight Shift in Ba-Ti Oxyhydride: An Indication of the Multiple Hydrogen Occupation;Tai Misaki et al.;《Chemistry of Materials》;第31卷(第18期);7178-7185 * |
| 固体高分辨核磁共振技术在有机固体研究中的应用;唐亚林;现代仪器(第03期);21-27 * |
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