Special zero-susceptibility alloy for nuclear magnetic resonance spectrometer and preparation method thereof

By preparing Cu-Rh-Fe-Mn copper-based alloys, the problem of high magnetic susceptibility of the detection probe of nuclear magnetic resonance spectrometer was solved, realizing an alloy material with high sensitivity and high conductivity, thus improving the detection performance of nuclear magnetic resonance spectrometer.

CN119410951APending Publication Date: 2025-02-11SHANGHAI HUANTONG SCI & EDUCATIONAL EQUIP CO LTD
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Patent Information

Application Number
CN202411324522.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-23
Publication Date
2025-02-11

AI Technical Summary

Technical Problem

The high magnetic susceptibility of the detection probe wires in existing nuclear magnetic resonance spectrometers leads to impaired magnetic field uniformity, affecting instrument resolution and detection sensitivity.

Method used

Using Cu-Rh-Fe-Mn copper alloys, alloy thin plates were prepared by vacuum metallurgy, and then heated under inert gas protection and finally cooled and quenched with liquid nitrogen to prepare alloy materials with extremely low magnetic susceptibility.

Benefits of technology

A high-sensitivity, zero-magnetic-susceptibility, and high-conductivity alloy material was developed, suitable for nuclear magnetic resonance spectrometers, improving the magnetic field uniformity and detection sensitivity of the detection probe and simplifying the winding process.

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Abstract

The invention discloses a special zero-magnetic-susceptibility alloy for a nuclear magnetic resonance spectrometer and a preparation method of the special zero-magnetic-susceptibility alloy. The special zero-magnetic susceptibility alloy for the nuclear magnetic resonance spectrometer is Cu-Rh-Fe-Mn copper alloy, and comprises the following components in percentage by mass: 0.5 to 0.6 percent of Rh, 0.03 to 0.05 percent of Fe, 0.015 to 0.02 percent of Mn and the balance of Cu. The special zero-magnetic-susceptibility alloy for the nuclear magnetic resonance spectrometer has the characteristics of high sensitivity, zero magnetic susceptibility, high strength and high conductivity. The magnetic susceptibility of the special zero-magnetic susceptibility alloy for the nuclear magnetic resonance spectrometer is 5lt; the prepared magnetic core has the advantages that the magnetic core is not diamagnetic or paramagnetic, the conductivity is larger than 95% ICS, the magnetic core can be used for a nuclear magnetic resonance spectrometer, tight winding is achieved, only the electromagnetic performance needs to be considered during winding, the influence of magnetic susceptibility does not need to be considered, and the optimal electromagnetic performance is easy to achieve.
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Description

Technical Field

[0001] The invention relates to an alloy metal, in particular to a zero magnetic susceptibility alloy special for a nuclear magnetic resonance spectrometer and a preparation method thereof. Background Art

[0002] Nuclear magnetic resonance spectrometer is an important instrument for chemical structure analysis. It uses the resonance between atomic nuclei and electromagnetic fields under magnetic fields to obtain chemical structure information. The magnetic field uniformity of the nuclear magnetic resonance spectrometer must reach 10-8 or 10-9, so as to achieve an instrument resolution of 10 -8 or 10 -9 The magnetic susceptibility of the NMR spectrometer probe wire reaches 10 6 In the process of realizing the present invention, the inventors found that the current nuclear magnetic resonance spectrometer uses a low magnetic susceptibility of 7*10 7 The conductor is loosely wound and magnetized to offset the winding, this method of probe detection sensitivity is low. Summary of the invention

[0003] In order to solve the above technical problems, the embodiment of the present invention provides a zero magnetic susceptibility alloy dedicated to nuclear magnetic resonance spectrometer and a preparation method thereof. The specific technical solution is as follows: In the first aspect, a zero magnetic susceptibility alloy dedicated to a nuclear magnetic resonance spectrometer is provided. The zero magnetic susceptibility alloy dedicated to a nuclear magnetic resonance spectrometer is a Cu-Rh-Fe-Mn copper alloy, wherein the mass percentage of Rh is 0.5-0.6%, the mass percentage of Fe is 0.03-0.05%, the mass percentage of Mn is 0.015-0.02%, and the rest is Cu.

[0004] In a second aspect, a method for preparing a zero magnetic susceptibility alloy for a nuclear magnetic resonance spectrometer is provided. The alloy thin plate is prepared by a vacuum metallurgical method, which comprises the following steps: weighing raw materials according to the percentage of each component of the zero magnetic susceptibility alloy for a nuclear magnetic resonance spectrometer of the first aspect; vacuum smelting the weighed raw materials into alloy ingots at a temperature of 1550-1560°C; rolling the alloy ingot into an alloy thin plate and processing it into shape; heating the processed alloy thin plate to 950°C-980°C under inert gas protection and maintaining it for 30-40 minutes; and cooling and quenching.

[0005] In a first possible implementation of the second aspect, in the step of weighing raw materials according to the percentage of each component of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to the first aspect, the purity of the weighed copper is 99.999%, the purity of the rhodium is 99.9%, and the purity of the iron and manganese is 99.9%.

[0006] In a second possible implementation of the second aspect, in the step of vacuum smelting the weighed raw materials into alloy ingots at a temperature of 1550-1560° C., the vacuum degree is 10*Pa.

[0007] In a third possible implementation of the second aspect, in the step of vacuum smelting the weighed raw materials into alloy ingots at a temperature of 1550-1560°C, the weighed raw materials are placed in a crucible and heated to 1550-1560°C in the crucible.

[0008] In a fourth possible implementation manner of the second aspect, in the step of rolling the alloy ingot into the alloy sheet and processing the alloy sheet into shape, the alloy sheet is processed into shape by wire cutting.

[0009] In a fifth possible implementation manner of the second aspect, in the cooling and quenching step, liquid nitrogen is used to cool and quench the annealed alloy thin plate.

[0010] In the embodiment of the present invention, the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer of the present invention has the characteristics of high sensitivity, zero magnetic susceptibility, high strength and high conductivity. The magnetic susceptibility of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer of the present invention is 5<10 8 (almost zero), that is, it is neither antimagnetic nor paramagnetic, and its conductivity is greater than 95% ICS. It can be used in nuclear magnetic resonance spectrometers to achieve tight winding. When winding, only the electromagnetic properties need to be considered without considering the influence of magnetic susceptibility, and it is easy to achieve the best electromagnetic properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings: Figure 1 The present invention is a flowchart of the steps of a method for preparing a zero magnetic susceptibility alloy dedicated to a nuclear magnetic resonance spectrometer according to an embodiment of the present invention. DETAILED DESCRIPTION

[0012] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0013] See also Figure 1, which is a step flow chart of the preparation method of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to one embodiment of the present invention; as shown in the figure, the preparation method of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer includes the following steps S1 to S5. The alloy sheet is prepared by vacuum metallurgy. First, in step S1, the raw materials are weighed according to the percentage of each component of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer. The zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer is a Cu-Rh-Fe-Mn copper alloy, wherein the mass percentage of Rh is 0.5-0.6%, the mass percentage of Fe is 0.03-0.05%, the mass percentage of Mn is 0.015-0.02%, and the rest is Cu. Preferably, the purity of the copper weighed above is 99.999%, the purity of rhodium is 99.9%, and the purity of iron and manganese is 99.9%.

[0014] In step S2, the weighed raw materials are vacuum smelted at 1550-1560°C to form an alloy ingot. Specifically, the weighed raw materials in step S1 are all put into a crucible, and the crucible is heated to 1550-1560°C in the crucible, while the vacuum degree is controlled to be 10*Pa, so that the raw materials are vacuum smelted at 1550-1560°C to form an alloy ingot.

[0015] In step S3, the alloy ingot is rolled into an alloy sheet and processed. In this embodiment, the alloy sheet is processed by wire cutting. Then, in step S4, the processed alloy sheet is heated to 950°C-980°C under the protection of an inert gas and maintained for 30-40 minutes. Finally, in step S5, the alloy sheet is cooled and quenched. In this embodiment, liquid nitrogen is used to cool and quench the annealed alloy sheet.

[0016] The zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer prepared by the preparation method of the present embodiment has the characteristics of high sensitivity, zero magnetic susceptibility, high strength and high conductivity. The magnetic susceptibility of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer of the present invention is 5<10 8 (almost zero), that is, it is neither antimagnetic nor paramagnetic, and its conductivity is greater than 95% ICS. It can be used in nuclear magnetic resonance spectrometers to achieve tight winding. When winding, only the electromagnetic properties need to be considered without considering the influence of magnetic susceptibility, and it is easy to achieve the best electromagnetic properties.

[0017] The beneficial effects of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer and the preparation method thereof according to the embodiments of the present invention will be described below with specific embodiments. Example

[0018] 1. Put high-purity raw materials in a crucible in proportion, including 0.5-0.6% Rh by mass, 0.03-0.05% Fe by mass, 0.015-0.02% Mn by mass, and the rest is copper. The purity of copper is 99.999%, the purity of rhodium is 99.9%, and the purity of iron and manganese is 99.9%.

[0019] 2. Heat the tungsten crucible to 1560℃ with 400A current in 10Pa vacuum, cool and solidify into ingot after melting, then roll into thin plate and wire cut into required shape.

[0020] 3. Heat to 980°C under inert gas, maintain for 30 minutes, and then place it in liquid nitrogen for cooling and quenching.

[0021] 4. Test the conductivity of the zero magnetic susceptibility alloy used for the nuclear magnetic resonance spectrometer of the above paper cups: 95% ICS (room temperature 25°C) and magnetic susceptibility: 8.2*10 8 (Room temperature 25℃).

[0022] In summary, the present invention provides a zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer and a preparation method thereof. The zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer of the present invention has the characteristics of high sensitivity, zero magnetic susceptibility, high strength and high conductivity. The magnetic susceptibility of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer of the present invention is 5<10 8 (almost zero), that is, neither antimagnetic nor paramagnetic, the conductivity is greater than 95% ICS, it can be used in nuclear magnetic resonance spectrometers to achieve tight winding, and when winding, only the electromagnetic performance needs to be considered without considering the influence of magnetic susceptibility, and it is easy to achieve the best electromagnetic performance It should be noted that, in this article, the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, an element defined by the sentence "comprises a ..." does not exclude the existence of other identical elements in the process, method, article or device including the element.

[0023] The embodiments of the present invention are described above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned specific implementation modes, which are merely illustrative rather than restrictive. Under the guidance of the present invention, ordinary technicians in this field can also make many forms without departing from the scope of protection of the present invention and the claims, all of which are within the protection of the present invention.

Claims

1. A zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer, characterized in that: The zero magnetic susceptibility alloy dedicated to the nuclear magnetic resonance spectrometer is a Cu-Rh-Fe-Mn copper alloy, wherein the mass percentage of Rh is 0.5-0.6%, the mass percentage of Fe is 0.03-0.05%, the mass percentage of Mn is 0.015-0.02%, and the rest is Cu.

2. A method for preparing a zero magnetic susceptibility alloy for a nuclear magnetic resonance spectrometer, characterized in that: The alloy sheet is prepared by vacuum metallurgy. The following steps are involved: Weigh the raw materials according to the percentage of each component of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 1; The weighed raw materials are vacuum smelted at 1550-1560°C to form alloy ingots; Rolling the alloy ingot into alloy thin plates and processing them into shapes; The formed alloy sheet is heated to 950° C.-980° C. under the protection of an inert gas, and maintained at the temperature for 30-40 minutes; Cooling and quenching.

3. The method for preparing the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 2, characterized in that: In the step of weighing the raw materials according to the percentage of each component of the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 1, the purity of the weighed copper is 99.999%, the purity of the rhodium is 99.9%, and the purity of the iron and manganese is 99.9%.

4. The method for preparing the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 2, characterized in that: In the step of smelting the weighed raw materials into the alloy ingot under vacuum at a temperature of 1550-1560° C., the vacuum degree is 10*Pa.

5. The method for preparing the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 2, characterized in that: In the step of smelting the weighed raw materials into the alloy ingot at a temperature of 1550-1560° C. in vacuum, the weighed raw materials are placed in a crucible and heated to 1550-1560° C. in the crucible.

6. The method for preparing the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 2, characterized in that: In the step of rolling the alloy ingot into the alloy sheet and processing the alloy sheet into a shape, the alloy sheet is processed into a shape by wire cutting.

7. The method for preparing the zero magnetic susceptibility alloy for nuclear magnetic resonance spectrometer according to claim 2, characterized in that: In the cooling and quenching step, liquid nitrogen is used to cool and quench the annealed alloy sheet.