CN115448383A - Preparation method of infinite-layer nickel-based superconductor precursor - Google Patents
Preparation method of infinite-layer nickel-based superconductor precursor Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002887 superconductor Substances 0.000 title claims abstract description 28
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 27
- 239000002243 precursor Substances 0.000 title claims abstract description 27
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 22
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 claims abstract description 15
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 11
- 230000005291 magnetic effect Effects 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 23
- 238000005303 weighing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 238000003980 solgel method Methods 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract 2
- 238000001816 cooling Methods 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910000480 nickel oxide Inorganic materials 0.000 description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000005298 paramagnetic effect Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
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- C01G53/70—Nickelates containing rare earth, e.g. LaNiO3
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Abstract
The invention discloses a preparation method of an infinite layer nickel-based superconductor precursor. The method comprises the following steps: dissolving neodymium nitrate, strontium nitrate and nickel nitrate in water according to a stoichiometric ratio to obtain nitric acid gel, putting the obtained nitric acid gel into an oven for concentration, then crushing a dried product by using an agate mortar, putting the crushed product into a mold, and putting the mold into a high-temperature high-pressure furnace for sintering to obtain an infinite-layer nickel-based superconductor precursor Nd 1‑x Sr x NiO 3 . The method combines the sol-gel method with a high-temperature high-pressure furnace, has the advantages of strong flexibility, simple preparation conditions, simple and convenient operation process, short period and good product stability, can prepare a large superconductor precursor, and has high product stability.
Description
Technical Field
The invention belongs to the technical field of superconducting material preparation, and particularly relates to an infinite-layer nickel-based superconductor precursor Nd 1- x Sr x NiO 3 The preparation method of (1).
Background
Copper-based superconductors and iron-based superconductors are the key and leading-edge fields of condensed physical research at present, nickel is positioned beside copper in a chemical element periodic table, and whether nickel-based oxides can become a new superconducting system is paid attention and hopefully. In 2019, nd was found 1-x Sr x NiO 2 The film has superconducting phenomenon, and initiates the research hot tide of superconducting boundary on nickel oxide system, nd 1-x Sr x NiO 2 The film being formed by reducing Nd 1-x Sr x NiO 3 The film is obtained, and the bulk sample of the nickel base in the current research is not discovered to have superconductivity temporarily, so that Nd 1-x Sr x NiO 3 The preparation of (A) has important significance.
At present, most of the existing infinite-layer nickel oxide film preparation methods need to reduce a precursor nickel oxide, and the perovskite-structure nickel oxide is a matrix material which is used in a large amount. Conventional preparation of Nd 1-x Sr x NiO 3 The method, such as magnetron sputtering, pulsed laser deposition, molecular beam epitaxy and the like, has strict requirements on experimental environment and equipment, is complex in operation process, long in preparation period and low in success rate. Therefore, a precursor Nd for simply and rapidly preparing the infinite layer nickel-based superconductor is sought 1-x Sr x NiO 3 The method has great significance for the current experimental research.
Disclosure of Invention
The invention aims to provide a simple and quick precursor Nd of an infinite layer nickel-based superconductor 1-x Sr x NiO 3 The preparation method combines the sol-gel method with a high-temperature high-pressure furnace, and has the advantages of strong flexibility, simple preparation conditions and simple and convenient operation processThe finished product has high stability and is a massive superconducting material, and the method effectively solves the problems that the existing method has strict requirements on experimental environment, experimental equipment is complex to operate and the like.
In order to achieve the above object, the present invention adopts the following technical means:
infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
1) Weighing neodymium nitrate, strontium nitrate and nickel nitrate according to a stoichiometric ratio, then sequentially pouring the weighed neodymium nitrate, strontium nitrate and nickel nitrate into deionized water, and stirring to obtain a gel product;
2) Placing the gel product in an oven for baking, and volatilizing excessive water to obtain xerogel;
3) The xerogel is put into an agate mortar and ground into powder;
4) Putting the powder into a graphite die, sintering the powder in a high-temperature and high-pressure furnace, and cooling the powder to room temperature along with the furnace to obtain Nd 1-x Sr x NiO 3 Wherein x =0.05 to 0.4.
The molar ratio of the neodymium nitrate to the strontium nitrate to the nickel nitrate is 0.6-0.95 and is as follows.
The stirring in the step 1) is stirring and dissolving on a heat collection type constant temperature magnetic stirrer, the temperature is 95-130 ℃, and the time is 4-75 min.
The baking temperature of the baking oven in the step 2) is 85-125 ℃, and the baking time is 600-950 min.
And 3) grinding for 30-100 min.
And 4) sintering at 700-1050 ℃ under 7-14 MPa for 510-720 min.
By adopting the technical scheme, the sol-gel method is combined with the high-temperature high-pressure furnace, so that the method has the advantages of strong flexibility, simple preparation conditions, simple and convenient operation process, short period and good product stability, and can be used for preparing a bulk superconductor precursor with high product stability. The method effectively solves the problems that the existing method has strict requirements on experimental environment, experimental equipment is complex to operate and the like.
Drawings
Figure 1 is an XRD spectrum of the product of example 1, example 2, example 3, example 4.
Figure 2 is an XRD pattern of the products of example 5, example 6, example 7, example 8.
FIG. 3 is a graph showing a comparison of lattice parameters of the products of examples 1, 2, 3 and 4 after sintering.
FIG. 4 is a graph showing a comparison of lattice parameters of sintered products of examples 5, 6, 7 and 8.
FIG. 5 is a graph of magnetization versus temperature for the products of examples 1, 2, 3, and 4 during zero field cooling at a magnetic field of 3000 Oe.
Detailed Description
Example 1
Infinite layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni =0.7 of 1, sequentially pouring samples into deionized water, and stirring and dissolving the samples on a heat collection type constant temperature heating magnetic stirrer at the temperature of 100 ℃ for 60min to obtain a gel-like product.
Step 2: and (3) putting the gel product into an oven, baking for 600min at 120 ℃, and volatilizing excessive water to obtain xerogel.
And 3, step 3: and pouring the xerogel into an agate mortar to be ground for 70min to obtain powder.
And 4, step 4: placing the obtained powder into a mold, placing in a high-temperature high-pressure furnace, sintering at 800 deg.C under 14Mpa for 630min, and furnace cooling to obtain Nd 0.7 Sr 0.3 NiO 3 。
Fig. 1 is an XRD spectrum of the product of this example, from which it can be seen that the diffraction peak of the product of this example is weakest relative to the products of examples 2, 3 and 4.
FIG. 3 is a graph comparing the lattice parameters of the product of this example with those of the products of examples 2, 3 and 4 after sintering in a high-temperature high-pressure furnace, and it can be seen that the lattice parameters b and c of the product of this example are the largest and a is the smallest.
FIG. 5 is the M-T curve of the product of this example showing the variation of magnetic susceptibility with temperature during zero field cooling at a magnetic field of 3000 Oe. The product of the embodiment has the highest magnetic susceptibility, the magnetic susceptibility is in a descending trend along with the temperature rise, and no obvious magnetic phase change, namely paramagnetic characteristic is observed.
Example 2
Infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: neodymium nitrate, strontium nitrate and nickel nitrate are weighed according to the stoichiometric ratio of Nd: sr: ni = 0.8.
Step 2: and (3) putting the gel product into an oven, baking for 800min at the temperature of 95 ℃, and volatilizing excessive water to obtain dry gel.
And step 3: pouring the xerogel into an agate mortar to be ground for 90min to obtain powder;
and 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 900 deg.C and 11Mpa for 540min, and cooling to obtain Nd 0.8 Sr 0.2 NiO 3 。
FIG. 1 is the XRD pattern of the product of this example, from which it can be seen that the peaks of the sample can correspond to the quadrature phase diffraction peaks, the space group is Pnma, and a small amount of impurities indicates that the purity of the sample is higher, and a small amount of Sr replaces Nd.
FIG. 3 is a graph comparing the lattice parameters of samples of the product of this example with those of examples 1, 3 and 4 after sintering in a high temperature and high pressure furnace.
FIG. 5 is an M-T curve of the product of this example showing the temperature dependence of magnetic susceptibility during zero field cooling at a magnetic field of 3000 Oe. The product of the embodiment has the lowest magnetic susceptibility, the magnetic susceptibility is in a descending trend along with the temperature rise, and no obvious magnetic phase change, namely paramagnetic characteristics, is observed.
Example 3
Infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni =0.95: 1, sequentially pouring the samples into deionized water, and stirring and dissolving the samples on a heat collection type constant temperature heating magnetic stirrer at the temperature of 120 ℃ for 75min to obtain a gel-like product.
Step 2: and (3) putting the gel product into an oven, baking for 900min at 110 ℃, and volatilizing the excessive water to obtain the xerogel.
And step 3: the xerogel is poured into an agate mortar to be ground for 40mi to obtain powder.
And 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 1050 deg.C and 10Mpa for 690min, and furnace cooling to obtain Nd 0.95 Sr 0.05 NiO 3 。
FIG. 1 is the XRD pattern of the product of this example, from which it can be seen that the peaks of the sample can correspond to the quadrature phase diffraction peaks, the space group is Pnma, and a small amount of impurities indicates that the purity of the sample is higher, and a small amount of Sr replaces Nd.
FIG. 3 is a graph comparing the lattice parameters of samples of the product of this example with those of examples 1, 2 and 4 after sintering in a high temperature and high pressure furnace.
FIG. 5 is the M-T curve of the product of this example showing the variation of magnetic susceptibility with temperature during zero field cooling at a magnetic field of 3000 Oe. The magnetic susceptibility of the product of this example is similar to that of the product of example 4, and the magnetic susceptibility tends to decrease with increasing temperature, with a slight change in magnetic susceptibility at a location of about 20K.
Example 4
Infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni = 0.9.
And 2, step: and (3) putting the gel product into an oven, baking for 700min at 85 ℃, and volatilizing excessive water to obtain dry gel.
And step 3: pouring the xerogel into an agate mortar to be ground for 100min to obtain powder;
and 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 750 deg.C and 12Mpa for 720min, and furnace cooling to obtain Nd 0.9 Sr 0.1 NiO 3 。
FIG. 1 is the XRD pattern of the product of this example, from which it can be seen that the peak of the sample corresponds to the quadrature phase diffraction peak, the space group is Pnma, and the diffraction peak of the product of this example is the strongest.
FIG. 3 is a graph comparing the lattice parameters of the sample after sintering in the high temperature and high pressure furnace with those of examples 1, 2 and 3, and it can be seen that the lattice parameters a are the largest and b and c are the smallest.
FIG. 5 is an M-T curve of the product of this example showing the temperature dependence of magnetic susceptibility during zero field cooling at a magnetic field of 3000 Oe. The magnetic susceptibility of the product of the embodiment is similar to that of the product of the embodiment 3, the magnetic susceptibility is in a descending trend along with the increase of the temperature, and no obvious magnetic phase change, namely paramagnetic characteristic, is observed.
Example 5
Infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni = 0.65.
Step 2: and (3) putting the gel product into an oven, baking for 950min at 105 ℃, and volatilizing excessive water to obtain xerogel.
And step 3: and pouring the xerogel into an agate mortar to be ground for 60min to obtain powder.
And 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 1000 deg.C and 9Mpa for 570min, and furnace cooling to obtain Nd 0.65 Sr 0.35 NiO 3 。
FIG. 1 is an XRD spectrum of the product of this example, from which it can be seen that the product of this example has a weak peak, a small amount of impurities, and a small amount of Sr replacing Nd.
Fig. 4 is a graph comparing the lattice parameters of the sample after the product of the present example is sintered in the high temperature and high pressure furnace with those of examples 6, 7 and 8, and it can be seen that the lattice parameters b and c of the product of the present example are the maximum and a is the minimum.
Example 6
Infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni = 0.6.
Step 2: and (3) putting the gel product into an oven, baking for 750min at 125 ℃, and volatilizing excessive water to obtain xerogel.
And 3, step 3: and pouring the xerogel into an agate mortar to be ground for 30min to obtain powder.
And 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 950 deg.C and 8Mpa for 510min, and cooling to obtain Nd 0.6 Sr 0.4 NiO 3 。
FIG. 2 is the XRD pattern of the product of this example, from which it can be seen that the peaks of the sample can correspond to the quadrature phase diffraction peaks, the space group is Pnma, and a small amount of impurities indicates that the purity of the sample is higher, and a small amount of Sr replaces Nd.
FIG. 4 is a graph comparing the lattice parameters of the sample after the product of this example is sintered in a high temperature and high pressure furnace with those of examples 5, 7 and 8, and it can be seen that the lattice parameters of the product of this example and the product of example 7 are not very different.
Example 7
Infinite layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni = 0.75.
Step 2: and (3) putting the gel product into an oven, baking for 650min at 90 ℃, and volatilizing excessive water to obtain xerogel.
And 3, step 3: and pouring the xerogel into an agate mortar to be ground for 50min to obtain powder.
And 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 850 deg.C and 7Mpa for 600min, and cooling to obtain Nd 0.75 Sr 0.25 NiO 3 。
FIG. 2 is the XRD pattern of the product of this example, from which it can be seen that the peaks of the sample correspond to the orthorhombic phase diffraction peaks, the space group is Pnma, and a small amount of impurities, which indicates that the purity of the sample is high, and a small amount of Sr replaces Nd.
FIG. 4 is a graph comparing the lattice parameters of samples with those of examples 5, 6 and 8 after sintering the product of this example in a high temperature and high pressure furnace.
Example 8
Infinite-layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method comprises the following steps:
step 1: weighing neodymium nitrate, strontium nitrate and nickel nitrate according to the stoichiometric ratio of Nd: sr: ni = 0.85.
And 2, step: and (3) putting the gel product into an oven, baking for 850min at the temperature of 100 ℃, and volatilizing excessive water to obtain xerogel.
And step 3: and pouring the xerogel into an agate mortar to be ground for 80min to obtain powder.
And 4, step 4: placing the obtained powder into a mold, sintering in a high temperature and high pressure furnace at 700 deg.C and 13Mpa for 660min, and cooling to obtain Nd 0.85 Sr 0.15 NiO 3 。
Fig. 2 is an XRD spectrum of the product of this example, from which it can be seen that the peak of the sample of this example corresponding to the orthorhombic phase diffraction is the strongest as compared to examples 5, 6 and 7, and the space group is Pnma, a small amount of impurities indicates that the purity of the sample is high and a small amount of Sr replaces Nd.
FIG. 4 is a graph showing the comparison of the lattice parameters of the sample after sintering in the high temperature and high pressure furnace with those of examples 5, 6 and 7, and it can be seen that the lattice parameters a are the largest and b and c are the smallest.
Claims (8)
1. Infinite layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method is characterized by comprising the following steps:
1) Weighing neodymium nitrate, strontium nitrate and nickel nitrate according to a stoichiometric ratio, then sequentially pouring the weighed materials into water, and stirring to obtain a gel product;
2) Placing the gel product in an oven for baking, and volatilizing excessive water to obtain xerogel;
3) Putting the xerogel into an agate mortar and grinding into powder;
4) Mixing the above powdersPlacing the powder into a mold, and sintering the powder in a high-temperature high-pressure furnace to obtain Nd 1-x Sr x NiO 3 Wherein x =0.05 to 0.4.
2. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The method for producing (1), wherein the molar ratio of the neodymium nitrate to the strontium nitrate to the nickel nitrate is 0.6 to 0.95.
3. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The preparation method is characterized in that the purity of the neodymium nitrate is more than or equal to 99.0 percent, the purity of the strontium nitrate is more than or equal to 99.5 percent, and the purity of the nickel nitrate is more than or equal to 98.0 percent.
4. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The preparation method is characterized in that the stirring in the step 1) is carried out on a magnetic stirrer for stirring and dissolving, the temperature is 95-130 ℃, and the time is 4-75 min.
5. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The preparation method is characterized in that the baking temperature of the baking oven in the step 2) is 85-125 ℃, and the baking time is 600-950 min.
6. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The preparation method is characterized in that the grinding time in the step 3) is 30-100 min.
7. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The preparation method is characterized in that the sintering temperature in the step 4) is 700-1050 ℃, the pressure is 7-14 MPa, and the sintering time is 510 to720min。
8. The infinite-layer nickel-based superconductor precursor Nd according to claim 1 1-x Sr x NiO 3 The preparation method is characterized in that after the sintering in the step 4) is finished, the mixture is cooled to room temperature along with the furnace.
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