CN116396077A - Lead-containing ceramic for nuclear power station and preparation method thereof - Google Patents
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 125000004429 atom Chemical group 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 238000004364 calculation method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000001568 sexual effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004215 lattice model Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
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Abstract
The invention discloses a lead-containing ceramic for a nuclear power station and a preparation method thereof, wherein the lead-containing ceramic has a chemical formula of Zr 3 PbC 2 Or Hf 3 PbC 2 The ternary lamellar carbide ceramic with the nano lamellar structure contains lead element, and belongs to 312 phases in MAX phase ceramic; the preparation method comprises the following steps: zr/Hf powder, pb powder and C powder according to the mol ratio of 3: (0.9-1.3): (2-2.3) mixing under the protection of argon to obtain mixed powder; heating the mixed powder to 1200-1400 ℃, cooling and grinding off the surface carbonized layer to obtain the sample. The lead-containing ceramic Zr discovered for the first time by the invention 3 PbC 2 And Hf 3 PbC 2 The discovery and preparation of new ceramics provide a new material for the development of the nuclear industryAnd safe operation of the nuclear reactor is ensured.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to lead-containing ceramic for a nuclear power station and a preparation method thereof.
Background
The nuclear power industry in China has rapid development in recent years, and nuclear reactors play a vital role in the nuclear power industry. In order to meet the normal operation conditions of the nuclear reactor, two brand new lead-containing ceramic materials are designed.
Lead (Pb) has the characteristics of high atomic number and high density, has good shielding capability on X rays, alpha rays, beta rays and gamma rays, and is widely applied to the protection of ray radiation. In addition, lead is also used to slow down fast neutrons in neutron radiation. Unfortunately, however, elemental lead does not itself have the ability to absorb slow neutrons, which also means that elemental lead does not shield neutron radiation well.
In order to obtain the material for nuclear reactor, the invention introduces Zr element and Hf element with slow neutron absorption capacity, and then introduces C element to stabilize the Zr element and Hf element, and designs a material with M 6 A layered ceramic material having an alternating arrangement of C (m=zr, hf) octahedral layers and Pb layers. The ceramic material has the advantages of retaining the ray shielding capability of lead element and slowing down the fast neutron velocity, and increasing M for absorbing slow neutrons 6 The C (M=Zr, hf) layer can effectively shield alpha rays, beta rays, gamma rays and absorb neutrons, ensures the safe operation of a nuclear reactor, and has a very large application prospect in the nuclear industry.
Disclosure of Invention
In order to achieve the above purpose, the invention provides a lead-containing ceramic for a nuclear power station and a preparation method thereof.
The lead-containing ceramic for the nuclear power station has the chemical formula of Zr 3 PbC 2 Or Hf 3 PbC 2 。
Zr 3 PbC 2 Is P6 3 /mmc；Zr 3 PbC 2 Is of the lattice parameter of
Zr atoms are located at (0, 0) and (1/3, 2/3,0.12586), pb atoms are located at (0, 1/4), and C atoms are located at (1/3, 2/3,0.56632).
Hf 3 PbC 2 Is P6 3 /mmc；Hf 3 PbC 2 Is of the lattice parameter of
Hf atoms are located at (0, 0) and (2/3, 1/3,0.12552), pb atoms are located at (0, 1/4), and C atoms are located at (1/3, 2/3,0.06413).
The invention relates to lead-containing ceramic for nuclear power stations: zr (Zr) 3 PbC 2 And Hf 3 PbC 2 . The lattice structure and the atomic position of the new phase are determined by detection and analysis methods such as X-ray diffraction, first sexual principle calculation, scanning electron microscope and the like. Zr (Zr) 3 PbC 2 And Hf 3 PbC 2 Is ternary lamellar carbide ceramic with nano lamellar structure containing lead element, belongs to 312 phases in MAX phase ceramic, and is also first proposed and successfully synthesized with Zr 3 PbC 2 And Hf 3 PbC 2 . The invention provides a new phase of lead-containing ceramic for two nuclear power stations and successful synthesis, provides new material support for the nuclear industry, and ensures the safe operation of a nuclear reactor.
The preparation method of the lead-containing ceramic for the nuclear power station comprises the following steps:
step 1: zr/Hf powder, pb powder and C powder according to the mol ratio of 3: (0.9-1.3): (2-2.3) mixing under the protection of argon gas to obtain mixed powder.
Step 2: heating the mixed powder to 1200-1400 ℃, cooling and grinding off the surface carbonized layer to obtain the sample.
Further, in the step 1, argon is used for protection and mixing, the mixing time is 10-14 h, and the mixing speed is 40-80 rpm.
Further, the temperature rising rate in the step 2 is 10-50 ℃/min, and the pressure is 20-40 MPa.
The beneficial technical effects of the invention are as follows:
1. the invention discovers a novel lead-containing ceramic Zr for nuclear power plants 3 PbC 2 And Hf 3 PbC 2 The lattice structure and the atomic position of the new phase are determined by detection and analysis methods such as X-ray diffraction, first sexual principle calculation, scanning electron microscope and the like.
2. The invention discloses lead-containing ceramic Zr for the first time 3 PbC 2 And Hf 3 PbC 2 The discovery and preparation of new ceramics provide new material support for the development of the nuclear industry and ensure the safe operation of the nuclear reactor.
Drawings
FIG. 1 is a view of the lead-containing ceramic Zr in example 1 3 PbC 2 And Hf 3 PbC 2 A comparison of the X-ray diffraction pattern of (c) with a theoretical X-ray diffraction pattern.
FIG. 2 is a view of Zr in the lead-containing ceramic of example 1 3 PbC 2 And Hf 3 PbC 2 SEM/EDS of (a).
FIG. 3 is a view showing a lead-containing ceramic Zr in example 1 3 PbC 2 (0 00 2) and (iv)
The atomic arrangement of the facets and the diffraction spots obtained by simulation.
FIG. 4 is a view showing a lead-containing ceramic Zr in example 1 3 PbC 2 Rietveld fitting pattern of (a).
FIG. 5 is a view showing the Hf ceramic containing lead in example 1 3 PbC 2 Rietveld fitting pattern of (a).
Detailed Description
The invention will be described in further detail with reference to the drawings and examples.
Example 1
Lead-containing ceramic material Zr for nuclear power plant 3 PbC 2 And Hf 3 PbC 2 The preparation method of (2) comprises the following steps:
(1) Zr/Hf powder (99.9%, 500 mesh), pb powder (99.99%, 500 mesh) and C powder (99.95%, 500 mesh) in a molar ratio of 3:1.2:2.2, mixing, namely mixing for 12 hours by using a drum mixer under the protection of argon gas to obtain mixed powder;
(2) 17g of the mixed powder is put into a graphite mold filled with graphite paper, covered with graphite felt, loaded into an SPS furnace, heated to 700 ℃ at a heating rate of 50 ℃/min under 20MPa, then heated to 1400 ℃ at 10 ℃/min, and then cooled with the furnace. And grinding the surface carbide layer to obtain the target block.
Example 2
Lead-containing ceramic material Zr for nuclear power plant 3 PbC 2 And Hf 3 PbC 2 The preparation method of (2) comprises the following steps:
(1) Zr/Hf powder (99.9%, 500 mesh), pb powder (99.99%, 500 mesh) and C powder (99.95%, 300 mesh) in a molar ratio of 3:1.3:2.2, mixing, namely mixing for 14 hours by using a drum mixer under the protection of argon gas to obtain mixed powder;
(2) 17g of the mixed powder is put into a graphite mould filled with graphite paper, covered with graphite felt, loaded into an SPS furnace, heated to 700 ℃ at a heating rate of 40 ℃/min under 20MPa, then heated to 1400 ℃ at 20 ℃/min, and then cooled with the furnace. And grinding the surface carbide layer to obtain the target block.
Example 3
Lead-containing ceramic material Zr for nuclear power plant 3 PbC 2 And Hf 3 PbC 2 The preparation method of (2) comprises the following steps:
(1) Zr/Hf powder (99.9%, 300 mesh), pb powder (99.99%, 800 mesh) and C powder (99.95%, 1500 mesh) in a molar ratio of 3:1.4:2.2, mixing, namely mixing for 10 hours by using a drum mixer under the protection of argon gas to obtain mixed powder;
(2) 17g of the mixed powder is put into a graphite mould filled with graphite paper, covered with graphite felt, loaded into an SPS furnace, heated to 700 ℃ at a heating rate of 70 ℃/min under 20MPa, then heated to 1400 ℃ at 15 ℃/min, and then cooled with the furnace. And grinding the surface carbide layer to obtain the target block.
Experimental example
1. Zr obtained in example 1 3 PbC 2 And Hf 3 PbC 2 The ceramic blocks were phase-detected using X-ray diffraction (XRD) and characteristic peaks of the new phase were identified corresponding to theoretical characteristic peaks calculated by Material Studio, as shown in fig. 1.
Zr prepared in example 1 according to the X-ray diffraction pattern of the ceramic block shown in FIG. 1 3 PbC 2 And Hf 3 PbC 2 Ceramic block X-ray diffractionHas a series of unknown peaks, and the peak positions of the unknown peaks are equal to Zr 3 PbC 2 And Hf 3 PbC 2 Is highly consistent with the theoretical value of (c).
2. Zr obtained in example 1 3 PbC 2 And Hf 3 PbC 2 Microscopic morphology observations (as shown in fig. 2) of the ceramic blocks were performed using a scanning electron microscope in combination with an energy spectrometer (SEM/EDS), confirming the microscopic layered structure and elemental composition of the samples.
According to the SEM image of ceramic powder shown in FIG. 2, example 1 shows Zr as powder 3 PbC 2 And Hf 3 PbC 2 Has typical lamellar features, and the white cross-position EDS results show Zr: pb=2.81: 1 and Hf: pb=3.19: 1, within the tolerance range.
3. Identifying the XRD pattern obtained in the step 1, and calculating Zr by using a Crystal Maker in combination with the theoretical Crystal structure calculated by the Material Studio 3 PbC 2 And Hf 3 PbC 2 Theoretical diffraction spots. Zr established according to example 1 shown in FIG. 3 3 PbC 2 The crystal lattice of the ceramic belongs to a typical MAX phase structure, wherein the atomic arrangement of the (0 00 2) plane and the theoretical diffraction spots show that it belongs to the hexagonal system,
the atomic arrangement of the face and the theoretical diffraction spots show typical lamellar arrangement, and Zr and Pb atoms follow [ 00 0 1 ]]The direction is regularly stacked in an ABABACACA mode.
4. Taking the XRD pattern obtained in the step 1 and the lattice model obtained after the step optimization as input, and performing Rietveld fitting in Full-Prof software to obtain Zr 3 PbC 2 And Hf 3 PbC 2 Rietveld fitting graphs of ceramics (shown in fig. 4 and 5) determine lattice constants, atomic positions (shown in table 1) of ceramic powders and 2 theta, d and I values (shown in tables 2 and 3) of different crystal plane corresponding calculations and experiments.
TABLE 1 Zr in example 1 3 PbC 2 And Hf 3 PbC 2 Lattice constant and atomic position of ceramics
TABLE 2 Zr in example 1 3 PbC 2 Corresponding calculation and experiment of 2 theta, d and I values of different crystal faces of ceramic
TABLE 3 Hf in example 1 3 PbC 2 Corresponding calculation and experiment of 2 theta, d and I values of different crystal faces of ceramic
According to Zr shown in FIG. 4 3 PbC 2 Rietveld fitting map of ceramic block, zr 3 PbC 2 The purity of the sample was 37.98wt% (55.28 wt% ZrC,1.82wt% Pb,4.92wt% Zr), R-P=6.50%, and R-WP=8.26%. At the same time obtain Zr 3 PbC 2 The lattice parameters and atomic positions of the ceramics (shown in table 1) and the corresponding calculated and experimental 2 theta, d and I values of different crystal faces (shown in table 2).
According to Hf shown in FIG. 5 3 PbC 2 Rietveld fitting map of ceramic block, hf 3 PbC 2 The purity of the sample was 40.10wt% (59.87 wt% hfc,0.03wt% pb contained therein), R-p=8.31%, R-wp=11.2%. At the same time obtain Hf 3 PbC 2 The lattice parameters and atomic positions of the ceramics (shown in table 1) and the corresponding calculated and experimental 2 theta, d and I values of different crystal faces (shown in table 3).
The invention relates to a novel lead-containing ceramic material Zr for nuclear power plants 3 PbC 2 And Hf 3 PbC 2 And the preparation method thereof, the method of the invention is adopted to successfully prepare new MAX phase Zr 3 PbC 2 And Hf 3 PbC 2 Ceramics, and give Zr 3 PbC 2 And Hf 3 PbC 2 The invention provides two lead-containing ceramics for nuclear power stations, provides new material support for the development of nuclear industry, and ensures the safe operation of nuclear reactors.
Claims (4)
1. A lead-containing ceramic for nuclear power station is characterized in that the chemical formula of the ceramic is Zr 3 PbC 2 Or Hf 3 PbC 2 ；
The Zr is 3 PbC 2 Is P6 3 /mmc；Zr 3 PbC 2 Is of the lattice parameter of
Zr atoms are located at (0, 0) and (1/3, 2/3,0.12586), pb atoms are located at (0, 1/4), and C atoms are located at (1/3, 2/3,0.56632);
the Hf 3 PbC 2 Is P6 3 /mmc；Hf 3 PbC 2 Is of the lattice parameter of
Hf atoms are located at (0, 0) and (2/3, 1/3,0.12552), pb atoms are located at (0, 1/4), and C atoms are located at (1/3, 2/3,0.06413).
2. The method for producing a lead-containing ceramic for nuclear power plants as defined in claim 1, comprising the steps of:
step 1: zr/Hf powder, pb powder and C powder according to the mol ratio of 3: (0.9-1.3): (2-2.3) mixing under the protection of argon to obtain mixed powder;
step 2: heating the mixed powder to 1200-1400 ℃, cooling and grinding off the surface carbonized layer to obtain the sample.
3. The method for preparing lead-containing ceramic for nuclear power plant according to claim 2, wherein the step 1 is performed with argon protection mixing for 10-14 hours at 40-80 rpm.
4. The method for preparing lead-containing ceramic for nuclear power plant according to claim 2, wherein the heating rate in step 2 is 10-50 ℃/min and the pressure is 20-40 MPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799185A (en) * | 2017-09-13 | 2018-03-13 | 中广核研究院有限公司 | Fuel can and fuel assembly |
| CN108147828A (en) * | 2017-12-13 | 2018-06-12 | 广东核电合营有限公司 | MAX phase ceramics tubing and preparation method thereof, cladding nuclear fuels pipe |
| CN114315369A (en) * | 2022-01-06 | 2022-04-12 | 西南交通大学 | Ternary layered boride ceramic and preparation method thereof |
| CN114669747A (en) * | 2022-03-21 | 2022-06-28 | 四川大学 | M based on Cr, Zr or NbnAlCn-1Method for preparing phase powder |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799185A (en) * | 2017-09-13 | 2018-03-13 | 中广核研究院有限公司 | Fuel can and fuel assembly |
| CN108147828A (en) * | 2017-12-13 | 2018-06-12 | 广东核电合营有限公司 | MAX phase ceramics tubing and preparation method thereof, cladding nuclear fuels pipe |
| CN114315369A (en) * | 2022-01-06 | 2022-04-12 | 西南交通大学 | Ternary layered boride ceramic and preparation method thereof |
| CN114669747A (en) * | 2022-03-21 | 2022-06-28 | 四川大学 | M based on Cr, Zr or NbnAlCn-1Method for preparing phase powder |
Non-Patent Citations (2)
| Title |
|---|
| 姚沛: "《MAX相陶瓷及其与SiC复合材料的微波吸收与屏蔽性能研究》", 中国博士学位论文全文数据库, no. 2023, pages 18 - 25 * |
| 成来飞 等: "《复合材料原理及工艺》", 西北工业大学出版社, pages: 66 - 67 * |
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