CN113186440A - Aluminum fluoride-based ceramic neutron moderating material and preparation method thereof - Google Patents
Aluminum fluoride-based ceramic neutron moderating material and preparation method thereof Download PDFInfo
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- CN113186440A CN113186440A CN202110463782.2A CN202110463782A CN113186440A CN 113186440 A CN113186440 A CN 113186440A CN 202110463782 A CN202110463782 A CN 202110463782A CN 113186440 A CN113186440 A CN 113186440A
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- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title claims abstract description 39
- 239000000919 ceramic Substances 0.000 title claims abstract description 25
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 238000005520 cutting process Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- 238000007731 hot pressing Methods 0.000 claims description 7
- 229910000838 Al alloy Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 abstract 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 206010028980 Neoplasm Diseases 0.000 description 3
- 201000011510 cancer Diseases 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000020610 powder formula Nutrition 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001959 radiotherapy Methods 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Manufacturing & Machinery (AREA)
- Radiation-Therapy Devices (AREA)
Abstract
The invention discloses an aluminum fluoride-based ceramic neutron moderating material and a preparation method thereof. The technical scheme of the invention is as follows: the composite material comprises the following components in percentage by mass: 0.5-5% of LiF, 15-40% of Al and 345-75% of AlF, and the particle sizes of LiF, Al and AlF3 powder are all less than 2.5 mu m. The preparation method provided by the invention can ensure that the moderator has high density, high hardness and good processability.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to an aluminum fluoride-based ceramic neutron moderating material and a preparation method thereof.
Background
According to the boron neutron capture cancer treatment device driven by the accelerator, accelerated protons (5 MeV-30 MeV) bombard a lithium target or a beryllium target to generate neutrons, and the neutrons are decelerated by a moderator to obtain thermal neutrons. The thermal neutrons are absorbed by boron-containing drugs in the tumor cells, and the boron atomic nucleus releases charged ions after absorbing the neutrons so as to kill cancer cells and realize accurate radiotherapy at a cellular level. In the whole process, the generation of thermal neutrons with high enough flux is a very important link. The ceramic sintered by using LiF \ Al \ AlF3 mixed powder can meet the requirement and provide enough thermal neutrons for cancer treatment, and how to provide an aluminum fluoride-based ceramic neutron moderating material and a preparation method thereof are the problems to be solved by the inventor.
Disclosure of Invention
In view of the shortcomings of the prior art, the main object of the present invention is to provide ….
In order to achieve the purpose, the invention provides the following technical scheme: the aluminum fluoride-based ceramic neutron moderating material comprises the following components in percentage by mass: 0.5-5% of LiF, 15-40% of Al and 345-75% of AlF, and the particle sizes of LiF, Al and AlF3 powder are all less than 2.5 mu m.
A preparation method of an aluminum fluoride-based ceramic neutron moderating material comprises the following steps:
a. mixing LiF, Al and AlF3 powder uniformly according to a proportion, putting the mixture into a molybdenum kettle for hot pressing, and placing the molybdenum kettle in a graphite mold;
b. slowly heating and pressurizing the graphite mould at 100-200 ℃ for 2-4 h to ensure the release of gas in the powder and ensure the drying of the powder;
c. gradually increasing the pressure and the temperature when the gas is completely released;
d. sintering at constant temperature and constant pressure for 8-12 hours under the conditions that the temperature is stabilized at 600-700 ℃ and the pressure is 30-40 Mpa;
e. standing for 10-20 h after constant-temperature and constant-pressure sintering is finished, and forming the aluminum fluoride-based ceramic neutron moderating material;
f. cutting the aluminum fluoride-based ceramic neutron moderating material formed in the step e into moderating bodies by using a linear cutting or water-cooling cutting process;
g. and sleeving the aluminum alloy sleeve into the cut slowing-down body.
Preferably, in the step c, the temperature and pressure increase curve is one of linear, step-like and S-like or a combination of any two of the above.
Preferably, in the step d, the temperature during constant-temperature and constant-pressure sintering is 655 ℃, the pressure is 34Mpa, and the sintering time is 10 hours.
Preferably, in the step e, the standing time is 15 h.
Preferably, in the step f, when water cooling cutting is used, the moderator needs to be vacuumized and dried, and the temperature is not increased to 100 ℃ in the drying process, and the drying time is 24 hours.
Compared with the prior art, the invention has the advantages of high density, high hardness and good processing performance of the moderator. LiF, Al and AlF3 are used in a powder formula, a graphite die is used in hot pressing production, and a layer of molybdenum kettle is used for isolating the graphite die from powder needing hot pressing, so that carbon atoms in graphite are prevented from diffusing into ceramic at high temperature and high pressure. The heating and pressurizing are preferably S-shaped curves, and the heating and pressurizing are slowly performed firstly, so that the release of gas in the powder is ensured, and the drying of the powder is ensured. The purpose is to exhaust air and dry firstly, and then ensure the diffusion fully at constant temperature and constant pressure. Heating and pressurizing for about 10 hr, stabilizing at 655 deg.C and 34MPa, standing for 15 hr, and pressing to obtain the final product with density higher than 2.3g/cm 3. Need cooling when using water-cooling cutting process, use water-cooling, but because water infiltration effect, need evacuation drying behind the water-cooling, ensure that the inside absorbed moisture can volatilize, the drying process can suitably be warmed up to no more than 100 ℃. Vacuum drying for 24 hr. If the ceramic is wrapped by the shell, the aluminum alloy material is used and is as thin as possible, so that the influence on neutron performance is minimized. The invention can be used for neutron moderation of boron neutron capture therapy devices (BNCT) to generate an optimal thermal neutron energy spectrum.
Drawings
FIG. 1 is a first graph of the present invention;
FIG. 2 is a second graph of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in fig. 1, the aluminum fluoride-based ceramic neutron moderating material comprises the following components in percentage by mass: 0.5-5% of LiF, 15-40% of Al and 345-75% of AlF, and the particle sizes of LiF, Al and AlF3 powder are all less than 2.5 mu m.
A preparation method of an aluminum fluoride-based ceramic neutron moderating material comprises the following steps:
a. mixing LiF, Al and AlF3 powder uniformly according to a proportion, putting the mixture into a molybdenum kettle for hot pressing, and placing the molybdenum kettle in a graphite mold;
b. slowly heating and pressurizing the graphite mould at 100-200 ℃ for 2-4 h to ensure the release of gas in the powder and ensure the drying of the powder;
c. gradually increasing the pressure and the temperature when the gas is completely released;
d. sintering at constant temperature and constant pressure for 8-12 hours under the conditions that the temperature is stabilized at 600-700 ℃ and the pressure is 30-40 Mpa;
e. standing for 10-20 h after constant-temperature and constant-pressure sintering is finished, and forming the aluminum fluoride-based ceramic neutron moderating material;
f. cutting the aluminum fluoride-based ceramic neutron moderating material formed in the step e into moderating bodies by using a linear cutting or water-cooling cutting process;
g. and sleeving the aluminum alloy sleeve into the cut slowing-down body.
Preferably, in the step c, the temperature and pressure increase curve is one of linear, step-like and S-like or a combination of any two of the above.
Preferably, in the step d, the temperature during constant-temperature and constant-pressure sintering is 655 ℃, the pressure is 34Mpa, and the sintering time is 10 hours. Sintering for 10 hours at constant temperature and constant pressure. If the sintering time is too short, the crystal bond is not tightly bonded, the hardness of the ceramic is not high enough, and ash falling may occur. Sufficient diffusion and bonding is generally ensured over 5 hours, and the increase in pressure makes up for the lack of time.
Referring to fig. 1 and 2, the graph of the present invention shows an example of the heating and pressurizing curves, wherein the curve with a higher node density is a pressure curve, the curve with a lower node density is a temperature curve, the temperature curve in fig. 1 is linear, the pressure curve is S-shaped, the temperature curve in fig. 2 is step-shaped, and the pressure curve is S-shaped.
Preferably, in the step e, the standing time is 15 h.
Preferably, in the step f, when water cooling cutting is used, the moderator needs to be vacuumized and dried, and the temperature is not increased to 100 ℃ in the drying process, and the drying time is 24 hours.
The aluminum fluoride-based ceramic neutron moderating material and the preparation method thereof can ensure that the moderating body has high density, high hardness and good processing performance. LiF, Al and AlF3 are used in a powder formula, a graphite die is used in hot pressing production, and a layer of molybdenum kettle is used for isolating the graphite die from powder needing hot pressing, so that carbon atoms in graphite are prevented from diffusing into ceramic at high temperature and high pressure. The heating and pressurizing are preferably S-shaped curves, and the heating and pressurizing are slowly performed firstly, so that the release of gas in the powder is ensured, and the drying of the powder is ensured. The purpose is to exhaust air and dry firstly, and then ensure the diffusion fully at constant temperature and constant pressure. Heating and pressurizing for about 10 hr, stabilizing at 655 deg.C and 34MPa, standing for 15 hr, and pressing to obtain the final product with density higher than 2.3g/cm 3. Need cooling when using water-cooling cutting process, use water-cooling, but because water infiltration effect, need evacuation drying behind the water-cooling, ensure that the inside absorbed moisture can volatilize, the drying process can suitably be warmed up to no more than 100 ℃. Vacuum drying for 24 hr. If the ceramic is wrapped by the shell, the aluminum alloy material is used and is as thin as possible, so that the influence on neutron performance is minimized. The invention can be used for neutron moderation of boron neutron capture therapy devices (BNCT) to generate an optimal thermal neutron energy spectrum.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (6)
1. The aluminum fluoride-based ceramic neutron moderating material is characterized by comprising the following components in percentage by mass: 0.5-5% of LiF, 15-40% of Al and AlF3 45-75%, and the particle sizes of LiF, Al and AlF3 powder are all less than2.5μm。
2. A preparation method of an aluminum fluoride-based ceramic neutron moderating material is characterized by comprising the following steps:
a. LiF, Al and AlF3Uniformly mixing the powder according to a proportion, putting the powder into a molybdenum kettle for hot pressing, and placing the molybdenum kettle in a graphite mold;
b. slowly heating and pressurizing the graphite mould at 100-200 ℃ for 2-4 h to ensure the release of gas in the powder and ensure the drying of the powder;
c. gradually increasing the pressure and the temperature when the gas is completely released;
d. sintering at constant temperature and constant pressure for 8-12 hours under the conditions that the temperature is stabilized at 600-700 ℃ and the pressure is 30-40 Mpa;
e. standing for 10-20 h after constant-temperature and constant-pressure sintering is finished, and forming the aluminum fluoride-based ceramic neutron moderating material;
f. cutting the aluminum fluoride-based ceramic neutron moderating material formed in the step e into moderating bodies by using a linear cutting or water-cooling cutting process;
g. and sleeving the aluminum alloy sleeve into the cut slowing-down body.
3. The method of claim 2, wherein the method comprises: in the step c, the increasing curves of the temperature and the pressure are one of linear, step-like and S-like or a combination of any two of the above.
4. The method of claim 2, wherein the method comprises: in the step d, the temperature is 655 ℃ and the pressure is 34Mpa when constant temperature and pressure sintering is carried out, and the sintering time is 10 h.
5. The method of claim 2, wherein the method comprises: and in the step e, the standing time is 15 h.
6. The method of claim 2, wherein the method comprises: in the step f, when water cooling cutting is used, vacuumizing and drying are needed for the moderator, the temperature is not higher than 100 ℃ in the drying process, and the drying time is 24 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897526A (en) * | 2021-09-26 | 2022-01-07 | 散裂中子源科学中心 | Neutron deceleration composite material |
| CN116375473A (en) * | 2023-03-30 | 2023-07-04 | 山东亚赛陶瓷科技有限公司 | Magnesium fluoride-based composite neutron moderating material and preparation method thereof |
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2021
- 2021-04-28 CN CN202110463782.2A patent/CN113186440A/en active Pending
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| CN116375473A (en) * | 2023-03-30 | 2023-07-04 | 山东亚赛陶瓷科技有限公司 | Magnesium fluoride-based composite neutron moderating material and preparation method thereof |
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