CN111470865B - Isotope of carbon monoxide10Sintering method of B material - Google Patents

Isotope of carbon monoxide10Sintering method of B material Download PDF

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CN111470865B
CN111470865B CN202010285703.9A CN202010285703A CN111470865B CN 111470865 B CN111470865 B CN 111470865B CN 202010285703 A CN202010285703 A CN 202010285703A CN 111470865 B CN111470865 B CN 111470865B
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column
sintering
filament
sintered
isotope
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CN111470865A (en
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樊启文
孟波
王�华
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China Institute of Atomic of Energy
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/421—Boron
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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Abstract

The invention belongs to the technical field of isotope target material preparation,discloses an isotope10And B, sintering the material. The method is that10Pressing the B material into carbon crucible, bombarding with intermittent electrostatic focusing and fine tuning electron bombardment under vacuum condition10B material, obtained after sintering10B. The method has the advantages of small single input amount, low loss and stable and reliable process.

Description

Isotope of carbon monoxide10Sintering method of B material
Technical Field
The invention belongs to the technical field of isotope target preparation, and particularly relates to an isotope10And B, sintering the material.
Background
10B is commonly used in nuclear reactors due to its large neutron absorption cross section10B as a protector, control rod, etc. in10B(n,α)7Detectors for Li reaction need to be used10The B film is used as a detection medium, so the B film is widely applied to the fields of nuclear engineering and nuclear physics.
High enrichment isotope10B (abundance over 90%) is a controlled nuclear material, expensive and extremely difficult to purchase. Currently, it is only available from a very small number of countries10B, powdery material. In order to meet the requirements of nuclear physics experiments, the powder is required to be prepared10The B material is firstly sintered into blocks and then the nucleation target material is prepared. Due to the fact that10B has a high melting point (about 2075 ℃), poor viscosity, and poor heat transfer, and it is difficult to evaporate, distill, or melt and condense it using high temperature distillation or resistance heating techniques. At the same time due to10B is high in price and small in amount (usually, hundreds of milligrams to several grams are purchased commercially), and sintering cannot be carried out by adopting an industrial high-temperature sintering method (the single-time input amount of industrial sintering is large). Therefore, there is a high necessity for a melting point alloy which is sufficiently small10And B, sintering the material.
Disclosure of Invention
Objects of the invention
According to the problems existing in the prior art, the invention provides a sintering method which has the advantages of small single input amount, small loss and stable and reliable process10And (B) a process.
(II) technical scheme
In order to solve the problems in the prior art, the technical scheme provided by the invention is as follows:
sintered isotope10The key point of the method of the B material is that the method is to mix10Pressing B material, setting in carbon crucible with boron nitride lining, and bombarding in vacuum condition by intermittent electrostatic focusing and fine tuning electron bombardment10B material, obtained after sintering10B。
Preferably, the sintering isotope10A method of B material, the method comprising the steps of:
(1) mixing the powdered isotope10Pressing the material B into the product by a press10A column B;
(2) the column shape obtained in the step (1) is10B, placing the carbon crucible into an intermittent electrostatic focusing electron bombardment device, wherein the inner surface of the carbon crucible is provided with a boron nitride lining;
(3) vacuumizing an intermittent electrostatic focusing electron bombardment device, starting an electron gun, and gradually increasing the high voltage; the focusing point of the electron beam is focused on from top to bottom10On column B, the temperature is conducted from top to bottom and rises to approach10Melting point of B, melting, sintering10A column B;
(4) gradually reducing the high pressure until the mixture is completely cooled to obtain sintered10And B, block.
Preferably, the pressure increase in step (3) is maintained for 20min per 200V increase.
Preferably, the step (4) is reduced in pressure in a manner of maintaining for 5min every 100V reduction.
Preferably, the filament of the electron gun in the intermittent electrostatic focusing electron bombardment device is a circular tungsten filament fixed on the filament10Top end of B column, distance10The top end of the B column is 10.5-11 mm; the tungsten filament is of a structure capable of moving up and down, and an electron beam is firstly focused on10Top surface of B pillar from10Sintering the top of the B column to the middle part gradually, and then sintering10The residual part of the column B is inversely sintered, and the plane of the filament of the electron gun is always kept10The top end of the B column is 10.5-11 mm.
Preferably, the filament of the electron gun in the intermittent electrostatic focusing electron bombardment device is a circular tungsten filament which is of a movable structure and can move up and down, move left and right and deflect at a small angle, so that the electron beam can be focused on10The top surface, the middle side surface and the bottom end side surface of the B column.
Preferably, the plane distance of the circular tungsten wire10The distance of the B column is kept between 10.5 and 11mm all the time.
Preferably, the sintering time in the step (3) is 1-2 hours.
Preferably, the10The diameter of the column B is 4-12 mm, and the height is 2-10 mm.
Preferably, the tungsten wire has a diameter of 0.2 mm.
(III) advantageous effects
The isotope provided by the invention is adopted10The sintering method of the material B is sintering in a batch type electrostatic focusing electron bombardment device10B material, after sintering10The column B does not collapse and does not crack, thereby facilitating the subsequent further target making operation. The concrete effects are as follows:
□ the method avoids the need for pressurizing the electron gun in a gradient manner for 20min every 200V rise10B, the vacuum performance in the equipment is deteriorated due to rapid heating and exhausting; at the same time due to10The material B has poor heat conductivity, and the pressurizing mode provided by the application is adopted, so that the phenomenon caused by rapid heating is well avoided10The local temperature of the B column is too high to cause cracking.
Top to bottom slow bombardment of filament10B column, avoiding first bombardment10Brought from the middle or bottom of the B-pillar10B collapse problem.
③ distance between ring-shaped tungsten filament of electron gun10The distance between the B column and the B column is 10.5-11 mm, which is of great importance, the problem of overheating of an electron gun flange caused by overlarge power of a high-voltage power supply due to overlarge distance is avoided, and the phenomenon that the focusing position of an electron beam is not at the position caused by the overlarge distance is also avoided10Top problems with B-pillars.
Fourthly, in the voltage reduction process, the voltage is not directly reduced to 0, and the situation that the voltage is reduced to 0 is avoided10The problem of the dry cracking of the B column.
Detailed Description
The present application will be further described with reference to specific examples.
Example 1
Sintered isotope10A method of preparing B material by reacting10Pressing B material, setting in carbon crucible with boron nitride lining, and bombarding in vacuum condition by intermittent electrostatic focusing and fine tuning electron bombardment10B material, obtaining a firedAfter knotting10B. The method comprises the following steps:
(1) mixing the powdered isotope10Pressing the material B into a column shape by a pressing machine10B；
(2) The column shape obtained in the step (1) is10B, placing the carbon crucible into an intermittent electrostatic focusing electron bombardment device, wherein a boron nitride lining is arranged in the carbon crucible;
(3) vacuumizing an intermittent electrostatic focusing electron bombardment device, starting an electron gun, and gradually increasing the high voltage; the focusing point of the electron beam is focused on the column from top to bottom10On column B, the temperature is conducted from top to bottom and rises to approach10Melting point of B, melting, sintering10B；
(4) Gradually reducing the high pressure until the mixture is completely cooled to obtain sintered10And B, block.
Example 2
In contrast to example 1, the method comprises the following steps:
(1) mixing the powdered isotope10Pressing the material B into a column shape by a pressing machine10B; the above-mentioned10The column B had a diameter of 8mm and a height of 7 mm.
(2) The column shape obtained in the step (1) is10B, placing the carbon crucible into an intermittent electrostatic focusing electron bombardment device, wherein a boron nitride lining is arranged in the carbon crucible;
(3) vacuumizing the intermittent electrostatic focusing electron bombardment equipment, starting an electron gun, gradually increasing the high voltage, and keeping the high voltage for 20min every 200V;
the filament of the electron gun is a circular tungsten filament and is of a structure capable of moving up and down. Firstly, the position and the plane distance of the filament of the electron gun are adjusted10The distance between the top ends of the B columns is 10.5-11 mm, so that the focusing point of the electron beam is focused on10On the top of the B column, the temperature is conducted from top to bottom and rises to near10Melting point of B to locally melt and sinter the upper part10B; then taking out10Turning the column B, putting it into carbon crucible again, and adjusting the position of the filament of the electron gun downward to make the plane of the filament and the plane of the filament10The top end of the B column is always kept at a distance of 10.5-11 mm to finish the other halfIn part10And (5) sintering the B column. The maximum current and voltage were 51mA and 1.56kV, respectively.
(4) After sintering, the high pressure is gradually reduced in a way of keeping for 5min every 100V reduction. Until completely cooled, to obtain sintered10And B, block.
Example 3
In contrast to example 1, the method comprises the following steps:
(1) mixing the powdered isotope10Pressing the material B into the product by a press10A column B; the above-mentioned10The column of B had a diameter of 5mm and a height of 5 mm.
(2) Subjecting the product obtained in step (1)10The B column is placed in a carbon crucible of intermittent electrostatic focusing electron bombardment equipment, and a boron nitride lining is arranged in the carbon crucible;
(3) vacuumizing the intermittent electrostatic focusing electron bombardment equipment, starting an electron gun, gradually increasing the high voltage, and keeping the high voltage for 20min every 200V;
the filament of the electron gun is a circular tungsten filament which is of a movable structure and can move up and down, move left and right and deflect at a small angle, so that an electron beam can be focused on10The top surface, the middle side surface and the bottom end side surface of the B column. Firstly, the position of the filament of the electron gun is adjusted to focus the focus point of the electron beam on10On the top of the B column, the temperature is conducted from top to bottom and rises to near10Melting point of B, melting, sintering10B; the maximum current and voltage were 42mA and 1.36kV, respectively.
(4) After sintering, the high pressure is gradually reduced in a way of keeping for 5min every 100V reduction.
Example 4
Unlike example 2, the tungsten wire had a diameter of 0.2 mm. The above-mentioned10The diameter of the B column was 10mm, and the maximum current and voltage were 54mA and 1.8kV, respectively.
Example 5
In contrast to example 3, the process described10The diameter of the B column was 12mm, and the maximum current and voltage were 58mA and 2.0kV, respectively.

Claims (6)

1. Sintered isotope10A method of forming a B material, characterized in that the method comprises10Pressing the B material into carbon crucible, bombarding with intermittent electrostatic focusing and fine tuning electron bombardment under vacuum condition10B material, obtained after sintering10B; the method comprises the following steps:
(1) mixing the powdered isotope10Pressing the material B into the product by a press10A column B;
(2) the column shape obtained in the step (1) is10B, placing the carbon crucible into an intermittent electrostatic focusing electron bombardment device, wherein the inner surface of the carbon crucible is provided with a boron nitride lining;
(3) vacuumizing an intermittent electrostatic focusing electron bombardment device, starting an electron gun, and gradually increasing the high voltage; the focusing point of the electron beam is focused on from top to bottom10On column B, the temperature is conducted from top to bottom and rises to approach10Melting point of B, melting, sintering10A column B; the high pressure is increased in a gradient way, and the pressure is maintained for 20min every time the pressure is increased by 200V; the filament of the electron gun in the intermittent electrostatic focusing electron bombardment equipment is a circular tungsten filament, and the plane distance of the filament10The top end of the B column is 10.5-11 mm; the filament of the electron gun is of a structure capable of moving up and down, and the electron beam is focused on10Top surface of B pillar from10Sintering the top of the B column to the middle part gradually, and then sintering10The column B is inverted to sinter the rest part, and the plane of the electron gun filament is always kept10The top end of the B column is 10.5-11 mm in distance;
(4) gradually reducing the high pressure until the mixture is completely cooled to obtain sintered10And B, block.
2. Sintered isotope according to claim 110The method for preparing the material B is characterized in that the pressure reduction in the step (4) is carried out in a manner of keeping for 5min every 100V reduction.
3. Sintered isotope according to claim 110Method of B material, characterized in that electricity in the intermittent electrostatic focusing electron bombardment deviceThe sub-gun filament is a circular ring-shaped tungsten filament, is of a movable structure, can move up and down, move left and right and deflect at a small angle, so that an electron beam can be focused on10The top surface, the middle side surface and the bottom end side surface of the B column.
4. Sintered isotope according to claim 110The method for preparing the material B is characterized in that the sintering time in the step (3) is 1-2 hours.
5. Sintered isotope according to claim 110Method of preparing material B, characterized in that10The diameter of the column B is 4-12 mm, and the height is 2-10 mm.
6. Sintered isotope according to claim 110The method of the material B is characterized in that the diameter of the tungsten wire is 0.2 mm.
CN202010285703.9A 2020-04-13 2020-04-13 Isotope of carbon monoxide10Sintering method of B material Active CN111470865B (en)

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