CN103754877A - Manufacturing method of boron carbide neutron absorber - Google Patents
Manufacturing method of boron carbide neutron absorber Download PDFInfo
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- CN103754877A CN103754877A CN201310545859.6A CN201310545859A CN103754877A CN 103754877 A CN103754877 A CN 103754877A CN 201310545859 A CN201310545859 A CN 201310545859A CN 103754877 A CN103754877 A CN 103754877A
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- norbide
- carbon nanotube
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention discloses a manufacturing method of a boron carbide neutron absorber. The method includes the preparation of boron carbide, and the preparation of boron carbide comprises the following steps: (1) the purification and dispersion of carbon nanotubes; (2) preparation of raw materials for synthesis; (3) chemical reactions and heat treatment of raw materials; (4) super high pressure synthesis; and (5) residual stress elimination. According to the method, the neutron absorber with good thermal stability and chemical properties can be prepared.
Description
Technical field
The present invention relates to a kind of manufacture method of neutron-absorbing material.
Background technology
Norbide (boron carbide), has another name called boron carbide, and molecular formula is B
4c, is generally dark gray powder.Norbide is commonly called as man-made diamond, its relative density 2.52, and 2350 ℃ of fusing points, 3500 ℃ of boiling point >, microhardness >=3500kgf/mm2, bending strength >=400Mpa, is a kind of very boride of high rigidity that has.With acid, alkaline solution Fails To Respond, easily manufacture and price are relatively cheap.Be widely used in grinding, grinding, boring and the polishing of mechanically resistant material, the manufacture of metal boride and smelting boron sodium, boron alloy and special welding etc.Norbide has high chemical potential, neutron-absorbing, wear-resisting and semi-conductor electroconductibility.Be one of material the most stable to acid, in all dense or rare acid or alkali aqueous solution, all stablize.
Because norbide can absorb a large amount of neutrons, can not form any radio isotope, therefore it in nuclear energy power generation field, he is very desirable neutron-absorbing material, and neutron-absorbing material be mainly control caryocinetic speed.Norbide is mainly to make controllable bar-shapedly in nuclear reaction stove field, but can it be made Powdered because of increasing surface-area sometimes.The boron carbide material that how to synthesize excellent performance is that those skilled in the art endeavour the problem solving always.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of neutron-absorbing material, and it has good thermostability and chemical property.
In order to solve the problems of the technologies described above, the manufacture method of norbide neutron-absorbing material provided by the invention comprises prepares norbide, wherein prepares norbide and comprises the steps:
(1) purifying of carbon nanotube and dispersion treatment:
The carbon nanotube of many walls or single wall adopts acetone soaking and washing, and purifying process, as ordinary method, is then positioned over carbon nanotube in mixing solutions and carries out ultra-sonic oscillation dispersion, finally puts into drying in oven;
(2) synthesis material is prepared:
Synthesis material formula: the carbon nanotube after massfraction 0.5～5% disperses, the boron oxide of its twice as high molar ratio, caking agent is 18～22%, surplus is the diadust of particle size range 5 μ m～20 μ m, hard alloy substrate; Before using, diadust carries out surface cleaning processing and pre-greying, and hard alloy substrate and caking agent carry out surface cleaning processing; Other subsidiary material that use carry out corresponding clean; Pyrophyllite block, agalmatolite ring before assembling must be removed moisture; By diadust, caking agent, carbon nanotube and boron oxide compound, first use dehydrated alcohol wet mixing, after oven dry, be dry mixed and make mixing raw material;
(3) chemical reaction of raw material and thermal treatment:
It is 800～900 ℃ that mixing raw material is heated to temperature, and the time is 0.5～1.5h; Then reacted raw material is placed on to temperature and is in the baking oven of 80～100 ℃ and save backup;
(4) ultra-high voltage is synthetic:
To synthesize piece and be positioned in pyrophyllite block mould, at additional agalmatolite ring, conducting steel ring and the catalyst sheet loaded onto of mould, in six-plane piercer, carry out high pressure high temperature compound experiment; Synthesis technologic parameter is: 1450～1600 ℃ of sintering temperatures, and sintering pressure 5～6GPa, the heat-insulation pressure keeping time is 3～5 minutes;
(5) unrelieved stress is eliminated:
After synthesizing, product carries out vacuum aging annealing.
Described mixing solutions is in 200ml dehydrated alcohol+0.1～1.0g sodium lauryl sulphate mixing solutions.
Described six-plane piercer is hinge type six-plane piercer, the synthetic middle liquid phase pressure transmission mode that adopts.
The surface cleaning processing of described hard alloy substrate and caking agent refers to: first in connection with surface, carry out sanding and polishing processing, erase zone of oxidation and the hole of mating surface, until expose unsalted surface, then deoil, washing, ultrasonic cleaning, infrared drying, finally pack in clean vessel standby.
Described caking agent is cobalt sheet and titanium sheet.
The present invention, by above-mentioned manufacture method, has prepared a kind of norbide with good thermal stability and chemical property, and then the neutron-absorbing material of processability excellence.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
The preparation method who is used to form the norbide of neutron-absorbing material comprises the steps:
(1) purifying of carbon nanotube and dispersion treatment
The carbon nanotube of many walls or single wall adopts acetone soaking and washing, purifying process is as ordinary method, then carbon nanotube is positioned in 200ml dehydrated alcohol+0.5g sodium lauryl sulphate mixing solutions, carries out ultra-sonic oscillation dispersion, finally put into drying in oven;
(2) synthesis material is prepared
Synthesis material formula: the carbon nanotube after massfraction 0.5% disperses, the boron oxide of its twice as high molar ratio, the diadust of particle size range 5～10 μ m, caking agent is 22%, hard alloy substrate; Before using, diadust must carry out surface cleaning processing and pre-greying, hard alloy substrate, cobalt sheet, titanium sheet raw and auxiliary material, first in connection with surface, carry out sanding and polishing processing, erase zone of oxidation and the hole of mating surface, until expose unsalted surface, then deoil, washing, ultrasonic cleaning, infrared drying, finally pack in clean vessel standby; Other subsidiary material that use also should carry out corresponding clean; Pyrophyllite block, agalmatolite ring before assembling must first carry out calcination process, to remove the moisture in agalmatolite; By diadust, caking agent, carbon nanotube and boron oxide compound, first use dehydrated alcohol wet mixing, after oven dry, be dry mixed, preserve mixing raw material;
(3) chemical reaction of raw material and thermal treatment
It is 850 ℃ that mixing raw material is heated to temperature, and time 1.5h, is then placed on reacted raw material in baking oven and saves backup, and oven temperature is 80 ℃;
(4) ultra-high voltage is synthetic
To synthesize piece and be positioned over by pyrophyllite block mould, at additional agalmatolite ring, conducting steel ring and the catalyst sheet loaded onto of mould, in hinge type six-plane piercer, carry out high pressure high temperature compound experiment; In synthetic, adopt liquid phase pressure transmission mode, synthesis technologic parameter is: 1600 degrees Celsius of sintering temperatures, and sintering pressure 5GPa, the heat-insulation pressure keeping time is 3 minutes;
(5) unrelieved stress is eliminated
After synthesizing, product carries out vacuum aging annealing.
Sample effect: the wear resistance ratio that utilizes grinding silicon carbide grinding wheel method to measure norbide is about 2.70461 × 105; Utilize the toughness of tension weight churning method test, single strike work 1.4J, sample average number of shocks is 13 times.
Embodiment 2:
The preparation method who is used to form the norbide of neutron-absorbing material comprises the steps:
(1) purifying of carbon nanotube and dispersion treatment
The carbon nanotube of many walls or single wall adopts acetone soaking and washing, purifying process is as ordinary method, then carbon nanotube is positioned in 200ml dehydrated alcohol+0.1g sodium lauryl sulphate mixing solutions, carries out ultra-sonic oscillation dispersion, finally put into drying in oven;
(2) synthesis material is prepared
Synthesis material formula: the carbon nanotube after massfraction 1% disperses, the boron oxide of its twice as high molar ratio, the diadust of particle size range 15～20 μ m, caking agent is 20%, hard alloy substrate; Before using, diadust must carry out surface cleaning processing and pre-greying, hard alloy substrate, cobalt sheet, titanium sheet raw and auxiliary material, first in connection with surface, carry out sanding and polishing processing, erase zone of oxidation and the hole of mating surface, until expose unsalted surface, then deoil, washing, ultrasonic cleaning, infrared drying, finally pack in clean vessel standby; Other subsidiary material that use also should carry out corresponding clean; Pyrophyllite block, agalmatolite ring before assembling must first carry out calcination process, to remove the moisture in agalmatolite; By diadust, caking agent, carbon nanotube and boron oxide compound, first use dehydrated alcohol wet mixing, after oven dry, be dry mixed, preserve mixing raw material;
(3) chemical reaction of raw material and thermal treatment
It is 800～900 ℃ that mixing raw material is heated to temperature, and time 1h, is then placed on reacted raw material in baking oven and saves backup, and oven temperature is 90 ℃;
(4) ultra-high voltage is synthetic
To synthesize piece and be positioned over by pyrophyllite block mould, at additional agalmatolite ring, conducting steel ring and the catalyst sheet loaded onto of mould, in hinge type six-plane piercer, carry out high pressure high temperature compound experiment; In synthetic, adopt liquid phase pressure transmission mode, synthesis technologic parameter is: 1500 ℃ of sintering temperatures, and sintering pressure 5.5GPa, the heat-insulation pressure keeping time is 5 minutes;
(5) unrelieved stress is eliminated
After synthesizing, product carries out vacuum aging annealing.
Sample effect: the wear resistance ratio that utilizes grinding silicon carbide grinding wheel method to measure norbide is about 2.70461 × 105; Utilize the toughness of tension weight churning method test, single strike work 1.4J, sample average number of shocks is 14 times.
Embodiment 3:
The preparation method who is used to form the norbide of neutron-absorbing material comprises the steps:
(1) purifying of carbon nanotube and dispersion treatment
The carbon nanotube of many walls or single wall adopts acetone soaking and washing, purifying process is as ordinary method, then carbon nanotube is positioned in 200ml dehydrated alcohol+1.0g sodium lauryl sulphate mixing solutions, carries out ultra-sonic oscillation dispersion, finally put into drying in oven;
(2) synthesis material is prepared
Synthesis material formula: the carbon nanotube after massfraction 5% disperses, the boron oxide of its twice as high molar ratio, the diadust of particle size range 10～20 μ m, caking agent is 18%, hard alloy substrate; Before using, diadust must carry out surface cleaning processing and pre-greying, hard alloy substrate, cobalt sheet, titanium sheet raw and auxiliary material, first in connection with surface, carry out sanding and polishing processing, erase zone of oxidation and the hole of mating surface, until expose unsalted surface, then deoil, washing, ultrasonic cleaning, infrared drying, finally pack in clean vessel standby; Other subsidiary material that use also should carry out corresponding clean; Pyrophyllite block, agalmatolite ring before assembling must first carry out calcination process, to remove the moisture in agalmatolite; By diadust, caking agent, carbon nanotube and boron oxide compound, first use dehydrated alcohol wet mixing, after oven dry, be dry mixed, preserve mixing raw material;
(3) chemical reaction of raw material and thermal treatment
Mixing raw material is heated to 620～680 ℃, and 0.5h, is then placed on reacted raw material in baking oven and saves backup, and oven temperature is 100 ℃;
(4) ultra-high voltage is synthetic
To synthesize piece and be positioned over by pyrophyllite block mould, at additional agalmatolite ring, conducting steel ring and the catalyst sheet loaded onto of mould, in hinge type six-plane piercer, carry out high pressure high temperature compound experiment; In synthetic, adopt liquid phase pressure transmission mode, synthesis technologic parameter is: 1550 ℃ of sintering temperatures, and sintering pressure 6GPa, the heat-insulation pressure keeping time is 4 minutes;
(5) unrelieved stress is eliminated
After synthesizing, product carries out vacuum aging annealing.
Sample effect: the wear resistance ratio that utilizes grinding silicon carbide grinding wheel method to measure norbide is about 2.70461 × 105; Utilize the toughness of tension weight churning method test, single strike work 1.4J, average number of shocks is 34 times.
Certainly; the present invention also can have other various embodiments; in the situation that not deviating from spirit of the present invention and essence thereof; those of ordinary skill in the art are when making according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (5)
1. a manufacture method for norbide neutron-absorbing material, comprises and prepares norbide, it is characterized in that, prepares norbide and comprises the steps:
(1) purifying of carbon nanotube and dispersion treatment:
The carbon nanotube of many walls or single wall adopts acetone soaking and washing, and purifying process, as ordinary method, is then positioned over carbon nanotube in mixing solutions and carries out ultra-sonic oscillation dispersion, finally puts into drying in oven;
(2) synthesis material is prepared:
Synthesis material formula: the carbon nanotube after massfraction 0.5～5% disperses, the boron oxide of its twice as high molar ratio, caking agent is 18～22%, surplus is the diadust of particle size range 5 μ m～20 μ m, hard alloy substrate; Before using, diadust carries out surface cleaning processing and pre-greying, and hard alloy substrate and caking agent carry out surface cleaning processing; Other subsidiary material that use carry out corresponding clean; Pyrophyllite block, agalmatolite ring before assembling must be removed moisture; By diadust, caking agent, carbon nanotube and boron oxide compound, first use dehydrated alcohol wet mixing, after oven dry, be dry mixed and make mixing raw material;
(3) chemical reaction of raw material and thermal treatment:
It is 850 ℃ that mixing raw material is heated to temperature, and the time is 1.5h; Then reacted raw material is placed on to temperature and is in the baking oven of 80～100 ℃ and save backup;
(4) ultra-high voltage is synthetic:
To synthesize piece and be positioned in pyrophyllite block mould, at additional agalmatolite ring, conducting steel ring and the catalyst sheet loaded onto of mould, in six-plane piercer, carry out high pressure high temperature compound experiment; Synthesis technologic parameter is: 1600 ℃ of sintering temperatures, and sintering pressure 5～6GPa, the heat-insulation pressure keeping time is 3～5 minutes;
(5) unrelieved stress is eliminated:
After synthesizing, product carries out vacuum aging annealing.
2. the manufacture method of norbide neutron-absorbing material according to claim 1, is characterized in that: described mixing solutions is in 200ml dehydrated alcohol+0.1～1.0g sodium lauryl sulphate mixing solutions.
3. the manufacture method of norbide neutron-absorbing material according to claim 1, is characterized in that: described six-plane piercer is hinge type six-plane piercer, the synthetic middle liquid phase pressure transmission mode that adopts.
4. the manufacture method of norbide neutron-absorbing material according to claim 1 and 2, it is characterized in that: the surface cleaning processing of described hard alloy substrate and caking agent refers to: first in connection with surface, carry out sanding and polishing processing, erase zone of oxidation and the hole of mating surface, until expose unsalted surface, then deoil, washing, ultrasonic cleaning, infrared drying, finally pack in clean vessel standby.
5. the manufacture method of norbide neutron-absorbing material according to claim 1, is characterized in that: described caking agent is cobalt sheet and titanium sheet.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103956192A (en) * | 2014-05-07 | 2014-07-30 | 镇江市纽科利核能新材料科技有限公司 | Novel high-density neutron absorption plate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717682A (en) * | 2009-11-20 | 2010-06-02 | 河北理工大学 | Solid lubricating composite material and manufacturing method thereof |
| CN101891214A (en) * | 2010-07-13 | 2010-11-24 | 北京科技大学 | Preparation method for synthesizing boron carbide powder at low temperature |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717682A (en) * | 2009-11-20 | 2010-06-02 | 河北理工大学 | Solid lubricating composite material and manufacturing method thereof |
| CN101891214A (en) * | 2010-07-13 | 2010-11-24 | 北京科技大学 | Preparation method for synthesizing boron carbide powder at low temperature |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103956192A (en) * | 2014-05-07 | 2014-07-30 | 镇江市纽科利核能新材料科技有限公司 | Novel high-density neutron absorption plate |
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Application publication date: 20140430 |