CN106082230A - A kind of submicron carbonized boron powder and its production and use - Google Patents
A kind of submicron carbonized boron powder and its production and use Download PDFInfo
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- CN106082230A CN106082230A CN201610447716.5A CN201610447716A CN106082230A CN 106082230 A CN106082230 A CN 106082230A CN 201610447716 A CN201610447716 A CN 201610447716A CN 106082230 A CN106082230 A CN 106082230A
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C7/00—Control of nuclear reaction
- G21C7/06—Control of nuclear reaction by application of neutron-absorbing material, i.e. material with absorption cross-section very much in excess of reflection cross-section
- G21C7/24—Selection of substances for use as neutron-absorbing material
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
- C09K3/1418—Abrasive particles per se obtained by division of a mass agglomerated by sintering
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F41—WEAPONS
- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H5/00—Armour; Armour plates
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/06—Ceramics; Glasses; Refractories
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
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- G21F1/103—Dispersions in organic carriers
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses and a kind of improve production efficiency, reduce production cost and prepare high-purity, the essence submicron carbonized boron powder of granularity and preparation method and use thereof.Wherein the purity of boron carbide is 98.5%～99.4%, and mean diameter is 0.4 5 μm, and proportion is more than 90%, the method preparing this submicron carbonized boron powder: with raw material, tentatively mix；Adding abrasive media, batch mixing is uniform；Raw material separates with abrasive media；It is pressed into green compact；Base substrate enters reaction unit and carries out the synthetic reaction of self-propagating；Product is crushed；Grind, separate；Pickling purifies；Material filtering, wash, be dried；Airflow crash.The boron carbide powder of the method synthesis can apply in nuclear reactor, with neutron absorber material and radiation protection material；Armour material can be made through High Temperature High Pressure sintering；Can also be as the abrasive material of fine senior grinding and grinding agent.
Description
Technical field
The invention discloses a kind of compound and its production and use, it particularly relates to a kind of raising produces effect
Rate, reduce production cost and prepare high-purity, submicron carbonized boron powder and its production and use of essence granularity.
Background technology
At present, the preparation method of the boron carbide powder mentioned in scientific documents has electric arc furnace carbothermic method, carbon shirt-circuiting furnace carbon
Thermal reduction, intermediate frequency furnace carbothermic method, Sol-Gel method, vapour deposition process and magnesium reduction process etc., these distinct methods
Purity and the granularity of prepared material are different.Currently, domestic only it is capable of technology path prepared by boron carbide industrialization
Having carbothermic method, wherein the production capacity with electric arc furnace carbothermic method is the highest.But boron carbide technique is prepared in electric arc furnace carbon thermal reduction
Energy consumption is high, production environment is severe, and the grinding purifying technique that the boron carbide lump of synthesis is follow-up is complicated, finally prepares the granule of powder
Thick (micron order), purity are relatively low, seriously reduce the performance of boron carbide powder sintered article.Superfine boron carbide powder can show
Write and reduce densification sintering temperature, but boron carbide is that (its hardness is only second to diamond and cube nitridation to a kind of high hardness material
Boron), it is unpractical for obtaining fine silicon carbide boron powder only by the method for mechanical lapping, and submicron order to be obtained is even more
Fine boron carbide powder, the other technologies route beyond exploitation carbothermic method is just particularly important.At present, Sol-Gel
Method and vapour deposition process can synthesis nano boron carbide powder, but cost is high, production efficiency is low, and distance industrialization also has the biggest
Distance.
Summary of the invention
The present invention is that it is solved the technical problem that in order to overcome problem present on existing boron carbide powder synthetic technology
It is to provide a kind of high-purity, the submicron order boron carbide of essence granularity, with and its production and use.
To this end, the invention provides a kind of submicron carbonized boron powder, wherein the purity of boron carbide be 98.5%～
99.4%, mean diameter is 0.4-5 μm, and proportion is more than 90%.
Present invention also offers a kind of method preparing submicron carbonized boron powder, including the following step:
Step 1 is equipped with raw material and tentatively mixes, and the present invention is with B2O3, nanometer carbon black be boron source and carbon source, with magnesium metal for reduction
Agent, by diboron trioxide (B after drying and dewatering2O3), nanometer carbon black (C) and magnesium metal (Mg) powder be according to mass ratio B2O3: C:Mg=
(182-210): 12:(151-159) dispensing, i.e. B are carried out2O3Excess (30-50) %, Mg excess (5-10) %, the grain of three kinds of raw materials
Degree is respectively less than 50 μm, and purity is higher than 98.5%, and wherein, the granularity of nanometer carbon black is at below 80nm, and purity is more than 99.99%,
Raw material tentatively mixes in batch mixer；
Step 2 adds abrasive media, and batch mixing is uniform, the abrasive media that the present invention adds, abrasive media and the quality of raw material
Ratio is (1-1.5): 1, and material mixing is uniform；
Step 3 raw material separates with abrasive media, batch mixing uniformly after, use sub-sieve raw material and abrasive media to be carried out point
From, obtain mixed powder；
Step 4 pressure makes green compact, and mixed powder is poured into rustless steel base substrate mould, applies 5-10MPa pressure at forcing press
A diameter of columned green compact of Φ 50mm it are pressed under power；
Step 5 base substrate enters reaction unit and carries out the synthetic reaction of self-propagating, and base substrate puts into the graphite boat of boring semicircle, graphite
Boat is sent into self-propagating reaction room, then to reative cell evacuation, then is passed through the Ar gas shielded of flowing.Reative cell electric connection of power supply
The two poles of the earth, be provided with the high temperature resistant heating reaching more than 800 DEG C in both junctions, the other end of this heating is to reaction
Indoor extend to graphite boat, when energized, heat heating, when the heating wire of white heat is heated to uniform temperature to material
Time, ignite material, and graphite boat heat transfer maintains combustion wave, now power-off, and material relies on the reaction of combustion wave self-propagating synthesis；
Product is crushed by step 6, treats that whole material reaction terminates, naturally cools to room temperature, collecting reaction product, adopt
With jaw crusher, product is crushed to 5mm；
Step 7 is ground, is separated, and after using abrasive media that combustion product is ground to below 30-50 μm, employing sub-sieve will
Raw material separates with abrasive media；
Step 8 pickling purifies, and powder thing is loaded glass reaction container, adds 2-5mol/L hydrochloric acid solution, and glass is anti-
Answer container to seal, material is carried out pickling purification, material is constantly stirred by acid cleaning process, heats, thus metal
Magnesium reduction stabilisation in hydrochloric acid solution, pickling temperature maintains 80-120 DEG C, pickling time 10h, after tested, after pickling
Material particles reaches submicron order；
Step 9 material filtering, wash, be dried, acid-leached product is filtered, and after being washed with deionized, obtains filter cake, filter
Vacuum drying oven put into by cake dries, and drying temperature is 100 DEG C, and drying time 12h forms micron and the Asia of below 5 μm particle diameters
The material of micron particles.
As a preferred version of preparation method of the present invention, further comprising the steps of: airflow crash, after drying material
Crushing through Jet Mill, agglomerated particle is opened again, obtain purity be 99.4%, mean diameter be 0.4-1 μm
Submicron order boron carbide powder.
As the further improvement in said method, described batch mixing uniformity basis for estimation up to standard is not exist in material
Soft-agglomerated piece, naked eyes invisible white scatterplot, entirety presents uniform Lycoperdon polymorphum Vitt or grey black.
As the further improvement in said method, the flowing protection gas that described self-propagating reaction room is passed through is Ar gas.
As the further improvement in said method, described abrasive media is zirconia ball, and described zirconia ball is a diameter of
Φ10mm。
As the further improvement in said method, the addition of hydrochloric acid solution needs mistake on the basis of theoretical addition amount
Amount 25%, the basis of theoretical addition amount is the pure HCl that 1mol Mg element needs to consume 2mol.
As the further improvement in said method, batch mixer uses the drum mixer of ladle alumina liner, cylinder
Rotating speed is at least 25r/min, mixing time at least 2 hours.
As the further improvement in said method, described heating high temperature resistant need to reach more than 800 DEG C, described electric heating unit
Part is Aludirome silk.
Present invention also offers the submicron order boron carbide powder prepared according to the method described above, because its characteristic is in industry
In have a wide range of applications.
The beneficial aspects of the present invention:
The present invention has feature simple to operate, that production efficiency improves, energy consumption reduces and dust generation amount is few, prepared carbon
Change boron powder purity height, fine size and there is higher sintering activity.Boron carbide belongs to orthorhombic system, due to non-stoichiometric
In boron carbide, it is expected to there is higher vacancy concentration, and the nonequilibrium condition of structural vacancy can be with the transfer of activated diffusion material
Mechanism, improves boron and Carbon diffusion motility, causes lattice distortion, reduces and combines energy, diffusion bond energy, diffusion activation energy and position
Wrong Shipment dynamic resistance, therefore can make sintering process be activated.
The hot self-spread synthesizing method of magnesium is to utilize the heat-producing chemical reaction between raw material, by the burning that after igniting, self maintains
Process carrys out a kind of advanced technology of synthesizing submicron dusty material, it have production efficiency powder purity high, prepared high,
The feature that grain is fine.So, use magnesium hot self-propagating synthesis high-purity, the boron carbide powder of high granularity to have industry greatly and send out
Exhibition potentiality.
Submicron order boron carbide is dark gray powder, has the low (2.52g/cm of density3), hardness is high, fusing point high (2450
DEG C), heat conductivity is good, high abrasion resistance, the feature big to neutron absorption capability, and has higher force performance and excellent
Antioxidation and decay resistance.Due to its high rigidity, submicron order boron carbide and composite thereof can be used to manufacture grinding agent
And bulletproof armour.Utilizing the feature that its density is low and elevated temperature strength is high, submicron order boron carbide can be applied and lead with Aero-Space
Territory.In submicron order boron carbide10B has higher neutron absorption cross-section, as a kind of nuclear screening and control material, submicron
Level boron carbide is because its high-purity, essence granularity have wider application in nuclear reactor.
The submicron order boron carbide powder quality that this method prepares meets the core of regulation in China's standard GB/T 5151-85
First level flour (HTP-1) requires [10], has a wide range of applications in nuclear reactor.The boron carbide powder of the method synthesis is permissible
It is applied in nuclear reactor, with neutron absorber material and radiation protection material.Such as, use the enrichment 10B of the method synthesis rich
The B4C of degree may be used for preparing fast breeder reactor control rod pellet and shielding rod pellet；May be used for preparing neutron absorption ball,
It is applied to the Second shutdown system of HTGR；Especially, the B4C powder that prepared by the method can preparation compound with metallic aluminium
Spentnuclear fuel screen work neutron absorber material；Or compound with polyethylene, epoxy resin etc. prepare fuel container neutron shield material
Material.
The B4C powder that the method can also be used to synthesize makes armour material through High Temperature High Pressure sintering, as light-duty anti-
Play clothing and the ballistic armor materials of ground vehicle, armed helicopter and airline carriers of passengers.
Additionally, the boron carbide powder changing method synthesis can be as the abrasive material of fine senior grinding and grinding agent, it is possible to achieve
The polishing the brightest and the cleanest to wear-resistant surface of the work.
Accompanying drawing explanation
Fig. 1 is self-propagating reaction device schematic diagram of the present invention:
1-pressure regulator, 2-vacuum pump, 3-shielding window, 4-reactor chamber door, 5-air vent,
6-adds thermode, 7-graphite boat, 8-air inlet, 9-effusion meter, 10-Ar gas cylinder,
11-is with the graphite boat cover plate of boring, 12-graphite boat base, 13-graphite boat sectional view；
Fig. 2 is the XRD figure spectrum of boron carbide powder；
Fig. 3 is the curve chart of grain size analysis test data；
Fig. 4 is self-propagating synthesis B4The chemical analysis results of C powder.
It is embodied as
Describing the present invention further in detail below in conjunction with the accompanying drawings, these accompanying drawings are the schematic diagram of simplification, only
The basic structure of the present invention is described in a schematic way, and the direction being originally embodied as is with Fig. 1 direction as standard.
The invention provides a kind of granularity is submicron order (100 μm) boron carbide powder and synthetic method, reality below
Execute example to be only intended to describe the present invention in detail, and limit the protection domain of invention never in any form.The inventive method is:
Step 1 is equipped with raw material and tentatively mixes
The present invention is with B2O3, nanometer carbon black be boron source and carbon source, with magnesium metal as reducing agent, after drying and dewatering by three aoxidize
Two boron (B2O3), nanometer carbon black (C) and magnesium metal (Mg) powder be according to mass ratio B2O3:C:Mg=(182-210): 12:(151-
159) carrying out dispensing, according to chemical equation, having a stoichiometric between these three raw material is B2O3:C:Mg=140:12:
144 i.e. B2O3 excess (30-50) %, Mg excess (5-10) %, the granularity of three kinds of raw materials is respectively less than 50 μm, and purity is higher than
98.5%, wherein, the granularity of nanometer carbon black is at below 80nm, and purity is more than 99.99%, and raw material is at ladle alumina liner
Tentatively mix in drum mixer.During charging, it is initially charged with B2O3With loading nanometer carbon black after magnesium powder, damage in order to avoid carbon black flies upward generation
Lose.
Step 2 adds abrasive media, and batch mixing is uniform
It is zirconia ball (Z that the present invention adds abrasive mediarO2), zirconia ball is (1-1.5) with the mass ratio of raw material: 1,
Zirconia ball (ZrO2) a diameter of Φ 10mm, material mixing is uniform, and drum rotation speed is 25r/min, mixing time at least 2 hours,
Batch mixing uniformity basis for estimation up to standard is not have soft-agglomerated piece in material, and naked eyes invisible white scatterplot, entirety presents all
Even Lycoperdon polymorphum Vitt or grey black.Abrasive media can also use other media in this area known to those skilled in the art.
Step 3 raw material separates with abrasive media
After batch mixing is uniform, uses sub-sieve to be separated by zirconia ball, obtain mixed powder.
Step 4 pressure makes green compact
Mixed powder is poured into rustless steel base substrate mould, is pressed into a diameter of under forcing press applies (5-10) MPa pressure
The columned green compact of Φ 50mm.The pressure in the range of choice can be needed, to suppress the green compact of different densities according to industry.
Step 5 base substrate enters reaction unit and carries out the synthetic reaction of self-propagating
Base substrate puts into the graphite boat of boring semicircle, and graphite boat is sent into self-propagating reaction room, then to reative cell evacuation, then
It is passed through the Ar gas shielded of flowing.The two poles of the earth of reative cell electric connection of power supply, are provided with in both junctions and high temperature resistant reach more than 800 DEG C
Heating, heating in the present embodiment uses Aludirome silk, and the other end of this heating is in reative cell
Extend to graphite boat, when energized, heat heating wire, meanwhile, utilize the heat conductivity heated material that graphite boat is good, graphite
It is fast that boat has heat transfer, the feature being heated evenly.When the heating wire of white heat is heated to uniform temperature to material, due to magnesium metal
(Mg) inflammable characteristic of being heated is ignited material, and graphite boat heat transfer maintains combustion wave, now power-off, and material relies on combustion wave self-propagating
Synthetic reaction.
Product is crushed by step 6
Treat that whole material reaction terminates, naturally cool to room temperature, collecting reaction product, chemical reaction occurs between raw material,
Generate B4The mixture of two kinds of materials of C and MgO, uses jaw crusher that product is crushed to 5mm.
Step 7 is ground, is separated
Use abrasive media zirconia ball (ZrO2) combustion product is ground to below (30-50) μm after, use sub-sieve
Ball material is separated.
Step 8 pickling purifies
Powder thing being loaded glass reaction container, adds (2-5) mol/L hydrochloric acid solution, the addition of hydrochloric acid solution needs
Excess 25% on the basis of theoretical addition amount, the basis of theoretical addition amount is that 1mol Mg element needs to consume 2mol
Pure HCl.Glass reaction container is sealed, material is carried out pickling purification.Material is constantly stirred by acid cleaning process,
Heating, thus the reduction stabilisation that magnesium metal is in hydrochloric acid solution, pickling temperature maintains (80-120) DEG C, pickling time 10h,
After tested, the material particles after pickling reaches submicron order.
Step 9 material filtering, wash, be dried
Being filtered by acid-leached product, and after being washed with deionized, obtain filter cake, vacuum drying oven drying put into by filter cake,
Drying temperature is 100 DEG C, drying time 12h.Dried through overpickling, multiple granules can soft-agglomerated caking, form 5 μm particle diameters
Following micron and the material of submicron particles.
Step 10 airflow crash
Material after drying crushes through Jet Mill again, utilizes this mode will not introduce impurity and pollutes, reunites
Granule is opened, obtain purity be 99.4%, mean diameter be the submicron order boron carbide powder of 0.4-1 μm can account for 90% with
On.
Present invention also offers a kind of self-propagating synthesis reaction unit, as it is shown in figure 1, it includes power supply 1, pressure regulator 2, anti-
Answer room 3, heating 4, graphite boat 5, vacuum pump 6, Ar gas cylinder 7 and effusion meter 8, wherein:
The positive and negative electrode of described power supply 1 is drawn and is connected with reative cell 3, and the middle pressure regulator 2 that passes through adjusts heating power, described
The positive and negative electrode two ends drawn arrange the heating 4 of high temperature resistant more than 800 DEG C, described heating 4, in the present embodiment,
Use Aludirome silk.
As shown in Figure 1, described reative cell is Horizontal tubular structure, and the inner chamber of described reative cell 3 has receiving graphite boat 5
First space 31 and protective gas encircle the second space 32 of graphite boat 5, and the left side of described reative cell 3 is provided with pushing away of reative cell
Sliding door 33, carrying blank graphite boat 5 send into from this sliding door 33, the center of this sliding door 33 is provided with shielding window
331 so that operator's up time observes the situation of synthetic reaction；The left end outer wall of described reative cell 3 is provided with steam vent 34,
Described steam vent 34 is connected with vacuum pump 6；The right-hand member outer wall of described reative cell 3 is provided with air inlet 35, described air inlet 35
Being connected with Ar gas cylinder 7, be provided with effusion meter 8 in the middle of both, in order to the flow-control of Ar gas, Ar gas cylinder is used for providing Ar
Gas shielded reacts；The outer wall entering boat end at reative cell 3 is additionally provided with the positive and negative electrode position 36 that the electrode with power supply 1 matches, institute
State positive and negative electrode position 36 to communicate with second space 32, in order to heating 4 stretches into from positive and negative electrode position 36, through second space
32, connect with the corresponding end of graphite boat 5.
Described graphite boat 5 includes the boat body 51 with base and the cover plate 52 with circular hole 54, and described boat body 51 is used for
Taking up blank, the shaft section of this boat body 51 is semicircle, and both sides are provided with dismountable block plate 53, and the opening part of this boat body 51 is arranged
Having the notch 511 for the horizontal pull of cover plate, described cover plate 52 is horizontally set at the opening part of this boat body 51, with described notch 511
It is connected on boat body 51, boat wall and top blind flange is all disposed with a diameter of Φ 3～5mm small sircle hole 54 not etc., in order to
When material reacts in graphite boat, heat dissipates and the volatilization of low melting point in time.
Submicron order boron carbide (B4C) it is dark gray powder, there is density low (2.52g/cm3), hardness height, fusing point height
(2450 DEG C), heat conductivity are good, high abrasion resistance, the feature big to neutron absorption capability, and have higher force performance and
Excellent antioxidation and decay resistance.
The submicron order boron carbide powder quality that this method prepares meets the core of regulation in China's standard GB/T 5151-85
First level flour (HTP-1) requires [10].The boron carbide powder of the method synthesis can apply to, in nuclear reactor, use neutron-absorbing
Material and radiation protection material.Such as, the enrichment 10 of the method synthesis is usedBThe B of abundance4C may be used for preparing fast neutron breeding
Heap control rod pellet and shielding rod pellet；May be used for preparing neutron absorption ball, be applied to the second shutdown system of HTGR
System；Especially, the B4C powder that prepared by the method compound with metallic aluminium can prepare spentnuclear fuel screen work neutron absorber material；Or
Compound with polyethylene, epoxy resin etc. prepare fuel container neutron shielding material.
The B that the method synthesizes can also be used4C powder makes armour material through High Temperature High Pressure sintering, as light-duty anti-
Play clothing and the ballistic armor materials of ground vehicle, armed helicopter and airline carriers of passengers.
Additionally, the boron carbide powder changing method synthesis can be as the abrasive material of fine senior grinding and grinding agent, it is possible to achieve
The polishing the brightest and the cleanest to wear-resistant surface of the work.
Although the present invention is described in detail the most in conjunction with the embodiments, but described those skilled in the art
It is understood that on the premise of without departing from present inventive concept, in claims, it is also possible to above-described embodiment is entered
Row change or change etc..
Claims (10)
1. a submicron carbonized boron powder, wherein the purity of boron carbide is 98.5%～99.4%, and mean diameter is 0.4-5
μm, proportion is more than 90%.
2. a preparation method for the submicron carbonized boron powder described in claim 1, comprises the following steps:
Step 1 is equipped with raw material, tentatively mixes, and the present invention is with B2O3, nanometer carbon black be boron source and carbon source, with magnesium metal as reducing agent,
By diboron trioxide, nanometer carbon black and metal magnesium powder according to mass ratio B after drying and dewatering2O3: C:Mg=182-210:12:151-
159 carry out dispensing, i.e. B2O3Excess 30-50%, Mg excess 5-10%, the granularity of three kinds of raw materials is respectively less than 50 μm, and purity is higher than
98.5%, wherein, the granularity of nanometer carbon black is at below 80nm, and purity is more than 99.99%, and raw material is the most mixed in batch mixer
Close；
Step 2 adds abrasive media, and batch mixing is uniform, and the abrasive media that the present invention adds, abrasive media with the mass ratio of raw material is
1-1.5:1, material mixing is uniform；
Step 3 raw material separates with abrasive media, after batch mixing is uniform, uses sub-sieve to be separated with abrasive media by raw material,
To mixed powder；
Step 4 is pressed into green compact, and mixed powder is poured into rustless steel base substrate mould, presses under forcing press applies 5-10MPa pressure
Make a diameter of columned green compact of Φ 50mm；
Step 5 base substrate enters reaction unit and carries out the synthetic reaction of self-propagating, and base substrate puts into the graphite boat of boring semicircle, and graphite boat send
Enter self-propagating reaction room, then to reative cell evacuation, then be passed through the protection gas shielded of flowing, the two of reative cell electric connection of power supply
Pole, is provided with the high temperature resistant heating reaching more than 800 DEG C in both junctions, and the other end of this heating is in reative cell
Extend to graphite boat, when energized, heat heating, when the heating wire of white heat is heated to uniform temperature to material,
Ignite material, and graphite boat heat transfer maintains combustion wave, now power-off, and material relies on the reaction of combustion wave self-propagating synthesis；
Product is crushed by step 6, treats that whole material reaction terminates, and naturally cools to room temperature, collecting reaction product, uses jaw
Product is crushed to 5mm by formula disintegrating machine；
Step 7 is ground, is separated, and after using abrasive media that combustion product is ground to below 30-50 μm, uses sub-sieve by raw material
Separate with abrasive media；
Step 8 pickling purifies, and powder thing is loaded glass reaction container, adds 2-5mol/L hydrochloric acid solution, is held by glass reaction
Device seals, and material is carried out pickling purification, is constantly stirred material, heats, thus magnesium metal exists in acid cleaning process
Reduction stabilisation in hydrochloric acid solution, pickling temperature maintains 80-120 DEG C, pickling time 10h, after tested, the material after pickling
Granule reaches submicron order；
Step 9 material filtering, washing, be dried, filtered by acid-leached product, and after being washed with deionized, obtain filter cake, filter cake is put
Drying in entering vacuum drying oven, drying temperature is 100 DEG C, and drying time 12h forms micron and the submicron of below 5 μm particle diameters
The material of grade particles.
In accordance with the method for claim 2, the most further comprising the steps of: airflow crash, the material after drying is again through air-flow
Disintegrating apparatus crushes, and agglomerated particle is opened, obtain purity be 99.4%, mean diameter be the submicron order carbon of 0.4-1 μm
Change boron powder.
The most in accordance with the method for claim 2, wherein: described batch mixing uniformity basis for estimation up to standard is not exist in material
Soft-agglomerated piece, naked eyes invisible white scatterplot, entirety presents uniform Lycoperdon polymorphum Vitt or grey black.
The most in accordance with the method for claim 2, wherein: described protection gas uses Ar gas.
The most in accordance with the method for claim 2, wherein: described abrasive media is zirconia ball, and described zirconia ball is a diameter of
Φ10mm。
The most in accordance with the method for claim 2, wherein: the addition of hydrochloric acid solution needs mistake on the basis of theoretical addition amount
Amount 25%, the basis of theoretical addition amount is the pure HCl that 1mol Mg element needs to consume 2mol.
The most in accordance with the method for claim 2, wherein: batch mixer uses the drum mixer of ladle alumina liner, cylinder
Rotating speed is at least 25r/min, mixing time at least 2 hours.
Submicron carbonized boron powder the most according to claim 1, the boron carbide powder of the method synthesis can apply to
In nuclear reactor, with neutron absorber material and radiation protection material；The boron carbide powder that the method synthesizes can be used through too high
Temperature high-pressure sinter makes armour material；The boron carbide powder changing method synthesis can be as the abrasive material of fine senior grinding and grinding
Agent.
10. the submicron carbonized boron powder described in claim 9, the application in nuclear reactor of the described boron carbide powder is for adopting
Enrichment 10 with the method synthesisBThe boron carbide of abundance, may be used for preparing fast breeder reactor control rod pellet and shielding rod
Pellet；May be used for preparing neutron absorption ball, be applied to the Second shutdown system of HTGR；Boron carbide prepared by the method
Powder compound with metallic aluminium can prepare spentnuclear fuel screen work neutron absorber material；Preparation compound with polyethylene, epoxy resin etc.
Fuel container neutron shielding material.
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| CN106976883A (en) * | 2017-05-10 | 2017-07-25 | 东北大学 | A kind of situ-combustion synthesis prepares B4The method of C nano powder |
| CN107226472A (en) * | 2017-05-10 | 2017-10-03 | 东北大学 | A kind of situ-combustion synthesis prepares B4The method of C nano pipe |
| CN107758670A (en) * | 2017-12-08 | 2018-03-06 | 中国科学院青海盐湖研究所 | A kind of preparation method of boron carbide superfine powder |
| CN108101059A (en) * | 2018-02-10 | 2018-06-01 | 潍坊锐能新材料技术有限公司 | A kind of production technology and process units of ultra tiny boron carbide micro powder |
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| CN109553396A (en) * | 2018-10-23 | 2019-04-02 | 西安建筑科技大学 | A kind of Low-carbon magnesia-carbon refractory material additive, preparation method and applications |
| CN110579102A (en) * | 2019-08-13 | 2019-12-17 | 山东德艾普节能材料有限公司 | ultra-high temperature sintering furnace and sintering method for oxide fiber product |
| CN111995401A (en) * | 2020-09-04 | 2020-11-27 | 牡丹江金钢钻碳化硼有限公司 | Preparation method of superfine boron carbide powder |
| CN114750049A (en) * | 2022-05-20 | 2022-07-15 | 贵溪奥泰铜业有限公司 | Preparation facilities of tin-phosphor bronze board with adjustable glossiness |
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