CN106853533B - A method of preparing high-purity ferro-boron superfine powder - Google Patents
A method of preparing high-purity ferro-boron superfine powder Download PDFInfo
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Abstract
The present invention relates to high performance alloys field of material technology, and in particular to a kind of method preparing high-purity ferro-boron superfine powder.This method only needs each component powder is dry-mixed uniformly, then it is suppressed with certain pressure, it is sent into processing in high temperature furnace and can be obtained high pure and ultra-fine ferro-boron powder, greatly reduce degree of dependence of the ferro-boron production to equipment, and dramatically reduce the security risk in production process.Simultaneously as reaction raw materials have just largely been uniformly mixed before being produced in feeding stove, so production temperature is greatly reduced, material loss greatly reduces, and ferro-boron homogeneity of ingredients is also dramatically improved.Since obtained product is also the tiny powder of granularity, also just reduces follow-up broken this link of processing needed for traditional smelting production ferro-boron, further save human and material resources.
Description
Technical field
The present invention relates to high performance alloys field of material technology, and in particular to preparing high-purity ferro-boron superfine powder to a kind of
Method.
Background technology
The continuous popularization and application of high-performance amorphous band and high-performance rare-earth permanent magnet material, to the purity and quality of raw material
Stability more stringent requirements are proposed.Ferro-boron is as the weight for introducing boron element in amorphous band or rare earth permanent-magnetic material
Want one of raw material, ingredient controllability and stability for obtaining high-performance amorphous band or rare earth forever in mass production levels
Magnetic material product simultaneously improves yield rate and plays a crucial role.
The traditional handicraft of ferro-boron industrialized production is normally based on following reaction formula, is made using scrap iron piece or steel cuttings
For source of iron, using boric anhydride, boric acid or borax as boron source, using coke or wood chip as carbon source, in ore-smelting electric furnace, with smelting
The mode of refining is produced (Cao Yi, the production method ferroalloy 1986 (03) of the pure ferro-boron of low-aluminium high, Wei Shounan；Shi Yunshi, low aluminium
The production of ferro-boron, ferroalloy .1986 (04), the optimal parameter of the refined sweet smell carbothermies production ferro-boron of rope, ferroalloy .1992 (05)).
4Fe+2B2O3+3C→4FeB+3CO2
In order to allow larger-size iron plate, wood chip etc. to be come into full contact between raw materials and boric anhydride, boric acid and react, usually
It needs to make boric anhydride melt with iron plate under the temperature (being higher than 1800-3000 DEG C) far beyond primary raw material boric anhydride and iron plate fusing point,
And make the ferro-boron melt obtained by smelting that there is lower viscosity, to keep different parts ferro-boron liquid alloy ingredient in stove equal
It is even and be easy to operation of coming out of the stove.
There is several main problems for this technique：(1) since production temperature is high, along with ore-smelting electric furnace has production ring
Border it is open with atmosphere the characteristics of, this allows for ferro-boron, and to produce that there is energy expenditures huge；(2) due to boric anhydride
Density is far below molten iron, is easy to float on molten iron surface at high temperature, and since the viscosity of boric anhydride and molten iron is all very high, lead to boric anhydride
Difficulty is mixed with molten iron and coke, it is uneven that this allows for different parts ferro-boron bath composition in ore-smelting electric furnace；(3) due to
The fusing point and boiling point of boric anhydride are all very low (being about 450 DEG C and 1680 DEG C respectively), under ferro-boron actual production conditions, it is easy to send out
Raw volatilization, causes the loss of expensive raw materials boric anhydride.While being smelted, boric anhydride can also be used as oxygen source, by coke or
Person's wood chip aoxidizes, and generates boron carbide (B4The by-products such as C), cause loss of material, also result in the serious pollution to environment；Boric anhydride or
Person's boron carbide can also be dissolved or be mingled with into ferro-boron frit, lead to impurity content increase, quality decline and post-processing
The increase of processing cost.
In addition, there are two factors, and ferro-boron impurity can be caused to increase, quality decline：(1) boric acid or boric anhydride etc. are anti-
It answers raw material to there is the phenomenon that residual moisture evaporation at high temperature, after in high-temperature fusant assembling to a certain extent, is easy to cause
Ferro-boron melt explodes in stove, causes great work safety accident.In order to reduce or avoid the generation of this phenomenon, lead to
It often needs that sawdust or wood chip is added simultaneously inside raw mixture, melt is maked somebody a mere figurehead between the material melted in stove, is formed
The channel for allowing vapor to escape.Naturally occurring ash impurities can make ferro-boron impurity content increase inside sawdust or wood chip
Add；(2) in order to save ferro-boron production cost or make full use of mineral resources, also it has been proposed that with the ferro-boron magnesium of boracic
Mine or main component are iron oxide (Fe2O3) Iron concentrate, agglomerates of sintered pellets or metallurgical grade coke as reactant (in bamboo
Suitable, assistant rattan has one, slope, and originally extensively bright high-purity ferroboron Chinese Patent Application No. 200610082571.X, Huang account for literary ferro-boron
Production method Chinese Patent Application No. 200810224192.9, Shi Yun stones motherland text Jia Zong lifes are a kind of burnt using prefabricated boron
Carbothermy production ferro-boron technique Chinese Patent Application No. 93108638.8, Cui Zhang Xianpeng passes Meng Liu Su orchids Ji spring continuous heavy rain Zhao
It is the method Chinese Patent Application No. 87101579 that benevolence ludwigite directly produces ferro-boron, Takao Hamada, Nobuo
Tsuchiya, Toshihiro Inatani, Yoshiyasu Takada, Mitsuo Sumito, Eiji Katayama,
Toshimitsu Koitabashi, Kyoji Okabe, Yo Ito, Method for producing Fe-B molten
Metal, US4397691,1983, Sunao Takeuchi, Yuichi Sato, Hiroaki Sakamoto, High-purity
Ferroboron, a mother alloy for iron-base amorphous alloy, an iron-base
Amorphous alloy, and methods for producing the same, US 2006/0292027A1).These are former
Although the utilization of material can reduce production cost to a certain extent, because containing too many impurity, it is also significantly reduced boron
The quality of ferroalloy productor, because reducing the use value of product.
It is large-scale to smelt production and cause in ferro-boron product there are a large amount of field trash, this just give amorphous band or
The component of rare earth permanent-magnetic material brings deviation, microstructure to rise and fall, and causes final products performance unstable.
Finally, in order to avoid under above-mentioned high temperature because of the explosion in ore-smelting electric furnace that vapor causes in raw material, in production
It is usually taken boric acid, borate elder generation high temperature dehydration, is converted into boric anhydride, then put into ore-smelting electric furnace and produce together with unclassified stores
Method.Additional workshop, equipment and manpower are needed since boric acid dehydration is converted into boric anhydride, and there is also under high temperature in dehydration
Volatilizing loss, this just brings additional cost to production.
Therefore, in order to solve the above technical problems, devising a kind of method preparing high-purity ferro-boron superfine powder, this method
Only need uniformly then to suppress each component powder is dry-mixed with certain pressure, be sent into processing in high temperature furnace can be obtained it is high-purity super
Thin ferro-boron powder greatly reduces degree of dependence of the ferro-boron production to equipment, and dramatically reduces production
Security risk in the process.Simultaneously as reaction raw materials have just largely obtained before being produced in feeding stove
To being uniformly mixed, so production temperature is greatly reduced, material loss greatly reduces, and ferro-boron homogeneity of ingredients is also very big
Degree it is improved.Since obtained product is also the tiny powder of granularity, also just reduce traditional smelting production boron
Follow-up broken this link of processing needed for ferroalloy, further saves human and material resources.In addition, this method it is easy to operate and
Safe, low for equipment requirements, energy-saving and emission-reduction, products obtained therefrom be high-purity and stay in grade, disclosure satisfy that high-end downstream to high-purity ferro-boron
The demand of superfine powder.
Invention content
In order to overcome defect present in background technology, the technical solution adopted by the present invention to solve the technical problems to be：
A method of high-purity ferro-boron superfine powder being prepared, step is：
(1) with iron powder, boron-containing compound powder and carbon dust, by Fe: B2O3: C=(1.7~2.3): (0.8~1.2): (2.7
~3.2) molar ratio ratio is dry-mixed uniformly mixed, is placed in mold in 1~250MPa forming under the pressure, dry-pressing formed rear institute
It is spare to obtain biscuit；
(2) biscuit for preparing step (1), is placed in high temperature furnace and is heat-treated, and the heating step of high temperature furnace is：With
15 DEG C/min of heating rate rises to 1000 DEG C from room temperature, and keeps the temperature 15 minutes；Then with 10 DEG C/min of heating rate from
1000 DEG C are warming up to 1200~1600 DEG C, and keep the temperature 30 minutes；Then high temperature furnace power supply is cut off, high temperature furnace natural cooling is made, etc.
When being cooled to room temperature in high temperature furnace, sample is taken out；In entire heat treatment process, nitrogen or argon gas are filled in high temperature furnace as guarantor
Atmosphere is protected, or makes to keep vacuum state in high temperature furnace；
(3) sample that step (2) is taken out and methanol are configured to solid content in the slurry of 5~85wt.%, while adding phase
For solid phase quality be 0.01~5wt.% maleic acid as dispersant, be then placed in sand mill and be ground, grinding is held
The continuous time is 5~300 minutes, after grinding, material is taken out drying, that is, prepares high-purity ferro-boron superfine powder.
The preferred boron-containing compound powder is boric anhydride, boric acid or borax, and the carbon dust is charcoal powder, graphitic carbon
Powder, coke carbon dust, petroleum coke or calcined coke.
The grain size of iron powder, boron-containing compound powder and carbon dust is less than 20 mesh in the preferred step (1), can be with dry
Mixed technique further adds a small amount of methylcellulose or after water mixed, is pressed into biscuit.
The preferred high temperature furnace is carbon shirt-circuiting furnace, molybdenum wire furnace, induction furnace, continuous tunnel furnace, electric arc furnaces or mineral hot furnace.
The preferred sand mill is vertical grinding machine or horizontal sand mill.
The granularity of preferred high-purity ferro-boron superfine powder is 0.5~5000 micron, and boron content is 8~17wt.%.
A kind of method preparing high-purity ferro-boron superfine powder according to the present invention, this method are only needed each component powder
It is dry-mixed uniformly then to be suppressed with certain pressure, it is sent into processing in high temperature furnace and can be obtained high pure and ultra-fine ferro-boron powder, significantly
Degree of dependence of the ferro-boron production to equipment is reduced, and dramatically reduces the security risk in production process.Together
When, it has just largely been uniformly mixed before being produced in feeding stove due to reaction raw materials, so production
Temperature is greatly reduced, and material loss greatly reduces, and ferro-boron homogeneity of ingredients is also dramatically improved.Due to
Obtained product is also the tiny powder of granularity, is also just reduced follow-up broken needed for traditional smelting production ferro-boron
This link is processed, human and material resources are further saved.In addition, this method is easy to operate and safe, low for equipment requirements, section
Can emission reduction, products obtained therefrom be high-purity and stay in grade, disclosure satisfy that demand of the high-end downstream to high-purity ferro-boron superfine powder.
Description of the drawings
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the X ray diffracting spectrum for high-purity ferro-boron superfine powder that the present invention is prepared according to specific embodiment two；
Fig. 2 is that the laser particle size sedimentometer for high-purity ferro-boron superfine powder that the present invention is prepared according to specific embodiment two is surveyed
The size distribution curve of examination；
Specific implementation mode
In conjunction with the accompanying drawings, the present invention is further explained in detail.Attached drawing is the schematic diagram of simplification, only with signal side
Formula illustrates the basic structure of the present invention, therefore it only shows the composition relevant to the invention.
Specific embodiment one, a method of high-purity ferro-boron superfine powder being prepared, step is：
(1) with iron powder, boron-containing compound powder and carbon dust, by Fe: B2O3: C=1.7: 0.8: 2.7 molar ratio ratio is dry
It is mixed to be uniformly mixed, it is placed in mold in 1MPa forming under the pressure, dry-pressing formed rear gained biscuit is spare；
(2) biscuit for preparing step (1), is placed in high temperature furnace and is heat-treated, and the heating step of high temperature furnace is：With
15 DEG C/min of heating rate rises to 1000 DEG C from room temperature, and keeps the temperature 15 minutes；Then with 10 DEG C/min of heating rate from
1000 DEG C are warming up to 1200 DEG C, and keep the temperature 30 minutes；Then high temperature furnace power supply is cut off, high temperature furnace natural cooling is made, waits until high temperature
When being cooled to room temperature in stove, sample is taken out；In entire heat treatment process, nitrogen or argon gas are filled in high temperature furnace as protection gas
Atmosphere, or make to keep vacuum state in high temperature furnace；
(3) sample that step (2) is taken out and methanol be configured to solid content 5wt.% slurry, while add relative to
Solid phase quality be 0.01wt.% maleic acid as dispersant, be then placed in sand mill and be ground, grind the duration be
5 minutes, after grinding, material is taken out into drying, that is, prepares high-purity ferro-boron superfine powder.
The boron-containing compound powder is boric anhydride, and the carbon dust is charcoal powder, iron powder, boracic chemical combination in the step (1)
The grain size of powder and carbon dust is less than 20 mesh, can be pressed into biscuit with dry mixing process.
The high temperature furnace is carbon shirt-circuiting furnace, and the sand mill is vertical grinding machine, the granularity of high-purity ferro-boron superfine powder
It it is 0.5~5000 micron, boron content is 8~17wt.%.
Specific embodiment two, a method of high-purity ferro-boron superfine powder being prepared, step is：
(1) with iron powder, boron-containing compound powder and carbon dust, by Fe: B2O3: C=2: 1: the 3 dry-mixed mixing of molar ratio ratio
Uniformly, it is placed in mold in 120MPa forming under the pressure, dry-pressing formed rear gained biscuit is spare；
(2) biscuit for preparing step (1), is placed in high temperature furnace and is heat-treated, and the heating step of high temperature furnace is：With
15 DEG C/min of heating rate rises to 1000 DEG C from room temperature, and keeps the temperature 15 minutes；Then with 10 DEG C/min of heating rate from
1000 DEG C are warming up to 1400 DEG C, and keep the temperature 30 minutes；Then high temperature furnace power supply is cut off, high temperature furnace natural cooling is made, waits until high temperature
When being cooled to room temperature in stove, sample is taken out；In entire heat treatment process, nitrogen or argon gas are filled in high temperature furnace as protection gas
Atmosphere, or make to keep vacuum state in high temperature furnace；
(3) sample that step (2) is taken out and methanol are configured to solid content in the slurry of 55wt.%, while adding opposite
In solid phase quality be 3wt.% maleic acid as dispersant, be then placed in sand mill and be ground, grind the duration be
200 minutes, after grinding, material is taken out into drying, that is, prepares high-purity ferro-boron superfine powder.
The boron-containing compound powder is boric acid, and the carbon dust is coke carbon dust, and iron powder in the step (1) contains boronation
The grain size for closing powder and carbon dust is less than 20 mesh, can be pressed into biscuit after further adding a small amount of methylcellulose mixing.
The high temperature furnace is induction furnace, and the sand mill is horizontal sand mill, the granularity of high-purity ferro-boron superfine powder
It it is 0.5~5000 micron, boron content is 8~17wt.%.
Products therefrom ingredient is ferro-boron pure phase as can see from Figure 1, and gained powdery pulp is to swash as can see from Figure 2
The size distribution curve of light bead degree sedimentometer test.
Specific embodiment three, a method of high-purity ferro-boron superfine powder being prepared, step is：
(1) with iron powder, boron-containing compound powder and carbon dust, by Fe: B2O3: C=2.3: 1.2: 3.2 molar ratio ratio is dry
It is mixed to be uniformly mixed, it is placed in mold in 250MPa forming under the pressure, dry-pressing formed rear gained biscuit is spare；
(2) biscuit for preparing step (1), is placed in high temperature furnace and is heat-treated, and the heating step of high temperature furnace is：With
15 DEG C/min of heating rate rises to 1000 DEG C from room temperature, and keeps the temperature 15 minutes；Then with 10 DEG C/min of heating rate from
1000 DEG C are warming up to 1600 DEG C, and keep the temperature 30 minutes；Then high temperature furnace power supply is cut off, high temperature furnace natural cooling is made, waits until high temperature
When being cooled to room temperature in stove, sample is taken out；In entire heat treatment process, nitrogen or argon gas are filled in high temperature furnace as protection gas
Atmosphere, or make to keep vacuum state in high temperature furnace；
(3) sample that step (2) is taken out and methanol are configured to solid content in the slurry of 85wt.%, while adding opposite
In solid phase quality be 5wt.% maleic acid as dispersant, be then placed in sand mill and be ground, grind the duration be
300 minutes, after grinding, material is taken out into drying, that is, prepares high-purity ferro-boron superfine powder.
The boron-containing compound powder is borax, the grain size of iron powder, boron-containing compound powder and carbon dust in the step (1)
Less than 20 mesh, biscuit can be pressed into after being mixed with water.
The high temperature furnace is mineral hot furnace, and the sand mill is vertical grinding machine., the granularity of high-purity ferro-boron superfine powder
It it is 0.5~5000 micron, boron content is 8~17wt.%.
A kind of method preparing high-purity ferro-boron superfine powder according to the present invention, this method are only needed each component powder
It is dry-mixed uniformly then to be suppressed with certain pressure, it is sent into processing in high temperature furnace and can be obtained high pure and ultra-fine ferro-boron powder, significantly
Degree of dependence of the ferro-boron production to equipment is reduced, and dramatically reduces the security risk in production process.Together
When, it has just largely been uniformly mixed before being produced in feeding stove due to reaction raw materials, so production
Temperature is greatly reduced, and material loss greatly reduces, and ferro-boron homogeneity of ingredients is also dramatically improved.Due to
Obtained product is also the tiny powder of granularity, is also just reduced follow-up broken needed for traditional smelting production ferro-boron
This link is processed, human and material resources are further saved.In addition, this method is easy to operate and safe, low for equipment requirements, section
Can emission reduction, products obtained therefrom be high-purity and stay in grade, disclosure satisfy that demand of the high-end downstream to high-purity ferro-boron superfine powder.
It is enlightenment with the above-mentioned desirable embodiment according to this patent, through the above description, relevant staff is complete
Various changes and amendments can be carried out in the range of without departing from this item patented technology thought entirely.The technology of this item patent
Property range is not limited to the contents of the specification, it is necessary to determine its technical scope according to right.
Claims (6)
1. a kind of method preparing high-purity ferro-boron superfine powder, it is characterised in that its step is：
(1) with iron powder, boron-containing compound powder and carbon dust, by Fe: B2O3: C=(1.7~2.3): (0.8~1.2): (2.7~
3.3) molar ratio ratio is dry-mixed uniformly mixed, is placed in mold in 1~250MPa forming under the pressure, dry-pressing formed rear gained
Biscuit is spare；
(2) biscuit for preparing step (1), is placed in high temperature furnace and is heat-treated, and the heating step of high temperature furnace is：With 15
DEG C/min heating rate rise to 1000 DEG C from room temperature, and keep the temperature 15 minutes；Then with 10 DEG C/min of heating rate from
1000 DEG C are warming up to 1200~1600 DEG C, and keep the temperature 30 minutes；Then high temperature furnace power supply is cut off, high temperature furnace natural cooling is made, etc.
When being cooled to room temperature in high temperature furnace, sample is taken out；In entire heat treatment process, nitrogen or argon gas are filled in high temperature furnace as guarantor
Atmosphere is protected, or makes to keep vacuum state in high temperature furnace；
(3) sample that step (2) is taken out and methanol be configured to solid content 5-85wt.% slurry, while add relative to
Solid phase quality be 0.01~5wt.% maleic acid as dispersant, be then placed in sand mill and be ground, grinding persistently when
Between be 5-300 minute, after grinding, will material taking-up drying, that is, prepare high-purity ferro-boron superfine powder.
2. a kind of method preparing high-purity ferro-boron superfine powder according to claim 1, which is characterized in that described to contain boronation
Conjunction powder is boric anhydride, boric acid or borax, and the carbon dust is charcoal powder, graphite carbon dust, coke carbon dust, petroleum coke or after forging
It is burnt.
3. a kind of method preparing high-purity ferro-boron superfine powder according to claim 1, which is characterized in that the step
(1) grain size of iron powder, boron-containing compound powder and carbon dust is less than 20 mesh in, can be a small amount of with dry mixing process or further addition
After methylcellulose or water are mixed, it is pressed into biscuit.
4. a kind of method preparing high-purity ferro-boron superfine powder according to claim 1, which is characterized in that the high temperature furnace
For carbon shirt-circuiting furnace, molybdenum wire furnace, induction furnace, continuous tunnel furnace, electric arc furnaces or mineral hot furnace.
5. a kind of method preparing high-purity ferro-boron superfine powder according to claim 1, which is characterized in that the sand mill
For vertical grinding machine or horizontal sand mill.
6. a kind of method preparing high-purity ferro-boron superfine powder according to claim 1, which is characterized in that the high purity boron
The granularity of iron superfine powder is 0.5~5000 micron, and boron content is 8~17wt.%.
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| CN1854322A (en) * | 2002-03-28 | 2006-11-01 | 新日本制铁株式会社 | High-purity ferroboron |
| CN101476077A (en) * | 2008-10-27 | 2009-07-08 | 黄占文 | Production method of ferroboron |
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| JPS5225000A (en) * | 1975-08-21 | 1977-02-24 | Komatsu Ltd | Method for production of feb powder |
| JPS5826025A (en) * | 1981-08-06 | 1983-02-16 | Mitsui Mining & Smelting Co Ltd | Manufacture of ferroboron |
| CN1083125A (en) * | 1993-07-17 | 1994-03-02 | 辽阳铁合金厂 | A kind of carbothermy of prefabricated boron Jiao that uses is produced ferro-boron technology |
| CN1854322A (en) * | 2002-03-28 | 2006-11-01 | 新日本制铁株式会社 | High-purity ferroboron |
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