CN105884371A - Self-propagating synthesis method for submicron-grade TiB2 powder - Google Patents
Self-propagating synthesis method for submicron-grade TiB2 powder Download PDFInfo
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Abstract
The invention belongs to the field of preparation of ceramic materials and boride powder and in particular relates to a self-propagating synthesis method for submicron-grade TiB2 powder. The self-propagating synthesis method comprises the following steps: mixing materials, compacting, igniting, breaking and grinding, carrying out acid pickling, filtering, drying, and carrying out airflow pulverization. When the self-propagating synthesis method is adopted for preparing the submicron-grade TiB2 powder, the obtained submicron-grade TiB2 powder is high in purity, low in granularity and relatively high in sintering activity; the purity can reach 98.5% or more, industrial production can be realized, a synthesis technology is mature, and production cost is relatively low; and the synthesis method is easy to operate, production efficiency is high, dust output is low, and the prepared TiB2 powder is high in purity, low in granularity and relatively high in sintering activity.
Description
Technical field
The invention belongs to the preparation field of ceramic material and boride powder, be specifically related to a kind of submicron order
TiB2The self-propagating synthesis method of powder body.
Background technology
Titanium diboride (TiB2) there is high-melting-point (2980 DEG C), low-density (4.5g/cm3), high rigidity
(HV=34GPa), higher bending strength and fracture toughness, excellent heat conduction, electric conductivity, anti-wear performance
With chemical stability, especially molten-metal-resistant corrode.Titanium diboride can by metal aluminium liquid complete wetting,
Be known today in ceramic/metal system uniquely can be with the material system of complete wetting.The hardness of titanium diboride
It is only second to diamond, cubic boron nitride (c-BN) and boron carbide, higher than oxide and nitride ceramics.
Based on above excellent characteristic, TiB2 is at cutting element, wear resistant tools and part, military armor and shellproof structure
The application neck of some uniquenesses such as part, metallization evaporator boat, aluminium electrolytic cell cathode coating, industry heating electrode
Territory demonstrates the serviceability of excellence, and shows the most wide application and development in many applications
Prospect.
At present, TiB2The preparation method of powder mainly has carbothermic method, self-propagating high-temperature synthesis, boron heat
Reducing process, sol-gal process, fused salt electrolysis process, element direct synthesis technique and gas-phase reaction method.Carbon heat is also
TiB is prepared in former method industrialization2Technique relative maturity, will TiO2、B2O3With the mixing raw material of carbon black through carbon
Pipe furnace, induction furnace or electric arc furnace high-temperature process, product is polished obtains micron order TiB2Powder, this side
Method can not prepare submicron order or nano-scale particle size powder.Although sol-gal process can prepare the higher powder of purity
End, but commercial processes is the most immature, the most only rests on laboratory level.Boron thermal reduction method preparation cost
Height, purity is difficult to control.Gas-phase reaction method can prepare nanoscale TiB2Powder, but raw material and equipment cost
Height, production capacity is little, and production efficiency is low.In sum, existing TiB2Technology of preparing is at quality, cost and product
There is certain technical bottleneck in industry efficiency aspect.
Summary of the invention
In order to solve the problems referred to above that prior art exists, the invention provides a kind of submicron order TiB2Powder body
Self-propagating synthesis method.
The technical solution adopted in the present invention is:
The present invention provides a kind of above-mentioned submicron order TiB2The self-propagating synthesis method of powder body, including walking as follows
Rapid:
Step 1: weigh TiO respectively according to the ratio of weight ratio 80:91-105:120-1322、B2O3And metal
Magnesium powder, and carry out batch mixing, batch mixing is complete obtains batch mixing powder；
Step 2: after batch mixing is uniform, batch mixing powder is pressed into cylindric base substrate；
Step 3: described cylindric base substrate is put into graphite boat, then graphite boat is loaded self-propagating reaction room
In, it is passed through the Ar gas of flowing after the evacuation of self-propagating reaction room again, it is ensured that self-propagating reaction indoor are deposited without air
?；
Step 4: add the cylindric base substrate of thermal ignition to cause self-propagating reaction, end to be combusted, cool down cylinder
Shape base substrate, obtains the loose porous cylindric product that surface is black or grey black；
Step 5: by described cylindric product grind into powder；Addition hydrochloric acid solution carries out pickling to powder and carries
Pure, pickle constantly it is stirred by acid cleaning process and heats, being filtrated to get filter cake, washing filter cake, so
After filter cake is dried, after drying filter cake through grinding, obtain the submicron order TiB that granularity is 0.4-1 μm2
Powder body.
SHS process (is called for short SHS), is also called combustion synthesis technology, is to utilize height between reactant
The self-heating of chemical reaction heat and carry out a kind of technology of synthetic material from conduction, when reactant once by
Igniting, the regional spread that not yet will react from trend, until reaction completely, is to prepare inorganic compound height
A kind of new method of adiabator.
In step 2, described batch mixing uniformity basis for estimation up to standard is not have soft-agglomerated piece in material,
Naked eyes invisible white scatterplot, entirety presents uniform Lycoperdon polymorphum Vitt or grey black.Graphite boat used by step 3 is half
Circle boat, both sides with dismountable block plate, opening part equipped with can pull cover plate, boat wall and top blind flange are made
Small sircle hole.In step 5, use distilled water wash filter cake.
Further, by TiO in step 12、B2O3Add in drum mixer with metal magnesium powder and carry out batch mixing,
The drum rotation speed of described drum mixer is 25-30r/min, and mixing time is at least 2h；Described cylinder batch mixing
The liner material of machine is aluminium oxide；Having ball milling in described drum mixer, described ball milling is diameter
10-20mm zirconia ball mill.The volume of described drum mixer is generally 70L.
Further, described TiO2、B2O3The weight sub with described ball milling with the gross weight sum of metal magnesium powder
Ratio be 1:1-1.5.
In step 2, the pressure that batch mixing powder is pressed into cylindric base substrate is 5-10MPa.
Further, described self-propagating reaction room is horizontal tubular reactor room, described self-propagating reaction room anti-
Air inlet and air vent should be respectively provided with in pipe two ends.Add the cylindric base substrate of thermal ignition with cause self-propagating reaction it
Before, first to reative cell evacuation, it is passed through the Ar gas of flowing the most again from described air inlet, by air from described
Air vent is discharged；Flowing Ar gas is continued until that reaction terminates rear material and is cooled to room temperature.
The described thermal ignition mode that adds is that electric-heating-wire-heating ignites, and heating wire is a diameter of 0.5-1mm tantalum wire；Logical
After electricity, ignited in one end of cylindric base substrate by heating wire；One end of cylindric base substrate is drawn by the heating wire of white heat
Electric current can be cut off after combustion, stop heating, spread maintenance reaction by combustion wave and complete.
Further, in step 5, in airtight glass lined reactor container, carry out pickling operation, described
Before pickling operation, use jaw crusher that described cylindric product is broken into the little of a diameter of 5-15mm
Block, then with rod milling or ball-grinding machine, described fritter ground to form the powder that granularity is 5-20 μm.
Described pickling purification process uses 2-5mol/L hydrochloric acid solution, the quality of described hydrochloric acid and the quality of magnesium powder
Ratio is 1:2.5；Pickling temperature controls at 80-100 DEG C, and pickling time is 10-20 hour.Add the total of hydrochloric acid
Amount needs to increase at least 25% on the basis of theoretical addition amount；The basis of theoretical addition hydrochloric acid content is
1mol Mg element needs to consume the pure HCl of 2mol.
In step 5, combustion product is after overpickling, and the filter cake being filtrated to get is put into vacuum drying oven and carried out
Drying, vacuum drying temperature is 80-120 DEG C, and the time is 10-15h.After drying, filter cake is through ball milling or air-flow
Disintegrating apparatus grinds further, obtains the high-purity Ti B of 0.4-1 μm2Powder.
The invention have the benefit that the present invention uses self-propagating synthesis method to prepare submicron order TiB2Powder body,
Gained submicron order TiB2Powder purity is high, fine size and have higher sintering activity；Purity can reach
More than 98.5%, it is possible to industrialization produces, synthesis technique is ripe, and production cost is relatively low.Its synthetic method operates
Simply, production efficiency is high, and dust generation amount is little, prepared TiB2Powder purity is high, fine size and having
Higher sintering activity.
Accompanying drawing explanation
Fig. 1 is self-propagating reaction device schematic diagram；
Fig. 2 is the cross-sectional view of graphite boat；
Fig. 3 is the TiB of preparation in the embodiment of the present invention 22The XRD figure spectrum of powder.
In figure, 1, pressure regulator；2, vacuum pump；3, shielding window；4, reactor chamber door；5, air vent；
6, thermode is added；7, graphite boat；8, air inlet；9, effusion meter；10, Ar gas cylinder；11, with brill
The graphite boat cover plate in hole；12, graphite boat base.
Detailed description of the invention
Embodiment 1
By TiO2、B2O3With magnesium powder according to mass ratio TiO2:B2O3: Mg=80:105:120 dispensing, i.e. B2O3
Excess 50%, magnesium metal excess 5%.In stainless steel cask after preliminary mixing, load with alumina liner
Drum mixer, adds the zirconia ball of a diameter of 10mm, zirconia ball and TiO2、B2O3And magnesium metal
The mass ratio of the gross weight sum of powder is 1:1, batch mixing 2 hours under the rotating speed of 25 turns/min, and raw material mixes
Uniformly.Use stainless steel mould that material is pressed under 5MPa pressure the cylindric base substrate of a diameter of 50mm.
The cylindric base substrate suppressed is put into graphite boat, after plugging plate, graphite boat is put into self-propagating reaction room,
To the Ar gas shielded being passed through flowing after the evacuation of self-propagating reaction room.After energising, the heating wire of white heat is by material
Igniting in one end, cuts off electric current, maintains whole material reaction to terminate by combustion wave self-propagating, naturally cools to room
Temperature, collecting reaction product.After using jaw crusher that product is crushed to 5mm, ball milling is used burning to be produced
Thing is ground to below 20 μm.Ball milling product is loaded glass reaction still, adds 5mol/L hydrochloric acid solution, salt
The addition of acid solution needs excess 25% on the basis of theoretical addition amount, to material after being sealed by reactor
Carry out pickling purification.Material is constantly stirred by acid cleaning process, heats, it is ensured that temperature maintains 80 DEG C,
Pickling time 10h.Pickling terminate after by material filtering, washing, be dried 12h at 100 DEG C of vacuum drying ovens,
Dried material i.e. can get submicron order high-purity Ti B through comminution by gas stream2Powder.
Embodiment 2
By TiO2、B2O3With magnesium powder according to mass ratio TiO2:B2O3: Mg=80:91:132 dispensing, i.e. B2O3
Excess 30%, magnesium metal excess 10%.In stainless steel cask after preliminary mixing, load with alumina liner
Drum mixer, add the zirconia ball of a diameter of 10mm, zirconia ball and TiO2、B2O3And metal
The mass ratio of the gross weight sum of magnesium powder is 1:1, batch mixing 2 hours under the rotating speed of 25 turns/min, and raw material mixes
Close uniformly.Use stainless steel mould that material is pressed under 7MPa pressure the cylindric base of a diameter of 50mm
Body.The cylindric base substrate suppressed is put into graphite boat, after plugging plate, graphite boat is put into self-propagating reaction
Room, to the Ar gas shielded being passed through flowing after reative cell evacuation.After energising, the heating wire of white heat is by the one of material
End ignites, and cuts off electric current, maintains whole material reaction to terminate by combustion wave self-propagating, naturally cools to room temperature,
Collecting reaction product.After using jaw crusher that product is crushed to 5mm, ball milling is used to be ground by combustion product
It is milled to below 10 μm.Ball milling product being loaded glass reaction still, adds 4mol/L hydrochloric acid solution, hydrochloric acid is molten
The addition of liquid needs excess 25% on the basis of theoretical addition amount, after being sealed by reactor carries out material
Pickling purifies.Material is constantly stirred by acid cleaning process, heats, it is ensured that temperature maintains 90 DEG C, acid
Wash time 10h.Pickling terminate after by material filtering, washing, be dried 12h at 100 DEG C of vacuum drying ovens, dry
Dry rear material i.e. can get submicron order high-purity Ti B through comminution by gas stream2Powder.
Embodiment 3
By TiO2、B2O3With magnesium powder according to mass ratio TiO2:B2O3: Mg=80:105:132 dispensing, i.e. B2O3
Excess 50%, magnesium metal excess 10%.In stainless steel cask after preliminary mixing, load with alumina liner
Drum mixer, add the zirconia ball of a diameter of 10mm, zirconia ball and TiO2、B2O3And metal
The mass ratio of the gross weight sum of magnesium powder is 1.5:1, batch mixing 2 hours, raw material under the rotating speed of 25 turns/min
Mix homogeneously.Use stainless steel mould that material is pressed under 10MPa pressure a diameter of 50mm cylindric
Base substrate.The cylindric base substrate suppressed is put into graphite boat, after plugging plate, graphite boat is put into self-propagating anti-
Answer room, to the Ar gas shielded being passed through flowing after reative cell evacuation.After energising, the heating wire of white heat is by material
Igniting in one end, cuts off electric current, maintains whole material reaction to terminate by combustion wave self-propagating, naturally cools to room
Temperature, collecting reaction product.After using jaw crusher that product is crushed to 5mm, ball milling is used burning to be produced
Thing is ground to below 5 μm.Ball milling product is loaded glass reaction still, adds 3mol/L hydrochloric acid solution, salt
The addition of acid solution needs excess 25% on the basis of theoretical addition amount, to material after being sealed by reactor
Carry out pickling purification.Material is constantly stirred by acid cleaning process, heats, it is ensured that temperature maintains 100 DEG C,
Pickling time 10h.Pickling terminate after by material filtering, washing, be dried 12h at 100 DEG C of vacuum drying ovens,
Dried material i.e. can get submicron order high-purity Ti B through comminution by gas stream2Powder.
Embodiment 4
By TiO2、B2O3With magnesium powder according to mass ratio TiO2:B2O3: Mg=80:105:132 dispensing, i.e. B2O3
Excess 50%, magnesium metal excess 10%.In stainless steel cask after preliminary mixing, load with alumina liner
Drum mixer, add the zirconia ball of a diameter of 10mm, zirconia ball and TiO2、B2O3And metal
The mass ratio of the gross weight sum of magnesium powder is 1.5:1, batch mixing 2 hours, raw material under the rotating speed of 25 turns/min
Mix homogeneously.Use stainless steel mould that material is pressed under 10MPa pressure a diameter of 50mm cylindric
Base substrate.The cylindric base substrate suppressed is put into graphite boat, after plugging plate, graphite boat is put into self-propagating anti-
Answer room, to the Ar gas shielded being passed through flowing after reative cell evacuation.After energising, the heating wire of white heat is by material
Igniting in one end, cuts off electric current, maintains whole material reaction to terminate by combustion wave self-propagating, naturally cools to room
Temperature, collecting reaction product.After using jaw crusher that product is crushed to 5mm, ball milling is used burning to be produced
Thing is ground to below 5 μm.Ball milling product is loaded glass reaction still, adds 2mol/L hydrochloric acid solution, salt
The addition of acid solution needs excess 25% on the basis of theoretical addition amount, to material after being sealed by reactor
Carry out pickling purification.Material is constantly stirred by acid cleaning process, heats, it is ensured that temperature maintains 120 DEG C,
Pickling time 10h.Pickling terminate after by material filtering, washing, be dried 12h at 100 DEG C of vacuum drying ovens,
Dried material i.e. can get submicron order high-purity Ti B through comminution by gas stream2Powder.
The TiO used in the embodiment of the present invention2、B2O3It is technical grade product, wherein TiO with magnesium powder2For sharp
Titanium ore crystal formation, the granularity of three kinds of raw materials is respectively less than 50 μm.
As depicted in figs. 1 and 2, the submicron order TiB that the present invention provides2The self-propagating reaction device bag of powder body
Include pressure regulator 1, vacuum pump 2, graphite boat and self-propagating reaction room；Pressure regulator 1 is connected by adding thermode 6,
It is provided with shielding window 3 on the reactor chamber door 4 of self-propagating reaction room, can be observed certainly by shielding window 3
Spread the situation in reative cell；It is provided with on the reaction tube of self-propagating reaction room and adds thermode 6, reaction tube
Two ends are respectively provided with air inlet 8 and air vent 5；Air vent 5 is connected with vacuum pump 2, air inlet 8 and Ar
Gas cylinder 10 is connected, and is additionally provided with the flow for measuring Ar throughput between air inlet 8 and Ar gas cylinder 10
Meter 9.
Add the cylindric base substrate of thermal ignition to cause before self-propagating reaction, start vacuum pump 2, first to self-propagating
Reative cell evacuation, is passed through the Ar gas of flowing the most again, is discharged from air vent 5 by air from air inlet 8；
Flowing Ar gas is continued until that reaction terminates rear material and is cooled to room temperature.Graphite boat 7 is semicircle boat, including this
Body and graphite boat base 12, the both sides of graphite boat 7 are with dismountable block plate, and opening part is equipped with can the band of pull
Having the graphite boat cover plate of boring, Zhou Bishang is also with boring.
Embodiment 2 gained submicron order TiB2The XRD figure spectrum of powder body is as it is shown on figure 3, the present invention uses certainly
Spread synthetic method and prepare submicron order TiB2Powder body, gained submicron order TiB2Powder purity can reach
More than 98.5%, and can industrialization produce, synthesis technique is ripe, and production cost is relatively low.
The present invention is not limited to above-mentioned preferred forms, and anyone can draw it under the enlightenment of the present invention
His various forms of products, no matter but in its shape or structure, make any change, every have and the application
Technical scheme as same or like, within all falling within protection scope of the present invention.
Claims (10)
1. a submicron order TiB2The self-propagating synthesis method of powder body, it is characterised in that: include walking as follows
Rapid:
Step 1: weigh TiO respectively according to the ratio of weight ratio 80:91-105:120-1322、B2O3And metal
Magnesium powder, and carry out batch mixing, batch mixing is complete obtains batch mixing powder；
Step 2: after batch mixing is uniform, batch mixing powder is pressed into cylindric base substrate；
Step 3: described cylindric base substrate is put into graphite boat, then graphite boat is loaded self-propagating reaction room
In, it is passed through the Ar gas of flowing after the evacuation of self-propagating reaction room again, it is ensured that self-propagating reaction indoor are deposited without air
?；
Step 4: add the cylindric base substrate of thermal ignition to cause self-propagating reaction, end to be combusted, cool down cylinder
Shape base substrate, obtains the loose porous cylindric product that surface is black or grey black；
Step 5: by described cylindric product grind into powder；Addition hydrochloric acid solution carries out pickling to powder and carries
Pure, pickle constantly it is stirred by acid cleaning process and heats, being filtrated to get filter cake, washing filter cake, so
After filter cake is dried, after drying filter cake through grinding, obtain the submicron order TiB that granularity is 0.4-1 μm2
Powder body.
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, its feature
It is: by TiO in step 12、B2O3Add in drum mixer with metal magnesium powder and carry out batch mixing, described rolling
The drum rotation speed of cylinder batch mixer is 25-30r/min, and mixing time is at least 2h；Described drum mixer interior
Lining material matter is aluminium oxide；Having ball milling in described drum mixer, described ball milling is diameter 10-20mm oxygen
Change zirconium ball milling.
Submicron order TiB the most according to claim 22The self-propagating synthesis method of powder body, its feature
It is: described TiO2、B2O3With the weight sum of metal magnesium powder with the weight ratio of described ball milling it is
1:1-1.5。
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, its feature
Being: in step 2, the pressure that batch mixing powder is pressed into cylindric base substrate is 5-10MPa.
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, its feature
It is: described self-propagating reaction room is horizontal tubular reactor room, the reaction tube two ends of described self-propagating reaction room
It is respectively provided with air inlet and air vent.
Submicron order TiB the most according to claim 52The self-propagating synthesis method of powder body, its feature
It is: add the cylindric base substrate of thermal ignition to cause before self-propagating reaction, first to reative cell evacuation, then
It is passed through the Ar gas of flowing again from described air inlet, air is discharged from described air vent；Flowing Ar gas is always
Last till that reaction terminates rear material and is cooled to room temperature.
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, its feature
Be: described in add thermal ignition mode be that electric-heating-wire-heating ignites, heating wire is a diameter of 0.5-1mm tantalum wire；
After energising, ignited in one end of cylindric base substrate by heating wire.
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, its feature
It is: in step 5, in airtight glass lined reactor container, carries out pickling operation, described pickling operation
Before, use jaw crusher that described cylindric product is broken into the fritter of a diameter of 5-15mm, then use
Described fritter is ground to form the powder that granularity is 5-20 μm by rod milling or ball-grinding machine.
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, its feature
Being: in step 5, described pickling purification process uses 2-5mol/L hydrochloric acid solution, the quality of described hydrochloric acid
It is 1:2.5 with the mass ratio of magnesium powder；Pickling temperature controls at 80-100 DEG C, and pickling time is 10-20 hour.
Submicron order TiB the most according to claim 12The self-propagating synthesis method of powder body, it is special
Levying and be: in step 5, combustion product is after overpickling, and vacuum drying oven put into by the filter cake being filtrated to get
Drying, vacuum drying temperature is 80-120 DEG C, and the time is 10-15h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110817896A (en) * | 2019-12-15 | 2020-02-21 | 合肥中航纳米技术发展有限公司 | Preparation method of nano titanium diboride powder |
| CN114873600A (en) * | 2022-04-29 | 2022-08-09 | 淄博晟钛复合材料科技有限公司 | Preparation method of high-purity titanium diboride ceramic powder |
| CN115448360A (en) * | 2022-09-27 | 2022-12-09 | 攀枝花学院 | Method for preparing TiO material |
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| CN101891215A (en) * | 2010-07-15 | 2010-11-24 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN103265048A (en) * | 2013-06-14 | 2013-08-28 | 兰州理工大学 | Preparation method of TiB2 ultrafine powder material |
| CN103466649A (en) * | 2013-08-28 | 2013-12-25 | 东北大学 | Cleaner production method for preparing superfine boride powder through self-propagating metallurgy method |
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| CN101891215A (en) * | 2010-07-15 | 2010-11-24 | 武汉工程大学 | Method for preparing nano titanium diboride polycrystalline powder |
| CN103265048A (en) * | 2013-06-14 | 2013-08-28 | 兰州理工大学 | Preparation method of TiB2 ultrafine powder material |
| CN103466649A (en) * | 2013-08-28 | 2013-12-25 | 东北大学 | Cleaner production method for preparing superfine boride powder through self-propagating metallurgy method |
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| CN110817896A (en) * | 2019-12-15 | 2020-02-21 | 合肥中航纳米技术发展有限公司 | Preparation method of nano titanium diboride powder |
| CN110817896B (en) * | 2019-12-15 | 2022-07-01 | 合肥中航纳米技术发展有限公司 | Preparation method of nano titanium diboride powder |
| CN114873600A (en) * | 2022-04-29 | 2022-08-09 | 淄博晟钛复合材料科技有限公司 | Preparation method of high-purity titanium diboride ceramic powder |
| CN115448360A (en) * | 2022-09-27 | 2022-12-09 | 攀枝花学院 | Method for preparing TiO material |
| CN115448360B (en) * | 2022-09-27 | 2024-01-16 | 攀枝花学院 | Method for preparing TiO material |
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