CN103769592B - A kind of preparation method of spherical TiC/Fe cermet composite particles - Google Patents
A kind of preparation method of spherical TiC/Fe cermet composite particles Download PDFInfo
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Abstract
The invention provides a kind of preparation method of spherical TiC/Fe composite particles, belong to ceramic-metal composite field.With the Ti/Fe powder of cheapness and sucrose for raw material, obtain precursor powder by mechanical ball milling, drying, carbonization, fragmentation and screening, when inductively coupled plasma meltallizing, cause autoreaction synthesis, finally obtain spherical TiC/Fe composite particles.The cermet composite particles sphericity of preparation is good, and compact structure, Metal Phase and the mutual disperse of pottery are uniformly distributed, and wetability is good.Method technique of the present invention is simple, and flow process is short, and energy consumption is low, and abundant raw material is easy to get, and cost is low.
Description
Technical field
The present invention relates to composite and manufacture field, belong to the category of ceramic-metal composite.Specifically provide a kind of preparation method of spherical TiC/Fe cermet composite particles.
Background technology
Ceramic Reinforced MMCs combines the advantage of pottery and metal, not only possessed the high rigidity of ceramic material, high strength, high-melting-point simultaneously but also possess the performances such as the good machining property of metal and electric-conductivity heat-conductivity high, it is applied in and is developed greatly in recent years.
TiC ceramic phase, because having low friction coefficient, high rigidity, low-density and good high-temperature stability, is widely used in preparation TiC grain reinforced metal ceramic composite.Wherein TiC/Fe composite is because of its distinctive high specific strength, high ratio modulus, wearability and the premium properties such as high temperature resistant, has progressively developed into a kind of abrasion-resistant coating material and the cutter material with wide range of industrial applications prospect.
In powder metallurgical production technique, material powder is one of key factor affecting the final performance of goods.And be no matter the plasma-coated raw meal for material protection, or for the preparation of the raw meal of hard tool and ceramic/metal composite materials, be all the multicomponent mixture that hard phase combines together with metal or alloy.It is more difficult for only obtaining uniform composite powder by mechanical mixture mode.Further, there is the bad problem of wetability in TiC ceramic phase and Fe metallic matrix, easily causes combination interface to pollute, and reduces the performance of goods.
Composite particles is the surface consolidation material of rising in recent years and the quality raw materials of high-performance composite materials, it can be utilized to prepare the coating with performances such as wear-resisting, corrosion-resistant, heat-resisting and resistance to high temperature oxidation, also can prepare multi-element metal and metal-ceramic body composite material.The production of current China composite particles mainly adopts liquid-phase hydrogenatin reducing process, and this method complex process, influence factor is many and product variety is limited; Other production methods existing can not satisfy social needs.
The inductively coupled plasma technology risen have temperature high, pollute less, atmosphere the is adjustable advantage such as controlled.Inductively coupled plasma technology is that preparation component is even, defect is few, the good approach of the spherical powder of good fluidity, has both lower production cost and higher productivity ratio.In order to make that metal is pre-alloyed, the heterogeneous mixture homogenizing that makes density difference larger, densification, and then obtain the good nodularization powder of the mutual dispersivity of metal/ceramic two-phase, rely on inductively coupled plasma technology to prepare the method for spherical TiC/Fe composite particles, yet there are no relevant report.
Summary of the invention
The uniform technique of two-phase disperse is simple, the preparation method of process control, spherical metal ceramic composite particles with low cost to the object of the present invention is to provide a kind of energy acquisition to have, and solves the shortcomings such as existing method cost is high, complex process, wayward, the production cycle is long.
The technical solution adopted in the present invention is: adopt cheap Ti/Fe powder and sucrose as raw material, obtains precursor powder through mechanical ball milling, vacuum drying, carbonization treatment, fragmentation and the technique such as to sieve.Again by precursor powder through plasma spray, precursor powder, through causing autoreaction synthesis while plasma high-temperature district, obtains TiC phase and the uniform spherical composite pellets of the mutual disperse of Fe phase two-phase.
A preparation method for spherical TiC/Fe cermet composite particles, comprises following processing step:
1, the preparation of precursor powder: with cheap Ti/Fe powder and sucrose for raw material, the proportioning of powder is carried out according to Ti:C atomic ratio 1:1, be that medium carries out mechanical ball milling with absolute ethyl alcohol, gained slurry is carried out vacuum drying, then under nitrogen protection atmosphere, carry out carbonization treatment, gained cellular block is carried out fragmentation, sieving obtains precursor powder;
2, the preparation of spherical TiC/Fe composite particles: utilize inductively coupled plasma technology, after forvacuum, each technological parameter of adjustment plasma, obtains the plasma torch of stable operation; Gained precursor powder is carried out the process of inductively coupled plasma meltallizing: precursor powder absorbs heat rapidly when passing plasma high-temperature district and causes autoreaction synthesis, powder melts under the effect of dual heat also gathers cold curing globulate powder, obtains spherical TiC/Fe cermet composite particles.
Mechanical ball milling described in step 1, ratio of grinding media to material 5:1, Ball-milling Time 24 ~ 48h, by gained slip at 120 DEG C of vacuum drying 12h.Powder after drying is carried out carbonization treatment in nitrogen protection atmosphere, and carbonization system is 250 DEG C of insulation 1h, 350 insulation 2 ~ 4h, broken, sieving obtains precursor powder.
The preparation of spherical TiC/Fe composite particles described in step 2 is to 1.0 × 10 by the forvacuum of diffusion pump unit
-3pa, sets up the inductively coupled plasma of stable operation, and its major parameter is: power 40KW, argon gas working gas flow 30 ~ 60slpm, argon gas limit throughput 100 ~ 200slpm, system negative pressure 1000 ~ 1200mm water column.For carrying gas, above-mentioned precursor powder is axially sent into plasma high-temperature district with argon gas, carrier gas flux 3.5 ~ 10slpm, powder feed rate is 10 ~ 30g/min.
The present invention is raw materials used is Ti/Fe powder, and cost is low; There is provided carbon source with sucrose, the amorphous carbon reactivity obtained is high, act as the effect of bonding agent simultaneously.
Adopt above technical scheme, the invention has the advantages that:
1, abundant raw material is easy to get, with low cost.
2, the time is short, economize energy, reduces costs.
3, utilize plasma technique to cause autoreaction synthesis, technique is simple, and flow process is short, and production efficiency is high.
4, prepared cermet composite particles sphericity is good, and compact structure, Metal Phase and the mutual disperse of ceramic phase are uniformly distributed, and wetability is good.
Accompanying drawing explanation
Fig. 1 is the cross section QBSD photo of precursor powder.
Fig. 2 is the cross section QBSD photo of spherical TiC/Fe composite particles prepared by the present invention.
Detailed description of the invention
Embodiment 1:
1, the preparation of precursor powder
With Ti/Fe powder and sucrose for raw material, stoichiometrically 1:1 carries out proportioning, is that medium carries out mechanical ball milling, ratio of grinding media to material 5:1 with absolute ethyl alcohol, and Ball-milling Time 24h, by gained slip at 120 DEG C of vacuum drying 12h.Powder after drying is carried out carbonization treatment in nitrogen protection atmosphere, and carbonization system is 250 DEG C of insulation 1h, 350 insulation 2h, broken, sieving obtains precursor powder.
2, the preparation of spherical TiC/Fe composite particles
By the forvacuum of diffusion pump unit to 1.0 × 10
-3pa, sets up the inductively coupled plasma of stable operation, and its major parameter is: power 40KW, argon gas working gas flow 35slpm, argon gas limit throughput 150slpm, system negative pressure 1000mm water column.For carrying gas, above-mentioned precursor powder is axially sent into plasma high-temperature district with argon gas, carrier gas flux 10slpm, powder feeding rate is 10g/min.Precursor powder is heat absorption melting when passing plasma high-temperature district, and cause autoreaction synthesis, molten melt drop is polycondensation globulate TiC/Fe composite particles under surface tension effects finally simultaneously.
Embodiment 2:
1, the preparation of precursor powder
With Ti/Fe powder and sucrose for raw material, stoichiometrically 1:1 carries out proportioning, is that medium carries out mechanical ball milling, ratio of grinding media to material 5:1 with absolute ethyl alcohol, and Ball-milling Time 36h, by gained slip at 120 DEG C of vacuum drying 12h.Powder after drying is carried out carbonization treatment in the atmosphere of nitrogen limit, and carbonization system is 250 DEG C of insulation 1h, 350 insulation 3h, broken, sieving obtains precursor powder.
2, the preparation of spherical TiC/Fe composite particles
By the forvacuum of diffusion pump unit to 1.0 × 10
-3pa, sets up the inductively coupled plasma of stable operation, and its major parameter is: power 40KW, argon gas working gas flow 60slpm, argon gas limit throughput 100slpm, system negative pressure 1100mm water column.For carrying gas, above-mentioned precursor powder is axially sent into plasma high-temperature district with argon gas, carrier gas flux 3.5slpm, powder feeding rate is 15g/min.Precursor powder is heat absorption melting when passing plasma high-temperature district, and cause autoreaction synthesis, molten melt drop is polycondensation globulate TiC/Fe composite particles under surface tension effects finally simultaneously.
Embodiment 3:
1, the preparation of precursor powder
With Ti/Fe powder and sucrose for raw material, stoichiometrically 1:1 carries out proportioning, is that medium carries out mechanical ball milling, ratio of grinding media to material 5:1 with absolute ethyl alcohol, and Ball-milling Time 48h, by gained slip at 120 DEG C of vacuum drying 12h.Powder after drying is carried out carbonization treatment in the atmosphere of nitrogen limit, and carbonization system is 250 DEG C of insulation 1h, and 350 insulation 4h, fragmentation is sieved and obtained precursor powder.
2, the preparation of spherical TiC/Fe composite particles
By the forvacuum of diffusion pump unit to 1.0 × 10
-3pa, sets up the inductively coupled plasma of stable operation, and its major parameter is: power 40KW, argon gas working gas flow 60slpm, argon gas limit throughput 120slpm, system negative pressure 1200mm water column.For carrying gas, above-mentioned precursor powder is axially sent into plasma high-temperature district with argon gas, carrier gas flux 5slpm, powder feeding rate is 20g/min.Precursor powder is heat absorption melting when passing plasma high-temperature district, and cause autoreaction synthesis, molten melt drop is polycondensation globulate TiC/Fe composite particles under surface tension effects finally simultaneously.
Claims (5)
1. a preparation method for spherical TiC/Fe cermet composite particles, is characterized in that: comprise following processing step:
1) preparation of precursor powder: with Ti/Fe powder and sucrose for raw material, the proportioning of powder is carried out according to Ti:C atomic ratio 1:1, be that medium carries out mechanical ball milling with absolute ethyl alcohol, gained slurry is carried out vacuum drying, then under nitrogen protection atmosphere, carry out carbonization treatment, gained cellular block is carried out fragmentation, sieving obtains precursor powder;
2) preparation of spherical TiC/Fe composite particles: utilize inductively coupled plasma technology, after forvacuum, each technological parameter of adjustment plasma, obtains the plasma torch of stable operation; Gained precursor powder is carried out the process of inductively coupled plasma meltallizing: precursor powder absorbs heat rapidly when passing plasma high-temperature district and causes autoreaction synthesis, powder melts under the effect of dual heat also gathers cold curing globulate powder, obtains spherical TiC/Fe cermet composite particles.
2. the preparation method of a kind of spherical TiC/Fe cermet composite particles according to claim 1, is characterized in that: step 1) described ball milling time material ball ratio 1:5, Ball-milling Time 24 ~ 48h; Vacuum drying temperature is 120 DEG C; Carbonization treatment system is: heating rate 5 DEG C/min, 250 DEG C of insulation 1h, 350 DEG C of insulation 2 ~ 4h.
3. the preparation method of a kind of spherical TiC/Fe cermet composite particles according to claim 1, is characterized in that: step 2) described inductively coupled plasma plays forearc, and carry out forvacuum by diffusion pump unit and reach 1.0 × 10
-3pa, prevents the oxidation of Ti/Fe and the reaction of C to run off.
4. the preparation method of a kind of spherical TiC/Fe cermet composite particles according to claim 1, it is characterized in that: step 2) described inductively coupled plasma, its main technologic parameters is: employing argon gas is work gas, limit gas and carrier gas, working gas flow 30 ~ 60slpm, limit throughput 100 ~ 200slpm, system negative pressure 1000 ~ 1200mm water column, powder carries throughput 3.5 ~ 10slpm, powder feed rate is 10 ~ 30g/min, equipment power output 40KW.
5. the preparation method of a kind of spherical TiC/Fe cermet composite particles according to claim 1, is characterized in that: cermet composite particles is of a size of 45 ~ 75 μm, is the spherical powder that the mutual dispersivity of metal/ceramic two-phase is good.
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