CN103769592A - Preparation method of spherical TiC/Fe metal-ceramic compound particles - Google Patents
Preparation method of spherical TiC/Fe metal-ceramic compound particles Download PDFInfo
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- CN103769592A CN103769592A CN201410018359.1A CN201410018359A CN103769592A CN 103769592 A CN103769592 A CN 103769592A CN 201410018359 A CN201410018359 A CN 201410018359A CN 103769592 A CN103769592 A CN 103769592A
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Abstract
The invention provides a preparation method of spherical TiC/Fe metal-ceramic compound particles, and belongs to the field of metal-ceramic compound materials. The method comprises the following steps: performing mechanical ball milling, drying, carbonization, crushing and sieving on cheap Ti/Fe powder and sugar cane serving as raw materials to obtain precursor powder; triggering self-reaction synthesis during inductive coupling plasma meltallizing to obtain the spherical TiC/Fe metal-ceramic compound particles. The prepared spherical TiC/Fe metal-ceramic compound particles have the advantages of high degree of sphericity, dense structure, mutual dispersion and uniform distribution of a metal phase and a ceramic phase, and excellent wetting property. The method provided by the invention has the advantages of simple process, short flow, low energy consumption, rich and readily available raw materials and low cost.
Description
Technical field
The present invention relates to composite and manufacture field, belong to the category of ceramic-metal composite.A kind of preparation method of spherical TiC/Fe cermet composite particles is provided especially.
Technical background
Ceramic Reinforced MMCs combines the advantage of pottery and metal, not only possess high rigidity, high strength, the high-melting-point while of ceramic material but also possess the performance such as machining property and electric-conductivity heat-conductivity high that metal is good, it is applied in recent years and is developed greatly.
TiC ceramic phase, because having low friction coefficient, high rigidity, low-density and good high-temperature stability, is widely used in preparing TiC grain reinforced metal ceramic composite.Wherein TiC/Fe composite, 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 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 no matter be the plasma-coated raw meal for material protection, still 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 only depending on mechanical mixture mode and obtaining uniform composite powder.And there is the bad problem of wetability in TiC ceramic phase and Fe metallic matrix, easily cause combination interface to pollute, reduce 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, can utilize it to prepare the coating of performances such as thering is wear-resisting, corrosion-resistant, heat-resisting and resistance to high temperature oxidation, also can prepare multi-element metal and metal-ceramic system composite.The at present production of China's composite particles mainly adopts liquid-phase hydrogenatin reducing process, and this method complex process, influence factor is many and product variety is limited; Existing other production methods can not satisfy social needs.
The inductively coupled plasma technology rising 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.For make metal pre-alloyed, make heterogeneous mixture homogenizing, densification that density difference is larger, and then the good nodularization powder of the acquisition 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 object of the present invention is to provide a kind of energy to obtain the preparation method with the spherical metal ceramic composite particles that the uniform technique of two-phase disperse is simple, process is controlled, with low cost, solve 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, make precursor powder through mechanical ball milling, vacuum drying, carbonization treatment, fragmentation and the technique such as sieve.By precursor powder process plasma spray, precursor powder, synthetic through causing autoreaction in plasma high-temperature district, obtains TiC phase and the uniform spherical composite pellets of the mutual disperse of Fe phase two-phase again.
A preparation method for spherical TiC/Fe cermet composite particles, comprises following processing step:
1, the preparation of precursor powder: take cheap Ti/Fe powder and sucrose as raw material, carry out the proportioning of powder according to Ti:C atomic ratio 1:1, carry out mechanical ball milling take absolute ethyl alcohol as medium, gained slurry is carried out to vacuum drying, then under nitrogen protection atmosphere, carry out carbonization treatment, by gained cellular block carry out fragmentation, sieving obtains precursor powder;
2, the preparation of spherical TiC/Fe composite particles: utilize inductively coupled plasma technology, after forvacuum, adjust the each technological parameter of plasma, obtain the plasma torch of stable operation; Gained precursor powder is carried out to the processing of inductively coupled plasma meltallizing: precursor powder absorbs heat rapidly and causes autoreaction and synthesize when through plasma high-temperature district, under the effect of dual heat, powder melts poly-cold curing globulate powder, obtain 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 ℃ of vacuum drying 12h.After being dried, powder carries out carbonization treatment in nitrogen protection atmosphere, and carbonization system is 250 ℃ of insulation 1h, and 350 insulation 2～4h are broken, sieving obtains precursor powder.
Described in step 2, the preparation of spherical TiC/Fe composite particles is by diffusion pump unit forvacuum 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 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; Provide carbon source with sucrose, the amorphous carbon reactivity obtaining is high, the effect of simultaneously having served as bonding agent.
Adopt above technical scheme, the invention has the advantages that:
1, abundant raw material is easy to get, with low cost.
2, the time short, save the energy, reduce costs.
3, utilize plasma technique to cause autoreaction synthetic, technique is simple, and flow process is short, and production efficiency is high.
4, prepared cermet composite particles sphericity is good, compact structure, and the mutual disperse of Metal Phase and ceramic phase is 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 the spherical TiC/Fe composite particles prepared of the present invention.
Specific embodiments
Embodiment 1:
1, the preparation of precursor powder
Take Ti/Fe powder and sucrose as raw material, carry out proportioning by stoichiometric proportion 1:1, carry out mechanical ball milling take absolute ethyl alcohol as medium, ratio of grinding media to material 5:1, Ball-milling Time 24h, by gained slip at 120 ℃ of vacuum drying 12h.After being dried, powder carries out carbonization treatment in nitrogen protection atmosphere, and carbonization system is 250 ℃ of insulation 1h, and 350 insulation 2h are broken, sieving obtains precursor powder.
2, the preparation of spherical TiC/Fe composite particles
By diffusion pump unit forvacuum 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, in the melting of absorbing heat when the plasma high-temperature district, causes autoreaction synthetic simultaneously, and molten melt drop is polycondensation globulate TiC/Fe composite particles under surface tension effects finally.
Embodiment 2:
1, the preparation of precursor powder
Take Ti/Fe powder and sucrose as raw material, carry out proportioning by stoichiometric proportion 1:1, carry out mechanical ball milling take absolute ethyl alcohol as medium, ratio of grinding media to material 5:1, Ball-milling Time 36h, by gained slip at 120 ℃ of vacuum drying 12h.After being dried, powder carries out carbonization treatment in the atmosphere of nitrogen limit, and carbonization system is 250 ℃ of insulation 1h, and 350 insulation 3h are broken, sieving obtains precursor powder.
2, the preparation of spherical TiC/Fe composite particles
By diffusion pump unit forvacuum 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, in the melting of absorbing heat when the plasma high-temperature district, causes autoreaction synthetic simultaneously, and molten melt drop is polycondensation globulate TiC/Fe composite particles under surface tension effects finally.
Embodiment 3:
1, the preparation of precursor powder
Take Ti/Fe powder and sucrose as raw material, carry out proportioning by stoichiometric proportion 1:1, carry out mechanical ball milling take absolute ethyl alcohol as medium, ratio of grinding media to material 5:1, Ball-milling Time 48h, by gained slip at 120 ℃ of vacuum drying 12h.After being dried, powder carries out carbonization treatment in the atmosphere of nitrogen limit, and carbonization system is 250 ℃ of insulation 1h, 350 insulation 4h, and fragmentation is sieved and is obtained precursor powder.
2, the preparation of spherical TiC/Fe composite particles
By diffusion pump unit forvacuum 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, in the melting of absorbing heat when the plasma high-temperature district, causes autoreaction synthetic simultaneously, and molten melt drop is polycondensation globulate TiC/Fe composite particles under surface tension effects finally.
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: take cheap Ti/Fe powder and sucrose as raw material, carry out the proportioning of powder according to Ti:C atomic ratio 1:1, carry out mechanical ball milling take absolute ethyl alcohol as medium, gained slurry is carried out to vacuum drying, then under nitrogen protection atmosphere, carry out carbonization treatment, by gained cellular block carry out fragmentation, sieving obtains precursor powder;
2) preparation of spherical TiC/Fe composite particles: utilize inductively coupled plasma technology, after forvacuum, adjust the each technological parameter of plasma, obtain the plasma torch of stable operation; Gained precursor powder is carried out to the processing of inductively coupled plasma meltallizing: precursor powder absorbs heat rapidly and causes autoreaction and synthesize when through plasma high-temperature district, under the effect of dual heat, powder melts poly-cold curing globulate powder, obtain 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: material ball ratio 1:5 when ball milling described in step 1), Ball-milling Time 24～48h; Vacuum drying temperature is 120 ℃; Carbonization treatment system is: 5 ℃/min of heating rate, 250 ℃ of insulation 1h, 350 ℃ 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 expanding pump assembly and reach 1.0 × 10
-3pa, prevents the oxidation of Ti/Fe and the reaction of C loss.
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: adopting 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 μ m, the good spherical powder of the mutual dispersivity of metal/ceramic two-phase.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106424746A (en) * | 2016-10-31 | 2017-02-22 | 湖南航天新材料技术研究院有限公司 | Device and method for preparing metal ceramic composite powder material |
| CN108080648A (en) * | 2017-12-18 | 2018-05-29 | 北京科技大学 | A kind of method that Fe/TiC composite granules are prepared in situ in vacuum carbothermal reduction |
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| CN102179521A (en) * | 2011-04-20 | 2011-09-14 | 北京科技大学 | Preparation method of ultra-fine spherical nickel coated titanium composite powder |
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Patent Citations (6)
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| US5350437A (en) * | 1991-05-27 | 1994-09-27 | Daido Tokushuko Kabushiki Kaisha | Method of manufacturing an alloy powder with hard particles dispersed therein |
| UA64966A (en) * | 2003-04-01 | 2004-03-15 | Serhii Serhiiovych Raiev | Method for production of the powder |
| CN1913200A (en) * | 2006-08-22 | 2007-02-14 | 深圳市贝特瑞电子材料有限公司 | Silicon carbone compound negative polar material of lithium ion battery and its preparation method |
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| CN106424746A (en) * | 2016-10-31 | 2017-02-22 | 湖南航天新材料技术研究院有限公司 | Device and method for preparing metal ceramic composite powder material |
| CN108080648A (en) * | 2017-12-18 | 2018-05-29 | 北京科技大学 | A kind of method that Fe/TiC composite granules are prepared in situ in vacuum carbothermal reduction |
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