CN106431416A - Zirconium carbide-zirconium diboride complex-phase ceramic powder synthesized through thermal explosion and preparation method thereof - Google Patents
Zirconium carbide-zirconium diboride complex-phase ceramic powder synthesized through thermal explosion and preparation method thereof Download PDFInfo
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Abstract
The invention relates to zirconium carbide-zirconium diboride complex-phase ceramic powder synthesized through thermal explosion and a preparation method thereof. The ceramic powder is prepared from, by mass, 0%-30% of Al powder and 70%-100% of Zr powder and B4C powder, wherein the molar ratio of Zr to B4C is 3:1, and the sum of the mass percent of the components is 100%. The preparation method comprises the steps that the Al powder, the Zr powder and the B4C powder which are dried are fully mixed and then pressed into green blank blocks, a thermal explosion chemical reaction is conducted in an induction furnace which is vacuumized and then is full of Ar gas, and the ceramic powder is obtained. The ceramic powder and the preparation method thereof have the advantages that reacting is rapid, energy saving and cleanliness are achieved, and the product compounding degree is high; the product is a ceramic compound mainly containing ZrC powder and ZrB2 powder and can be directly applied as a zirconium carbide-zirconium diboride complex-phase ceramic powder material, the zirconium carbide-zirconium diboride complex-phase ceramic powder can be separated after other impurities in the compound are washed off through extraction, and then the single pure zirconium carbide or pure zirconium diboride ceramic powder can be obtained for application.
Description
Technical field
The invention belongs to new transition metal carbide, boride composite ceramic powders field of material technology and in particular to
High-frequency induction thermal explosion is utilized to synthesize a kind of zirconium carbide, zirconium diboride composite ceramic powders and preparation method thereof under protective atmosphere.
Background technology
The chemical and physical features of zirconium carbide (ZrC) are stable, have high fusing point and hardness, excellent wear-and corrosion-resistant
Property, good chemical stability and certain metallic conduction, heat conductivility and be widely used in cutting tool, wear-resistance bit,
The fields such as the overcoat in electronic devices and components, atomic pile.As hardening constituent, ZrC is more used as in metal-base composites
Enhancing particle.ZrC has typical face-centred cubic structure, has the compound spy of comprehensive metallic bond, ionic bond and covalent bond
Property.ZrC also has great reaction and forms heat simultaneously, it can by the carbothermic reduction reaction under high temperature, magnesiothermic reduction reaction,
The methods such as mechanical alloying, chemical vapor deposition, sol-gel, microwave process for synthesizing are synthesizing or to prepare.Or these methods need
Want high temperature hyperpyrexia, and complex technical process, or the seriously polluted of product can be led to, thus leading to generated ZrC granule
Thick and impure, and then reduce its performance and application.Wherein traditional ZrC preparation is carbothermic method, the method by Zr or
ZrO2It is placed in the graphite tube furnace of vacuum with the mixture of C and is heated under 2200 DEG C of high temperature above carrying out carbonization, there is device
Complexity, response time length, high energy consumption, product phosphorus content be low and the low deficiency of purity.
Zirconium diboride (ZrB2) it is hexahedron crystal formation, gray crystallizes or powder, has good resistance to elevated temperatures, anti-corruption
Corrosion, conduction and heat conductivility, higher hardness, often/elevated temperature strength and chemical stability, and thermal shock resistance are good, resistance
The advantages of little, resistance to high temperature oxidation, be a kind of high-temperature structural material of excellent performance.Zirconium diboride is widely used in thermal structure pottery
The fields such as porcelain, composite, electrode material, thin-film material, refractory material, nuclear control material, such as aerospace exotic material,
The solid material of wear resistant smooth, the electrode material of cutting element, temperature difference heat galvanic couple protection pipe and electrolyzing fused compound or multiple
The hard of condensation material strengthens phase.It is particularly suited for use as the surface of rolling bearing ball.The preparation method that zirconium diboride is commonly used is main
There are metal zirconium and boron direct reaction method, boron carbide method, carbon reduction method, vapour deposition process.As zirconium diboride can be by metal zirconium and carbon
Change boron, be heated to 2000 DEG C in argon stream after boron nitride mixing and be obtained it is also possible to ZrO2、B4C, C adopt carbon heat also for raw material
Former method 2000～2100 DEG C in logical nitrogen carbon shirt-circuiting furnace at a temperature of synthesis or in vacuum arc furnace ignition synthesize.But these methods at present
The zirconium diboride powder granularity of preparation is big, activity is low, be difficult to sinter, and high pure and ultra-fine powder body is difficult to industry in a large number and is combined to, limit
Make it extensively to apply.
Easily lead to that carbonization is uneven, purity is low due to the process for producing of traditional zirconium carbide, zirconium diboride, sintering
Poor-performing, seriously constrains it as the impact of performance of hard enhanced particles, have impact on the exploitation of nonferrous materials and answer
With hindering the development of China's powder metallurgy industry.
Content of the invention
In view of this, the present invention be directed to traditional prepare zirconium carbide, the defect of zirconium diboride composite ceramic powders technology with
Not enough the problems such as, there is provided a kind of thermal explosion synthesis zirconium carbide, zirconium diboride composite ceramic powders and preparation method thereof.
In order to solve above-mentioned technical problem, the invention discloses a kind of thermal explosion synthesis zirconium carbide, zirconium diboride complex phase ceramic
Powder, is made up of following raw material by mass percentage：Al powder 0～30wt.%, Zr powder and B4C powder totally 70～100wt.%, wherein
Zr powder, B4The mol ratio of C powder is 3:1, above constituent mass percentage ratio sum is 100%.
Wherein raw material Zr powder, its purity is 98.5%, particle mean size～38 μm.
Wherein raw material B4C powder, its purity>98%, particle mean size～40 μm.
Wherein Al powder, its purity>99%, particle mean size～29 μm.
Above-mentioned thermal explosion synthesis zirconium carbide, the preparation method of zirconium diboride composite ceramic powders, specifically real according to following steps
Apply：
Step 1：Respectively by raw material A l powder, Zr powder and B4C powder is dried 4～6h at 80～90 DEG C；
Step 2：Al powder 0～30wt.%, Zr powder and B are weighed respectively according to mass ratio4C powder totally 70～100wt.%, wherein
Zr powder, B4The mol ratio of C powder is 3:1, above constituent mass percentage ratio sum is 100%；
Step 3：Al powder, Zr powder and the B that step 2 is weighed4C powder carries out ball milling and is sufficiently mixed, then by mixed powder 35
It is pressed into cylindric green briquette, diameter 20mm, thickness～15mm, relative density is 65 ± 3% under～40MPa pressure；
Step 4：Cylindric green briquette in step 3 is put into induction furnace and carries out thermal explosion chemical reaction, obtain zirconium carbide, two
The composite ceramic powders of zirconium boride.
The specific embodiment of thermal explosion chemical reaction is：Green briquette is positioned in the water-cooled induction coil in induction furnace,
It is full of Ar gas after first evacuation, connects SIT high frequency induction power supply, adjust what Efco-Northrup furnace was applied within 20～25s time
Voltage increases to 65～80 volts (electric current correspondingly can increase to 45～60 peaces from 0 therewith), the entirety of the briquet that now can ignite from 0
Reaction, there is overall very exothermic combustion reaction in briquet after the electrified regulation several seconds, entirely reacts after moment quickly completes
And power-off immediately, obtaining under the chilling of coil interior circulation water is in loose and the zirconium carbide of layer structure of expansion, two boronations
The composite ceramic powders of zirconium.
Compared with prior art, the present invention can obtain including following technique effect：
The present invention have be swift in response, the features such as process is simple, energy-saving clean, product Composite degree are high, based on product
Contain ZrC powder, ZrB2The ceramic complexes of powder, can directly as zirconium carbide, zirconium diboride composite ceramic powders materials application,
After the other impurities washing off in complex can be extracted, zirconium carbide, zirconium diboride composite ceramic powders are carried out separating, thus obtaining list
One pure zirconium carbide or pure zirconium diboride ceramic powder are applying.The present invention be zirconium carbide, zirconium diboride ceramic powder or the two
Composite powder produce provide a kind of new thinking.
Certainly, the arbitrary product implementing the present invention it is not absolutely required to reach all the above technique effect simultaneously.
Brief description
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the present invention, this
Bright schematic description and description is used for explaining the present invention, does not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 be thermal explosion of the present invention synthesize zirconium carbide, in the preparation method of zirconium boride composite ceramic powders induction furnace structure
Figure；
In figure, 1. reative cell, 2. graphite crucible, 3. green briquette, 4.SIT high frequency electric source, 5. water-cooled induction coil；
Fig. 2 is the XRD identification spectrogram of the synthetic product in embodiment.
Specific embodiment
The present invention is described in further detail by following embodiment, coordinates embodiment to describe the embodiment party of the present invention in detail
Formula, thereby to the present invention, how application technology means solve technical problem and to reach realizing process and fully managing of technology effect
Solution is simultaneously implemented according to this.According to the final observed result of the present invention, now the embodiment of the present invention is elaborated：This enforcement is real
Example is carried out under premised on technical solution of the present invention, contains detailed embodiment and specific operating process.
Following embodiment raw materials are wherein Al powder 0～30wt.%, Zr powder and B4C powder totally 70～100wt.%,
Wherein Zr powder, B4The mol ratio of C powder is 3：1, above constituent mass percentage ratio sum is 100%.
The principles of chemistry of the present invention are：3Zr+B4C=ZrC+2ZrB2, show raw material Zr powder：B4The mol ratio of C powder is 3:1.
Therefore, Al powder 0～30wt.%, Zr powder and B during dispensing4C powder totally 70～100wt.%, wherein Zr powder, B4C powder presses Zr:B4C=3:
1 mol ratio is allocated, and above constituent mass percentage ratio sum is 100%.
Al powder in the present invention, its purity>99%, particle mean size～29 μm；Zr powder, its purity is 98.5%, particle mean size
～38 μm；B4C powder, its purity>98%, particle mean size～40 μm.
In the present invention, additive A l powder plays to the granular size of the composite ceramic powders preparing zirconium carbide, zirconium diboride
Vital effect.On the one hand, in course of reaction, the relatively early of lower temperature liquid phase Al (fusing point about 933K) is easier to appearance, is powder
Phase counterdiffusion between end provides more easy passage, a large amount of Zr, B4C powder will be dissolved in Al liquid phase, and rapidly and fully spread
With sprawl so that the surface area that contacts with each other improves, thus in the violent exothermic chemical reaction of moment induction, generate stable ZrC,
ZrB2Granule.On the other hand, the Al of interpolation serves the effect of diluent during thermal expousure, reduces the burning of reaction
Temperature, thus greatly inhibit generated ZrC, ZrB2The growth of crystal grain and roughening.
The structure of the induction furnace that thermal explosion chemical reaction is adopted as is shown in fig. 1, is provided using SIT high frequency electric source 4 and adds
Thermal source, to be ignited briquet using the high-frequency water-cooling induction coil 5 being connected with heavy current, once being ignited, briquet will be overall in moment
There is thermal expousure, the reaction of whole briquet almost completes simultaneously.Immediately power-off, the urgency of the recirculated water in induction coil
Fast cooling under cold, the principal product that final acquisition is bulk is zirconium carbide, the composite ceramic powders of zirconium diboride.Due to this reaction
Formerly being full of after evacuation carries out so that thermal expousure product is not polluted by impurity such as oxygen in the environment of Ar gas shielded, its product
Can be directly as zirconium carbide, zirconium diboride composite ceramic powders materials application, after also can extracting the other impurities washing off in complex
Zirconium carbide, zirconium diboride composite ceramic powders are carried out separating, thus obtaining single zirconium carbide or pure zirconium diboride ceramic
End is applying.
Thermal explosion synthesis portion of product on the premise of not damaging its appearance structure levigate to make XRD (model D/Max
2500PC, Rigaku., Japan) Discriminating materials to be determining the composition of product.
Embodiment 1：Zr-B4C system
For Zr-B4C system, by mole composed of the following components：Zr powder 75mol.%, B4C powder 25mol.%,
The two mol ratio is 3:1st, molar percentage sum is 100mol.%.By at 80～90 DEG C be dried 4～6h after Zr powder and
B4C powder presses 3:After 1 16.0 grams of molar ratio weighing mix homogeneously, compressing cylindric green compact under 35～40MPa pressure
Block, diameter 20mm, thickness 15mm, relative density is 65 ± 3%.Then this briquet 3 is put in graphite crucible 2, then one piece
It is positioned in the reative cell 1 in induction furnace, be full of Ar gas after first evacuation to protect, connect SIT high frequency electric source 4, in 20～25s
The voltage that in time, regulation Efco-Northrup furnace is applied increases to 65 volts (electric current correspondingly can increase to 45 peaces from 0 therewith) from 0,
Now can ignite the W-response of briquet, and after the electrified regulation several seconds, briquet occurs overall very exothermic combustion reaction, entirely
Reaction power-off immediately after moment quickly completes, obtaining under the chilling of coil interior circulation water is in stratiform that is loose and expanding
The final product of structure.
XRD Discriminating materials are carried out to this thermal explosion product, shown in its result such as Fig. 2 (a), show this thermal explosion synthetic product only by
ZrC、ZrB2Two phase compositions.
Embodiment 2：10wt.%Al-Zr-B4C system
For 10wt.%Al-Zr-B4C system, raw material is composed of the following components by mass percentage：Al powder 10wt.%,
Zr powder and B4The common 90wt.% of C powder, wherein Zr powder, B4C powder presses Zr:B4C=3:1 mol ratio is prepared, three kinds of constituent masses
Percentage ratio sum is 100%.Al powder 4～6h after, Zr powder and B will be dried at 80～90 DEG C4C powder is claimed by this component ratio
Amount, wherein Zr powder and B4The mol ratio of C powder is 3:1, suppress under 35～40MPa pressure after 15.7 grams of total weight mix homogeneously
The cylindric green briquette of molding, diameter 20mm, thickness～15mm, relative density is 65 ± 3%.Then this briquet 3 is put into stone
In black crucible 2, then in one piece of reative cell being positioned in induction furnace 1, it is full of Ar gas after first evacuation to protect, connects SIT
High frequency electric source 4, adjust within 20～25s time the voltage that applied of Efco-Northrup furnace increase to from 0～70 volts (electric current therewith can
Correspondingly increase to～50 peaces from 0), the W-response of the briquet that now can ignite, there is entirety in briquet after the electrified regulation several seconds
Very exothermic combustion reaction, entirely react power-off immediately after moment quickly completes, under the chilling of coil interior circulation water
And obtaining is in loose and the layer structure of expansion final product.
XRD Discriminating materials are carried out to this thermal explosion product, shown in its result such as Fig. 2 (b), shows that this thermal explosion synthetic product is big absolutely
Part is by ZrC, ZrB2The biphase and extremely micro Al phase composition as diluent.
Embodiment 3：20wt.%Al-Zr-B4C system
For 20wt.%Al-Zr-B4C system, raw material is composed of the following components by mass percentage：Al powder 20wt.%,
Zr powder and B4The common 80wt.% of C powder, wherein Zr powder, B4C powder presses Zr:B4C=3:1 mol ratio is prepared, three kinds of constituent masses
Percentage ratio sum is 100%.Al powder 4～6h after, Zr powder and B will be dried at 80～90 DEG C4C powder is claimed by this component ratio
Amount, wherein Zr powder and B4The mol ratio of C powder is 3:1, suppress under 35～40MPa pressure after 15.4 grams of total weight mix homogeneously
The cylindric green briquette of molding, diameter 20mm, thickness～15mm, relative density is 65 ± 3%.Then this briquet 3 is put into stone
In black crucible 2, then in one piece of reative cell being positioned in induction furnace 1, it is full of Ar gas after first evacuation to protect, connects SIT
High frequency electric source 4, adjust within 20～25s time the voltage that applied of Efco-Northrup furnace increase to from 0～75 volts (electric current therewith can
Correspondingly increase to～55 peaces from 0), the W-response of the briquet that now can ignite, there is entirety in briquet after the electrified regulation several seconds
Very exothermic combustion reaction, entirely react power-off immediately after moment quickly completes, under the chilling of coil interior circulation water
And obtaining is in loose and the layer structure of expansion final product.
XRD Discriminating materials are carried out to this thermal explosion product, shown in its result such as Fig. 2 (c), shows that this thermal explosion synthetic product is main
By ZrC, ZrB2Biphase and micro Zr3Al3C5Phase, and a small amount of Al phase composition as diluent.
Embodiment 4：30wt.%Al-Zr-B4C system
For 30wt.%Al-Zr-B4C system, raw material is composed of the following components by mass percentage：Al powder 30wt.%,
Zr powder and B4The common 70wt.% of C powder, wherein Zr powder, B4C powder presses Zr:B4C=3:1 mol ratio is prepared, three kinds of constituent masses
Percentage ratio sum is 100%.Al powder 4～6h after, Zr powder and B will be dried at 80～90 DEG C4C powder is claimed by this component ratio
Amount, wherein Zr powder and B4The mol ratio of C powder is 3:1, suppress under 35～40MPa pressure after 15.0 grams of total weight mix homogeneously
The cylindric green briquette of molding, diameter 20mm, thickness～15mm, relative density is 65 ± 3%.Then this briquet 3 is put into stone
In black crucible 2, then in one piece of reative cell being positioned in induction furnace 1, it is full of Ar gas after first evacuation to protect, connects SIT
High frequency electric source 4, the voltage that regulation Efco-Northrup furnace is applied within 20～25s time increases to 80 volts from 0, and (electric current therewith can phase
Ground is answered to increase to 60 peaces from 0), the W-response of the briquet that now can ignite, there is overall play in briquet after the electrified regulation several seconds
Strong exothermic combustion reaction, entirely reacts power-off immediately after moment quickly completes, obtains under the chilling of coil interior circulation water
It must be in loose and the layer structure of expansion final product.
XRD Discriminating materials are carried out to this thermal explosion product, shown in its result such as Fig. 2 (d), shows that this thermal explosion synthetic product is main
By ZrC, ZrB2Biphase and a small amount of Zr3Al3C5Phase, and a small amount of Al phase composition as diluent.
Embodiment 1～4 shows, for Al-Zr-B4C powder systems, the Al powder mass percent of interpolation is 0～30wt.%
Shi Junneng thermal explosion synthesis zirconium carbide, zirconium boride multiphase ceramic powder material.Simply with the increase of Al powder addition, induction coil institute
The voltage that need to apply also can increase (electric current can accordingly increase therewith), impurities phase Zr in product3Al3C5Meet with diluent Al
Corresponding increase, thus reducing the temperature of thermal expousure and preparing relatively fine granular product.
This embodiment is carried out under premised on technical solution of the present invention.But as previously mentioned it should be understood that sending out
Bright be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and can be used for various other groups
Close, modification and environment, and can be in invention contemplated scope described herein, by the technology of above-mentioned teaching or association area or know
Knowledge is modified.But the technology contents that this embodiment is illustrated are only illustrative rather than determinate, should not come office according to this
Limit protection scope of the present invention, the change that those skilled in the art are carried out and change without departing from the spirit and scope of invention, are then all answered
In the protection domain of invention claims.
Claims (10)
1. thermal explosion synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：By mass percentage by following raw material group
Become：Al powder 0～30wt.%, Zr powder and B4C powder totally 70～100wt.%, wherein Zr powder and B4The mol ratio of C powder is 3:1, above
Constituent mass percentage ratio sum is 100%.
2. thermal explosion synthesis zirconium carbide as claimed in claim 1, zirconium diboride composite ceramic powders, is characterized in that being：Described
Raw material Zr powder, its purity is 98.5%, 38 μm of particle mean size.
3. thermal explosion as claimed in claim 1 synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：Described former
Material B4C powder, its purity>98%, 40 μm of particle mean size.
4. thermal explosion as claimed in claim 1 synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：Described Al
Powder, its purity>99%, 29 μm of particle mean size.
5. thermal explosion as claimed in claim 1 synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：For Zr-
B4C system, by mole composed of the following components：Zr powder 75mol.%, B4C powder 25mol.%, the two mol ratio is 3:1、
Molar percentage sum is 100mol.%.
6. thermal explosion as claimed in claim 1 synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：For
10wt.%Al-Zr-B4C system, composed of the following components by mass percentage：Al powder 10wt.%, Zr powder and B4C powder is altogether
90wt.%, wherein Zr powder and B4The mol ratio of C powder is 3:1, three kinds of constituent mass percentage ratio sums are 100%.
7. thermal explosion as claimed in claim 1 synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：For
20wt.%Al-Zr-B4C system, composed of the following components by mass percentage：Al powder 20wt.%, Zr powder and B4C powder is altogether
80wt.%, Zr powder and B4The mol ratio of C powder is 3:1, three kinds of constituent mass percentage ratio sums are 100%.
8. thermal explosion as claimed in claim 1 synthesis zirconium carbide, zirconium diboride composite ceramic powders it is characterised in that：For
30wt.%Al-Zr-B4C system, composed of the following components by mass percentage：Al powder 30wt.%, Zr powder and B4C powder is altogether
70wt.%, Zr powder and B4The mol ratio of C powder is 3:1, three kinds of constituent mass percentage ratio sums are 100%.
9. described thermal explosion synthesis zirconium carbide as arbitrary in claim 1～8, the preparation method of zirconium diboride composite ceramic powders,
It is characterized in that, specifically implement according to following steps：
Step 1：Respectively by raw material A l powder, Zr powder and B4C powder is dried 4～6h at 80～90 DEG C；
Step 2：Al powder 0～30wt.%, Zr powder and B are weighed respectively according to mass ratio4C powder totally 70～100wt.%, wherein Zr powder,
B4The mol ratio of C powder is 3:1, above constituent mass percentage ratio sum is 100%；
Step 3：Al powder, Zr powder and the B that step 2 is weighed4C powder carries out ball milling and is sufficiently mixed, then by mixed powder 35～
It is pressed into cylindric green briquette, diameter 20mm, thickness～15mm, relative density is 65 ± 3% under 40MPa pressure；
Step 4：Cylindric green briquette in step 3 is put into induction furnace and carries out thermal explosion chemical reaction, obtain zirconium carbide, two boronations
The composite ceramic powders of zirconium.
10. thermal explosion synthesis zirconium carbide as claimed in claim 9, the preparation method of zirconium diboride composite ceramic powders, its feature
It is, the specific embodiment of described thermal explosion chemical reaction is：Green briquette is positioned in the water-cooled induction coil in induction furnace,
It is full of Ar gas after first evacuation, connects SIT high frequency induction power supply, adjust what Efco-Northrup furnace was applied within 20～25s time
Voltage increases to 65～80 volts from 0, the W-response of the briquet that now can ignite, and after the electrified regulation several seconds, briquet occurs entirety
Very exothermic combustion reaction, entirely reacts power-off immediately after moment quickly completes, under the chilling of coil interior circulation water
Obtain is in loose and the zirconium carbide of layer structure of expansion, the composite ceramic powders of zirconium diboride.
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