CN104227010A - Preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction - Google Patents
Preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction Download PDFInfo
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- CN104227010A CN104227010A CN201310253904.0A CN201310253904A CN104227010A CN 104227010 A CN104227010 A CN 104227010A CN 201310253904 A CN201310253904 A CN 201310253904A CN 104227010 A CN104227010 A CN 104227010A
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Abstract
The invention discloses a preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction. According to the preparation method, Zr (zirconium) powder and carbon black powder are basic materials, a certain Al (aluminum) powder or Zn (zinc) powder or prepared ZrC (zirconium carbide) powder is added to serve as a booster to control reaction temperature, the molar ratio of Zr (zirconium) to C (carbon) of the basic materials is 1, and the additive amount of the Al powder is 30wt% when mixed powder of Al, Zr and C is used; when mixed powder of Al, Zn, Zr and C is used, the additive amount of the Al powder is 20wt%, and the additive amount of the Zn powder is 10wt%; when mixed powder of ZrC, Al, Zr and C is used, both the content of the ZrC powder and the content of the Al powder are 10wt%. The preparation method has the advantages of quick reaction, simple technology, good energy-saving effect, high efficiency, high product purity, high nanocrystallization level and the like.
Description
Technical field
The invention belongs to new transition metal carbide ceramic powder material technical field, specifically a kind of preparation method of ultra-fine zirconium carbide nano-powder material.
Background technology
As everyone knows, zirconium carbide (ZrC) is with its high fusing point and hardness, excellent wear resistance and corrosion resistance, good chemical stability and certain metallic conduction, heat conductivility and be widely used in the fields such as the overcoat in cutting tool, wear-resistance bit, electronic devices and components, atomic pile.As hardening constituent, ZrC is more used as the enhancing particle in metal-base composites.ZrC has typical face-centred cubic structure, has the composite attribute of comprehensive metallic bond, ionic bond and covalent bond.ZrC also has the heat of reaction formation greatly simultaneously, and it can be synthesized by methods such as the carbothermic reduction reaction under high temperature, magnesiothermic reduction reaction, mechanical alloying, chemical vapour deposition (CVD) and sol-gels or be prepared.But these methods or need the high heat of high temperature, and complex technical process, or the seriously polluted of product can be caused, thus cause the thick and impure of generated ZrC particle, and then reduce its performance and application.
In addition, the process for producing of traditional nano-zirconium carbide is easy to cause that carbonization is uneven, purity is low, nanometer degree is low, sintering character is poor, seriously constrain its impact of performance as hard enhanced particles, have impact on the development & application of nonferrous materials, hinder the development of China's powder metallurgy industry.
Summary of the invention
The object of the invention is to overcome traditional shortcomings and deficiencies preparing zirconium carbide powder technology, and a kind of newly preparation method of simple zirconium carbide nano particle is provided, the chemical thermal explosion method in combustion synthesis technology is adopted directly to prepare nanoscale zirconium carbide powder, efficiently solve the technological deficiency of existing nanometer zirconium carbide powder manufacture of materials, thus define that a kind of technique is simple, efficient energy-saving, product purity are high, nanometer degree is high and the zirconium carbide nano-powder material be evenly distributed.
A kind of preparation method of solid state reaction kinetics zirconium carbide nano powder, it comprises the following steps: with Zr powder, raw material based on carbon black, Al powder, Zn powder, ZrC powder is additive raw material, cylindric briquet is pressed into after fully being mixed by certain mixed-powder, chemical reactive synthesis is carried out in the atmosphere being full of Ar gas, adopt the radio-frequency induction coil being connected with heavy current to the briquet that ignites, briquet will at moment overall generation thermal expousure, finally obtain the nanoscale ZrC powder being mixed with part Al or Zn, this thermal expousure product is not by contaminating impurities such as oxygen, can directly use as nanometer ZrC/Al composite, also simple ZrC nano particle can be obtained after extraction is washed, described Zr/C atomic ratio is 1, be 30wt.% with the addition of Al powder during Al-Zr-C mixed powder, be 10wt.% with the addition that the addition of Al powder during Al-Zn-Zr-C mixed powder is 20wt.%, Zn powder, 10wt.% is with the content of ZrC powder during ZrC-Al-Zr-C mixed powder and Al powder.
Described Al powder, its purity > 99%, particle mean size ~ 29 μm.
Described Zr powder, its purity is 98.5%, and particle mean size is 38 μm.
Described Zn powder, its purity > 98%, particle mean size ~ 40 μm.
Described carbon black powder, its purity > 98%, amorphous, particle mean size ~ 5nm.
Described ZrC powder, for making powder by oneself by thermal expousure, its purity > 97%, particle mean size ~ 20 μm
Described briquet is cylindric briquetting, and diameter is about 20mm, and thickness is about 15mm, and relative density is 65 ± 3%.
Described inert gas is Ar gas.
The described mode of igniting is that SIT high frequency electric source is realized by water-cooled induction coil.
In the present invention, add Ji Al powder or Zn powder or ZrC powder and vital effect is played to preparation ZrC nanometer powder.On the one hand, in course of reaction, lower temperature liquid phase Zn's (fusing point is about 693K) or Al (fusing point is about 933K) comparatively early more easily occurs, for the phase counterdiffusion between powder provides more easy passage, a large amount of Zr, C powder will be dissolved in Zn (or Al) liquid phase, and spread rapidly and fully and sprawl, make the surface area raising that contacts with each other, thus bringing out violent exothermic chemical reaction instantaneously, generate stable ZrC particle.On the other hand, the Zn of interpolation (or Al, or ZrC) serves the effect of diluent in thermal expousure process, reduces the ignition temperature of reaction, thus greatly inhibits growth and the alligatoring of generated ZrC.Further, Zn or Al is easy to vaporize thus probably suppresses growing up of ZrC crystal grain, plays important facilitation to generation nanometer ZrC dusty material.
Existing research shows, the liquid combustion technology of solution is utilized to prepare multiple nanometer oxide material, some oxidizer materials of suitable heating more can cause violent solution combustion reaction, and prepare corresponding nanometer oxide material with violent vapography.The quick-fried combustion synthesis reaction of severe thermal of the mixed-powder that the present invention is brought out by SIT high frequency electric source induction coil also can see as a kind of special in the liquid combustion process of raw solution, in reaction, the comparatively morning of Zn (or Al) defines Al (or Zn)-Zr-C bath after comparatively easy melting, both facilitated the rapid diffusion of each powder, sprawled and dissolving, more facilitate the generation of the liquid combustion reaction of solution, in addition reacted fast break water-cooled, has finally synthesized nanometer ZrC powder.
Beneficial effect:
The present invention efficiently solves the technological deficiency of existing nanometer zirconium carbide powder manufacture of materials, thus defines that a kind of technique is simple, efficient energy-saving, product purity are high, nanometer degree is high and the zirconium carbide nano-powder material be evenly distributed.
Detailed description of the invention
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, below in conjunction with tool embodiment, setting forth the present invention further.
Embodiment 1:30wt%Al-Zr-C
The ternary mixed-powder of 30wt%Al-Zr-C is pressed into Φ 20 × 15mm after ball milling fully mixes, relative density be 65 ± 3% cylindric prefabricated briquet, then this briquet is positioned in the water-cooled induction coil in the induction furnace being full of Ar gas, by the W-response that SIT high frequency induction power supply provides energy to ignite briquet, there is overall very exothermic combustion reaction in briquet after the electrified regulation several seconds, whole reaction completed rapidly in moment, the layer structure that product expands in loosening.The qualification result of XRD test shows that this thermal explosion synthetic product is made up of Al and ZrC.The observed result of FE-SEM shows that the particle mean size of synthesized ZrC particle is 80 ~ 150nm.
Embodiment 2:10wt%ZrC-10wt%Al-Zr-C
The quaternary mixed-powder of 10wt%ZrC-10wt%Al-Zr-C is pressed into Φ 20 × 15mm after ball milling fully mixes, relative density is the cylindric prefabricated briquet of 65 ± 3%, wherein ZrC powder is original homemade through thermal expousure, the powder that granularity is about 20 μm, this briquet is positioned in the water-cooled induction coil in the induction furnace being full of Ar gas, by the W-response that SIT high frequency induction power supply provides energy to ignite briquet, there is overall very exothermic combustion reaction in briquet after the electrified regulation several seconds, whole reaction completed rapidly in moment, the layer structure that product expands in loosening.The qualification result of XRD test shows that this thermal explosion synthetic product is made up of Al and ZrC.The observed result of FE-SEM shows that the particle mean size of synthesized ZrC particle is 120 ~ 300nm.
Embodiment 3:10wt%Zn-20wt%Al-Zr-C
The quaternary mixed-powder of 10wt%Zn-20wt%Al-Zr-C is pressed into Φ 20 × 15mm after ball milling fully mixes, relative density is the cylindric prefabricated briquet of 65 ± 3%, wherein ZrC powder is original homemade through thermal expousure, the powder that granularity is about 20 μm, this briquet is positioned in the water-cooled induction coil in the induction furnace being full of Ar gas, by the W-response that SIT high frequency induction power supply provides energy to ignite briquet, there is overall very exothermic combustion reaction in briquet after the electrified regulation several seconds, whole reaction completed rapidly in moment, the layer structure that product expands in loosening.The qualification result of XRD test shows that this thermal explosion synthetic product is made up of Al and ZrC.Make Zn phase wherein be vaporized because reaction temperature is higher, the vaporization of Zn phase more can suppress the growth of ZrC, thus generates more tiny crystal grain.Therefore, find from the observed result of FE-SEM, synthesized ZrC particle is trickleer, and its particle mean size is 40 ~ 70nm.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (7)
1. a preparation method for zirconium carbide nano powder, is characterized in that: it is with Al powder, Zn powder, ZrC powder, Zr powder and carbon black powder for raw material, and wherein the mol ratio of Zr/C powder is 1, proportions: be 30wt.% with the addition of Al powder during Al-Zr-C mixed powder; Be 10wt.% with the addition that the addition of Al powder during Al-Zn-Zr-C mixed powder is 20wt.%, Zn powder; 10wt.% is with the content of ZrC powder during ZrC-Al-Zr-C mixed powder and Al powder, mixed-powder is carried out ball milling fully mix, and be pressed into prefabricated briquet, chemical synthesis is carried out in the induction furnace being full of Ar gas, there is provided strong energy by SIT high frequency electric source, adopt the water-cooled copper induction coil of heavy current to ignite whole compacting briquet and thermal expousure occurs, the reaction of whole briquet almost completes simultaneously, coil power-off chilling immediately subsequently, obtains mainly containing the composite particles of nanometer ZrC.
2. the preparation method of a kind of zirconium carbide nano powder according to claim 1, is characterized in that: described base stock Zr powder, particle mean size is 38 μm.
3. the preparation method of a kind of zirconium carbide nano powder according to claim 1, it is characterized in that: described base stock carbon black powder, particle mean size is 5nm.
4. the preparation method of a kind of zirconium carbide nano powder according to claim 1, it is characterized in that: described additive A l powder, particle mean size is 29 μm.
5. the preparation method of a kind of zirconium carbide nano powder according to claim 1, is characterized in that: described additive Zn powder, particle mean size is 40 μm.
6. the preparation method of a kind of zirconium carbide nano powder according to claim 1, is characterized in that: described additive ZrC powder is for making powder by oneself through thermal expousure, and particle mean size is 20 μm.
7. the preparation method of a kind of zirconium carbide nano powder according to claim 1, it is characterized in that: described compacting briquet is cylindric briquetting, and diameter is about 20mm, and thickness is about 15mm, relative density is 65 ± 3%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108504891A (en) * | 2018-05-09 | 2018-09-07 | 台州学院 | The one-step method for synthesizing of ultra-fine zirconium carbide-zirconium boride ceramic complex intensifying copper electrode material |
| CN108588471A (en) * | 2018-05-09 | 2018-09-28 | 台州学院 | The one-step method for synthesizing of the copper base electrode material of ceramic particle containing nano-zirconium carbide |
| CN108584958A (en) * | 2018-05-09 | 2018-09-28 | 台州学院 | A kind of in-situ synthetic method of zirconium carbide nano-powder |
| CN108611514A (en) * | 2018-05-09 | 2018-10-02 | 九江学院 | A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof |
| WO2019095715A1 (en) * | 2017-11-15 | 2019-05-23 | 泰州市艾瑞斯克模具有限公司 | High-temperature sensitive nano-material and preparation method therefor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019095715A1 (en) * | 2017-11-15 | 2019-05-23 | 泰州市艾瑞斯克模具有限公司 | High-temperature sensitive nano-material and preparation method therefor |
| CN108504891A (en) * | 2018-05-09 | 2018-09-07 | 台州学院 | The one-step method for synthesizing of ultra-fine zirconium carbide-zirconium boride ceramic complex intensifying copper electrode material |
| CN108588471A (en) * | 2018-05-09 | 2018-09-28 | 台州学院 | The one-step method for synthesizing of the copper base electrode material of ceramic particle containing nano-zirconium carbide |
| CN108584958A (en) * | 2018-05-09 | 2018-09-28 | 台州学院 | A kind of in-situ synthetic method of zirconium carbide nano-powder |
| CN108611514A (en) * | 2018-05-09 | 2018-10-02 | 九江学院 | A kind of ultra-fine zirconium carbide particle-zirconium boride stick crystalline substance enhancing copper base electrode material and preparation method thereof |
| CN108588471B (en) * | 2018-05-09 | 2020-01-10 | 台州学院 | One-step synthesis method of copper-based electrode material containing nano zirconium carbide ceramic particles |
| CN108584958B (en) * | 2018-05-09 | 2020-04-21 | 台州学院 | In-situ synthesis method of zirconium carbide nano powder |
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Application publication date: 20141224 |