CN101367520A - Preparation method for nano- zirconium carbide material - Google Patents
Preparation method for nano- zirconium carbide material Download PDFInfo
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- CN101367520A CN101367520A CNA2008102012510A CN200810201251A CN101367520A CN 101367520 A CN101367520 A CN 101367520A CN A2008102012510 A CNA2008102012510 A CN A2008102012510A CN 200810201251 A CN200810201251 A CN 200810201251A CN 101367520 A CN101367520 A CN 101367520A
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Abstract
The invention relates to the technical field of the composite material, and discloses a method for preparing the nanometer zirconium carbide material; Copper powder or aluminum power, the zinc powder and the carbon soot are adopted as the raw materials; the atomic ratio of the zinc and carbon is 1; in the mixed powder of the copper, zinc and carbon, the content of the copper powder is 10 to 30 percent at wt; in the mixed powder of the aluminum powder, the zinc powder and the carbon soot, the content of the aluminum powder is 30 to 40 percent at wt; after the copper or aluminum powder, zinc powder and carbon soot are adequately mixed, the mixture is compressed to a briquet; in the environment that is full of inert gases, the briquet is combusted and synthesized; tungsten arc on the bottom of the briquet is adopted for ignition; after the briquet is ignited, the combustion wave is spontaneously spread until the entire reaction is completed, so that the nanometer carbon zinc that is mixed with copper or aluminum is obtained. The invention has the advantages of simple craftwork, energy conservation, high efficiency, high purity of the quality, and the like; the product is the composite material of copper or aluminum, so that the product not only can be used as Cu-nanometer ZrC composite material or Al-nanometer ZrC composite material, but also can obtain the pure nanometer carbon zinc particles adopting the acid to wash the metal copper or aluminum.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of composite materials, specifically is a kind of preparation method of nano-zirconium carbide material.
Background technology
Zirconium carbide (ZrC) has high fusing point and hardness, and excellent wear resistance and corrosion resistance and good chemical stability are widely used in protective layer in cutting tool, wear-resistance bit, electronic devices and components, the reactor and the enhancing particle in the matrix material.The nanometer of ZrC grain-size can increase substantially the mechanical property of material.ZrC prepares by methods such as carbothermic reduction reaction, mechanical alloying, chemical vapor deposition (CVD) under the high temperature usually, also can prepare by burning synthesis method simple by technology, that save the energy, but resulting ZrC particle thicker (more than the 10 μ m) is synthesized in the burning of Zr and C usually), other processing method commonly used also is difficult to prepare effectively nanometer ZrC material.
Find through literature search prior art, " Synthesis of nanosizedzirconium carbide by a sol-gel route " (Mickael Doll ＇ e etc. that Mickael Doll ＇ e etc. deliver on " Journal of the EuropeanCeramic Society " 27 (2007) 2061-2067, " utilize sol-gel process synthesis of nano zirconium carbide ", the ceramic journal in Europe, 2007 27 volume 2061-2067 pages or leaves) literary composition, propose to utilize sol-gel process synthesis of nano zirconium carbide in this article, the raw material that sets out is Zr (OPr) 4, AcOH and sucrose, the zirconium carbide particle that sol-gel processing that process is complicated and high-temperature heat treatment have obtained about 100 nanometers of median size, but oxygen contamination is serious in the product, and technological process is very complicated.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of nano-zirconium carbide the preparation method, make it adopt combustion synthesis technology directly to prepare nano-zirconium carbide material, thereby it is simple to form a kind of technology, the nano-zirconium carbide material that efficient energy-saving and product purity are high.
The present invention is achieved by the following technical solutions, the present invention is a raw material with Cu or Al powder and Zr powder, carbon black, to be pressed into briquet behind Cu or Al and Zr, the C ternary mixed powder thorough mixing, it is synthetic to burn in being full of the environment of rare gas element, adopt the tungsten electrode arc of briquet bottom to ignite, after briquet is lighted, combustion wave will spontaneously be propagated, finish until entire reaction, obtain being mixed with the nanometer ZrC of portion C u or Al.This product is not subjected to contaminating impurities such as oxygen, both can directly use and can fall metal Cu or the simple nanometer ZrC particle of Al acquisition with pickling as Cu (or Al)-nanometer ZrC matrix material.
The atomic ratio of described Zr and C is 1, and the content of Cu powder is 10-30wt% during with the Cu-Zr-C powder mix, and the content of Al powder is 30-40wt% during with the Al-Zr-C powder mix.
Described Cu powder, its purity are more than 99%, and median size is 44 μ m.
Described Al powder, its purity are more than 99%, and median size is 29 μ m.
Described Zr powder, its purity are more than 99%, and median size is 38 μ m.
Described carbon black, its purity〉98%, amorphous.
Described briquet is cylindric briquet, and diameter is Φ 22 * 10mm, and relative density is about 60 ± 5%.
Described rare gas element is an Ar gas.
Described burning, its temperature is gathered by the thermopair that is inserted in the raw material briquet.
Among the present invention, the interpolation of Cu or Al powder plays a part crucial to the preparation nano-zirconium carbide.On the one hand, the appearance of liquid Cu in the reaction process (the about 1356K of melting point) or Al (the about 933K of melting point), for the phase mutual diffusion between powder provides easier passage, a large amount of Zr, C powder will be dissolved in Cu (or Al) liquid, and rapidly diffusion with sprawl, make that being in contact with one another surface-area improves rapidly, thereby cause violent exothermic chemical reaction, generate the ZrC particle.On the other hand, Cu (or Al) plays thinner in reaction process, reduces the temperature of combustion of reaction, thereby suppresses the ZrC growth.In addition, the vaporization of Cu (or Al) may obtain nanometer ZrC material and play an important role suppressing the ZrC growth.
Utilize solution combustion can prepare multiple nanometer oxide material.Suitably heat some solution that contain oxygenant and can cause violent solution combustion, follow violent vaporization, thereby make corresponding nano-oxide.The combustion synthesis reaction of Cu (or Al)-Zr-C ternary mixed powder is also permitted and is seen a kind of special interior living solution combustion as, after melting, Cu in the reaction process (or Al) formed Cu (or Al)-Zr-C solution, and then produce the solution combustion phenomenon, obtain nanometer ZrC particle.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The used starting material of following examples are Cu powder (purity is 99%, and median size is 44 μ m), Al powder (purity is 99%, and median size is 29 μ m), Zr powder (purity is 99%, and median size is 38 μ m), carbon black (purity〉98%, amorphous).The atomic ratio of Zr and C is 1, and the content of Cu powder is 10-30wt.% during with the Cu-Zr-C powder mix, and the content of Al powder is 30-40wt% during with the Al-Zr-C powder mix.Portion of product is clayed into power, and (D/Max 2500PC Rigaku, Japan) thing detects mutually as XRD.Use field emission scanning electron microscope (FE-SEM, model is JSM-6700F) to observe the fracture apperance of product.Temperature of combustion is gathered by the W-La thermopair that is inserted in the raw material briquet.
Embodiment 1:
With 10wt%Cu-Zr-C ternary mixed powder behind thorough mixing, be pressed into Φ 22 * 10mm, relative density is about 60 ± 5% cylindric briquet, be placed on then in the glove box that is full of Ar, ignite by the tungsten electrode arc that is installed in the sample bottom, Cu began fusing (temperature reaches about 1100 ℃) after tungsten electrode arc heated the several seconds, produce violent heat release combustion reactions (temperature is up to 2450 ℃) subsequently, combustion wave is spontaneously propagated, and finishes until entire reaction.The result of X-ray diffraction test shows that this combustion synthesized product is made of Cu and ZrC.The result that field emission scanning electron microscope is observed shows that the median size of ZrC is about 100nm.
Embodiment 2:
With 20wt%Cu-Zr-C ternary mixed powder behind thorough mixing, be pressed into Φ 22 * 10mm, relative density is about 60 ± 5% cylindric briquet, be placed on then in the glove box that is full of Ar, ignite by the tungsten electrode arc that is installed in the sample bottom, Cu began fusing after tungsten electrode arc heated the several seconds, produce violent heat release combustion reactions (temperature is up to 2430 ℃) subsequently, combustion wave is spontaneously propagated, and finishes until entire reaction.The result of X-ray diffraction test shows that this combustion synthesized product is made of Cu and ZrC two-phase.The result that field emission scanning electron microscope is observed shows that the median size of ZrC is about 70nm.
Embodiment 3:
With 30wt%Cu-Zr-C ternary mixed powder behind thorough mixing, be pressed into Φ 22 * 10mm, relative density is about 60 ± 5% cylindric briquet, be placed on then in the glove box that is full of Ar, ignite by the tungsten electrode arc that is installed in the sample bottom, tungsten electrode arc heats after about 12 seconds Cu and begins fusing, produce violent heat release combustion reactions (temperature is up to 2400 ℃) subsequently, combustion wave is spontaneously propagated, and finishes until entire reaction.The result of X-ray diffraction test shows that this combustion synthesized product is made of Cu and ZrC two-phase.The result that field emission scanning electron microscope is observed shows that the median size of ZrC is about 50nm.
Embodiment 4:
With 30wt%Al-Zr-C ternary mixed powder behind thorough mixing, be pressed into Φ 22 * 10mm, relative density is about 60 ± 5% cylindric briquet, be placed on then in the glove box that is full of Ar, ignite by the tungsten electrode arc that is installed in sample bottom, tungsten electrode arc heats after about 4 seconds between the Al-Zr at 650 ℃ and the solid phase thermopositive reaction has taken place and generates ZrAl
3Compound, Al-Zr solid state reaction institute liberated heat impels part A l fusing, thereby make temperature decrease, this melts the caused temperature fluctuation of absorbing heat by heat release of Al-Zr solid state reaction and Al may produce violent heat release combustion reactions (temperature is up to 1675 ℃) because the Zr particle promptly is added to also to react with it in the Al liquid after lasting about 1 second, generates a large amount of ZrAl
3Intermetallic compound, C and liquid ZrAl subsequently
3Further thermopositive reaction generates ZrC and Al, and temperature also further rises to 1953 ℃, and combustion wave is spontaneously propagated, and finishes until entire reaction.The formation in above-mentioned each stage of reaction is determined by the X-ray diffraction test.The result that field emission scanning electron microscope is observed shows that the median size of ZrC is about 100nm.
Embodiment 5:
With 40wt%Al-Zr-C ternary mixed powder behind thorough mixing, be pressed into Φ 22 * 10mm, relative density is about 60 ± 5% cylindric briquet, be placed on then in the glove box that is full of Ar, ignite by the tungsten electrode arc that is installed in sample bottom, the solid phase thermopositive reaction took place and has generated ZrAl at 650 ℃ between the Al-Zr after the heating several seconds in tungsten electrode arc
3Compound, Al-Zr solid state reaction institute liberated heat impels part A l fusing, thereby make temperature decrease, this melts the caused temperature fluctuation of absorbing heat by heat release of Al-Zr solid state reaction and Al may produce violent heat release combustion reactions because the Zr particle promptly is added to also to react with it in the Al liquid after lasting about 1 second, generates a large amount of ZrAl
3Intermetallic compound, C and liquid ZrAl subsequently
3Further thermopositive reaction generates ZrC and Al, and temperature also further rises to 1630 ℃, and combustion wave is spontaneously propagated, and finishes until entire reaction.The formation in above-mentioned each stage of reaction is determined by the X-ray diffraction test.The result that field emission scanning electron microscope is observed shows that the median size of ZrC is about 80nm.
Claims (8)
- A nano-zirconium carbide material the preparation method, it is characterized in that, be raw material with Cu or Al powder and Zr powder, carbon black, and the atomic ratio of described Zr and C is 1, to be pressed into briquet behind Cu or Al and Zr, the C ternary mixed powder thorough mixing, it is synthetic to burn in being full of the environment of stating rare gas element, adopts the tungsten electrode arc of briquet bottom to ignite, after briquet is lighted, combustion wave will spontaneously be propagated, finish until entire reaction, obtain being mixed with the nanometer ZrC of portion C u or Al, wherein:The weight percent content of Cu powder is 10-30% during with the Cu-Zr-C powder mix, and the weight percent content of Al powder is 30-40% during with the Al-Zr-C powder mix.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that, described Cu powder, its purity is more than 99%, median size is 44 μ m.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that, described Al powder, its purity is more than 99%, median size is 29 μ m.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that, described Zr powder, its purity is more than 99%, median size is 38 μ m.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that described carbon black, its purity〉98%.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that described briquet is cylindric briquet, diameter is Φ 22 * 10mm, relative density is 60 ± 5%.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that described rare gas element is an Ar gas.
- Nano-zirconium carbide material as claimed in claim 1 the preparation method, it is characterized in that, described burning, its temperature is gathered by the thermopair that is inserted in the raw material briquet.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844766A (en) * | 2010-06-12 | 2010-09-29 | 武汉理工大学 | Method for rapidly preparing zirconium carbide ceramics powder |
| CN104227010A (en) * | 2013-06-14 | 2014-12-24 | 铜仁学院 | Preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction |
| CN106475092A (en) * | 2016-11-23 | 2017-03-08 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of alumina base platinum catalyst |
| CN106495156A (en) * | 2016-11-24 | 2017-03-15 | 景德镇陶瓷大学 | A kind of method for preparing zirconium carbide nano-powder |
| CN108531767A (en) * | 2018-05-09 | 2018-09-14 | 台州学院 | A kind of preparation method of the ultra-fine zirconium carbide particle dispersed and strengthened copper-based composite material of spot-wedling electrode |
| CN108570570A (en) * | 2018-05-09 | 2018-09-25 | 九江学院 | A kind of nano-zirconium carbide ceramic strengthening copper base electrode material and preparation method thereof |
| CN108584958A (en) * | 2018-05-09 | 2018-09-28 | 台州学院 | A kind of in-situ synthetic method of zirconium carbide nano-powder |
| 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 |
-
2008
- 2008-10-16 CN CNA2008102012510A patent/CN101367520A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844766A (en) * | 2010-06-12 | 2010-09-29 | 武汉理工大学 | Method for rapidly preparing zirconium carbide ceramics powder |
| CN101844766B (en) * | 2010-06-12 | 2012-01-11 | 武汉理工大学 | Method for rapidly preparing zirconium carbide ceramics powder |
| CN104227010A (en) * | 2013-06-14 | 2014-12-24 | 铜仁学院 | Preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction |
| CN106475092A (en) * | 2016-11-23 | 2017-03-08 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of alumina base platinum catalyst |
| CN106475092B (en) * | 2016-11-23 | 2019-08-20 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of alumina base platinum catalyst |
| CN106495156B (en) * | 2016-11-24 | 2018-11-16 | 景德镇陶瓷大学 | A method of preparing zirconium carbide nano-powder |
| CN106495156A (en) * | 2016-11-24 | 2017-03-15 | 景德镇陶瓷大学 | A kind of method for preparing zirconium carbide nano-powder |
| CN108570570A (en) * | 2018-05-09 | 2018-09-25 | 九江学院 | A kind of nano-zirconium carbide ceramic strengthening copper base electrode material and preparation method thereof |
| CN108584958A (en) * | 2018-05-09 | 2018-09-28 | 台州学院 | A kind of in-situ synthetic method of zirconium carbide nano-powder |
| 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 |
| CN108531767A (en) * | 2018-05-09 | 2018-09-14 | 台州学院 | A kind of preparation method of the ultra-fine zirconium carbide particle dispersed and strengthened copper-based composite material of spot-wedling electrode |
| 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 |
| CN108570570B (en) * | 2018-05-09 | 2020-01-10 | 九江学院 | Nano zirconium carbide ceramic reinforced copper-based electrode material and preparation method thereof |
| 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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