CN104495848B - A kind of preparation method of monodisperse spherical zirconium carbide superfine powder - Google Patents
A kind of preparation method of monodisperse spherical zirconium carbide superfine powder Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of monodisperse spherical zirconium carbide superfine powder, described preparation method includes: 1) by single dispersing ZrO2Powder body ultrasonic disperse is in water, then is dispersed with ZrO to this2Adding soluble sugar in the water of powder body, stirring forms suspension；2) after suspension step 1) prepared carries out hydro-thermal reaction at 160 190 DEG C, it is performing centrifugal separation on being precipitated thing, and precipitate is carried out, dries and obtain ZrO2/ C composite granule；3) by step 2) prepare ZrO2/ C composite granule carries out carburizing reagent under an inert atmosphere, obtains described monodisperse spherical zirconium carbide superfine powder.
Description
Technical field
The present invention relates to the preparation method of a kind of dispersed nano-micron order Zirconium carbide powder, belong to powder body synthesis field.
Background technology
In the past few decades, inorganic nano-particle is all widely used (Y. in respective scientific research and application
N.Xia,B.Gates,Y.D.Yin,and X.Lu,Monodispersed colloidal spheres:old materials with new
applications.Adv.Mater.12(2000)693–713.Schartl.W.Crosslinked spherical nanoparticles with
core-shell topology.Adv.Mater.12(2000)1899-1908.]).Owing to nano material has reduced size, more greatly
Specific surface area, higher chemism, thus have uniqueness performance.And the performance of final products is had very by powder characteristics
Big impact.Powder body preparation is not only to improving material sintering character and microstructure has great significance, and to ultra-fine grain
The theoretical research of material itself has a major impact.If able to obtain ultra-fine, single dispersing, regular shape (as spherical), less group
Poly-powder granule, all play a very important role (M.Van de Graaf, J. to the reduction of sintering temperature and the research of performance
Ter Maat,A.Burggraaf,Microstructure and sintering kinetics of highly reactive ZrO2-Y2O3
ceramics.Mater.Sci.20(1985)1407–1418)。
ZrC zirconium carbide is owing to having high-melting-point, and high rigidity, high intensity, the capacity of heat transmission is good, and saturated vapor forces down, without solid-state
The features such as phase transformation and good neutron control ability, thus at cutting tool, superhigh temperature structural ceramics, composite, fire proofed wood
The aspects such as material, nuclear control material have preferably application.Because ZrC has less neutron absorption cross-section and preferable radioresistance
Can the covering material of forth generation nuclear fuel have potential application (C.R.Rambo, J.Cao, O.Rusina,
H.Sieber.Manufacturing of biomorphic(Si,Ti,Zr)-carbide ceramics by sol–gel processing.Carbon.
43(2005)1174–1183；D.Gosset,M.Dollé,D.Simeone,G.Baldinozzi,L.Thomé.Structural
behavior of nearly stoichiometric ZrC under ionirradiation.Nucl Instrum Methods Phys Res:SectB
266(2008)2801–2805).Because of ZrC, there is noble metal electronic structure again, the binary catalyst being combined into Pt, catalytic
Can have compared with single catalyst and significantly increase.Cause is ZrC supporting Pt in binary catalyst, so ZrC block
Pre-treatment is needed to improve the specific surface area of ZrC.ZrC is due to stronger covalent bond in sintering process, and the sintering of ZrC needs bigger
Pressure and higher temperature or use sintering aid.Theoretical research and experimental data show, ZrC powder is from the model of submicron order
Enclosing and be reduced to nanoscale, sintering kinetics activity has had significant raising in fact.The most either reduction of the sintering temperature of powder body
On, or all need in the raising of catalytic performance to seek a kind of synthesis uniform particle diameter monodispersed ZrC nanometer powder.
The serial of methods preparing ZrC at present all makes some progress (A.Maitre, P.Lefort.Solid state
reaction of zirconia with carbon.Solid State Ionics.104(1997)109–122；M.D.Sacks,C.A.Wang,
Z.H.Yang,A.Jain.Carbothermal reduction synthesis of nanocrystalline zirconium carbide and
Hafnium carbide powders using solution-derived precursors.Mater.Sci.39 (2004) 6,057 6066),
Solid reaction process and wet chemistry method is mainly had on ZrC chemical preparation process.Solid state reaction mainly includes carbothermic method, self-propagating
High-temperature synthesis (SHS), laser Gaseous reaction method, high-energy ball milling method, solid phase exchange process.Solid state reaction mainly passes through inorganic powder
Prepared by end reaction, use metal dust, metal oxide powder, metal compound powder and carbon source reaction to prepare zirconium carbide ceramics
Powder.Dynamics Controlling course of reaction, molecular diffusion rate determines the speed that reaction is carried out and the degree completed.Due to mummification
Method uses powder body as raw material, only has contact between reactant on surface, and microcosmic point is separated, and it is prominent that molecule is needed
Interface of being marred by a scar, etc. just can be spread to react inside powder body, and speed is very slow, and when oxide surface is transformed into corresponding nitridation
After thing or carbide form involucrum, carbon source, nitrogen source are more difficult to be diffused into inside powder body.For making reaction be carried out and react
Entirely, need to react the most for a long time.Even if therefore material powder is nanoscale, but through the highest
Temperature processes, and inorganic particulate includes that the particle diameter of initiation material and product all significantly increases.Wet chemistry method refers mainly to precursor process, forerunner
Body method is a kind of newer ceramic material preparation method, and owing to the method is in phase uniformity, the fine adjustments of chemical composition is controlled
Make the aspects such as final material shape and microstructure and have the incomparable superiority of powder method, be that ceramic material grinds the most both at home and abroad
The emphasis studied carefully and focus, especially receive much attention in terms of preparing Nano Ceramic Particles.Sol-gal process is the one of precursor process
Kind, it is a kind of milling method by means of colloidal dispersion, ultimate principle is: the catalyst of metal alkoxide, water, alcohol and necessity
Composition solution, forms wet gel through hydrolytie polycondensation, and wet gel, through dry, heat treatment, then crushes and obtains superfines.?
It is remaining that sol-gel process usually can introduce oxygen, and heat treatment removes the way that oxygen impurities is the most frequently used, and oxygen removal process often causes
The increase of crystallite dimension.As long as the reason causing this phenomenon is above ZrO when 1300 DEG C2The growth of appearance crystal grain, and this temperature
The initial temperature of zirconium oxide carbonization just.ZrO2The reduction of growth inducing carburizing reagent activity, to final synthesis single dispersing ZrC
Nano-particle has the impact of the most negative effect.As can be seen here, synthesizing good single dispersing zirconium carbide nano-powder is still current carbonization
One difficult point of zirconium split synthesis.
Summary of the invention
It is contemplated that overcome prior art cannot realize synthesizing the technical barrier of good monodisperse spherical Zirconium carbide powder,
The invention provides the preparation method of a kind of monodisperse spherical zirconium carbide superfine powder.
The invention provides the preparation method of a kind of monodisperse spherical zirconium carbide superfine powder, described preparation method includes:
1) by single dispersing ZrO2Powder body ultrasonic disperse is in water, then is dispersed with ZrO to this2The water of powder body adds soluble sugar, stirs
Mix formation suspension；
2) by step 1) after the suspension prepared carries out hydro-thermal reaction at 160-190 DEG C, it is performing centrifugal separation on being precipitated thing, and right
Precipitate is carried out, dry and obtain ZrO2/ C powder body；
3) by step 2) prepare ZrO2/ C powder body carries out carburizing reagent under an inert atmosphere, obtains described monodisperse spherical zirconium carbide and surpasses
Fine powder body.
It is preferred that step 1) in, single dispersing ZrO2The particle diameter of powder body is 50-150nm, preferably 120nm.
It is preferred that step 1) in, single dispersing ZrO2The preparation method of powder body includes:
Carbamide is dissolved in water as precipitation from homogeneous solution agent, inorganic zirconium salts is dissolved in water as mother solution, precipitation from homogeneous solution agent is joined mother solution
In, after stirring, carry out water-bath ageing, then be centrifuged separating, wash by washing, alcohol successively, dry, it is thus achieved that single point
Dissipate ZrO2Powder body.
It is preferred that inorganic zirconium salts includes Zr (SO4)2·4H2O、ZrOCl2·8H2O、Zr(NO3)4·5H2In O at least one
Kind, carbamide is (1～4) with the mass ratio of inorganic zirconium salts: 1.
It is preferred that water-bath Aging Temperature is 70～90 DEG C, the time is 30～60 minutes, and centrifuge speeds is
5000～10000r/ minute, the time is 5～20 minutes.
It is preferred that step 1) in, described soluble sugar include the water solublity monosaccharide containing glucose building blocks, disaccharide and
Polysaccharide, preferably glucose, sucrose and/or maltose.
It is preferred that step 1) in, soluble sugar and single dispersing ZrO2The mass ratio of powder body is (10～50): 1.
It is preferred that step 2) in, the hydro-thermal reaction time is 180～300 minutes, and hydro-thermal reaction is entered in autoclave
OK, the pressure in course of reaction is 600-850KPa, preferably 690KPa.
It is preferred that step 2) in, centrifuge speeds is 5000～10000r/ minute, and the time is 5～20 minutes.
It is preferred that step 3) in, carbonation reaction temperature is 1400～1600 DEG C, and the time is 60～180 minutes.
Beneficial effects of the present invention:
1. it is prepared for the ZrO of carbon cladding2(ZrO2@C) structure, completely cut off the contact between zirconium oxide by carbon-coating, hinder carbonization
During ZrO2Growth and reunion, advantageously form monodispersed Zirconium carbide powder；
2. zirconates selects inorganic salt, and carbon encapsulated material selects soluble saccharide cheap and easy to get, makes production preparation cost reduce；
3. use the method can obtain mono-dispersed nano powder body at 1400～1600 DEG C, reduce than the temperature of prior art report
100～200 DEG C；
4. the microstructure of the dispersed nano powder body obtained is spherical, and this monodispersed spherical morphology nano-powder has bigger ratio
Surface area, reactivity is high, advantageously reduces sintering temperature and the raising of catalytic efficiency of pottery；
5. due to ZrO2For unformed, dehydration under the high temperature conditions, volume contraction.Simultaneously can ZrO under the protection of carbon-coating2
Carbon thermal reduction can split into multiple ZrC spherical powder.Gained ZrC particle diameter can be less than initial ZrO2Particle diameter.
Accompanying drawing explanation
Fig. 1 shows that in an embodiment of the invention, the single dispersing of preparation, micron order, microstructure are spherical carbon
Change zirconium powder body TEM photo；
Fig. 2 shows that in an embodiment of the invention, the single dispersing of preparation, nanoscale, microstructure are spherical Zirconium carbide powder
TEM photo；
Fig. 3 shows the single dispersing of preparation in an embodiment of the invention, spherical zirconium carbide superfine powder XRD figure spectrum.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
The present invention solves the problem being difficult to obtain monodisperse spherical ZrC ceramic powder in prior art, disclose a kind of single
Dispersion, nano-micrometre level, microstructure are spherical Zirconium carbide powder and preparation method thereof, to fill up the sky of prior art
In vain.The invention discloses a kind of monodisperse spherical zirconium carbide superfine powder and preparation method thereof, belong to powder body synthesis field.Described
Zirconium carbide powder be single dispersing, nanoscale-micron order, microstructure powder body spherical in shape, its particle size range is
30～4000nm.
The preparation method of this Zirconium carbide powder comprises the steps: in short
First, using inorganic zirconium salts and carbamide is raw material, obtains monodisperse spherical ZrO by precipitation from homogeneous solution2Powder body；
Secondly, the ZrO that will obtain2Powder body and soluble saccharide carry out water under high pressure thermal response, it is thus achieved that single dispersing ZrO2@C powder body；
Finally, the single dispersing ZrO that will obtain2@powder body carries out high temperature cabonization reaction under inert atmosphere protection, obtains monodisperse spherical
Zirconium carbide superfine powder.
The preparation method of described single dispersing Zirconium carbide powder, comprises the steps:
(a) monodisperse spherical ZrO2Preparation: carbamide is dissolved in deionized water as precipitation from homogeneous solution agent, inorganic zirconium salts is dissolved in
Precipitation from homogeneous solution agent, as mother solution, is joined in mother solution by deionized water, after stirring, carries out water-bath ageing, then is centrifuged
Separate, wash by washing, alcohol successively, dry, it is thus achieved that monodisperse spherical ZrO2Powder body；
B () is by the monodisperse spherical ZrO of preparation in (a)2Powder body joins in deionized water and after ultrasonic disperse, adds solubility
Saccharide also stirs formation suspension, then continues at after carrying out hydro-thermal reaction in autoclave, by precipitation and centrifugal separation, through successively
After washing, alcohol are washed, are dried, it is thus achieved that single dispersing ZrO2@C (i.e. ZrO2/ C) powder body；
C () is by the single dispersing ZrO of gained in (b)2@C powder body carries out high temperature cabonization reaction under inert atmosphere protection, obtains single point
Dissipate, microstructure is spherical Zirconium carbide powder.
Inorganic zirconium salts described in step (a) can be Zr (SO4)2·4H2O、ZrOCl2·8H2O、Zr(NO3)4·5H2O。
Carbamide described in step (a) is (1～4) with the mass ratio of inorganic zirconium salts: 1.
Water-bath Aging Temperature described in step (a) is 70～90 DEG C, and the time is 30～60min.
Centrifuge speeds described in step (a) and (b) is 5000～10000r/min, and the time is 5～20min.
Soluble saccharide described in step (b) is water solublity monosaccharide, disaccharide and the polysaccharide containing glucose building blocks,
Such as glucose, sucrose, maltose etc..
Soluble saccharide described in step (b) and ZrO2Mass ratio be (10～50): 1.
Hydrothermal temperature in autoclave described in step (b) is 160～190 DEG C, and the time is
180～300min.
High temperature cabonization reaction temperature described in step (c) is 1400～1600 DEG C, and the time is 60～180min.
Inert atmosphere described in step (c) is argon gas atmosphere.
Compared with prior art, there is advantages that
1. it is prepared for the ZrO of carbon cladding2(ZrO2@C) structure, completely cut off the contact between zirconium oxide by carbon-coating, hinder carbonization
During ZrO2Growth and reunion, advantageously form monodispersed Zirconium carbide powder；
2. zirconates selects inorganic salt, and carbon encapsulated material selects soluble saccharide cheap and easy to get, makes production preparation cost reduce；
3. use the method can obtain mono-dispersed nano powder body at 1400～1600 DEG C, reduce than the temperature of prior art report
100～200 DEG C；
4. the microstructure of the dispersed nano powder body obtained is spherical, and this monodispersed spherical morphology nano-powder has bigger ratio
Surface area, reactivity is high, advantageously reduces sintering temperature and the raising of catalytic efficiency of pottery；
5. due to ZrO2For unformed, dehydration under the high temperature conditions, volume contraction.Simultaneously can ZrO under the protection of carbon-coating2
Carbon thermal reduction can split into multiple ZrC spherical powder.Gained ZrC particle diameter can be following in initial ZrO2Particle diameter.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
For preparing single dispersing, nanoscale, microstructure are spherical Zirconium carbide powder: 4.5 grams of carbamide are dissolved in 500ml by (1)
Ionized water is as precipitation from homogeneous solution agent, by 1.775 grams of Zr (SO4)2It is dissolved in 500ml deionized water as mother solution, by precipitation from homogeneous solution
Agent joins in mother solution, after stirring, carries out water-bath ageing, and water-bath Aging Temperature is 90 DEG C, and the time is 30min.Enter again
Row centrifugation, centrifuge speeds is 8000r/min, and the time is 10min.Wash by washing, alcohol successively, dry, obtain
Obtain monodisperse spherical ZrO2Powder body.(2) by the monodisperse spherical ZrO of preparation in (1)2Powder body 1 gram joins 250ml and goes
In ionized water and after ultrasonic disperse, add 25 grams of sucrose and stir formation suspension, then continuing at and autoclave carries out water
Thermal response, hydrothermal temperature is 170 DEG C, and the time is 210min, pressure is 790KPa.By precipitation and centrifugal separation, centrifugal
Separating rate is 8500r/min, and the time is 15min.After washing, alcohol are washed, are dried successively, it is thus achieved that single dispersing ZrO2@C
Powder body.(3) by the single dispersing ZrO of gained in (2)2@C powder body carries out high temperature cabonization reaction under argon gas atmosphere is protected, high
Temperature carbonation reaction temperature is 1400 DEG C, and the time is 120min.Obtain single dispersing, nanoscale, microstructure are subglobose carbon
Change zirconium powder body.
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its grain
Footpath is 150nm.
Embodiment 2
Powder body, the except for the difference that carbamide employed in step (1) and Zr (SO is obtained by with embodiment 1 exact same way4)2's
Quality is respectively 2.25 grams and 1.775 grams；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
100nm。
Embodiment 3
Powder body, the except for the difference that carbamide employed in step (1) and Zr (SO is obtained by with embodiment 1 exact same way4)2's
Quality is respectively 1.775 grams and 1.775 grams；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
50nm (Fig. 2).
Embodiment 4
Powder body, the except for the difference that ZrO employed in step (2) is obtained by with embodiment 1 exact same way2Powder body and sucrose
Quality is respectively 2.5 grams and 25 grams；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
200nm。
Embodiment 5
Powder body, the except for the difference that ZrO employed in step (2) is obtained by with embodiment 1 exact same way2Powder body and sucrose
Quality is respectively 0.5 gram and 25 grams；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
300nm。
Embodiment 6
Obtaining powder body by with embodiment 1 exact same way, the soluble saccharide except for the difference that used is glucose, hydro-thermal reaction
Temperature is 160 DEG C, and the time is 180min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
50nm。
Embodiment 7
Obtaining powder body by with embodiment 1 exact same way, the soluble saccharide except for the difference that used is glucose, hydro-thermal reaction
Temperature is 190 DEG C, and the time is 300min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
1500nm (Fig. 1).
Embodiment 8
Obtaining powder body by with embodiment 1 exact same way, the soluble saccharide except for the difference that used is maltose, high temperature cabonization
Reaction temperature is 1400 DEG C, and the time is 120min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
100nm。
Embodiment 9
Obtaining powder body by with embodiment 1 exact same way, the soluble saccharide except for the difference that used is glucose, high temperature cabonization
Reaction temperature is 1500 DEG C, and the time is 180min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
80nm。
Embodiment 10
Obtaining powder body by with embodiment 1 exact same way, the inorganic zirconium salts except for the difference that used is ZrOCl2·8H2O, high temperature
Carbonation reaction temperature is 1500 DEG C, and the time is 180min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
3000nm。
Embodiment 11
Obtaining powder body by with embodiment 1 exact same way, the inorganic zirconium salts except for the difference that used is Zr (NO3)4·5H2O is high
Temperature carbonation reaction temperature is 1500 DEG C, and the time is 180min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
1000nm。
Embodiment 12
Powder body, the ZrO except for the difference that used is obtained by with embodiment 10 exact same way2The quality of powder body and sucrose is respectively
2.5 grams and 25 grams, high temperature cabonization reaction temperature is 1500 DEG C, and the time is 180min；
Learnt by tem observation: gained Zirconium carbide powder be single dispersing, microstructure be the powder body of regular spherical, its particle diameter is
4000nm。
Claims (11)
1. the preparation method of a monodisperse spherical zirconium carbide superfine powder, it is characterised in that described preparation method includes:
1) by single dispersing ZrO2Powder body ultrasonic disperse is in water, then is dispersed with ZrO to this2Adding soluble sugar in the water of powder body, stirring forms suspension, wherein soluble sugar and single dispersing ZrO2The mass ratio of powder body is (10-50): 1；
2) suspension step 1) prepared carries out hydro-thermal reaction at 160-190 DEG C, the hydro-thermal reaction time is 180-300 minute, and the pressure in course of reaction is 600-850Kpa, after hydro-thermal reaction, it is performing centrifugal separation on being precipitated thing, and precipitate is carried out, dries and obtain single dispersing ZrO2/ C composite granule；
3) by step 2) prepare single dispersing ZrO2/ C composite granule carries out carburizing reagent under an inert atmosphere, obtains described monodisperse spherical zirconium carbide superfine powder.
Preparation method the most according to claim 1, it is characterised in that in step 1), single dispersing ZrO2The particle diameter of powder body is 50-150nm.
Preparation method the most according to claim 2, it is characterised in that single dispersing ZrO2The particle diameter of powder body is 120nm.
Preparation method the most according to claim 1, it is characterised in that in step 1), single dispersing ZrO2The preparation method of powder body includes:
Carbamide is dissolved in water as precipitation from homogeneous solution agent, inorganic zirconium salts is dissolved in water as mother solution, precipitation from homogeneous solution agent is joined in mother solution, after stirring, carries out water-bath ageing, then be centrifuged separating, wash by washing, alcohol successively, dry, it is thus achieved that single dispersing ZrO2Powder body.
Preparation method the most according to claim 4, it is characterised in that inorganic zirconium salts includes Zr (SO4)2·4H2O、ZrOCl2·8H2O、Zr(NO3)4·5H2At least one in O, carbamide is (1-4) with the mass ratio of inorganic zirconium salts: 1.
Preparation method the most according to claim 4, it is characterised in that water-bath Aging Temperature is 70-90 DEG C, the time is 30-60 minute, and centrifuge speeds is 5000-10000r/ minute, and the time is 5-20 minute.
Preparation method the most according to claim 1, it is characterised in that in step 1), described soluble sugar includes water solublity monosaccharide, disaccharide and polysaccharide containing glucose building blocks.
Preparation method the most according to claim 7, it is characterised in that in step 1), described soluble sugar is glucose, sucrose and/or maltose.
Preparation method the most according to claim 1, it is characterised in that step 2) in, hydro-thermal reaction is carried out in autoclave, and the pressure in course of reaction is 790KPa.
Preparation method the most according to claim 1, it is characterised in that step 2) in, centrifuge speeds is 5000-10000r/ minute, and the time is 5-20 minute.
11. according to described preparation method arbitrary in claim 1-9, it is characterised in that in step 3), carbonation reaction temperature is 1400-1600 DEG C, and the time is 60-180 minute.
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| CN103626179A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing nanometer zirconium carbide powder |
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