CN1312218A - Titania nitriding process for preparing nanometer titanium nitride powder - Google Patents
Titania nitriding process for preparing nanometer titanium nitride powder Download PDFInfo
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Abstract
The preparation method of nanometer titanium nitride powder body is characterized by that nanometer titanium dioxide is used as raw material, and the titanium dioxide is subjected to high-temp. nitridization in tubular reactor furnace in ammonia atmosphere so as to obtain nanometer titanium nitride. By selecting and using nanometer titanium dioxide with different forms and sizes and changing the technological conditions of nitridization temp., nitridization time and ammonia gas flow rate, etc. the nanometer titanium nitride with different crystal grain size and form can be obtained. Said invented method is suitable for preparing titanium nitride nanometer powder and several nanometer composite powder of titanium nitride and other nitride and titanium nitride and oxide, etc.
Description
The present invention relates to the preparation method of Nano titanium nitride powder, the method for titania nitriding process for preparing nanometer titanium nitride powder belongs to the nano-powder field more precisely.
Titanium nitride is a kind of type material, has hardness height (microhardness is 21GPa), fusing point height (2950 ℃), characteristics that chemical stability is good, is a kind of good refractory high-abrasive material.Titanium nitride also has good electrical conductivity, can be used as the superconducting material of electro-conductive materials such as the electrode of fused salt electrolysis and electrical contact and higher superconduction critical temperature.In addition, it also has excellent biological compatibility, can be used as biomaterial.But the sintering character of titanium nitride micro mist is poor, influences and limited the widespread use of this material.
The Nano titanium nitride powder be meant its grain-size in 100 nanometers with interior nitride powder, replace micron order nitride powder to make raw material with its and can reduce sintering temperature, improve sintering character; As wild phase, can effectively improve the intensity and the toughness of metal, ceramic matrix with it.And, because particle is little, specific surface area is big, can be dispersed in other material and form conductive network, improves the conductivity of matrix material greatly.So Nano titanium nitride is a kind of material with broad prospect of application.At present, the common method of preparation Nano titanium nitride powder has plasma vapor deposition processes and high-energy ball milling method, preceding a kind of method needs expensive production unit, be difficult to suitability for industrialized production, a kind of method production efficiency in back is low, and contain impurity, coating of particles irregularity in the product, be difficult to obtain the high Nano titanium nitride powder of purity.
The object of the present invention is to provide a kind of short-cut method of titania nitriding process for preparing nanometer titanium nitride powder, the required production unit of this production technique is simple, be easy to realize suitability for industrialized production, the Nano titanium nitride powder that obtains has that particle diameter is little, good dispersity, shape is regular and characteristics such as purity height.
The objective of the invention is to implement like this: with titaniferous compound is main raw material, with the hydrolysis under suitable condition of titaniferous compound, obtains nano-titanium dioxide powder; In tubular react furnace, under mobile ammonia condition, high-temperature ammonolysis makes the Nano titanium nitride powder with nano titanium oxide.
Concrete enforcement can be divided into two and go on foot greatly:
The first step prepares nano-titanium dioxide powder; Second step prepared the Nano titanium nitride powder with the nano titanium oxide nitrogenize.Now details are as follows respectively:
1, the preparation of nano-titanium dioxide powder
By titaniferous compound hydrolysis, can obtain the hydrated titanium dioxide precipitation.The mentioned titaniferous compound of the present invention can be titanium tetrachloride, metatitanic acid, butyl (tetra) titanate, isopropyl titanate.These compounds are made into the solution of proper concn, under vigorous stirring, dropwise join in the distilled water that contains hydrolyst or hydrolysis in the basic solution, hydrolysate is filtered, use distilled water wash, remove impurity, use the absolute ethanol washing secondary again, remove the moisture in the hydrolysate, avoid the generation of hard aggregation, can obtain the armorphous nano titanium oxide of favorable dispersity, with this product under 450 ℃, calcining 2h obtains anatase-phase nano titanium dioxide.Catalyzer commonly used is oxalic acid, acetate, sodium hydroxide.Titanium/water mol ratio is 1: 100～200 in the final hydrolysate, and hydrolysis temperature is 20～50 ℃, and 1～24 hour time, the hydrolysate drying condition is 120 ℃, 8 hours, grinds 200 mesh sieves.
2, the preparation of Nano titanium nitride powder
The anatase-phase nano titanium dioxide powder that obtains is put into quartz crucible, the tubular type of packing into atmosphere furnace, feed ammonia, ammonia flow is 0.5～5 liter/minute, is warming up to 800-1100 ℃, temperature rise rate is 10～25 ℃/minute, under this temperature, be incubated 2～5 hours, then, under the ammonia that flows, naturally cool to room temperature.Obtain Nano titanium nitride.Can control the particle diameter and the nitriding velocity of Nano titanium nitride by temperature of reaction; Particle diameter by controlling reaction time control Nano titanium nitride; Shorten the reaction times by control ammonia flow velocity.So the selection of these three parameters all has fundamental influence to particle diameter, the output of reaction after product, these three parameters of choose reasonable, it is very important making it organic coupling.
The method of titania nitriding process for preparing nanometer titanium nitride powder provided by the invention is applicable to that preparation Nano titanium nitride and other nitride are (as Si
3N
4, AlN) composite nano-powder, be applicable to that preparation Nano titanium nitride and oxide compound are (as Al
2O
3, ZrO
2) composite nano-powder.Only need nitride such as Si with micron or submicron order
3N
4, AlN, oxide compound such as Al
2O
3, ZrO
2, be dispersed in required ratio in the solution of titanium salt, dropwise add in the distilled water, be hydrolyst with acetate or oxalic acid, be 1: 100～200 in titanium/water mol ratio, the hydrolysate drying condition is dried through 8 hours at 120 ℃, grinds 200 mesh sieves.Then through 450 ℃, calcining in 2 hours, make armorphous nano titanium oxide be converted into anatase-phase nano titanium dioxide, thereby be prepared into nitride-titanium dioxide or oxide compound-titanium dioxide compound, under above-mentioned nitridation conditions, carry out nitrogenize again, make titanium dioxide be nitrided into titanium nitride, thereby be prepared into the composite nano-powder of titanium nitride and other nitride or titanium nitride and oxide compound.
The preparation method's of Nano titanium nitride provided by the invention characteristics are:
1. little, the good dispersity of Zhi Bei Nano titanium nitride diameter of particle, regular shape and purity height.
2. simple, the required production unit of production technique is cheap, is easy to realize suitability for industrialized production.
3. use ammonia in the production process as reductive agent, more safer, reliable than make reductive agent with hydrogen.
Fig. 1 is the X-ray diffractogram of the Nano titanium nitride of embodiment 1 preparation.
Fig. 2 is the transmission electrolysis photo of the Nano titanium nitride of embodiment 1 preparation.
Fig. 3 is the transmission electrolysis photo of the Nano titanium nitride of embodiment 2 preparations.
Fig. 4 is the X diffractogram of the titanium nitride-silicon nitride nano composite granule of embodiment 3 preparations.
Fig. 5 is the transmission electrolysis photo of the titanium nitride-silicon nitride nano composite granule of embodiment 3 preparations.
The X-coordinate of Fig. 1 and Fig. 4 is a diffraction angle, and ordinate zou is a peak strength.
Further specify embodiment and effect with following indefiniteness embodiment.
Embodiment 1
Get butyl (tetra) titanate 20g, be dissolved in the 180ml ethanol solution, add 1g oxalic acid as hydrolyst, with the ethanol solution of butyl (tetra) titanate, under vigorous stirring, dropwise join in the distilled water that contains hydrolyst, controlling final titanium/water mol ratio is 1: 150, hydrolysate is filtered, use distilled water wash, remove impurity, use twice of absolute ethanol washing again, filter cake at 120 ℃ of oven dry 8h, is ground, crosses 200 mesh sieves, then at 450 ℃ of calcining 2h.The nano titanium oxide that obtains is put into quartz crucible, and the tubular type of packing into atmosphere furnace feeds ammonia, and ammonia flow is 1 liter/minute, is warming up to 800 ℃, and temperature rise rate is 10 ℃/minute.Insulation is 5 hours under this temperature, then, under the ammonia that flows, naturally cools to room temperature.Obtain Nano titanium nitride.Fig. 1 is the X-ray diffractogram of the Nano titanium nitride of present embodiment preparation, show 800 ℃ of ammonia nitrogenize 5 hours, what obtain is pure titanium nitride, peak 1 expression titanium nitride (111) crystal face diffraction peak among the figure, peak 2 is (200) crystal face diffraction peak, and peak 3 is (220) crystal face diffraction peak.Fig. 2 is its transmission electron microscope photo, shows that its particle size is about 20 nanometers, and size evenly.
Embodiment 2
Drip the sodium hydroxide solution of 1M under the room temperature toward the 1M titanium tetrachloride solution, be neutralized to pH=7, obtain white precipitate, behind the distilled water repetitive scrubbing, use the absolute ethanol washing secondary again, filter cake is dried 8h at 120 ℃, grind, cross 200 mesh sieves, then 450 ℃ of calcining 2h.To obtain nano titanium oxide, put into quartz crucible, the tubular type of packing into atmosphere furnace, feed ammonia, ammonia flow is 1 liter/minute, is warming up to 1000 ℃, and temperature rise rate is 10 ℃/minute, under this temperature, be incubated 2 hours, then, under the ammonia that flows, naturally cool to room temperature, obtain Nano titanium nitride.The X-ray diffractogram of the Nano titanium nitride powder of present embodiment preparation is identical with embodiment 1, as shown in Figure 1.Show 1000 ℃ of ammonia nitrogenize 2 hours, what obtain is pure titanium nitride.Fig. 3 is its transmission electron microscope photo, and particle size is about 70 nanometers, and the nitriding temperature height is described, titanium nitride crystal grain is easily grown up.All the other are with embodiment 1.
Embodiment 3
Get silicon nitride 80g and be scattered in the 500ml distilled water ball milling 24h.With butyl (tetra) titanate 200g, be dissolved in the 1800ml ethanol solution, add 10g oxalic acid as hydrolyst, with the ethanol solution of butyl (tetra) titanate, under vigorous stirring, dropwise join in the silicon nitride aqueous solution that contains 10g oxalic acid hydrolyst, controlling final titanium/water mol ratio is 1: 150, hydrolysate is filtered, use distilled water wash, remove impurity, use the absolute ethanol washing secondary again, filter cake at 120 ℃ of oven dry 8h, is ground, crosses 200 mesh sieves, then at 450 ℃ of calcining 2h.With the silicon nitride-nano titanium oxide composite granule that obtains, put into quartz crucible, the tubular type of packing into atmosphere furnace feeds ammonia, ammonia flow is 3 liters/minute, be warming up to 900 ℃, temperature rise rate is 10 ℃/minute, under this temperature, be incubated 5 hours, then, under the ammonia that flows, naturally cool to room temperature.Obtain the multiple powder of silicon nitride-Nano titanium nitride.Fig. 4 shows 900 ℃ for the X-ray diffractogram of the silicon nitride-Nano titanium nitride composite granule of present embodiment preparation, ammonia nitrogenize 5 hours, and nitrogenizing reaction is complete.Wherein the diffraction peak of silicon be in the silicon that in test, adds mark to calibrate diffraction angle caused.Fig. 5 is its transmission electron microscope photo, and macrobead is a silicon nitride, and what particle size was little is the Nano titanium nitride particle.
Claims (9)
1. the method for a titania nitriding process for preparing nanometer titanium nitride powder, comprise the preparation of nano titanium oxide, it is to utilize titaniferous materials to be main raw material, hydrolysis under normal temperature, normal pressure, obtain unbodied white precipitate, unbodied white precipitate is through 450 ℃, high-temperature calcination in 2 hours obtains anatase-phase nano titanium dioxide, it is characterized in that nano titanium oxide is in tubular react furnace, under mobile ammonia condition, dominant discharge, reaction times and nitriding temperature make the Nano titanium nitride powder at high-temperature ammonolysis.
2. by the method for the described a kind of titania nitriding process for preparing nanometer titanium nitride powder of claim 1, it is characterized in that described titaniferous compound comprises titanium tetrachloride, metatitanic acid, butyl (tetra) titanate, isopropyl titanate.
3. by claim 1 or 2 described preparation methods, it is characterized in that, at 20-50 ℃ of hydrolysis 1-24 hour, use acetate, oxalic acid, sodium hydroxide, titanium/water mol ratio 1: 100～200 in the final hydrolysate as hydrolyst with titaniferous compound.The hydrolysate drying condition is 120 ℃, 8 hours.
4. by the described preparation method of claim 1, it is characterized in that the high-temperature ammonolysis temperature is 800-1100 ℃, controls the particle diameter and the nitriding velocity of Nano titanium nitride by controlled temperature.
5. by the described preparation method of claim 1, it is characterized in that controlling by controlling reaction time the particle diameter of Nano titanium nitride, the reaction times is 2～5 hours.
6. by the described preparation method of claim 1, it is characterized in that shortening the reaction times by control ammonia flow velocity, the ammonia flow velocity is 0.5～5 liter/minute.
7. by the described preparation method of claim 1, it is characterized in that the Nano titanium nitride particle diameter for preparing is little: the Nano titanium nitride particle diameter is 20-70nm.
8. the method for the described titania nitriding process for preparing nanometer titanium nitride powder of claim 1 is applicable to preparation Nano titanium nitride and Si
3N
4Or the composite nano-powder of other nitride of AlN; Be applicable to preparation Nano titanium nitride and Al
2O
3Or ZrO
2The oxidate nano composite granule.
9. by the method for the described titania nitriding process for preparing nanometer titanium nitride powder of claim 8, it is characterized in that only need be with the nitride such as the Si of micron or submicron order
3N
4, AlN, oxide compound such as Al
2O
3, ZrO
2Be dispersed in required ratio in the solution of titanium salt, dropwise add in the distilled water, with acetate or oxalic acid is hydrolyst, in titanium/water mol ratio is 1: 100～200, the hydrolysate drying condition is dried through 8 hours at 120 ℃, ground 200 mesh sieves, then through 450 ℃, calcining in 2 hours, make armorphous nano titanium oxide be converted into anatase-phase nano titanium dioxide, be prepared into nitride-titanium dioxide or oxide compound-titanium dioxide compound earlier,, carry out nitrogenize under the 2-5 hour nitridation conditions again at 800-1100 ℃, ammonia flow is a 0.5-5 liter/minute make titanium dioxide be nitrided into titanium nitride, thereby is prepared into the composite nano-powder of titanium nitride and other nitride or titanium nitride and oxide compound.
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