CN109835875B - Method for preparing nano titanium nitride powder by normal pressure chemical vapor deposition method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 49
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000010936 titanium Substances 0.000 claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 238000001878 scanning electron micrograph Methods 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 229920000877 Melamine resin Polymers 0.000 description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 1
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 229910000048 titanium hydride Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for preparing nano titanium nitride powder by a normal pressure chemical vapor deposition method, which comprises the steps of fully mixing a titanium source and a nitrogen source and grinding; and then putting the ground powder into a tubular furnace, heating the tubular furnace to a specified temperature in an inert atmosphere and a reducing atmosphere, preserving the heat, and cooling to room temperature after the reaction is finished to obtain gray black powder, namely the target product TiN. The invention adopts the chemical vapor deposition method to synthesize the high-purity nano titanium nitride powder, avoids the reaction process with high temperature and high time consumption, requires less raw materials for the preparation method, has less synthesis steps, and is convenient and simple to operate in the whole related process, low in cost and easy for large-scale production.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing nano titanium nitride powder by using a normal-pressure chemical vapor deposition method.
Background
Nitrogen is the most abundant element in air, but since nitrogen is chemically very stable, it is difficult to chemically react, but under some specific conditions, it may form nitrides with some transition elements, such as titanium nitride, vanadium nitride, zirconium nitride, etc., among which titanium nitride is studied and paid much attention. Titanium nitride has many excellent physical and chemical properties, such as high melting point (2950 ℃), high hardness, 8-9 mohs hardness, high thermochemical stability and excellent heat conduction and electrical conductivity, and in addition, titanium nitride also has excellent magnetic and optical properties, and based on the excellent properties of titanium nitride, titanium nitride is widely applied to various fields, mainly applied to the fields of high temperature resistance, wear resistance, electrode materials in the photoelectric industry, the field of catalysis and the like.
At present, there are many methods for preparing titanium nitride, including (1) direct nitridation of metallic titanium powder and (2) microwave carbon nitridationA thermal reduction method, (3) a titanium oxide reduction nitridation method, (4) a self-propagating high-temperature synthesis method, (5) a solvothermal synthesis method, (6) a mechanical alloying method, (7) a sol-gel method, and (8) a chemical vapor deposition method. All the preparation methods have respective advantages and disadvantages, but in general, no preparation method can quickly and simply prepare the titanium nitride nano powder, so that the search for a quick and simple preparation method is very important. The direct titanium powder nitriding method is characterized in that titanium powder reacts with nitrogen or ammonia gas to generate titanium nitride, the reaction temperature is 1200-1400 ℃, the method is relatively simple to operate, but the method has the defects that the reaction time is too long, about 30 hours is needed, and the powder sintering phenomenon is easily generated in the reaction process. The microwave carbothermic process is an oxidation-reduction reaction carried out at a relatively high temperature using inorganic carbon as a reducing agent, and has the advantages of low reaction temperature and short synthesis period. The titanium oxide reduction nitridation method is TiO2As raw material, reducing agent is carbon graphite in N2TiN is generated by reaction under the atmosphere, but the TiN prepared by the method has low purity, higher contents of O and C, higher reaction temperature and longer reaction time. The self-propagating high-temperature synthesis method is to ignite titanium powder (blank) and ammonia gas under certain pressure to obtain titanium nitride. The solvent thermal synthesis method is to add reactants and organic solvent into a closed system and control the reaction temperature and pressure to obtain the product. The method prepares titanium nitride as TiH2And NH4Cl is used as a raw material and is added into H at 500-800 DEG C2And N2The mixed gas is reacted to obtain the titanium nitride. The mechanical alloying method is to put titanium powder in ammonia gas and nitrogen gas atmosphere, and then ball milling is carried out by using a high-energy ball mill to obtain the nano titanium nitride. The sol-gel method is that the compound containing high chemical activity component is used as precursor, these raw materials are uniformly mixed in liquid phase, and undergone the processes of hydrolysis and condensation chemical reaction to form stable transparent sol system in the solution, the sol is undergone the process of ageing and slow polymerization between colloidal particles to form gel with three-dimensional network structure, then the gel is undergone the process of gelation treatmentThe material with molecular or even nano-substructure can be prepared by drying, sintering and curing. Zheng Yajie et al use this method to prepare titanium nitride powder. The chemical vapor deposition method is to generate titanium nitride with higher purity at 1100-1500 ℃ by taking titanium tetrachloride and ammonia gas as raw materials under hydrogen reduction. The existing scheme is that titanium dioxide, metal soluble chloride or hydrate thereof and melamine are mixed and ball-milled according to a certain mass, and then the mixture is put into a tubular furnace to react for 1-4 hours at 900-1400 ℃ to obtain the flaky titanium nitride nano material. The method has over-high reaction temperature and over-long reaction time, so that the method is particularly important for preparing the titanium nitride nano material with lower cost and simpler operation method.
At present, the preparation of TiN nano-materials by using a chemical vapor deposition method has two technical difficulties. First, Ti is easily oxidized to titanium dioxide at high temperature, which requires the reaction system to be in an oxygen-free condition, and usually requires the reaction to be carried out in an inert atmosphere. Secondly, although the melamine is synthesized by chemical vapor deposition, the reactant melamine can be decomposed at high temperature to generate highly toxic cyanide gas, which is not good for the health of experimenters.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing nano titanium nitride powder by using an atmospheric pressure chemical vapor deposition method, which has the advantages of low cost, less required raw materials, less synthesis steps, short time and easy large-scale production, and aims to overcome the defects in the prior art.
The invention adopts the following technical scheme:
a method for preparing nanometer titanium nitride powder by normal pressure chemical vapor deposition method comprises mixing titanium source and nitrogen source thoroughly and grinding; and then putting the ground powder into a tubular furnace, heating the tubular furnace to 600-1200 ℃ in an inert atmosphere and a reducing atmosphere, preserving the heat for 20-60 min, and cooling to room temperature after the reaction is finished to obtain the target gray-black TiN powder.
Specifically, the titanium source is titanium powder, and the nitrogen source is ammonium chloride.
Further, the mass ratio of the titanium source to the nitrogen source is 1: (8-15).
Specifically, the vacuum degree in the tube furnace is lower than 100 Pa.
Specifically, the heating rate of the tubular furnace is 2-10 ℃/min.
Specifically, the inert gas is high-purity argon, and the flow rate is 50-400 sccm.
Specifically, the reducing gas is hydrogen, and the flow rate is 20-80 sccm.
Specifically, the size of the prepared TiN powder particles is 20-200 nm.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention adopts a chemical vapor deposition method to fully mix and grind a titanium source and a nitrogen source; then putting the ground powder into a tube furnace, and vacuumizing the tube furnace; and heating the tube furnace to a specified temperature in an inert atmosphere and a reducing atmosphere, preserving heat, and cooling to room temperature after the reaction is finished to obtain black powder, namely the target product TiN. Compared with the conventional synthesis method, the method for synthesizing the high-purity titanium nitride nanopowder by adopting the chemical vapor deposition method is simpler, more efficient and safer, has the great advantage of avoiding a high-temperature and high-time-consuming reaction process, is convenient and simple to operate in the whole process, and only needs to keep the temperature at 600-1200 ℃ for 20-60 min, and is short in time and high in repeatability in the whole experimental process.
Furthermore, titanium powder has high activity at high temperature, and is easy to generate nitridation reaction to generate titanium nitride; and the titanium powder is an important industrial raw material, and the raw material is easy to obtain, thereby laying a foundation for subsequent batch production. The ammonium chloride is used as a nitrogen source, so that the price is low, and the cost is reduced for subsequent chemical industrial production; and the ammonium chloride is easily decomposed at high temperature to react with the titanium powder.
Further, the vacuum degree is lower than 100Pa, so that the oxygen content in the furnace is reduced, and the titanium powder and the residual oxygen can be effectively prevented from reacting at high temperature to generate titanium dioxide.
Furthermore, high-purity argon is used as inert gas, so that oxygen in the atmosphere is prevented from entering the furnace, and the titanium powder and the residual oxygen are effectively prevented from reacting at high temperature.
Furthermore, hydrogen is used as reducing gas, so that titanium oxide with partially oxidized surface can be effectively reduced into simple substance titanium, and titanium nitride with higher purity can be obtained. The flow rate is set so that the reduction of the surface titanium oxide cannot be achieved by a too low flow rate, and the flow rate is set so that the cost is increased and the risk factor is increased.
In conclusion, the method for synthesizing the high-purity titanium nitride nanopowder by adopting the chemical vapor deposition method is simpler, more efficient and safer.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD pattern of the product produced in example 1 of the present invention;
FIG. 2 is an SEM image of a product prepared in example 1 of the present invention;
FIG. 3 is an XRD pattern of the product prepared in example 2 of the present invention;
FIG. 4 is an SEM image of a product prepared in example 2 of the present invention;
FIG. 5 is an XRD pattern of the product prepared in example 3 of the present invention;
FIG. 6 is an SEM image of a product prepared in example 3 of the present invention;
FIG. 7 is an XRD pattern of the product prepared in example 4 of the present invention;
FIG. 8 is an SEM image of a product prepared according to example 4 of the present invention;
FIG. 9 is an XRD pattern of the product prepared in example 5 of the present invention;
FIG. 10 is an SEM image of a product prepared in example 4 of the present invention.
Detailed Description
The invention provides a method for preparing nano titanium nitride powder by a normal pressure chemical vapor deposition method, which comprises the steps of fully mixing a titanium source and a nitrogen source and grinding; and then putting the ground powder into a tubular furnace, heating the tubular furnace to 600-1200 ℃ in an inert atmosphere and a reducing atmosphere, preserving the heat for 20-60 min, and cooling to room temperature after the reaction is finished to obtain gray black powder, namely the target product TiN. The invention adopts the chemical vapor deposition method to synthesize the high-purity nano titanium nitride powder, avoids the reaction process with high temperature and high time consumption, requires less raw materials for the preparation method, has less synthesis steps, and is convenient and simple to operate in the whole related process, low in cost and easy for large-scale production.
The invention relates to a method for preparing nano titanium nitride powder by a normal pressure chemical vapor deposition method, which comprises the following steps:
s1, fully mixing and grinding a titanium source and a nitrogen source, wherein the titanium source is titanium powder, the nitrogen source is ammonium chloride, and the mass ratio of the titanium source to the nitrogen source is 1: (8-15);
s2, putting the ground powder into a tube furnace, and vacuumizing the tube furnace to ensure that the tube furnace is in an oxygen-free environment, wherein the vacuumizing vacuum degree of the tube furnace is lower than 100 Pa;
s3, introducing inert gas and reducing gas into the tube furnace, heating to 600-1200 ℃ at a heating rate of 2-10 ℃/min, and preserving heat for 20-60 min;
the inert gas is high-purity argon with the flow rate of 50-400 sccm, and the reducing gas is hydrogen with the flow rate of 20-80 sccm.
And S4, cooling to room temperature after heat preservation is finished, and obtaining the high-purity nano titanium nitride powder.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Firstly, fully mixing 1mmol of titanium powder and 15mmol of ammonium chloride, grinding, putting the ground powder into a tube furnace, and vacuumizing the tube furnace for 20 min;
then, introducing argon and hydrogen, wherein the flow of the argon is 50sccm, the flow of the hydrogen is 20sccm, heating the tube furnace to 1200 ℃ at the heating rate of 2 ℃/min, preserving the temperature for 20min to finish the growth of the nanocrystalline, then stopping heating, and cooling to room temperature to obtain black powder, namely the target product.
Fig. 1 is an X-ray diffraction spectrum of TiN nanopowder grown according to example 1, without impurity peaks appearing, indicating that the product is pure TiN.
FIG. 2 is an SEM image of TiN nanopowder grown according to example 1, showing that the size of TiN particles is 100-200 nm and agglomeration occurs between the particles.
Example 2
Firstly, fully mixing 1mmol of titanium powder and 8mmol of ammonium chloride, grinding, putting the ground powder into a tube furnace, and vacuumizing the tube furnace for 20 min;
then, introducing argon and hydrogen, wherein the flow of the argon is 400sccm, the flow of the hydrogen is 80sccm, heating the tubular furnace to 900 ℃ at the heating rate of 3 ℃/min, preserving the temperature for 60min to finish the growth of the nanocrystalline, then stopping heating, and cooling to room temperature to obtain black powder, namely the target product.
Fig. 3 is an X-ray diffraction spectrum of TiN nano-powder grown according to example 2, and it can be seen that the main component of the product is TiN and the crystallinity is good.
FIG. 4 is an SEM image of TiN nanopowder grown according to example 2, and it can be seen that TiN particle size is 50-100 nm.
Example 3
Firstly, fully mixing 1mmol of titanium powder and 10mmol of ammonium chloride, grinding, putting the ground powder into a tube furnace, and vacuumizing the tube furnace for 20 min;
then, introducing argon and hydrogen, wherein the flow of the argon is 200sccm, the flow of the hydrogen is 40sccm, heating the tubular furnace to 800 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 30min to finish the growth of the nanocrystalline, then stopping heating, and cooling to room temperature to obtain black powder, namely the target product.
Fig. 5 is an X-ray diffraction spectrum of TiN nano-powder grown according to example 3, and it can be seen that the main component of the product is TiN and the crystallinity is good.
FIG. 6 is an SEM image of TiN nanopowder grown according to example 3, showing that the TiN particle size is 50-100 nm and agglomeration occurs between particles.
Example 4
Firstly, fully mixing 1mmol of titanium powder and 11mmol of ammonium chloride, grinding, putting the ground powder into a tube furnace, and vacuumizing the tube furnace for 20 min;
then, introducing argon and hydrogen, wherein the flow of the argon is 200sccm, the flow of the hydrogen is 40sccm, heating the tube furnace to 700 ℃ at the heating rate of 8 ℃/min, preserving the temperature for 30min to finish the growth of the nanocrystalline, then stopping heating, and cooling to room temperature to obtain black powder, namely the target product.
Fig. 7 is an X-ray diffraction spectrum of TiN nanopowder grown in accordance with example 4, without impurity peaks appearing, indicating that the product is pure TiN.
FIG. 8 is an SEM image of TiN nanopowder grown according to example 4, showing that the size of TiN particles is 20-50 nm and agglomeration occurs between particles.
Example 5
Firstly, fully mixing 1mmol of titanium powder and 13mmol of ammonium chloride, grinding, putting the ground powder into a tube furnace, and vacuumizing the tube furnace for 20 min;
then, introducing argon and hydrogen, wherein the flow of the argon is 200sccm, the flow of the hydrogen is 40sccm, heating the tubular furnace to 600 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 30min to finish the growth of the nanocrystalline, then stopping heating, and cooling to room temperature to obtain black powder, namely the target product.
FIG. 9 is an X-ray diffraction pattern of TiN nano-powder grown according to example 5, and it can be seen that TiN is a main component of the product and that agglomeration occurs between particles.
Fig. 10 is an SEM morphology photograph of TiN nano-powder grown according to example 5, and it can be seen that the TiN particles were seriously agglomerated.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (1)
1. A method for preparing nanometer titanium nitride powder by normal pressure chemical vapor deposition is characterized in that 1mmol of titanium source and 11mmol of nitrogen source are fully mixed and ground, the titanium source is titanium powder, and the nitrogen source is ammonium chloride; and putting the ground powder into a tubular furnace, vacuumizing the tubular furnace for 20min, heating the tubular furnace to 700 ℃ in an inert atmosphere and a reducing atmosphere, wherein the vacuum degree in the tubular furnace is lower than 100Pa, the heating rate of the tubular furnace is 8 ℃/min, the inert gas is high-purity argon, the flow rate is 200sccm, the reducing gas is hydrogen, the flow rate is 40sccm, the temperature is kept for 30min, cooling to room temperature after the reaction is finished, and obtaining a gray-black target product TiN powder, wherein the particle size of the TiN powder is 20 nm.
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| CN101759163A (en) * | 2009-12-29 | 2010-06-30 | 山东大学 | Process for preparing porous titanium nitride at low temperature |
| CN102910910A (en) * | 2012-11-16 | 2013-02-06 | 四川理工学院 | Method for preparing micro-nano titanium carbonitride powder with controllable carbon-nitrogen ratio by adopting solid state nitrogen source |
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| JP2010084181A (en) * | 2008-09-30 | 2010-04-15 | Tokyo Electron Ltd | Exhaust system structure of film deposition device, film deposition device and method for treating exhaust gas |
| CN106586984B (en) * | 2016-11-25 | 2018-06-19 | 湖北工程学院 | The method that chemical vapour deposition technique prepares sheet titanium nitride nano material |
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| CN101759163A (en) * | 2009-12-29 | 2010-06-30 | 山东大学 | Process for preparing porous titanium nitride at low temperature |
| CN102910910A (en) * | 2012-11-16 | 2013-02-06 | 四川理工学院 | Method for preparing micro-nano titanium carbonitride powder with controllable carbon-nitrogen ratio by adopting solid state nitrogen source |
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