CN109928763A - Tantalum-based oxynitride nano powder and preparation method thereof - Google Patents
Tantalum-based oxynitride nano powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of tantalum-based oxynitride nano powder, which comprises the following steps: s1, dissolving alkaline earth metal salt, tantalum salt and a nitrogen source in alcohol, and drying after ball milling to obtain a mixed precursor; s2, placing the mixed precursor obtained in the step S1 in a reaction container, and carrying out non-pressure discharge plasma calcination under a protective atmosphere to obtain the tantalum base oxynitride nano powder.
Description
Technical field
The present invention relates to high performance dielectric ceramic technical field of material more particularly to a kind of tantalum base oxynitride nanometers
Powder and preparation method thereof.
Background technique
Perovskite oxynitride SrTaO2N and BaTaO2N causes state because it has high dielectric constant at room temperature
The extensive concern of inside and outside scholar.In the two crystal structure, Ta atom and O/N atomic building Ta (O, N)6Octahedra and Ta is located at eight
Face body center, A atom is located between octahedron and occupies eight vertex of structure cell, due to the difference of A atom and Ta atomic radius
And the various arrangement mode of N atom, so that Ta (O, N)6Different degrees of inclination occurs for octahedron, changes Ta-O/N-Ta
Bond distance and bond angle, Ta ion deflection center and generate spontaneous polarization.In addition to excellent dielectric properties, they also have both gold
The advantages of belonging to oxide and nitride, there are good thermal stability and acid-alkali-corrosive-resisting, it is considered to be novel high-performance electricity
The ideal material of container.
Currently, SrTaO2N and BaTaO2The synthetic method of N nano powder mainly has two-step method and one-step method.Two-step method is first closed
At the composite oxides presoma (Sr comprising various metals cation2Ta2O7And Ba5Ta4O15), then in the ammonia atmosphere of flowing
Neutralize (> 1000 °C) progress ammoniated treatments under high temperature.Since slowly, yield to be improved exists for gas-solid reaction diffusion in ammonifying process
It needs to stop repeatedly among reaction and grinds nano powder, only the preparation time of calcining step is typically for up to tens hours.One-step method is
It does not use or does not use ammonia directly, using Ta3N5, TaON, urea, melamine etc. be used as nitrogen source, single step reaction synthesizes oxygen nitrogen
Compound.This method substantially increases reaction efficiency, but preparation time still needs to a few hours.Meanwhile the heating that conventional calcination is excessively slow
Rate decomposes the nitrogen sources such as urea totally below the temperature for generating oxynitride, and nitrogen source is largely lost, and efficiency of nitridation is low,
The purity that will lead to oxynitride in product reduces.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of tantalum base oxynitriding of high-purity
Object nano powder, correspondingly, the present invention also provides a kind of short preparation periods, tantalum base oxynitride nano powder at low cost and with high purity
Preparation method.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of preparation method of tantalum base oxynitride nano powder, comprising the following steps:
S1, alkali salt, tantalum salt and nitrogen source are dissolved in alcohol, it is dry after ball milling, obtain mixing presoma;
S2, the resulting mixing presoma of step S1 is placed in reaction vessel, plasma discharging calcining is carried out under protective atmosphere,
Obtain tantalum base oxynitride nano powder.
As further improvement to above-mentioned technical proposal:
Preferably, in the step S2, the specific steps of the calcining are as follows: with 50 DEG C/min~500 DEG C/min heating rate
It is warming up to 800 DEG C~1400 DEG C, keeps the temperature 1min~30min, then with being furnace-cooled to room temperature.
It is furthermore preferred that in the step S2, the specific steps of the calcining are as follows: with 50 DEG C/min~300 DEG C/min liter
Warm rate is warming up to 900 DEG C~1300 DEG C, keeps the temperature 1min~10min, then with being furnace-cooled to room temperature.
Preferably, in the step S2, the reaction vessel includes container casing, the top and bottom of the container casing
It is symmetrically arranged with rotary table lid, offers more than two through-holes on the container casing side wall.
Preferably, the bottom surface of the rotary table lid is arranged close to container casing side.
Preferably, the through-hole close to container casing top side and be symmetrical arranged.
Preferably, in the step S1, the alkali salt is strontium carbonate or barium carbonate, and the tantalum salt is five oxidations two
Tantalum, the nitrogen source are urea, and the alcohol is dehydrated alcohol.
Preferably, the mass volume ratio of the alkali salt, tantalum salt, nitrogen source and alcohol be 1g~8g: 2g~8g: 0.1g~
10g: 5mL~100mL.
It is furthermore preferred that the alkali salt, tantalum salt, nitrogen source and alcohol ratio be 2g~6g: 2g~6g: 0.5g~6g: 5
ML~50mL.
Preferably, in the step S1, the specific steps of the drying are as follows: 1h~72h is kept the temperature at 30 DEG C~80 DEG C.
It is furthermore preferred that the drying temperature is 50 DEG C~80 DEG C, drying time is 6h~48h.
Preferably, the protective atmosphere is the one or more of nitrogen, helium or argon gas.
The inventive concept total as one, the present invention also provides a kind of tantalum base oxynitride nano powders, by preparation above-mentioned
Method is prepared.
Compared with the prior art, the advantages of the present invention are as follows:
1, the present invention prepares tantalum base oxynitride in such a way that plasma discharging calcining is combined with nitrogen source one-step synthesis, by
In Joule effect and field effect, heat transfer efficiency is high, and heating is very efficient, and whole process only needs several minutes, tradition preparation relatively
Method (a few hours or even tens of hours) substantially reduces preparation time, and cost is also cheaper, and discharge plasma sintering liter
It is warm rapid, it can be from the decomposition for kinetically inhibiting nitrogen source.
2, the present invention uses the mode that is rapidly heated of 50 DEG C/min~300 DEG C/min heating rate, forges compared to tradition
Burning mode (1 DEG C/min~50 DEG C of heating rate/min) further chemically can kinetically inhibit the decomposition of nitrogen source, retain
Under the premise of a large amount of nitrogen sources, temperature of reaction system is made to be rapidly reached the temperature needed for oxynitride generates, to occur sufficient
Nitridation reaction greatly shortens the reaction time and improves product purity.
3, the reaction vessel that the present invention places raw material mixing nano powder includes container casing, the top and bottom of container casing
Be symmetrically arranged with rotary table lid, rotary table lid is small relative to traditional cylindrical body lid cross-sectional area, corresponding current density with regard to big, generation
Joule's heat energy is more, higher relative to traditional cylindrical body lid heat transfer efficiency, effect is more preferable, and being beneficial to energy conservation reduces cost,
Reaction temperature is reduced to a certain extent.
Detailed description of the invention
Fig. 1 is reaction vessel and sample schematic diagram in the embodiment of the present invention 1.
Fig. 2 is the XRD spectra of tantalum base oxynitride nano powder made from the embodiment of the present invention 1.
Fig. 3 is the SEM photograph of tantalum base oxynitride nano powder made from the embodiment of the present invention 1.
Fig. 4 is the XRD spectra of tantalum base oxynitride nano powder made from the embodiment of the present invention 2.
Fig. 5 is the SEM photograph of tantalum base oxynitride nano powder made from the embodiment of the present invention 2.
Each label indicates in figure:
1, container casing;11, through-hole;12, rotary table lid;2, presoma is mixed.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
Raw material employed in following embodiment and instrument are commercially available.
A kind of fast preparation method of tantalum base oxynitride nano powder of the invention, comprising the following steps:
S1, alkali salt, tantalum salt and nitrogen source are dissolved in alcohol, it is dry after ball milling, obtain mixing presoma;
S2, the resulting mixing presoma of step S1 is placed in reaction vessel, plasma discharging calcining is carried out under protective atmosphere,
Obtain tantalum base oxynitride nano powder.
The present invention prepares tantalum base oxynitride in such a way that plasma discharging calcining is combined with nitrogen source one-step synthesis,
Due to Joule effect and field effect, heating is very efficient, and whole process only needs several minutes, and (number is small for opposite traditional preparation methods
Shi Naizhi tens of hours) preparation time is substantially reduced, cost is also cheaper.
Embodiment 1:
A kind of fast preparation method of the tantalum base oxynitride nano powder of the present embodiment, comprising the following steps:
S1,3.5g strontium carbonate, 4.5g tantalum pentoxide and 4.8g urea are added in 35ml dehydrated alcohol, and ball milling
240min obtains mixed slurry;
S2, gained mixed slurry after step S1 ball milling is dried, drying process are as follows: it is kept the temperature at 60 DEG C for 24 hours,
Obtain mixing presoma;
S3, the resulting mixing presoma of step S2 is placed in reaction vessel, reaction vessel is placed in and is set without pressure plasma calcining
In standby, plasma discharging calcining is carried out in nitrogen atmosphere, heating rate is 300 DEG C/min, 1000 DEG C of temperature, soaking time
1min;Finally with room temperature is furnace-cooled to, SrTaO is obtained2N nitride oxide powder, i.e. tantalum base oxynitride nano powder, object phase composition
And microscopic appearance difference is as shown in Figures 2 and 3.
In the present invention, it is not vacuum degree that " no pressure " in no pressure plasma calcining, which refers to no mechanical pressure,.It is conventional
Discharge plasma sintering be to be densified under conditions of mechanical compression to powder-mixed presoma, finally obtain block
Material.Plasma discharging calcining of the invention is will to mix powdery precursor to calcine under conditions of no mechanical compression,
Finally obtained is still pulverulent material.
As shown in Figure 1, reaction vessel includes container casing 1, it is hollow cylinder graphite crucible, the top of container casing 1
It is equipped with rotary table lid 12 with bottom symmetrical, offers more than two through-holes 11,2 laying of mix precursor on 1 side wall of container casing
In in container casing 1,2 through-holes 11 are in close 1 top side of container casing and are symmetrical arranged;Rotary table lid 12 is graphite cover, circle
The bottom surface of platform lid 12 is arranged close to 1 side of container casing.
By Fig. 2 and Fig. 3 it is found that the SrTaO that the present embodiment is prepared2N nitride oxide powder is almost pure phase SrTaO2N,
Color is bright orange green;Its form is uniform in size, crystallite dimension about 50~150nm.
Comparative example 1:
A kind of preparation method of tantalum base oxynitride nano powder of this comparative example is roughly the same with embodiment 1, the difference is that:
In step S3, plasma discharging calcining is not carried out using without pressure plasma sintering equipment, using traditional non-pressure sintering furnace
Conventional calcination is carried out, reaction vessel is the crucible (sealing container) with lid, and the heating rate of calcining is 20 DEG C/min, calcining
Temperature is 1100 DEG C, soaking time 60min.
The SrTaO that this comparative example is prepared2N nitride oxide powder object phase composition is SrTaO2N(is a small amount of), Sr2Ta2O7
(a large amount of) and Ta3N5(a small amount of), color are canescence, by the color contrast with tantalum base oxynitride nano powder in embodiment 1,
Qualitatively analysis knows that its purity is low compared with embodiment 1.As it can be seen that being calcined using plasma discharging, it is only necessary to temperature more lower than conventional method
Degree and shorter soaking time, can obtain the higher nitride oxide powder of purity.
Embodiment 2:
A kind of fast preparation method of the tantalum base oxynitride nano powder of the present embodiment, comprising the following steps:
S1,4.8g barium carbonate, 4.5g tantalum pentoxide and 4.8g urea are added in 40ml dehydrated alcohol, and ball milling
240min obtains mixed slurry;
S2, gained mixed slurry after step S1 ball milling is dried, drying process are as follows: it is kept the temperature at 60 DEG C for 24 hours,
Obtain mixing presoma;
S3, the resulting mixing presoma of step S2 is placed in reaction vessel, reaction vessel is placed in and is set without pressure plasma calcining
In standby, plasma discharging calcining is carried out in nitrogen atmosphere, heating rate is 300 DEG C/min, 1000 DEG C of temperature, soaking time
1min;Finally with being furnace-cooled to room temperature to get to BaTaO2N nitride oxide powder, i.e. tantalum base oxynitride nano powder, object phase group
At and microscopic appearance difference it is as shown in Figure 4 and Figure 5.
The reaction vessel that the present embodiment uses is same as Example 1.
By Fig. 4 and Fig. 5 it is found that the BaTaO that the present embodiment is prepared2N nitride oxide powder is almost pure phase BaTaO2N,
Color is sepia;Its form is uniform in size, crystallite dimension about 50~150nm.
Comparative example 2:
A kind of preparation method of tantalum base oxynitride nano powder of this comparative example is roughly the same with embodiment 1, the difference is that:
In step S3, plasma discharging calcining is not carried out using without pressure plasma calciner, using tradition without pressure calcining furnace
Conventional calcination is carried out, reaction vessel is the crucible (sealing container) with lid, and the heating rate of calcining is 20 DEG C/min, calcining
Temperature is 1100 DEG C, soaking time 60min.
The BaTaO that this comparative example is prepared2N nitride oxide powder object phase composition is BaTaO2N(is a small amount of), Ba5Ta4O15
(a large amount of) and Ta3N5(a small amount of), color are canescence, by the color contrast with tantalum base oxynitride nano powder in embodiment 2,
Qualitatively analysis knows that its purity is low compared with embodiment 2.As it can be seen that being calcined using plasma discharging, it is only necessary to temperature more lower than conventional method
Degree and shorter soaking time, can obtain the higher nitride oxide powder of purity.
Embodiment 3:
A kind of fast preparation method of the tantalum base oxynitride nano powder of the present embodiment, comprising the following steps:
S1,3.5g strontium carbonate, 4.5g tantalum pentoxide and 4.8g urea are added in 40ml dehydrated alcohol, and ball milling
240min obtains mixed slurry;
S2, gained mixed slurry after step S1 ball milling is dried, drying process are as follows: it is kept the temperature at 60 DEG C for 24 hours,
Obtain mixing presoma;
S3, the resulting mixing presoma of step S2 is placed in reaction vessel, reaction vessel is placed in and is set without pressure plasma calcining
In standby, plasma discharging calcining is carried out in nitrogen atmosphere, heating rate is 200 DEG C/min, 1100 DEG C of temperature, soaking time
1min;Finally with being furnace-cooled to room temperature to get to SrTaO2N nitride oxide powder, i.e. tantalum base oxynitride nano powder.
The reaction vessel that the present embodiment uses is same as Example 1.
Through detecting, SrTaO that the present embodiment is prepared2N nitride oxide powder is almost pure phase SrTaO2N, color are bright
Yellow green;Its form is uniform in size, crystallite dimension about 100~200nm.
Embodiment 4:
A kind of fast preparation method of the tantalum base oxynitride nano powder of the present embodiment, comprising the following steps:
S1,4.8g barium carbonate, 4.5g tantalum pentoxide and 4.8g urea are added in 40ml dehydrated alcohol, and ball milling
240min obtains mixed slurry;
S2, gained mixed slurry after step S1 ball milling is dried, drying process are as follows: it is kept the temperature at 60 DEG C for 24 hours,
Obtain mixing presoma;
S3, the resulting mixing presoma of step S2 is placed in reaction vessel, reaction vessel is placed in and is set without pressure plasma calcining
In standby, plasma discharging calcining is carried out in nitrogen atmosphere, heating rate is 200 DEG C/min, 1100 DEG C of temperature, soaking time
1min;Finally with being furnace-cooled to room temperature to get to BaTaO2N nitride oxide powder, i.e. tantalum base oxynitride nano powder.
The reaction vessel that the present embodiment uses is same as Example 1.
Through detecting, BaTaO that the present embodiment is prepared2N nitride oxide powder is almost pure phase BaTaO2N, color are palm fibre
Brown;Its form is uniform in size, crystallite dimension about 100~200nm.
Comparative example 3:
A kind of preparation method of tantalum base oxynitride nano powder of this comparative example is roughly the same with embodiment 1, the difference is that:
In step S3, reaction vessel upper and lower covers are traditional cylindrical body lid, and the height of cylindrical body lid is identical as rotary table lid in embodiment 1,
The cross section of cylindrical body lid is identical as rotary table base face cross section.
In calcination process, output power needed for equipment is high compared with embodiment 1, i.e. the energy of same process parameter cylindrical body lid
Consumption is high, heat transfer efficiency is low, more energy efficient using reaction vessel of the invention, advantageously reduces cost, reduces to a certain extent anti-
Answer temperature.
Although the present invention has been disclosed as a preferred embodiment, however, it is not intended to limit the invention.It is any to be familiar with ability
The technical staff in domain, without deviating from the scope of the technical scheme of the present invention, all using the technology contents pair of the disclosure above
Technical solution of the present invention makes many possible changes and modifications or equivalent example modified to equivalent change.Therefore, all
Without departing from the content of technical solution of the present invention, according to the present invention technical spirit any simple modification made to the above embodiment,
Equivalent variations and modification, all shall fall within the protection scope of the technical scheme of the invention.
Claims (9)
1. a kind of preparation method of tantalum base oxynitride nano powder, it is characterised in that: the following steps are included:
S1, alkali salt, tantalum salt and nitrogen source are dissolved in alcohol, it is dry after ball milling, obtain mixing presoma;
S2, the resulting mixing presoma of step S1 is placed in reaction vessel, is carried out under protective atmosphere without pressure plasma discharging
Calcining, obtains tantalum base oxynitride nano powder;
In the step S2, the specific steps of the calcining are as follows: be warming up to 50 DEG C/min~500 DEG C/min heating rate
800 DEG C~1400 DEG C, 1min~30min is kept the temperature, then with being furnace-cooled to room temperature.
2. preparation method according to claim 1, it is characterised in that: in the step S2, the specific steps of the calcining
Are as follows: 900 DEG C~1300 DEG C are warming up to 50 DEG C/min~300 DEG C/min heating rate, keeps the temperature 1min~10min, then with furnace
It is cooled to room temperature.
3. preparation method according to claim 1 or 2, it is characterised in that: in the step S2, the reaction vessel includes
Container casing (1) is symmetrically arranged with rotary table lid (12) at the top and bottom of the container casing (1), container casing (1) side wall
On offer more than two through-holes (11).
4. preparation method according to claim 3, it is characterised in that: the bottom surface of the rotary table lid (12) is close to container casing
(1) side is arranged.
5. the preparation method according to claim 4, it is characterised in that: top of the through-hole (11) close to container casing (1)
Portion side is simultaneously symmetrical arranged.
6. preparation method according to claim 3, it is characterised in that: in the step S1, the alkali salt is carbon
Sour strontium or barium carbonate, the tantalum salt are tantalum pentoxide, and the nitrogen source is urea, and the alcohol is dehydrated alcohol, the alkaline earth gold
The mass volume ratio for belonging to salt, tantalum salt, nitrogen source and alcohol is 1g~8g: 2g~8g: 0.1g~10g: 5mL~100mL.
7. preparation method according to claim 1 or 2, it is characterised in that: in the step S1, the specific step of the drying
Suddenly are as follows: 1h~72h is kept the temperature at 30 DEG C~80 DEG C.
8. preparation method according to claim 1 or 2, it is characterised in that: the protective atmosphere is nitrogen, helium or argon gas
It is one or more.
9. a kind of tantalum base oxynitride nano powder, it is characterised in that: the tantalum base oxynitride nano powder is by claim 1 to 8
Any one of described in preparation method be prepared.
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CN114906827A (en) * | 2022-04-20 | 2022-08-16 | 巢湖学院 | Microwave-assisted one-step rapid preparation method of metal oxynitride |
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CN114906827A (en) * | 2022-04-20 | 2022-08-16 | 巢湖学院 | Microwave-assisted one-step rapid preparation method of metal oxynitride |
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