CN108328587A - It is a kind of that Ti is synthesized using Al fluxing agents3B2The method of N - Google Patents
It is a kind of that Ti is synthesized using Al fluxing agents3B2The method of N Download PDFInfo
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- CN108328587A CN108328587A CN201810169742.5A CN201810169742A CN108328587A CN 108328587 A CN108328587 A CN 108328587A CN 201810169742 A CN201810169742 A CN 201810169742A CN 108328587 A CN108328587 A CN 108328587A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0602—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with two or more other elements chosen from metals, silicon or boron
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The present invention provides a kind of using Al fluxing agents synthesis Ti3B2The method of N, includes the following steps：TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: (2.5~3.5) B: BN=: (0.7~1.3): (0.7~1.3).The TiH that will be weighed2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain mixture；The metal Al powder of the mixture weight ratio 5~15% is added into mixture as fluxing agent, is uniformly mixed, tabletting, 700~1000 DEG C is then warming up under inert protective atmosphere, keep the temperature 2~12h；It waits for obtaining sample after the completion of above-mentioned steps；Under inert protective atmosphere, after sample cooled to room temperature, then using remaining Al in dilute hydrochloric acid removing sample, Ti is obtained3B2N.The present invention is by adding Al powder fluxing agents, successfully by Ti3B2N synthesis temperatures are reduced to 700~1000 DEG C, therefore the present invention can be substantially reduced Ti3B2The synthesis temperature of N, it is particularly significant for practical application, it is suitble to industrial scale production, reduces production cost.
Description
Technical field
The invention belongs to structural material fields, and in particular to be it is a kind of using Al fluxing agents synthesize Ti3B2The method of N.
Background technology
Ti3B2N is a kind of novel ternary layered compound, it has high-modulus, and (Young's modulus 430.22GPa shears mould
Measure 181.06GPa), high intensity etc..Meanwhile Ti3B2N has very low density (theoretical density 4.80g/cm3)。
Chinese patent application 2016100610872 discloses a kind of new ceramics crystal Ti3B2N and preparation method thereof, the Shen
High-temperature solid phase reaction method please be use to synthesize Ti3B2N, but the synthesis temperature that this application needs is 1100-1200 DEG C higher, is unfavorable for
The actual production of product, and high temperature production cost is higher, and synthetic technology disclosed in this application is still immature, also needs to continue to change
Into.
Therefore, other synthetic methods are found, synthesis temperature are reduced, for Ti3B2The practical application of N materials has good
Realistic meaning.
Invention content
Purpose of the present invention is to overcome above-mentioned new material Ti in the prior art3B2The high problem defect of the synthesis temperature of N, and carry
What is gone out is a kind of using Al fluxing agents synthesis Ti3B2The method of N.Ti can be greatly reduced in synthetic method provided by the invention3B2N's
Synthesis temperature is suitble to industrial scale production, reduces production cost.
To achieve the goals above, the present invention provides the following technical solutions：
It is a kind of that Ti is synthesized using Al fluxing agents3B2The method of N, the synthesis Ti3B2The method of N includes the following steps：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And the TiH2The molar ratio TiH of three kinds of powder, the unformed B powder and the hexagonal AlN powder raw materials2: B: BN=
(2.5~3.5): (0.7~1.3): (0.7~1.3)；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
3) the metal Al powder of the mixture weight ratio 5~15% is added into the mixture in step 2) as fluxing agent,
It is uniformly mixed, tabletting, 700~1000 DEG C is then warming up under inert protective atmosphere, keep the temperature 2~12h；
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature, then using dilute
Hydrochloric acid removes remaining Al in sample, obtains Ti3B2N。
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that in step 2), the TiH2It is powder, unformed
B powder and hexagonal AlN powder, which are put into reactor, to be mixed evenly process and is：In TiH2Powder, unformed B powder, the mixing of hexagonal AlN powder are stirred
It is added in mixing after absolute ethyl alcohol is mixed evenly, naturally dry.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that absolute ethyl alcohol is added, 5~30h is mixed
Afterwards, naturally dry.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that the addition of absolute ethyl alcohol must satisfy this
Absolute ethyl alcohol liquid level floods completely exceeds TiH2Powder, unformed B powder and the mixed material of hexagonal AlN powder.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that the addition of absolute ethyl alcohol must satisfy this
Absolute ethyl alcohol liquid level floods completely exceeds TiH2Powder, unformed B powder and the mixed 1~5mm of material of hexagonal AlN powder.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that in step 1), the TiH2Powder, the nothing
The molar ratio TiH of sizing three kinds of raw materials of B powder and the hexagonal AlN powder2: (2.5~3) B: BN=: (1~1.3): (1~1.3)；It is excellent
Selection of land, the TiH2The molar ratio TiH of three kinds of powder, the unformed B powder and the hexagonal AlN powder raw materials2: B: BN=3: 1: 1.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that in step 3), under inert protective atmosphere
700~1000 DEG C are warming up to the rate of 5~10 DEG C/min, keeps the temperature 2~12h；Preferably, with 6~8 under inert protective atmosphere
DEG C/rate of min is warming up to 700~1000 DEG C, keep the temperature 2~12h.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that in step 3), under inert protective atmosphere
700~1000 DEG C are warming up to, 3~5h or 7-11h is kept the temperature；Preferably, 700~900 DEG C are warming up under inert protective atmosphere；It is excellent
Selection of land keeps the temperature 4~5h or 7-11h.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that in step 3), the inert protective atmosphere
Under inert gas be argon gas or nitrogen；Preferably, the inert gas is argon gas.
Ti is synthesized using Al fluxing agents as described above3B2The method of N, it is preferable that in step 4), the concentration of the dilute hydrochloric acid
For 10-20%；Preferably, the time that the sample impregnates in the dilute hydrochloric acid is 24~96h.
Compared with the immediate prior art, technical solution provided by the invention has following excellent effect：
1, Ti can be greatly reduced in synthetic method provided by the invention3B2The synthesis temperature of N, the synthetic method are simply easily grasped
Make, is suitble to industrial scale production, reduces production cost.
2, in the present invention by adding Al powder fluxing agents, successfully by Ti3B2N synthesis temperatures are reduced to 700~1000 DEG C,
Therefore the present invention can be substantially reduced Ti3B2The synthesis temperature of N, it is particularly significant for practical application.
Description of the drawings
Fig. 1：The Ti that in the present invention prepared by specific embodiment 13B2The XRD spectrum of N samples.
Fig. 2：Ti3B2The theoretical XRD spectrum of N compounds.
Fig. 3：The XRD spectrum of reference examples 1 in the present invention.
Fig. 4：The Ti that in the present invention prepared by specific embodiment 23B2The XRD spectrum of N samples.
Fig. 5：The Ti that in the present invention prepared by specific embodiment 33B2The XRD spectrum of N samples.
Fig. 6：The Ti that in the present invention prepared by specific embodiment 43B2The XRD spectrum of N samples.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
The every other embodiment that logical technical staff is obtained, shall fall within the protection scope of the present invention.
The present invention will be described in detail below with reference to the accompanying drawings and embodiments.It should be noted that in the feelings not conflicted
Under condition, the feature in embodiment and embodiment in the present invention can be combined with each other.
Specific embodiments of the present invention provide a kind of using Al fluxing agents synthesis Ti3B2The method of N synthesizes Ti3B2The side of N
Method includes the following steps：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: (2.5~3.5) B: BN=(such as
2.6,2.7,2.8,2.9,3,3.1,3.2,3.3,3.4): (0.7~1.3) (such as 0.7,0.9,1.0,1.1,1.15,1.2,
1.25,1.26,1.27): (0.7~1.3) (such as 0.7,0.9,1.0,1.1,1.15,1.2,1.25,1.26,1.27)；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
3) be added into the mixture in step 2) the mixture weight ratio 5~15% (such as 6%, 7%, 8%, 9%,
10%, 11%, 12%, 13%, 14%) metal Al powder is uniformly mixed, tabletting as fluxing agent, then protects gas in inertia
Be warming up under atmosphere 700~1000 DEG C (such as 750 DEG C, 760 DEG C, 780 DEG C, 800 DEG C, 820 DEG C, 840 DEG C, 860 DEG C, 880 DEG C, 900
DEG C, 920 DEG C, 940 DEG C, 960 DEG C, 980 DEG C, 990 DEG C), heat preservation 2~12h (such as 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h,
6.5h、7h、7.5h、8h、8.5h、9h、9.5h、10h、10.5h、11h、11.5h)；
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature, then using dilute
Hydrochloric acid removes remaining Al in sample, obtains Ti3B2N。
In step 3), pressure in tableting processes must 3-8MPa (such as 4MPa, 4.5MPa, 5MPa, 5.5MPa,
6MPa、6.5MPa、7MPa、7.5MPa、7.8MPa).Preferably, the pressure in tableting processes must be in 5MPa.
To keep material mixing more uniform, in TiH2Powder, unformed B powder, hexagonal AlN powder blending process in preferably add
Absolute ethyl alcohol is as dispersant.In step 2), TiH2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed
Even process is：In TiH2Powder, unformed B powder, hexagonal AlN powder are added in being mixed after absolute ethyl alcohol is mixed evenly, from
So dry.Preferably, be added absolute ethyl alcohol be mixed 5~30h (such as 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 15h,
18h, 20h, 21h, 22h, 23h, 25h, 26h, 28h, 29h) after, naturally dry.
In a specific embodiment of the present invention, further preferably, the addition of absolute ethyl alcohol ensures that its liquid level did not had material,
That is the addition of absolute ethyl alcohol, which must satisfy the absolute ethyl alcohol liquid level and flood completely, exceeds TiH2Powder, unformed B powder and hexagonal AlN
The mixed material of powder.Further preferably, the addition of absolute ethyl alcohol must satisfy the absolute ethyl alcohol liquid level and flood completely and exceeds
TiH2Powder, unformed B powder and the mixed 1~5mm of material of hexagonal AlN powder (such as 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm,
4mm、4.5mm、4.8mm)。
In a specific embodiment of the present invention, further preferably, in step 1), TiH2Powder, unformed B powder and hexagonal AlN powder
The molar ratio TiH of three kinds of raw materials2: (2.5~3) B: BN=(such as 2.65,2.75,2.85,2.95): (1~1.3) (such as
1.1,1.15,1.2,1.25,1.26,1.27): (1~1.3) (such as 1.1,1.15,1.2,1.25,1.26,1.27)；Further preferably
Ground, the TiH2The molar ratio TiH of three kinds of powder, the unformed B powder and the hexagonal AlN powder raw materials2: B: BN=3: 1: 1.
In a specific embodiment of the present invention, further preferably, in step 3), under inert protective atmosphere with 5~10 DEG C/
Min (such as 5.5 DEG C/min, 6 DEG C/min, 6.5 DEG C/min, 7 DEG C/min, 7.5 DEG C/min, 8 DEG C/min, 8.5 DEG C/min, 9 DEG C/
Min, 9.5 DEG C/min) rate be warming up to 700~1000 DEG C (such as 750 DEG C, 760 DEG C, 780 DEG C, 800 DEG C, 820 DEG C, 840
DEG C, 860 DEG C, 880 DEG C, 900 DEG C, 920 DEG C, 940 DEG C, 960 DEG C, 980 DEG C, 990 DEG C), keep the temperature 2~12h.Preferably, in inertia
With 6~8 DEG C/min (such as 6.2 DEG C/min, 6.5 DEG C/min, 7.3 DEG C/min, 7.6 DEG C/min, 7.8 DEG C/min) under protective atmosphere
Rate heating.
In a specific embodiment of the present invention, further preferably, in step 3), 700 are warming up under inert protective atmosphere
~1000 DEG C (such as 750 DEG C, 760 DEG C, 780 DEG C, 800 DEG C, 820 DEG C, 840 DEG C, 860 DEG C, 880 DEG C, 900 DEG C, 920 DEG C, 940
DEG C, 960 DEG C, 980 DEG C, 990 DEG C), keep the temperature 3~5h or 7-11h；Preferably, 700~900 are warming up under inert protective atmosphere
DEG C (such as 750 DEG C, 760 DEG C, 780 DEG C, 800 DEG C, 820 DEG C, 840 DEG C, 860 DEG C, 870 DEG C, 900 DEG C).More preferably, 4 are kept the temperature
~5h or 7-11h.
In a specific embodiment of the present invention, further preferably, in step 3), the inert gas under inert protective atmosphere is
Argon gas or nitrogen；Preferably inert gas is argon gas.
In a specific embodiment of the present invention, further preferably, in step 4), a concentration of 10-20% of dilute hydrochloric acid (such as
11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%)；Preferably, the time that sample impregnates in dilute hydrochloric acid
For 24~96h (such as 26h, 27h, 28h, 29h, 30h, 35h, 40h, 45h, 50h, 55h, 60h, 65h, 70h, 75h, 80h,
85h, 90h, 95h), specific soaking time depends on the content of Al in sample, and this is not limited by the present invention.
To sum up, the present invention synthesizes Ti using Al fluxing agents3B2The method of N：By TiH2Powder, unformed B powder, hexagonal AlN
The molar ratio TiH of three kinds of raw materials of powder2: (2.5~3.5) B: BN=: (0.7~1.3): (0.7~1.3) weighs TiH2Powder, nothing are fixed
Type B powder and hexagonal AlN powder；The TiH that will be weighed2The metal of weight ratio 5~15% is added in powder, unformed B powder, hexagonal AlN powder mixing
Al powder is uniformly mixed, then tabletting is warming up to 700 under inert protective atmosphere with the rate of 5~10 DEG C/min as fluxing agent
~1000 DEG C, keep the temperature 2~12h；After the completion of reaction, under inert protective atmosphere, sample cooled to room temperature；Using dilute hydrochloric acid
Remaining Al in sample is removed, Ti is obtained3B2N.In synthetic method of the present invention, by adding Al powder fluxing agents, successfully by Ti3B2N
Synthesis temperature is reduced to 700~1000 DEG C.The main reason for technical scheme of the present invention can successfully reduce synthesis temperature be：
At a lower temperature, it is melted using lower melting-point fluxing agent, in the environment of having liquid in this way, can promote to participate in solid phase
The diffusion of the raw material of reaction, so as to start to react at a lower temperature.I.e. the present invention selects the reason of Al powder fluxing agents：1)
Al fusing points are 660 DEG C low；2) although Al and B has Binary-phase compound AlB12In the presence of, but its synthesis temperature needs 1000 DEG C or more；Al
With N with the presence of Binary-phase compound AlN, but its synthesis temperature needs 1200 DEG C or more；There is no the ternary of Al-B-N simultaneously
Close object.Therefore synthesis temperature can effectively be reduced by making fluxing agent using lower melting-point Al powder.
Therefore the present invention can be substantially reduced Ti3B2The synthesis temperature of N, it is particularly significant for practical application.
Al powder, TiH in following embodiment2Powder, unformed B powder and hexagonal AlN powder are commercial product, purity 99.9%
More than.
Embodiment 1
Ti is synthesized using Al fluxing agents the present embodiment provides a kind of3B2The method of N synthesizes Ti3B2The method of N includes as follows
Step：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: B: BN=3: 1: 1；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
TiH2Powder, unformed B powder and hexagonal AlN powder, which are put into container, to be mixed evenly process and is：In TiH2It is powder, unformed
B powder, hexagonal AlN powder add absolute ethyl alcohol mixing 18h in being mixed after, naturally dry.Wherein, absolute ethyl alcohol plus
Enter amount and must satisfy the absolute ethyl alcohol liquid level and flood completely to exceed TiH2Powder, unformed B powder and the mixed material of hexagonal AlN powder
3mm。
3) the metal Al powder of the mixture weight ratio 10% is added into the mixture in step 2) as fluxing agent, in agate
It is uniformly mixed in Nao mortars, tabletting (pressure in tableting processes must be in 5MPa) is cold-pressed into biscuit block；Biscuit block is placed in
Then tube furnace is warming up to 900 DEG C under inert protective atmosphere with the rate of 10 DEG C/min, keep the temperature 3h.
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature；Sample is set
It is impregnated in a concentration of 15% dilute hydrochloric acid and removes remaining Al in sample, the time of immersion is 48h, is diluted with distilled water, is filtered
Centrifugation, can obtain Ti3B2N black samples.
Ti manufactured in the present embodiment3B2The XRD spectrum of N products is shown in Fig. 1.Due to Ti3B2N is a kind of newly synthesized substance, because
It is not yet included in this X-ray diffraction standard card valut.Using crystal XRD spectra simulation softward poudrix, Ti can be obtained3B2The reason of N
By XRD spectrum, Fig. 2 is seen.Fig. 1 and Fig. 2 are compared, it may be determined that main phase is Ti in synthetic sample3B2N compounds.Meanwhile sample
Also contain a small amount of dephasign (TiN, JCPDS card number in product：38-1420；TiB2, JCPDS card numbers：35-0741).
Reference examples 1
This reference examples difference from example 1 is that：Al fluxing agents are not added.The same embodiment of other synthesis steps
1。
The XRD spectrum of product prepared by this reference examples is shown in Fig. 3.From figure 3, it can be seen that the comparative example and embodiment 1 its
Its condition is identical, but in the case of being added without Al fluxing agents, and comparative example can not obtain Ti3B2N phases.
Embodiment 2
The present embodiment difference from example 1 is that：TiH2Powder, unformed B powder, hexagonal AlN powder three kinds of raw materials rub
You compare TiH2: B: BN=2.5: 1.3: 1.3.Other are same as Example 1.
The XRD spectrum of product manufactured in the present embodiment is shown in Fig. 4.Although being still containing Ti3B2N、TiB2With tri- kinds of phases of TiN,
But embodiment 2 and embodiment 1 compare it is found that Ti in the sample of the embodiment 2 synthesis3B2The content of N is compared in embodiment 1
It is reduced.
Embodiment 3
The present embodiment difference from example 1 is that：Reaction temperature under an inert atmosphere is 700 DEG C.Other with
Embodiment 1 is identical.
The XRD spectrum of product manufactured in the present embodiment is shown in Fig. 5.Although the present embodiment is still containing Ti3B2N、TiB2With
Tri- kinds of phases of TiN, but Ti in the sample of the embodiment 3 synthesis3B2The content of N compares being reduced in embodiment 1.
Embodiment 4
The present embodiment difference from example 1 is that：The metal Al powder of mixture weight ratio 5% is added as fluxing
Agent, while the pyroreaction time is 12h.Other are same as Example 1.
The XRD spectrum of product manufactured in the present embodiment is shown in Fig. 6.Although being still containing Ti3B2N、TiB2With tri- kinds of phases of TiN,
But Ti in the sample of the embodiment 3 synthesis3B2The content of N compares being reduced in embodiment 1.
Embodiment 5
Ti is synthesized using Al fluxing agents the present embodiment provides a kind of3B2The method of N synthesizes Ti3B2The method of N includes as follows
Step：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: B: BN=3.5: 0.7: 1；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
TiH2Powder, unformed B powder and hexagonal AlN powder, which are put into container, to be mixed evenly process and is：In TiH2It is powder, unformed
B powder, hexagonal AlN powder add absolute ethyl alcohol mixing 30h in being mixed after, naturally dry.The addition of absolute ethyl alcohol must
It the absolute ethyl alcohol liquid level must be met floods completely and exceed TiH2Powder, unformed B powder and the mixed material 2mm of hexagonal AlN powder.
3) the metal Al powder of the mixture weight ratio 15% is added into the mixture in step 2) as fluxing agent, in agate
It is uniformly mixed in Nao mortars, tabletting (pressure in tableting processes must be in 3MPa) is cold-pressed into biscuit block；Biscuit block is placed in
Then tube furnace is warming up to 700 DEG C under inert protective atmosphere with the rate of 6 DEG C/min, keep the temperature 4h.
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature；Sample is set
It is impregnated in a concentration of 15% dilute hydrochloric acid and removes remaining Al in sample, the time of immersion is 30h, is diluted with distilled water, is filtered
Centrifugation, can obtain Ti3B2N black samples.
The XRD spectrum of product manufactured in the present embodiment is not shown.The present embodiment contains Ti3B2N、TiB2With tri- kinds of phases of TiN,
And Ti in the sample of embodiment synthesis3B2The content of N is close in embodiment 1.
Embodiment 6
Ti is synthesized using Al fluxing agents the present embodiment provides a kind of3B2The method of N synthesizes Ti3B2The method of N includes as follows
Step：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: B: BN=3: 0.8: 0.8；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
TiH2Powder, unformed B powder and hexagonal AlN powder, which are put into container, to be mixed evenly process and is：In TiH2It is powder, unformed
B powder, hexagonal AlN powder add absolute ethyl alcohol mixing 25h in being mixed after, naturally dry.The addition of absolute ethyl alcohol must
It the absolute ethyl alcohol liquid level must be met floods completely and exceed TiH2Powder, unformed B powder and the mixed material 4mm of hexagonal AlN powder.
3) the metal Al powder of the mixture weight ratio 8% is added into the mixture in step 2) as fluxing agent, in agate
It is uniformly mixed in Nao mortars, tabletting (pressure in tableting processes must be in 8MPa) is cold-pressed into biscuit block；Biscuit block is placed in
Then tube furnace is warming up to 800 DEG C under inert protective atmosphere with the rate of 8 DEG C/min, keep the temperature 7h.
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature；Sample is set
It is impregnated in a concentration of 12% dilute hydrochloric acid and removes remaining Al in sample, the time of immersion is 40h, is diluted with distilled water, is filtered
Centrifugation, can obtain Ti3B2N black samples.
The XRD spectrum of product manufactured in the present embodiment is not shown.The present embodiment contains Ti3B2N、TiB2With tri- kinds of phases of TiN,
And Ti in the sample of embodiment synthesis3B2The content of N is close in embodiment 1.
Embodiment 7
Ti is synthesized using Al fluxing agents the present embodiment provides a kind of3B2The method of N synthesizes Ti3B2The method of N includes as follows
Step：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: B: BN=2.5: 1: 1.3；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
TiH2Powder, unformed B powder and hexagonal AlN powder, which are put into container, to be mixed evenly process and is：In TiH2It is powder, unformed
B powder, hexagonal AlN powder add absolute ethyl alcohol mixing 10h in being mixed after, naturally dry.The addition of absolute ethyl alcohol must
It the absolute ethyl alcohol liquid level must be met floods completely and exceed TiH2Powder, unformed B powder and the mixed material 5mm of hexagonal AlN powder.
3) the metal Al powder of the mixture weight ratio 12% is added into the mixture in step 2) as fluxing agent, in agate
It is uniformly mixed in Nao mortars, tabletting (pressure in tableting processes must be in 4MPa) is cold-pressed into biscuit block；Biscuit block is placed in
Then tube furnace is warming up to 850 DEG C under inert protective atmosphere with the rate of 7 DEG C/min, keep the temperature 10h.
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature；Sample is set
It is impregnated in a concentration of 16% dilute hydrochloric acid and removes remaining Al in sample, the time of immersion is 80h, is diluted with distilled water, is filtered
Centrifugation, can obtain Ti3B2N black samples.
The XRD spectrum of product manufactured in the present embodiment is not shown.The present embodiment contains Ti3B2N、TiB2With tri- kinds of phases of TiN,
And Ti in the sample of embodiment synthesis3B2The content of N is close in embodiment 1.
Embodiment 8
Ti is synthesized using Al fluxing agents the present embodiment provides a kind of3B2The method of N synthesizes Ti3B2The method of N includes as follows
Step：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And TiH2The molar ratio TiH of three kinds of powder, unformed B powder and hexagonal AlN powder raw materials2: B: BN=2.8): 1.1: 0.9；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and obtain
Mixture；
TiH2Powder, unformed B powder and hexagonal AlN powder, which are put into container, to be mixed evenly process and is：In TiH2It is powder, unformed
B powder, hexagonal AlN powder add absolute ethyl alcohol mixing 21h in being mixed after, naturally dry.The addition of absolute ethyl alcohol must
It the absolute ethyl alcohol liquid level must be met floods completely and exceed TiH2Powder, unformed B powder and the mixed material 1mm of hexagonal AlN powder.
3) the metal Al powder of the mixture weight ratio 8% is added into the mixture in step 2) as fluxing agent, in agate
It is uniformly mixed in Nao mortars, tabletting (pressure in tableting processes must be in 7MPa) is cold-pressed into biscuit block；Biscuit block is placed in
Then tube furnace is warming up to 750 DEG C under inert protective atmosphere with the rate of 7 DEG C/min, keep the temperature 5h.
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature；Sample is set
It is impregnated in a concentration of 12% dilute hydrochloric acid and removes remaining Al in sample, the time of immersion is 96h, is diluted with distilled water, is filtered
Centrifugation, can obtain Ti3B2N black samples.
The XRD spectrum of product manufactured in the present embodiment is not shown.The present embodiment contains Ti3B2N、TiB2With tri- kinds of phases of TiN,
And Ti in the sample of embodiment synthesis3B2The content of N is close in embodiment 1.
In conclusion the present invention has the following technical effect that：
1, Ti can be greatly reduced in synthetic method provided by the invention3B2The synthesis temperature of N, the synthetic method are simply easily grasped
Make, is suitble to industrial scale production, reduces production cost.
2, in the present invention by adding Al powder fluxing agents, successfully by Ti3B2N synthesis temperatures are reduced to 700~1000 DEG C,
Therefore the present invention can be substantially reduced Ti3B2The synthesis temperature of N, it is particularly significant for practical application.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God and principle within, any modification, equivalent replacement, improvement and so on, accompanying claims protection domain of the present invention it
It is interior.
Claims (10)
1. a kind of synthesizing Ti using Al fluxing agents3B2The method of N, which is characterized in that the synthesis Ti3B2The method of N includes as follows
Step：
1) TiH is weighed respectively2Powder, unformed B powder and hexagonal AlN powder, it is spare；
And the TiH2The molar ratio TiH of three kinds of powder, the unformed B powder and the hexagonal AlN powder raw materials2: B: BN=(2.5~
3.5): (0.7~1.3): (0.7~1.3)；
2) TiH that will be weighed in step 1)2Powder, unformed B powder and hexagonal AlN powder are put into container and are mixed evenly, and must mix
Material；
3) the metal Al powder of the mixture weight ratio 5~15% is added into the mixture in step 2) as fluxing agent, mixing
Uniformly, then tabletting is warming up to 700~1000 DEG C under inert protective atmosphere, keep the temperature 2~12h；
4) it waits for obtaining sample after the completion of step 3)；Under inert protective atmosphere, after sample cooled to room temperature, then dilute hydrochloric acid is used
Remaining Al in sample is removed, Ti is obtained3B2N。
2. synthesizing Ti using Al fluxing agents as described in claim 13B2The method of N, which is characterized in that described in step 2)
TiH2Powder, unformed B powder and hexagonal AlN powder, which are put into reactor, to be mixed evenly process and is：In TiH2Powder, unformed B powder, six
Square BN powder is added in being mixed after absolute ethyl alcohol is mixed evenly, naturally dry.
3. synthesizing Ti using Al fluxing agents as claimed in claim 23B2The method of N, which is characterized in that it is mixed that absolute ethyl alcohol is added
After closing 5~30h of stirring, naturally dry.
4. synthesizing Ti using Al fluxing agents as claimed in claim 23B2The method of N, which is characterized in that the addition of absolute ethyl alcohol
Amount, which must satisfy the absolute ethyl alcohol liquid level and flood completely, exceeds TiH2Powder, unformed B powder and the mixed material of hexagonal AlN powder.
5. synthesizing Ti using Al fluxing agents as described in claim 2 or 43B2The method of N, which is characterized in that absolute ethyl alcohol adds
Enter amount and must satisfy the absolute ethyl alcohol liquid level and flood completely to exceed TiH2Powder, unformed B powder and the mixed material of hexagonal AlN powder 1
~5mm.
6. synthesizing Ti using Al fluxing agents as described in claim 13B2The method of N, which is characterized in that described in step 1)
TiH2The molar ratio TiH of three kinds of powder, the unformed B powder and the hexagonal AlN powder raw materials2: (2.5~3) B: BN=: (1~1.3)
: (1~1.3)；
Preferably, the TiH2The molar ratio TiH of three kinds of powder, the unformed B powder and the hexagonal AlN powder raw materials2: B: BN=3:
1∶1。
7. synthesizing Ti using Al fluxing agents as described in claim 13B2The method of N, which is characterized in that in step 3), in inertia
700~1000 DEG C are warming up to the rate of 5~10 DEG C/min under protective atmosphere, keeps the temperature 2~12h；
Preferably, 700~1000 DEG C are warming up to the rate of 6~8 DEG C/min under inert protective atmosphere, keep the temperature 2~12h.
8. synthesizing Ti using Al fluxing agents as described in claim 13B2The method of N, which is characterized in that in step 3), in inertia
It is warming up to 700~1000 DEG C under protective atmosphere, keeps the temperature 3~5h or 7-11h；
Preferably, 700~900 DEG C are warming up under inert protective atmosphere；
Preferably, 4~5h or 7-11h is kept the temperature.
9. synthesizing Ti using Al fluxing agents as described in claim 13B2The method of N, which is characterized in that described lazy in step 3)
Property protective atmosphere under inert gas be argon gas or nitrogen；
Preferably, the inert gas is argon gas.
10. synthesizing Ti using Al fluxing agents as described in claim 13B2The method of N, which is characterized in that described in step 4)
A concentration of 10-20% of dilute hydrochloric acid；
Preferably, the time that the sample impregnates in the dilute hydrochloric acid is 24~96h.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810169742.5A CN108328587A (en) | 2018-02-08 | 2018-02-08 | It is a kind of that Ti is synthesized using Al fluxing agents3B2The method of N |
| CN201910091841.0A CN109607559B (en) | 2018-02-08 | 2019-01-30 | Method for synthesizing ternary layered compound by adopting metal powder fluxing agent |
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| CN201810169742.5A CN108328587A (en) | 2018-02-08 | 2018-02-08 | It is a kind of that Ti is synthesized using Al fluxing agents3B2The method of N |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108911794A (en) * | 2018-09-18 | 2018-11-30 | 河南理工大学 | A kind of raising Ti3B2The processing method of N material purity |
| CN109437327A (en) * | 2018-12-26 | 2019-03-08 | 台州学院 | It is a kind of to prepare pure phase Sr97Nd3Co200As200The method of compound |
-
2018
- 2018-02-08 CN CN201810169742.5A patent/CN108328587A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108911794A (en) * | 2018-09-18 | 2018-11-30 | 河南理工大学 | A kind of raising Ti3B2The processing method of N material purity |
| CN108911794B (en) * | 2018-09-18 | 2020-07-03 | 河南理工大学 | Improve Ti3B2Method for processing purity of N material |
| CN109437327A (en) * | 2018-12-26 | 2019-03-08 | 台州学院 | It is a kind of to prepare pure phase Sr97Nd3Co200As200The method of compound |
| CN109437327B (en) * | 2018-12-26 | 2020-09-29 | 台州学院 | Preparation of pure phase Sr97Nd3Co200As200Method for preparing compounds |
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