CN107215897A - A kind of preparation method of black transparent amorphous niobium pentaoxide - Google Patents
A kind of preparation method of black transparent amorphous niobium pentaoxide Download PDFInfo
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- CN107215897A CN107215897A CN201710445794.6A CN201710445794A CN107215897A CN 107215897 A CN107215897 A CN 107215897A CN 201710445794 A CN201710445794 A CN 201710445794A CN 107215897 A CN107215897 A CN 107215897A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/02—Amorphous compounds
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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Abstract
The invention provides a kind of preparation method of black transparent amorphous niobium pentaoxide, by monoclinic phase H Nb2O5It is forced into 21.3~30.0GPa and obtains black transparent amorphous niobium pentaoxide.The present invention obtains black, amorphous Nb with good light permeability matter using the method for HIGH PRESSURE TREATMENT2O5Material；Unload to normal pressure, Nb2O5Stable non crystalline structure and good light transmitting property can be kept；And the operating process of the present invention is simple, easily operated.
Description
Technical field
The present invention relates to the high pressure preparing technical field of functional material, more particularly to a kind of black transparent amorphous five oxidation two
The preparation method of niobium.
Background technology
Nb2O5It is a kind of important raw material of industry, can be used as drawing niobic acid Ni-monocrystal, prepare special optical glass, high frequency and low
Frequency capacitor and piezo ceramic element, it can also be used to produce the various niobium alloys that ferro-niobium and special steel need.Nb2O5It is to produce niobium
And its raw material of compound, catalyst, refractory material are also served as, there is important application prospect in chemical industry field.
In recent years, non-crystalline material is aroused great concern due to its excellent physicochemical properties, some of
Non-crystalline material is also widely used, and amorphous Nb is prepared in the prior art2O5Method be thermal oxidation method (referring to《Amorphous state
The luminescence generated by light of Nb oxide nano-film visible regions》, Tao Shufen etc., Acta Optica, 2009,29 (10):2934-2937),
Up to the present, to Nb2O5Light transmitting property research under phase transition under high pressure and its non crystalline structure is still a challenging work
Make.Simultaneously as being usually associated with its lattice structure when obtaining the high pressure phase of material and non crystalline structure using high pressure technique
The invertibity of sample phase transformation after change and release, therefore pass through high pressure technique research material phase transition under high pressure and material high pressure phase
Property seems particularly difficult.So far, domestic and foreign countries are there is not yet relevant monoclinic phase H-Nb2O5Using high pressure tactics prepare amorphous and
Amorphous printing opacity Nb2O5Relevant report.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of black transparent amorphous niobium pentaoxide, with
Monoclinic phase H-Nb2O5For original material, black transparent amorphous Nb is obtained using high pressure tactics2O5, black transparent amorphous Nb2O5Can be with
Keep stable non crystalline structure and good light transmitting property.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
A kind of preparation method of black transparent amorphous niobium pentaoxide, comprises the following steps：
By monoclinic phase H-Nb2O5It is forced into 21.3~30.0GPa and obtains black transparent amorphous niobium pentaoxide.
Preferably, the monoclinic phase H-Nb2O5Purity be more than 99.9985%.
Preferably, the pressure process is specifically included：
Using diamond anvil cell press precompressed T301 steel discs or rhenium piece, impression is obtained；
In impression centre-drilling hole, by monoclinic phase H-Nb2O5It is placed in after hole, load pressure.
Preferably, the pressure of the precompressed is 17~19GPa.
Preferably, the thickness of the impression is 40~60 μm.
Preferably, a diameter of 110~160 μm of described hole.
Preferably, a diameter of 200~500 μm of the diamond anvil cell press diamond anvil face.
Preferably, the thickness of the T301 steel discs or rhenium piece independently is 0.2~0.3mm.
Preferably, it is described by monoclinic phase H-Nb2O5Being placed in after hole also includes addition ruby microballoon as pressure mark.
Preferably, a diameter of 5~25 μm of the ruby microballoon.
The invention provides a kind of preparation method of black transparent amorphous niobium pentaoxide, by monoclinic phase H-Nb2O5It is forced into
21.3~30GPa obtains black transparent amorphous niobium pentaoxide.The present invention is obtained with good using the method for HIGH PRESSURE TREATMENT
The amorphous Nb of light transmitting property2O5Material；Unload to normal pressure, Nb2O5Stable non crystalline structure and good translucency can be kept
Matter；And the operating process of the present invention is simple, easily operated.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the monoclinic phase H-Nb of comparative example 12O5Top light optical photograph under 0GPa pressure；
Fig. 2 is the monoclinic phase H-Nb of comparative example 12O5Back light optical photograph under 0GPa pressure；
Fig. 3 is Nb under comparative example 27.7GPa pressure2O5Back light optical photograph；
Fig. 4 is black transparent amorphous Nb under embodiment 121.3GPa pressure2O5Top light optical photograph；
Fig. 5 is black transparent amorphous Nb under embodiment 121.3GPa pressure2O5Back light optical photograph；
Fig. 6 is the monoclinic phase H-Nb of embodiment 12O5X ray diffracting spectrum under 0GPa (normal pressure)；
Fig. 7 is black transparent amorphous Nb under embodiment 121.3GPa pressure2O5X ray diffracting spectrum；
Fig. 8 is black transparent amorphous Nb under embodiment 230.0GPa pressure2O5Back light optical photograph；
Fig. 9 is black transparent amorphous Nb made from embodiment 22O5Unload the X ray diffracting spectrum for being depressed into 0GPa；
Figure 10 is black transparent amorphous Nb made from embodiment 22O5Unload the electronic diffraction collection of illustrative plates for being depressed into 0GPa；
Figure 11 is black transparent amorphous Nb made from embodiment 22O5Unload the back light optical photograph for being depressed into 0GPa.
Embodiment
The invention provides a kind of preparation method of black transparent amorphous niobium pentaoxide, comprise the following steps：
By monoclinic phase H-Nb2O5It is forced into 21.3~30.0GPa and obtains black transparent amorphous niobium pentaoxide.
In the present invention, the monoclinic phase H-Nb2O5Purity be preferably greater than 99.9985%；The monoclinic phase H-
Nb2O5Particle diameter be preferably 0.2~10 μm, more preferably 0.5~2 μm.The present invention is to the monoclinic phase H-Nb2O5Source do not have
There is special restriction, using product made from commercial goods well known to those skilled in the art or conventional technical means；
It is preferably the monoclinic phase H-Nb of Alpha Co., Ltd's production in the embodiment of the present invention2O5。
In the present invention, the pressure of the pressurization is preferably 21.3~30.0GPa, more preferably 23.0~25.6GPa.This
Invention was not limited the time of the pressurization, as long as pressure, which reaches, can obtain the oxidation of black transparent amorphous five after the pressure
Two niobiums.In the present invention, the initial monoclinic phase H-Nb under the pressure2O5Experience interphase orthohormbic structure is changed into amorphous phase, thoroughly
Light property be improved significantly, obtain the black non-crystalline material with good light transmission features.
In the present invention, the pressure process is preferably specifically included：
Using diamond anvil cell press precompressed T301 steel discs or rhenium piece, impression is obtained；
In impression centre-drilling hole, by monoclinic phase H-Nb2O5It is placed in after hole, load pressure.
The present invention utilizes diamond anvil cell press precompressed T301 steel discs or rhenium piece, obtains impression.In the present invention, it is described
The pressure of precompressed is preferably 17~19GPa, more preferably 17.5~18.5GPa.
In the present invention, preferably 200~500 μm of the diameter of the diamond anvil cell press diamond anvil face, more preferably
For for 300~400 μm.
In the present invention, the thickness of the T301 steel discs or rhenium piece is preferably independently 0.2~0.3mm, more preferably
0.25~0.28mm；The present invention does not have special restriction to the length and width of the T301 steel discs or rhenium piece, can be according to need
Select the T301 steel discs or rhenium piece of suitable length and width.
In the present invention, the thickness of the impression is preferably 40~60 μm, more preferably 45~55 μm, most preferably 50 μ
m.The present invention does not have special restriction to the area of the impression, and those skilled in the art can select impression according to actual needs
Area.The present invention was not limited the time of the precompressed, can reach the thickness of the impression.In the present invention,
The effect that the precompressed obtains impression is that sample preferably is sealed in into diamond and T301 steel discs or the high pressure-like of rhenium piece formation
Product intracavitary.
Obtain after impression, the present invention is in impression centre-drilling hole, by monoclinic phase H-Nb2O5It is placed in after hole, load pressure.
In the present invention, the diameter of described hole is preferably 110~160 μm, more preferably 120~150 μm, most preferably 130~140 μ
m.The present invention does not have special restriction to the depth of described hole, can make the monoclinic phase H-Nb in described hole2O5Reach described
Pressure.
In the present invention, it is described by monoclinic phase H-Nb2O5Being placed in after hole also includes addition ruby microballoon as pressure mark,
The ruby microballoon can detect the pressure in hole.The present invention is preferably by monoclinic phase H-Nb2O5It is completely filled with after hole and adds again
Plus ruby microballoon.
In the present invention, the diameter of the ruby microballoon is preferably 5~25 μm, more preferably 10~15 μm.The present invention
To originating without special restriction for the ruby microballoon, using commercial goods well known to those skilled in the art；This
Invention does not have special restriction to the consumption of the ruby microballoon, and those skilled in the art's use can detect hole internal pressure power
Consumption ruby microballoon.
The invention provides a kind of preparation method of black transparent amorphous niobium pentaoxide, by monoclinic phase H-Nb2O5It is forced into
21.3~30.0GPa obtains black transparent amorphous niobium pentaoxide.The present invention is obtained with good using the method for HIGH PRESSURE TREATMENT
The amorphous Nb of good light transmitting property2O5Material；Unload to normal pressure, Nb2O5Stable non crystalline structure and good translucency can be kept
Matter；And the operating process of the present invention is simple, easily operated.
The preparation method of the black transparent amorphous niobium pentaoxide provided with reference to embodiment the present invention carries out detailed
Explanation, but they can not be interpreted as limiting the scope of the present invention.
Comparative example 1
Using anvil face for 400 μm diamond anvil cell press in 17GPa precompressed T301 steel discs (about 0.25mm × 10mm ×
10mm), impression thickness is at 60 μm, and in the hole of a diameter of 130 μm of impression centre drill, by monoclinic phase H-Nb2O5Original material is filled out
Steel disc hole is attached to, is fully filled with after hole, then adds 5 μm of ruby microballoons as pressure and marks (pressure that intracavitary is pressed in detection), so
After seal press, carry out 0GPa pressurizations.
Obtained Nb under 0GPa pressure2O5Top light optical photograph is shown in Fig. 1, and back light optical photograph is shown in Fig. 2, can be with by Fig. 1~2
Find out, when pressure is 0GPa, monoclinic phase H-Nb2O5Show as white, light-proof material.
Comparative example 2
Using anvil face for 500 μm diamond anvil cell press in 19GPa precompressed T301 steel discs (about 0.3mm × 10mm ×
10mm), impression thickness is at 40 μm, and in the hole of a diameter of 160 μm of impression centre drill, by monoclinic phase H-Nb2O5Original material is filled out
Steel disc hole is attached to, is fully filled with after hole, then adds 25 μm of ruby microballoons as pressure and marks (pressure that intracavitary is pressed in detection), so
After seal press, carry out 7.7GPa pressurizations.
Obtained Nb under 7.7GPa pressure2O5Back light optical photograph under 7.7GPa is shown in Fig. 3, as seen from Figure 3, when
When pressure reaches 7.7GPa, monoclinic phase H-Nb2O5Raw material starts light transmitting property occur.
Embodiment 1
Using the diamond anvil cell press that anvil face is 400 μm in 17.5GPa precompressed T301 steel discs (about 0.25mm × 10mm
× 10mm), impression thickness is at 55 μm, and in the hole of a diameter of 140 μm of impression centre drill, by monoclinic phase H-Nb2O5Original material
Steel disc hole is filled into, is fully filled with after hole, hole is sample cavity, then adds 15 μm of ruby microballoons as pressure mark (inspection
Pressure in pressure measuring cavity), press is then sealed, 21.3GPa pressurizations are carried out, black transparent amorphous niobium pentaoxide is made.
Obtained Nb under 21.3GPa pressure2O5, the top light optical photograph under 21.3GPa is shown in Fig. 4, by Fig. 1 and Fig. 4 ratios
Relatively as can be seen that raw material H-Nb2O5Black is changed into by white under 21.3GPa；Back light optical photograph under 21.3GPa is shown in
Fig. 5, by Fig. 2 and Fig. 5 compare it can be seen from when pressure reaches 21.3GPa, obtained Nb2O5With good light transmitting property.
To raw material monoclinic phase H-Nb2O5Original material carries out X-ray diffraction analysis, as a result as shown in fig. 6, being made to embodiment 1
The printing opacity amorphous niobium pentaoxide obtained, carries out situ high pressure X-ray diffraction analysis (Beijing Synchrotron Radiation 4W2 lines under 21.3GPa
Station is measured), as a result as shown in fig. 7, by comparing Fig. 6 and Fig. 7, it can be seen that obtained amorphous niobium pentaoxide and monoclinic phase
H-Nb2O5Original material has different X-ray diffraction peaks, and compacting amorphous phase-change takes place in 21.3GPa in original material.
Embodiment 2
Using the diamond anvil cell press that anvil face is 300 μm in 18.5GPa precompressed T301 steel discs, impression thickness is in 45 μ
M, and in the hole of a diameter of 110 μm of impression centre drill, by monoclinic phase H-Nb2O5Original material is filled into steel disc hole, fills out completely
After full hole, then 10 μm of ruby microballoons are added as pressure mark (pressure of intracavitary is pressed in detection), then seal press, carry out
Black transparent amorphous niobium pentaoxide is made in 30GPa pressurizations.
Obtained Nb under 30.0GPa pressure2O5, the back light optical photograph under 30.0GPa is shown in Fig. 8, as seen from Figure 8,
When pressure reaches 30.0GPa, obtained Nb2O5With good light transmitting property.
The obtained black transparent amorphous niobium pentaoxide of 30.0GPa pressurizations is unloaded and is depressed into 0GPa, is depressed into unloading under 0GPa
Nb2O5X-ray diffraction analysis are carried out, as a result as shown in figure 9, to unloading the Nb being depressed under 0GPa2O5Carry out electron diffraction analysis, knot
Fruit as shown in Figure 10, unloads the Nb being depressed under 0GPa2O5Back light optical photograph is shown in Figure 11, by analysis chart 9~11, works as monocline
H-Nb2O5Raw material is increased to 30.0Pa in sample cavity pressure, unloads and is depressed into after 0GPa, Nb2O5Keep non crystalline structure stably and good
Good light transmitting property.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of black transparent amorphous niobium pentaoxide, comprises the following steps：
By monoclinic phase H-Nb2O5It is forced into 21.3~30.0GPa and obtains black transparent amorphous niobium pentaoxide.
2. preparation method according to claim 1, it is characterised in that the monoclinic phase H-Nb2O5Purity be more than
99.9985%.
3. preparation method according to claim 1, it is characterised in that the pressurization is specifically included：
Using diamond anvil cell press precompressed T301 steel discs or rhenium piece, impression is obtained；
In impression centre-drilling hole, by monoclinic phase H-Nb2O5It is placed in after hole, load pressure.
4. preparation method according to claim 3, it is characterised in that the pressure of the precompressed is 17~19GPa.
5. preparation method according to claim 3, it is characterised in that the thickness of the impression is 40~60 μm.
6. preparation method according to claim 3, it is characterised in that a diameter of 110~160 μm of described hole.
7. preparation method according to claim 3, it is characterised in that the diamond anvil face of the diamond anvil cell press
A diameter of 200~500 μm.
8. preparation method according to claim 3, it is characterised in that the thickness of the T301 steel discs and rhenium piece independently is
0.2~0.3mm.
9. preparation method according to claim 3, it is characterised in that described by monoclinic phase H-Nb2O5It is placed in after hole and also wraps
Addition ruby microballoon is included to mark as pressure.
10. preparation method according to claim 9, it is characterised in that a diameter of 5~25 μm of the ruby microballoon.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110745780A (en) * | 2019-12-02 | 2020-02-04 | 吉林大学 | High-pressure preparation method of amorphous GeH |
| CN111111645A (en) * | 2019-12-27 | 2020-05-08 | 吉林大学 | Enhanced LiTaO3Photocatalytic method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389750A (en) * | 2011-10-04 | 2012-03-28 | 吉林大学 | Ultra-high pressure device based on hinged-type hexahedral press |
| CN103011270A (en) * | 2012-10-31 | 2013-04-03 | 吉林大学 | Method for preparing high-pressure alpha-PbO2-phase TiO2 nanometer material |
-
2017
- 2017-06-14 CN CN201710445794.6A patent/CN107215897B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389750A (en) * | 2011-10-04 | 2012-03-28 | 吉林大学 | Ultra-high pressure device based on hinged-type hexahedral press |
| CN103011270A (en) * | 2012-10-31 | 2013-04-03 | 吉林大学 | Method for preparing high-pressure alpha-PbO2-phase TiO2 nanometer material |
Non-Patent Citations (1)
| Title |
|---|
| GEORGE C.SERGHIOU等: "Pressure-Induced Amorphization and Reduction of T-Nb2O5", 《PHYSICAL REVIEW LETTERS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110745780A (en) * | 2019-12-02 | 2020-02-04 | 吉林大学 | High-pressure preparation method of amorphous GeH |
| CN110745780B (en) * | 2019-12-02 | 2021-06-08 | 吉林大学 | High-pressure preparation method of amorphous GeH |
| CN111111645A (en) * | 2019-12-27 | 2020-05-08 | 吉林大学 | Enhanced LiTaO3Photocatalytic method |
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