CN105154812B - A kind of preparation method of the micro Nano material of metal and its oxide core shell structure - Google Patents
A kind of preparation method of the micro Nano material of metal and its oxide core shell structure Download PDFInfo
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- CN105154812B CN105154812B CN201510608599.1A CN201510608599A CN105154812B CN 105154812 B CN105154812 B CN 105154812B CN 201510608599 A CN201510608599 A CN 201510608599A CN 105154812 B CN105154812 B CN 105154812B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
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Abstract
The present invention provides a kind of preparation method of the micro Nano material of metal and its oxide core shell structure, includes the following steps：Step S1：It is that 10 μm or metal unit below are placed on substrate by size, and making that there is the space grown for metal oxide around metal unit, the size of the growing space is at least suitable with space size occupied after the micro nano structure complete growth of metal oxide；Step S2：It is passed through oxygen, substrate is heated and kept the temperature, the metal unit on substrate is made to grow the micro nano structure of metal oxide.The localization preparation method of metallic film is utilized in compared with the existing technology, often prepare the tungsten oxide micro nano structure of adhesion, the present invention around metal unit by being arranged growing space, make oxide micro-nano rice structure can complete growth, the determination of micro nano structure pattern, the adhesion of gained are prepared, large specific surface area, quantum effect are apparent, crystallinity is high.
Description
Technical field
The present invention relates to a kind of preparation method of metal oxide more particularly to a kind of metals and its oxide core shell structure
Micro Nano material preparation method and metal and its oxide core shell structure micro Nano material.
Background technology
Micro Nano material refers to the material that grain size reaches micron or Nano grade, in structure, photoelectricity, chemical property etc.
With unique characteristic, possess huge application prospect.For the metal oxide of micro nano structure, specific surface area
Greatly, Active sites are more, have extensively in petrochemical industry catalytic field, petrochemical industry lube oil additive, photocatalysis field etc.
Application.
A kind of thermal oxidation method preparation three is disclosed in the Chinese patent document that number of patent application is 201210377609.1
The method of tungstic oxide nano-sheets, this method plates metal W film on substrate first, then obtained sample is heated, and generates three oxygen
Change tungsten nanometer sheet.Specifically, the preparation of metal W film full wafer is being served as a contrast by magnetron sputtering, electron beam evaporation or electric plating method
On bottom, or use up can send out, mask means or silk screen print method prepare tungsten film pattern localization on substrate.The preparation side
The shortcomings that method is：Either full wafer or localization by tungsten film preparation on substrate, the oxide of the tungsten formed after heating is equal
Micro nano structure for island structure, tungsten oxide links together, and reunionization is serious, thus the specific surface area of metal oxide
Low, quantum effect unobvious, and can not accurately control the growth of metal oxide.
Invention content
In order to solve the above technical problem, the present invention provides the metals and its oxygen of a kind of structural integrity, large specific surface area
The preparation method of the micro Nano material of compound nucleocapsid.
The technical solution adopted in the present invention is：
Include the following steps：
Step S1：It is that 10 μm or metal unit below are placed on substrate, and make to have around metal unit by size
Have a space grown for metal oxide, the size of the growing space at least with the micro nano structure complete growth of metal oxide
Occupied space size is suitable afterwards；
Step S2：It is passed through oxygen, substrate is heated and kept the temperature, the metal unit on substrate is made to grow metal oxide
Micro nano structure.
The present invention metal and its oxide core shell structure micro Nano material preparation method, compared with the existing technology in
Using the localization preparation method of metallic film, the tungsten oxide micro nano structure of adhesion is often prepared, the present invention passes through in metal
Growing space is set around unit, make oxide micro-nano rice structure can complete growth, prepare gained micro nano structure pattern it is true
Fixed, adhesion, large specific surface area, quantum effect are apparent, crystallinity is high.
Further, in step S1, the error range of the placement position of the metal unit controls within 1-10 μm.
Further, in step S1, single metal unit is placed on substrate；Or multiple metal units are placed in base
On piece, and the spacing distance between adjacent metal unit is made to be 3 μm or more.
Further, the metal unit be single metal particle or the metal unit be multiple metallic particles continuously
Away from stacking.
Further, the metallic particles is tungsten particle, and granular size is 1-3 μm, between the adjacent metal unit between
Gauge is from being 3 μm or more；Or the metallic particles is titanium particle, granular size is 10 μm, between the adjacent metal unit
Spacing distance is 20 μm or more.
Further, in step sl, metal unit is placed on substrate by dispensing, electrophoresis, magnetic field or manipulator.
Further, in step s 2, under the vacuum condition of 5Pa, the mixing of inert gas and oxygen is placed the substrate in
It is heated in gas, oxygen flow 1.5-2.5sccm, argon flow amount is 100-200sccm；Or heat base under air conditions
Piece.
Further, in step sl, tungsten metal unit is placed on substrate；In step s 2, in the vacuum item of 5Pa
Under part, substrate is heated in the mixed gas of constant ratio, the inert gas of constant flow rate and oxygen to 1000 DEG C, and keep the temperature 5-
It is down to room temperature after 15 minutes.
Further, in step sl, titanium unit is placed on substrate；In step s 2, in the vacuum item of 5Pa
Under part, substrate is heated in the mixed gas of constant ratio, the inert gas of constant flow rate and oxygen to 1200 DEG C, and keep the temperature 15
It is down to room temperature after minute.
The present invention also provides a kind of metal and its micro Nano material of oxide core shell structure, according to above-mentioned metal and its
The preparation method of the micro Nano material of oxide core shell structure is prepared.
In order to better understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Description of the drawings
Fig. 1 is the tungsten and tungsten oxide micro nano structure SEM figures of the embodiment of the present invention one；
Fig. 2 is the tungsten and tungsten oxide micro nano structure SEM figures of the embodiment of the present invention two；
Fig. 3 is the tungsten and tungsten oxide micro nano structure SEM figures of the embodiment of the present invention three；
Fig. 4 is the tungsten that the soaking time of the embodiment of the present invention four is 5-15 minutes and tungsten oxide micro nano structure SEM figures；
Fig. 5 is the tungsten and tungsten oxide micro nano structure XRD spectra that the soaking time of the embodiment of the present invention four is 5-15 minutes；
Fig. 6 is the tungsten and tungsten oxide micro nano structure XRD spectra that the soaking time of the embodiment of the present invention four is 10 minutes；
Fig. 7 is the tungsten and tungsten oxide micro nano structure SEM figures of the embodiment of the present invention five；
Fig. 8 is the titanium and titanium oxide micro nano structure SEM figures of the embodiment of the present invention six.
Specific implementation mode
The preparation method of the metal of the present invention and its micro Nano material of oxide core shell structure, includes the following steps：
Step S1：Size is placed in for 10 μm (microns) or metal unit below on substrate by manipulator, makes phase
Spacing distance between adjacent metal unit is 3 μm or more；
Step S2：Under the vacuum condition of 5Pa, will be placed with the substrate of metal unit in oxygen flow is 2.5sccm
(standard-state cubic centimeter per minute), argon flow amount be heat under conditions of 200sccm, or
Substrate is heated under air conditions, the metal unit on substrate is made to grow the micro nano structure of oxide.
The metal unit is placed on quartz substrate, and the size of metal unit is 10 μm or less.Wherein, the metal unit
It can be single metallic particles, can also be that multiple metallic particles are formed without stacked spaced apart.Metallic particles can be tungsten, titanium or
Other metals.In addition, other than quartz substrate, substrate can also use potsherd, silicon chip or other heat-resisting materials.
Above-mentioned metal unit is isolated with adjacent metal unit at certain intervals, is supplied with ensureing to have around metal unit
The growing space of oxide micro-nano rice noodles complete growth.Structural integrity, the specific surface of the oxide micro-nano rice noodles to grow out
Product is big, quantum effect is apparent, when for making devices, high sensitivity.The size of above-mentioned spacing distance can be according to different metal
It is specific need to set, it is suitable with the size of the micro nano structure of the metal oxide.
In step sl, pass through dispensing mode (metal unit is selected and is dripped on substrate), electrophoretic (charged metal unit
Under electric field action, to electrically opposite electrode movement), Movement in Magnetic Field mode or manipulator (under the microscope, utilize degaussing
Property microprobe push metal unit) metal unit is placed on substrate.The placement position of metal unit is accurate to micron
Grade, specifically, the error range of the placement position control within 1-10 μm, roughly the same with the size of metal unit.Metal
The accuracy of the placement position of unit will influence whether the accurate of the growing space (or spacing distance) around single metal unit
Degree, if the error for putting operation is larger, it is likely that cause metal unit to be stacked, can not ensure each metal unit
Surrounding has growing space.Therefore the placement position for working as metal unit is accurate, and has (oxide) raw around metal unit
When long spacing, it is achieved that prepared by the fixed point of metal unit, the localization preparation with metallic film in the prior art distinguishes.Localization
In the case of preparation, the position of multiple metallic particles close-packed arrays distributions, single metal particle does not know, does not have between metallic particles
There are spacing distance or spacing distance uncertain, therefore the growth structure of oxide and pattern not can determine that, typically result in oxide
Micro nano structure link together, reunionization is serious, and specific surface area is low, quantum effect unobvious.And the fixed point system of the present invention
It is standby, it is meant that metal unit with accurate position individually or with other metal units it is separated by a distance be positioned at substrate
On, the micro nano structure for the oxide that growth comes out is controllable, complete, pattern is determining, adhesion, large specific surface area, quantum effect
It should apparent, crystallinity height.
Furthermore it is possible to by putting metal unit according to specific pattern, to prepare with specific one-dimensional, two-dimentional or three
Tie up pattern metal and its oxide core shell structure micro Nano material, can also by by metallic particles according to specific three dimensional knot
Structure is put without stacked spaced apart as a metal unit, and the metal unit is made to grow metal and its oxide core with specific structure
The micro Nano material of shell structure, can be sheet, tubular structure, such as will each and every one tens of metallic particles it is in blocks without stacked arrangement is spaced
The metal unit of shape, or multiple metallic particles are connected into rodlike metal unit without spaced linear, oxygen then is passed through to it
And heating and thermal insulation, make to grow complete, large specific surface area oxide micro-nano rice knot in the metal unit with specific shape
Structure.In these cases, even if not being spaced between the metallic particles of stacking, as long as being formed by the size control of metal unit
System at 10 μm or hereinafter, and the metal unit as a whole, around have growing space, i.e., still can guarantee and grow
The metal oxide come has more complete structure, larger specific surface area, has the preferable quantum effect (ruler of metal unit
Very little smaller, oxide growth precision is higher, effect is better), crystallinity is high, and (size is much big with utilization in the prior art
In 10 μm) metallic film carry out localization preparation method distinguish, have the effect of excellent.In addition, in addition to sheet, tubulose knot
Outside structure, flower-shaped, tree-shaped, spherical, network-like or other structures are can also be.
With the increase of heating time, go out metal oxide, metal oxidation in the surrounding growth of metal unit this core
Object is equivalent to the shell being enclosed in outside core, therefore metal unit and metal oxide form a kind of nucleocapsid.
In addition, the present invention also provides the preparation sides according to above-mentioned metal and its micro Nano material of oxide core shell structure
The micro Nano material of metal and its oxide core shell structure made of prepared by method, the structure include positioned at core metal unit with
And the metal oxide grown around metal unit.
Embodiment one
The preparation method of the metal of the embodiment of the present invention one and its micro Nano material of oxide core shell structure, including it is following
Step：
Step S1：Four tungsten metallic particles that size is 3 μm are placed on quartz substrate by manipulator, make four tungsten
About 10 μm of mode is arranged in one-dimensional patterns Roman number " 1 " to metallic particles at equidistant intervals (i.e. spacing distance is about 10 μm).
Wherein,
Step S2：Under the vacuum condition of 5Pa, oxygen flow be 2.5sccm, under conditions of argon flow amount is 200sccm,
Substrate is heated to 1000 DEG C from room temperature, and is kept the temperature and be cooled to room temperature after ten minutes.
Referring to Fig. 1, it schemes (scanning electron microscopy for the tungsten and tungsten oxide micro nano structure SEM of the embodiment of the present invention one
Mirror figure).After heated and heat preservation, the tungsten oxide micro-nano rice noodles that length is about 1 μm -5 μm are grown on tungsten particle.
Above-mentioned tungsten metallic particles is isolated with adjacent tungsten metallic particles at certain intervals, which can be arranged
It is 3 μm, this is because the length of the tungsten oxide micro-nano rice noodles grown on each tungsten particle is about 1 μm -5 μm, and with oxygen
Change the growth of tungsten, the volume of tungsten metallic particles gradually decreases, therefore when spacing distance is greater than or equal to 3 μm, you can ensures tungsten gold
There is the growing space for tungsten oxide micro-nano rice noodles complete growth around metal particles.
Embodiment two
The preparation method of the metal of the embodiment of the present invention two and its micro Nano material of oxide core shell structure, including it is following
Step：
Step S1：Four tungsten metallic particles that size is 3 μm are placed on quartz substrate by manipulator, make four tungsten
Metallic particles is arranged respectively as four vertex spacings of parallelogram, and formation is about 40 μm of four sides parallel with 50 μm on one side
Form point battle array two-dimensional pattern (i.e. spacing distance is about 40 μm or 50 μm).
Step S2：Under the vacuum condition of 5Pa, oxygen flow be 2.5sccm, under conditions of argon flow amount is 200sccm,
Substrate is heated to 1000 DEG C from room temperature, and is kept the temperature and be cooled to room temperature after ten minutes.
Referring to Fig. 2, its tungsten and tungsten oxide micro nano structure SEM figures for the embodiment of the present invention two.It is heated and keep the temperature
Afterwards, a large amount of tungsten oxide micro-nano rice noodles are grown around tungsten metallic particles.
Embodiment three
The preparation method of the metal of the embodiment of the present invention three and its micro Nano material of oxide core shell structure, including it is following
Step：
Step S1：Multiple tungsten particles that size is 3 μm are stacked in a manner of nonseptate by manipulator, are formed three-dimensional
The tungsten metal unit of " monkey " shape, is placed on quartz substrate, and as a whole, size is about 10 to the tungsten metal unit
μm, it is individually placed on substrate and prepares tungsten oxide.
Step S2：Under the vacuum condition of 5Pa, oxygen flow be 2.5sccm, under conditions of argon flow amount is 200sccm,
Substrate is heated to 1000 DEG C from room temperature, and is kept the temperature and be cooled to room temperature after ten minutes.
Referring to Fig. 3, its tungsten and tungsten oxide micro nano structure SEM figures for the embodiment of the present invention three.It is heated and keep the temperature
Afterwards, a large amount of tungsten oxide micro-nano rice noodles are grown in the tungsten metal unit.
Example IV
The preparation method of the metal of the embodiment of the present invention four and its micro Nano material of oxide core shell structure, including it is following
Step：
Step S1：Multiple tungsten particles that size is 3 μm are stacked into tungsten metal list in a manner of nonseptate by manipulator
Member is placed on quartz substrate, and as a whole, size is about 10 μm to the tungsten metal unit, is individually placed in substrate
On prepare tungsten oxide.
Step S2：Under the vacuum condition of 5Pa, oxygen flow be 2.5sccm, under conditions of argon flow amount is 200sccm,
Substrate is heated to 1000 DEG C from room temperature, and is cooled to room temperature after keeping the temperature 5 minutes, 10 minutes or 15 minutes respectively.
Referring to Fig. 4, its tungsten and tungsten oxide micro nano structure SEM figures for the embodiment of the present invention four, wherein Fig. 4 (a),
Fig. 4 (b), Fig. 4 (c) be respectively soaking time be 5 minutes, 10 minutes, 15 minutes when be formed by tungsten and the micro-nano knot of tungsten oxide
Structure is labelled with soaking time and engineer's scale in figure.The length and number of tungsten oxide micro-nano rice noodles with the increase of soaking time and
Increase, and the volume of tungsten metal unit is gradually reduced.Other than soaking time, by the size of metal unit, heating temperature,
The different settings of the preparation conditions such as heating speed, oxygen content, air pressure, can obtain the micro-nano knot of tungsten oxide of different-shape
Structure.
Referring to Fig. 5, its micro nano structure XRD spectra (X-ray diffractogram) for the tungsten oxide of the embodiment of the present invention four,
Wherein, correspond to respectively from top to bottom soaking time be 5 minutes, 10 minutes, 15 minutes tungsten and tungsten oxide micro nano structure.It can
See, the diffraction maximum in all XRD spectras both corresponds to the W of γ phases18O49Structure, no dephasign peak have high crystallinity, and
With the extension of evaporation time, the diffraction maximum in (020) face is more and more stronger, illustrates that growth course has according to γ phases direction preferentially
The orientation of growth shows that this kind of crystal is W18O49。
Referring to Fig. 6, it is the micro nano structure for the tungsten oxide that the soaking time of the embodiment of the present invention four is 10 minutes
XRD spectra.Wherein, the diffraction maximum in XRD spectra corresponds respectively to the cubic crystal structure and monocline γ phase structures of W (tungsten)
W18O49, prove that there are W and W in sample respectively18O49, show that W itself is not depleted, as core support and surround it
The W of growth18O49Structure.
Embodiment five
The preparation method of the metal of the embodiment of the present invention five and its micro Nano material of oxide core shell structure, including it is following
Step：
Step S1：The tungsten metallic particles that size is 1 μm is placed on quartz substrate by manipulator.
Step S2：Under the vacuum condition of 5Pa, oxygen flow be 1.5sccm, under conditions of argon flow amount is 100sccm,
Substrate is heated to 1000 DEG C from room temperature, and is kept the temperature and be cooled to room temperature after ten minutes.
Referring to Fig. 7, its tungsten and tungsten oxide micro nano structure SEM figures for the embodiment of the present invention five.It is heated and keep the temperature
Afterwards, the tungsten oxide micro-nano rice noodles that length is about 0.5 μm -1.5 μm are grown on tungsten particle.
Embodiment six
The preparation method of the metal of the embodiment of the present invention six and its micro Nano material of oxide core shell structure, including it is following
Step：
Step S1：The titanium metal particles that size is 10 μm are placed on substrate by dispenser, make adjacent titanium
The spacing distance of grain is 20 μm；
Step S2：Under conditions of the vacuum condition of 5Pa, oxygen flow are 2.5sccm, argon flow amount is 200sccm, from
Room temperature heats substrate to 1200 DEG C, and is cooled to room temperature after keeping the temperature 15 minutes.
Referring to Fig. 8, its titanium and titanium oxide micro nano structure SEM figures for the embodiment of the present invention six.The micro-nano of titanium oxide
Rice structure is in divergent shape, and a large amount of titanium oxide micro-and nanorods that collimate are around titanium granular center homoepitaxial, the length of 8-
10 μm, tip-shape or sheet is presented in the end of micro-and nanorods.
The preparation method and metal and its oxide of the metal of the present invention and its micro Nano material of oxide core shell structure
The micro Nano material of nucleocapsid, the middle localization preparation method using metallic film, is often prepared viscous compared with the existing technology
Tungsten oxide micro nano structure even, the present invention make oxide micro-nano rice structure by the way that growing space is arranged around metal unit
Can complete growth, the micro nano structure pattern for preparing gained is determining, adhesion, and large specific surface area, quantum effect be apparent, crystallinity
It is high.
The invention is not limited in the above embodiments, if the various changes or deformation to the present invention do not depart from the present invention
Spirit and scope, if these changes and deformation belong within the scope of the claim and equivalent technologies of the present invention, then this hair
It is bright to be also intended to comprising these changes and deformation.
Claims (6)
1. a kind of preparation method of the micro Nano material of metal and its oxide core shell structure, it is characterised in that including following step
Suddenly：
Step S1：It is 10 μm or multiple metal units below by size, is placed in by dispensing, electrophoresis, magnetic field or manipulator
On substrate, and make that there is the space that is grown for metal oxide around metal unit, the size of the growing space at least with gold
Occupied space size is suitable after the micro nano structure complete growth of category oxide；
Step S2：It is passed through oxygen, substrate is heated and kept the temperature, the metal unit on substrate is made to grow the micro-nano of metal oxide
Rice structure；
Wherein, in step S1, the error range of the placement position of the metal unit controls within 1-10 μm, adjacent metal list
Spacing distance between member is 3 μm or more；In step S2, under the vacuum condition of 5Pa, inert gas and oxygen are placed the substrate in
Mixed gas in be heated to 1000~1200 DEG C, and room temperature is down to after keeping the temperature 5-15 minutes, wherein oxygen flow is 1.5-
2.5sccm, inert gas flow are 100-200sccm, or heat substrate under air conditions.
2. the preparation method of the micro Nano material of metal according to claim 1 and its oxide core shell structure, feature
It is：The metal unit is single metal particle or the metal unit is that multiple metallic particles are formed without pitch stacking.
3. the preparation method of the micro Nano material of metal according to claim 2 and its oxide core shell structure, feature
It is：The metallic particles is tungsten particle, and granular size is 1-3 μm, the spacing distance between the adjacent metal unit be 3 μm or
More than；Or the metallic particles is titanium particle, granular size is 10 μm, and the spacing distance between the adjacent metal unit is 20 μm
Or more.
4. the preparation of the micro Nano material of metal according to any one of claim 1 to 3 and its oxide core shell structure
Method, it is characterised in that：In step sl, tungsten metal unit is placed on substrate；In step s 2, in the vacuum item of 5Pa
Under part, substrate is heated in the mixed gas of constant ratio, the inert gas of constant flow rate and oxygen to 1000 DEG C, and keep the temperature 5-
It is down to room temperature after 15 minutes.
5. the preparation of the micro Nano material of metal according to any one of claim 1 to 3 and its oxide core shell structure
Method, it is characterised in that：In step sl, titanium unit is placed on substrate；In step s 2, in the vacuum item of 5Pa
Under part, substrate is heated in the mixed gas of constant ratio, the inert gas of constant flow rate and oxygen to 1200 DEG C, and keep the temperature 15
It is down to room temperature after minute.
6. the micro Nano material of a kind of metal and its oxide core shell structure, it is characterised in that：According to any in claim 1-5
The preparation method of the micro Nano material of metal and its oxide core shell structure described in is prepared.
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