CN110172668A - A kind of preparation method and its nano particle of metal/oxide Core-shell Structure Nanoparticles - Google Patents
A kind of preparation method and its nano particle of metal/oxide Core-shell Structure Nanoparticles Download PDFInfo
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
A kind of method and its nano particle prepared the invention belongs to field of nano material preparation more particularly to metal/oxide Core-shell Structure Nanoparticles.The present invention sputters the target of needs as follows: target being made to form the plasma nanometer line of metal or alloy kernel in sputtering chamber；Subsequently into transition chamber, being passed through the adjustable oxygen of flow in transition chamber makes the particle superficial oxidation of plasma nanometer line form oxide shell layer, obtains the Core-shell Structure Nanoparticles of size uniformity.The present invention is suitable for the preparation of the Core-shell Structure Nanoparticles of the oxide cladding of a variety of easy oxidation metals sputtered or alloy；The oxidated layer thickness of cladding can be controlled by controlling oxygen flow；Sputter the size uniformity that environment cooling system guarantees prepared nano particle.
Description
Technical field
The invention belongs to field of nano material preparation more particularly to a kind of metal/oxide Core-shell Structure Nanoparticles systems
Standby method and its nano particle.
Background technique
Core-shell Structure Nanoparticles are to combine the material of two kinds of different performances in the form of core and cladding shell
Come, keeps the two performance compound.Nano particle performance can be improved to meet answering in particular surroundings by this structure
With receiving the extensive concern of each field scholar.The wherein nuclear shell structure nano that metal or alloy and autoxidation object are constituted
Grain embodies a variety of properties, and in optical device, biology, medicine, there is good application prospect in the fields such as information.
The Core-shell Structure Nanoparticles of this type oxide cladding are mostly made by chemical method at present, usually utilize reduction legal system
Metal or alloy nano particle is obtained, then oxide shell is obtained by oxidation reaction.Such as Inderhees and Borchers et al. exist
By Co in the mixed liquor of oleic acid and trioctyl phosphine oxide2(Co)8Thermal reduction obtains Co nano particle, then passes through air or oxygen again
Co nano particle is aoxidized in compression ring border to obtain the Co/CoO Core-shell Structure Nanoparticles of different-thickness.
(Inderhees S E,Borchers J A,Green K S,et al.Manipulating the Magnetic
Structure of Co Core/CoO Shell Nanoparticles:Implications for Controlling the
Exchange Bias [J] .Physical Review Letters, 2008,101 (11): 117202.) prepared by such methods
Journey is many and diverse, and manufacturing cycle is longer.Zeng and Li et al. propose that a kind of to be immersed in lauryl sodium sulfate water-soluble using laser ablation
The method of metallic target in liquid come prepare with oxide shell Core-shell Structure Nanoparticles (Haibo Zeng, Li Z,
Weiping Cai,et al.Microstructure Control of Zn/ZnO Core/Shell Nanoparticles
and Their Temperature-Dependent Blue Emissions[J]. Journal of Physical
Chemistry B,2007,111(51):14311-7.).This method and step is relatively easy, but is difficult to ensure prepared nanometer
Particle size uniformity.In addition above-mentioned method is both needed to chemical reagent as auxiliary, and preparation process can generate waste liquid and pollute.
Physical method in the prior art is usually not related to preparing the Core-shell Structure Nanoparticles of oxide cladding, example
Such as:
Present applicant formerly has developed a kind of nano-particular film that uniform high-compactness is prepared using physical method
Device and technology, referring to Chinese invention patent No.20140279632.3, title ' it is a kind of uniformly, high-compactness nano particle
The preparation method of film ', structure includes the sputtering chamber for being mounted with target rifle, the settling chamber of nanoparticle deposition and both connections
Transition chamber thereof etc..The ion beam that target rifle sputters when work flows through transition chamber by sputtering chamber due to the air pressure of sputtering chamber and settling chamber
Eventually enter into settling chamber.Sputtering chamber outlet and deposition chamber inlet are two taper screening mouths, can screen to particle, make to deposit
Product size is uniform.
Present applicant has also applied for Chinese utility model patent No. 201720755090.4, ' under a kind of vacuum
Cooling device ' (publication number CN 207035643U) for nano particle preparation.The device can maintain working region in a vacuum
Temperature is constant, improves the homogeneity of nano particle diameter.In addition, the adjusting by temperature can change the big of nano particle diameter
It is small；But the physical method in currently available technology is unable to get the Core-shell Structure Nanoparticles of oxide cladding.
Summary of the invention
The object of the present invention is to overcome the drawbacks described above of chemistry and physical preparation method in the prior art, joined by technique
Several improvement, using the magnetic control sputtering device of the prior art, obtain in a kind of vacuum for of uniform size, preparation process is simple,
The method and its particle of the free of contamination Core-shell Structure Nanoparticles preparation with oxide shell.
In order to achieve the above object, the present invention provides the following technical scheme that
A kind of preparation method of metal/oxide Core-shell Structure Nanoparticles, the Core-shell Structure Nanoparticles with metal or
Alloy is kernel, and the oxide of the metal or alloy is shell, and the kernel and oxide shell layer of the nano particle are in same system
It is formed continuously during standby；
Method includes the following steps:
A) transition chamber vacuum system and settling chamber's vacuum system are opened, until vacuum degree is higher than 5 × 10-4Pa；
B) temperature of sputtering chamber is adjusted；
C) gas needed for being passed through sputtering to sputtering chamber；
D) oxygen is passed through to transition chamber；
E) transition chamber molecule pump steam inlet plate valve is adjusted, sputtering chamber air pressure > transition chamber air pressure > settling chamber's air pressure is formed
Stepped differential pressures；
F) stable gas pressure sputters the target of needs as follows: in sputtering chamber target being formed after mixed gas is abundant
The plasma nanometer line of metal or alloy kernel；Subsequently into transition chamber, being passed through the adjustable oxygen of flow in transition chamber makes
The particle superficial oxidation of ion nanometer line forms oxide shell layer, obtains the Core-shell Structure Nanoparticles of size uniformity.
In step f), the sputtering includes: the first sputtering and the second sputtering, forms stable plasma in the first sputtering
After nano particle line, opens baffle (5) and start the second sputtering, the Core-shell Structure Nanoparticles to be formed is made to enter settling chamber (2).
Prepared Core-shell Structure Nanoparticles are that Co is kernel, and CoO is the nano particle of the core-shell structure of shell, or
CoFe is kernel, and the oxide of Co, Fe are the nano particle of the core-shell structure of shell.
Gas and oxygen needed for the gas being passed through when sputtering is divided into sputtering each leads into sputtering chamber and transition chamber.
In step b), the temperature of sputtering chamber is adjusted by the cooling system of unlatching sputtering chamber, adjusts sputtering chamber cavity interlayer
In coolant temperature realize, sputtering room temperature be -50 DEG C~30 DEG C.
Gas needed for sputtering described in step c) includes the mixed gas of cooling gas and sputter gas, including nitrogen, argon
One or more of gas, helium.
It is 40SCCM~100SCCM that the flow of gas is passed through described in step c) to be passed through flow.
The flow that oxygen is passed through described in step d) is 0.3SCCM~5SCCM.
Target described in step f) is selected from one kind of target made of following oxidable metal and alloy: Co, Fe, Al,
Cu, Zn, Ni, Ag, Mo, Mn and its alloy.
The draught head of transition chamber air pressure described in step f) and settling chamber's air pressure is maintained at 10-2Pa magnitude.
Regulate and control oxide shell layer thickness by adjusting oxygen flow.
A kind of nano particle that the preparation method using the metal/oxide Core-shell Structure Nanoparticles obtains, should
For Core-shell Structure Nanoparticles using metal or alloy as kernel, the oxide of the metal or alloy is shell；
The nano particle is prepared using following magnetron sputtering technique: target being made to form metal or alloy in sputtering chamber
The plasma nanometer line of kernel；Subsequently into transition chamber, being passed through the adjustable oxygen of flow in transition chamber makes plasma nanometer bundle
The particle superficial oxidation of stream forms oxide shell layer.
The nano-particle diameter is 7.54~22.6nm, and oxide shell layer is with a thickness of 1.96~4.5nm.
The thickness of the oxide shell layer is passed through the oxygen flow regulation of transition chamber by adjusting.
The nano particle is that Co is kernel, and CoO is the core-shell structure of shell.
When the nano particle is used for magnetic material, coercivity is 20.68~24.5Oe, saturation magnetization 269.78
~388.65emu/g, remanence magnetisation are 227.61~325.59emu/g.
Compared with the conventional method, the beneficial effects of the present invention are:
By the way that in the plasma nanometer line that is formed in the target as sputter of corresponding kernel, being passed through appropriate oxygen makes nanometer
Grain superficial oxidation generates core-shell structure, and the generating process of the core and oxide shell that make nano particle continuously produces in a system
Raw, operating process is simpler；Only need to by control oxygen flow can direct regulation and control oxide shell thickness；Cooling system guarantees
Working environment constant temperature is sputtered, prepared even particle size is made；Any pollution or by-product is not present in preparation process.By more
Different targets are changed, this method is suitable for a variety of oxidizable metals and alloy.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of this preparation method.
Fig. 2 a is the TEM pattern and size distribution statistics of nano particle prepared by embodiment 1；
Fig. 2 b is the TEM pattern and size distribution statistics of nano particle prepared by embodiment 2；
Fig. 2 c is the TEM pattern and size distribution statistics of nano particle prepared by embodiment 3；
Fig. 2 d is the TEM pattern and size distribution statistics of nano particle prepared by embodiment 4；
Fig. 3 a is the HTEM pattern of nano particle prepared by embodiment 1；
Fig. 3 b is the HTEM pattern of nano particle prepared by embodiment 2；
Fig. 3 c is the HTEM pattern of nano particle prepared by embodiment 3；
Fig. 3 d is the HTEM pattern of nano particle prepared by embodiment 4；
Fig. 4 a is the hysteresis loop schematic diagram of nano particle prepared by embodiment 1,2,3；
Fig. 4 b is coercivity, saturation magnetization and the remanence magnetisation of nano particle prepared by embodiment 1,2,3.
Appended drawing reference:
1 transition chamber, 2 settling chamber, 3 target rifle
4 transition chamber vacuum system, 5 baffle, 6 settling chamber's vacuum system
7 sputtering chambers
Specific embodiment
The present invention is with reference to the accompanying drawing further elaborated embodiment:
As shown in Figure 1, the present invention prepares Core-shell Structure Nanoparticles using magnetic control sputtering device, which includes transition chamber
1, settling chamber 2, target rifle 3, transition chamber vacuum system 4, baffle 5, settling chamber's vacuum system 6 and sputtering chamber 7.
A kind of method of Core-shell Structure Nanoparticles preparation, comprising the following steps:
(1) transition chamber vacuum system 4 and settling chamber's vacuum system 6 are opened, makes vacuum degree better than 5 × 10-4Pa；
(2) cooling system for opening sputtering chamber 7 adjusts coolant temperature, and coolant temperature is -50 DEG C~30 DEG C；
(3) gas needed for being passed through sputtering to sputtering chamber 7, gas needed for the sputtering includes cooling gas and sputter gas
One or more of mixed gas, including nitrogen, argon gas, helium, being passed through flow is 40SCCM~100SCCM；
(4) it is passed through oxygen to transition chamber 1, the flow for being passed through oxygen is 1SCCM-5SCCM；By adjusting oxygen flow regulation
Oxide shell layer thickness, the bigger oxide shell layer thickness of oxygen flow increase.
(5) transition chamber vacuum system air inlet plate valve (not shown) is adjusted, 7 air pressures of sputtering chamber > transition chamber, 1 gas is formed
The draught head of the stepped differential pressures of 2 air pressure of pressure > settling chamber, 1 air pressure of transition chamber and 2 air pressure of settling chamber is maintained at 10-2Pa or so；
(6) after stable gas pressure, it is uniform to mix gas, carries out pre-sputtering (first sputtering) to required target, formed it is stable it is equal from
Sub- nano particle line, the target include one kind of target made of oxidizable metal and alloy；After pre-sputtering i.e.
It can produce the Core-shell Structure Nanoparticles of the size uniformity with oxide shell layer；
(7) baffle (5) are then opened and starts the second sputtering, the Core-shell Structure Nanoparticles to be formed is made to enter settling chamber (2).
Embodiment 1:
(1) Co target is installed on sputtering target rifle 3；
(2) transition chamber vacuum system and settling chamber's vacuum system are opened, until vacuum degree is better than 5 × 10-4Pa；
(3) it is 20 DEG C that the cooling system for opening sputtering chamber, which adjusts the temperature of coolant liquid,；
(4) being passed through argon flow to sputtering chamber is 82SCCM；
(5) being passed through oxygen flow to transition chamber thereof is 1SCCM；
(6) transition chamber molecule pump steam inlet plate valve is adjusted, sputtering chamber air pressure > transition chamber air pressure > settling chamber's air pressure is formed
Stepped differential pressures；Wherein transition chamber air pressure is 2pa, and settling chamber's air pressure is 1*10-2Pa。
(7) after stable gas pressure, mixed gas uniformly carries out pre-sputtering (the first sputtering), forms stable plasma nano particle beam
Stream；Then it opens baffle 5 and starts the second sputtering, the Core-shell Structure Nanoparticles to be formed is made to enter settling chamber 2.Prepare Co@CoO
The nano particle of core-shell structure, particle size range are 7.49~22.6nm, and average grain diameter is 10~15nm.TEM pattern and granularity system
Meter result is as shown in Figure 2 a, and HTEM pattern is as shown in Figure 3a.
Embodiment 2:
Using step same as Example 1, the oxygen flow that wherein step (5) is passed through is 3SCCM.TEM pattern and granularity
Statistical result is as shown in Figure 2 b, and HTEM pattern is as shown in Figure 3b.
Embodiment 3:
Using step same as Example 1, the oxygen flow that wherein step (5) is passed through is 5SCCM.TEM pattern and granularity
Statistical result is as shown in Figure 2 c, and HTEM pattern is as shown in Figure 3c.
Embodiment 4:
Wherein, step (1) installs CoFe alloy target on sputtering target rifle 3；The oxygen flow that wherein step (5) is passed through is
0.3SCCM.After step (7) stable gas pressure, mixed gas uniformly carries out pre-sputtering (the first sputtering), forms stable plasma nanometer
Grain line；Then it opens baffle 5 and starts the second sputtering, the Core-shell Structure Nanoparticles to be formed is made to enter settling chamber 2.It prepares
CoFe is kernel, CoFe2O4Oxide be shell core-shell structure nano particle, TEM pattern and grain size statistics result are such as
Shown in Fig. 2 d, HTEM pattern is as shown in Figure 3d.
Can be seen that prepared nano particle under different parameters from Fig. 2 a~2c has good uniformity, average
Partial size is in 11nm~12nm.
The shell thickness of nano particle prepared by embodiment 1,2,3 is respectively 1.96nm, 2.75nm, 4.5nm；From figure
3a~3c can be seen that as the increase oxide cladding layers of oxygen flow increase therewith.
Fig. 2 d, 3d show the logical available even-grained nuclear shell structure nano of oxygen of target using other metal or alloy
Particle.
Fig. 4 is hysteresis loop (Fig. 4 a), the coercivity, saturation magnetization of nano particle prepared by embodiment 1,2,3
With remanence magnetisation (Fig. 4 b).Logical oxygen flow is the coercivity difference of nanoparticle prepared by 1SCCM, 3SCCM and 5SCCM
For 20.68Oe, 23.66Oe, 24.54Oe；Saturation magnetization is respectively 269.78emu/g, 301.24emu/g,
388.65emu/g；Remanence magnetisation is respectively 227.61emu/g, 246.90emu/g, 325.59emu/g.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent structure and flow change made by Spirit Essence or modification, should be covered by the protection scope of the present invention.
Claims (16)
1. a kind of preparation method of metal/oxide Core-shell Structure Nanoparticles, which is characterized in that
For the Core-shell Structure Nanoparticles using metal or alloy as kernel, the oxide of the metal or alloy is shell, the nanometer
The kernel and oxide shell layer of particle are formed continuously in same preparation process；
Method includes the following steps:
A) transition chamber vacuum system and settling chamber's vacuum system are opened, until vacuum degree is higher than 5 × 10-4Pa；
B) temperature of sputtering chamber is adjusted；
C) gas needed for being passed through sputtering to sputtering chamber；
D) oxygen is passed through to transition chamber；
E) transition chamber molecule pump steam inlet plate valve is adjusted, sputtering chamber air pressure > transition chamber air pressure > settling chamber's air pressure ladder pressure is formed
Difference；
F) stable gas pressure sputters the target of needs after mixed gas is abundant as follows: target being made to form metal in sputtering chamber
Or the plasma nanometer line of alloy core；Subsequently into transition chamber, being passed through the adjustable oxygen of flow in transition chamber makes plasma
The particle superficial oxidation of nanometer line forms oxide shell layer, obtains the Core-shell Structure Nanoparticles of size uniformity.
2. the method as described in claim 1, which is characterized in that
In step f), the sputtering includes: the first sputtering and the second sputtering, forms stable plasma nanometer in the first sputtering
After particle line, opens baffle (5) and start the second sputtering, the Core-shell Structure Nanoparticles to be formed is made to enter settling chamber (2).
3. the method as described in claim 1, which is characterized in that
Prepared Core-shell Structure Nanoparticles are that Co is kernel, and CoO is the nano particle of the core-shell structure of shell or CoFe is
Kernel, the oxide of Co, Fe are the nano particle of the core-shell structure of shell.
4. the method as described in claim 1, which is characterized in that
Gas and oxygen needed for the gas being passed through when sputtering is divided into sputtering each leads into sputtering chamber and transition chamber.
5. the method as described in claim 1, which is characterized in that
In step b), the temperature of sputtering chamber is adjusted by the cooling system of unlatching sputtering chamber, is adjusted in sputtering chamber cavity interlayer
Coolant temperature realizes that sputtering room temperature is -50 DEG C~30 DEG C.
6. the method as described in claim 1, which is characterized in that
Gas needed for sputtering described in step c) includes the mixed gas of cooling gas and sputter gas, including nitrogen, argon gas, helium
One or more of gas.
7. the method as described in claim 1, which is characterized in that
It is 40SCCM~100SCCM that the flow of gas is passed through described in step c) to be passed through flow.
8. the method as described in claim 1, which is characterized in that
The flow that oxygen is passed through described in step d) is 0.3SCCM~5SCCM.
9. the method as described in claim 1, which is characterized in that
Target described in step f) is selected from one kind of target made of following oxidable metal and alloy: Co, Fe, Al, Cu,
Zn, Ni, Ag, Mo, Mn and its alloy.
10. the method as described in claim 1, which is characterized in that
The draught head of transition chamber air pressure described in step f) and settling chamber's air pressure is maintained at 10-2Pa magnitude.
11. the method as described in claim 1, which is characterized in that
Regulate and control oxide shell layer thickness by adjusting oxygen flow.
12. what a kind of preparation method using metal/oxide Core-shell Structure Nanoparticles as described in claim 1 obtained receives
Rice grain, which is characterized in that
For the Core-shell Structure Nanoparticles using metal or alloy as kernel, the oxide of the metal or alloy is shell；
The nano particle is prepared using following magnetron sputtering technique: target being made to form metal or alloy kernel in sputtering chamber
Plasma nanometer line；Subsequently into transition chamber, being passed through the adjustable oxygen of flow in transition chamber makes plasma nanometer line
Particle superficial oxidation forms oxide shell layer.
13. nano particle according to claim 12, which is characterized in that
The nano-particle diameter is 7.54~22.6nm, and oxide shell layer is with a thickness of 1.96~4.5nm.
14. nano particle according to claim 12, which is characterized in that
The thickness of the oxide shell layer is passed through the oxygen flow regulation of transition chamber by adjusting.
15. nano particle according to claim 12, which is characterized in that
The nano particle is that Co is kernel, and CoO is the core-shell structure of shell.
16. nano particle according to claim 15, which is characterized in that
When the nano particle be used for magnetic material when, coercivity be 20.68~24.5Oe, saturation magnetization be 269.78~
388.65emu/g, remanence magnetisation are 227.61~325.59emu/g.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111659404A (en) * | 2020-06-30 | 2020-09-15 | 天津大学 | Supported core-shell structure ZnO catalyst and preparation method and application thereof |
| CN111892014A (en) * | 2020-07-30 | 2020-11-06 | 钢铁研究总院 | Getter film and preparation method thereof |
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| CN113319271A (en) * | 2021-05-28 | 2021-08-31 | 北京理工大学 | Oxide coated powder with core-shell structure and preparation method and application thereof |
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| WO2022000923A1 (en) * | 2020-06-30 | 2022-01-06 | 天津大学 | Supported core-shell structure zno catalyst, preparation method therefor and application thereof |
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| CN111892014B (en) * | 2020-07-30 | 2023-10-31 | 钢铁研究总院 | Air suction film and preparation method thereof |
| CN113275559A (en) * | 2021-05-21 | 2021-08-20 | 北京理工大学 | Cage type generating device for powder with oxide shell layer coated core-shell structure |
| CN113299535A (en) * | 2021-05-21 | 2021-08-24 | 北京理工大学 | Annular generating device for powder with oxide shell layer coated core-shell structure |
| CN113299535B (en) * | 2021-05-21 | 2022-05-10 | 北京理工大学 | Annular generating device for powder with oxide shell layer coated core-shell structure |
| CN113319271A (en) * | 2021-05-28 | 2021-08-31 | 北京理工大学 | Oxide coated powder with core-shell structure and preparation method and application thereof |
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