CN109913771A - A kind of VAlTiCrSi high-entropy alloy film and its application under briny environment - Google Patents
A kind of VAlTiCrSi high-entropy alloy film and its application under briny environment Download PDFInfo
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Abstract
The present invention provides a kind of VAlTiCrSi high-entropy alloy film.In the film containing 14~15% V, 12~13% Al, 12~13% Ti, 29~30% Cr, 30~31% Si, be to be deposited and is obtained in matrix surface using magnetron sputtering technique, in non crystalline structure.The film has high rigidity and excellent corrosion resistance, the matrix protection that can be used under the environment such as seawater.
Description
Technical field
The invention belongs to technical field of surface, and in particular to a kind of VAlTiCrSi high-entropy alloy film and its in sea
Application under water environment.
Background technique
With the formulation and implementation of ocean development strategy, ocean national defence has become the most important thing of modern state safety.
Advanced marine settings are the necessary supports for reinforcing the important leverage and Development of Marine economy of ocean defense force.But due to
The particularity of marine environment, the degree of injury of marine settings components are higher than terrestrial environment from far away, and service life is significantly
Equipment of reduction, especially underwater operation mechanical hand, Marine fish system, sea water pump etc. the work in briny environment.
For marine corrosion problem, Conventional marine mostly uses stainless steel, titanium alloy, engineering ceramics and polymer with material
Equal resistant materials.But stainless steel and titanium alloy wear no resistance in the seawater, engineering ceramics impact resistance and machine-shaping property
Difference, polymer hardness strength are low.Surface-coating technology is to improve one of the important means of material surface property, with minimal amount of material
Material assigns the properties such as part and wear-resisting, corrosion-resistant, the heat-resisting, endurance of component surface.In recent years, the modified protective coating in surface
Technology has become the secondary components reinforcing of seawater friction and corrosion resistant important means, is to improve marine settings stability and military service
Service life technological approaches the most feasible.
Traditional has become using one or two kinds of elements, compound as the alloy system of pivot by the long-term research of people
In mature, saturation.The performance of traditional metal materials is no longer satisfied people's demand in production and living.In this context, high
Entropy alloy comes into being, and high-entropy alloy is excellent in fields such as thermal stability, mechanics.
Summary of the invention
Status in view of the above technology, the present invention is intended to provide a kind of multicomponent alloy film of matrix surface, has height
Hardness and excellent corrosion resistance, the matrix protection that can be used under the environment such as seawater.
To realize the above-mentioned technical purpose, the technical scheme adopted by the invention is as follows: a kind of VAlTiCrSi high-entropy alloy is thin
Film selects corrosion resistance element V, Al, Ti, Cr, Si, and the atomic percentage content for controlling each element is as follows:
V:14~15%
Al:12~13%
Ti:12~13%
Cr:29~30%
Si:30~31%
Also, the VAlTiCrSi film is deposited in matrix surface using magnetron sputtering technique, on the one hand due to each element original
Size difference between son is big and be easy to cause distortion of lattice, on the other hand comes not in sputtering process since cooling velocity is fast
And crystal is formed, therefore the VAlTiCrSi film obtained using this method is in amorphous state.
Preferably, the VAlTiCrSi high-entropy alloy film with a thickness of 1 μm~20 μm, further preferably 1 μm
~10 μm.
The basis material is unlimited, including stainless steel and other metal materials, such as 304 stainless steels, 316 stainless steels etc..
As a kind of preparation method, magnetron sputtering composition target, matrix surface after cleaning deposits to obtain described
VAlTiCrSi high-entropy alloy film, wherein the composition target selects V target, Al target, Ti target, Cr target, Si target structure
At in vertical direction by five kinds of target stacked arrangements one target periods of formation, the composition target is being vertically included at least
One target period.
Preferably, each target content is 99.9% or more.
Preferably, being followed successively by V target, Al target, Ti target, Cr target, Si target from top to bottom in the period target
Material.
Preferably, V thickness is 5mm~50mm in a target period.
Preferably, Al thickness is 5mm~50mm in a target period.
Preferably, Ti thickness is 5mm~50mm in a target period.
Preferably, Cr thickness is 5mm~50mm in a target period.
Preferably, Si thickness is 5mm~50mm in a target period.
Preferably, the composition target includes 1~15 target period.
Preferably, carrying out Ar ion bombardment to composition target first, the impurity and oxide of target material surface are removed, and splashing
Logical Ar protective atmosphere during penetrating, to prevent from generating oxide in sputtering process.
Preferably, sputtering power is 1000W~3000W in sputtering process, substrate bias is -30V~-70V, matrix
Temperature is 100 DEG C~400 DEG C, deposits 5~10h.
Preferably, being evacuated to vacuum degree lower than 1.0 × 10 to deposition chamber before sputtering sedimentation–3Pa。
Preferably, glow discharge principle etch cleaner matrix surface is utilized before sputtering sedimentation, to remove matrix surface
Oxide layer or pollutant.
The present invention selects corrosion resistance constituent element V, Al, Ti, Cr, Si to constitute high-entropy alloy film, passes through control each element
Atomic percentage content and using magnetron sputtering technique matrix surface deposition obtain amorphous VAlTiCrSi film, have
It has the advantages that:
(1) on the one hand the high-entropy alloy film is made of corrosion resistance constituent element V, Al, Ti, Cr, Si；On the other hand magnetic is used
It controls sputtering technology and is in amorphous structure, metallic atom arrangement is in unordered shape in amorphous structure, and there is no amorphous metals to be had
The uneven defect of the local organizations such as some crystal boundaries, fault, segregation, therefore the VAlTiCrSi film has high rigidity and excellent
Corrosion resistance, hardness can be higher than 10Gpa, and corrosion current density be even lower than 304 stainless steel an order of magnitude, because
This is a kind of material of wear resistant corrosion resistant, can wear in height, carry out good protection to matrix in the adverse circumstances of high corrosion, such as
The matrix protection etc. that can be used under briny environment.
(2) currently, high-entropy alloy film multiselect high-entropy alloy target or individual element and low constituent element during the preparation process
The combination of alloy target material.But high-entropy alloy target is difficult to constituent content, and cost of manufacture is high；Using the only of individual element
Vertical target is difficult to obtain ingredient uniformly high entropy coating.The present invention stacks gradually each element target, periodic arrangement, not only makes
It is at low cost, and the uniform VAlTiCrSi film of ingredient can be obtained.
Detailed description of the invention
Fig. 1 is the cross section structure schematic diagram of the VAlTiCrSi composition target in the embodiment of the present invention 1.
Fig. 2 is the XRD diffracting spectrum of VAlTiCrSi high-entropy alloy film obtained in the embodiment of the present invention 1.
Fig. 3 is that VAlTiCrSi high-entropy alloy film obtained is surveyed with 304 stainless steels through electrochemistry in the embodiment of the present invention 1
Try the dynamic polarization curve obtained.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail with attached drawing, it should be pointed out that reality as described below
It applies example to be intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1:
In the present embodiment, basis material is 304 stainless steels, and matrix surface is that the VAlTiCrSi high entropy of non-crystal structure closes
Gold thin film.
The VAlTiCrSi high-entropy alloy film the preparation method is as follows:
Using magnetron sputtering technique, VAlTiCrSi high-entropy alloy film is prepared in matrix surface, main includes following step
It is rapid:
(1) as shown in Figure 1, V target, Al target, Ti target, Cr target, Si target are selected, in vertical direction according to V-Al-Ti-Cr-Si
Sequence stack gradually from top to bottom arrangement with a thickness of 10mm each target, form a target period；Then, in vertical direction packet
12 target periods are included, composition target is formed.
(2) Mechanical polishing processing is carried out to matrix surface, carries out ultrasonic cleaning 3 times with petroleum ether, acetone and alcohol respectively,
Then being dried with nitrogen with flowing；Then, matrix is put into magnetron sputtering cavity, being evacuated to vacuum degree is 10-3Pa utilizes Ar
Ion pair composition target bombards 20min, and carries out ion etching 20min to matrix sample.
(3) nitrogen that purity is 99.99at.%, flow set 24sccm, magnetron sputtering step (1) are filled in cavity
In composition target 10min, deposit 6h in step (2) treated matrix surface, obtain VAlTiCrSi high-entropy alloy film, splash
During penetrating, sputtering power 2000W, substrate bias are -50V, substrate temperature is 100 DEG C.
The element component content of VAlTiCrSi high-entropy alloy film sample obtained above is as shown in table 1 below:
Table 1:VAlTiCrSi high-entropy alloy film element component content
As it can be seen from table 1 the atomic percentage content of each element is all satisfied in the VAlTiCrSi high-entropy alloy film sample
The requirement that the atomic percentage content of element is 5%~35% in high-entropy alloy.
Being pressed into six depth to the high-entropy alloy film sample surface VAlTiCrSi by nano impress equipment is
The point of 250nm measures hardness and elastic modulus, as a result as shown in table 2 below.As can be seen from Table 2, the film wear resistence is good.
The hardness and elastic modulus of table 2:VAlTiCrSi high-entropy alloy film
Fig. 2 is the XRD diffracting spectrum of the VAlTiCrSi high-entropy alloy film sample, and display only nearby has at 45 ° one wide
General steamed bun peak, characterizing the VAlTiCrSi high-entropy alloy film is amorphous structure.
Fig. 3 is the dynamic polarization that the VAlTiCrSi high-entropy alloy film sample and 304 stainless steels are obtained through electro-chemical test
Curve.If the following table 3 is the corrosion potential and corrosion current of the VAlTiCrSi high-entropy alloy film sample and 304 stainless steels
Density.From Fig. 3 in table 3 as can be seen that the VAlTiCrSi high-entropy alloy film corrosion current density it is very low, not with 304
Rust steel is compared, and corrosion current density even reduces an order of magnitude.
The corrosion potential and corrosion current density of table 3:VAlTiCrSi high-entropy alloy film
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of VAlTiCrSi high-entropy alloy film, it is characterized in that: being made of five kinds of elements, each element and its atomic percent contain
It measures as follows:
V:14~15%
Al:12~13%
Ti:12~13%
Cr:29~30%
Si:30~31%
Also, the VAlTiCrSi high-entropy alloy film is to be deposited and obtained in matrix surface using magnetron sputtering technique, in non-
Crystal structure.
2. VAlTiCrSi high-entropy alloy film as described in claim 1, it is characterized in that: hardness is higher than 10Gpa.
3. VAlTiCrSi high-entropy alloy film as described in claim 1, it is characterized in that: corrosion current density is not lower than 304
Rust steel an order of magnitude.
4. VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3, it is characterized in that: magnetron sputtering composition target,
Matrix surface after cleaning deposits to obtain the VAlTiCrSi high-entropy alloy film；
The composition target is made of V target, Al target, Ti target, Cr target, Si target, in vertical direction by five kinds of targets
Material stacked arrangement forms a target period, and the composition target is vertically including at least one described target period.
5. VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3, it is characterized in that: in the period target, from upper
V target, Al target, Ti target, Cr target, Si target are followed successively by under.
6. VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3, it is characterized in that: the composition target include 1~
15 target periods.
7. VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3, it is characterized in that: V target is thick in a target period
Degree is 5mm~50mm；
Preferably, Al target is in a target period with a thickness of 5mm~50mm；
Preferably, Ti target is in a target period with a thickness of 5mm~50mm；
Preferably, Cr target is in a target period with a thickness of 5mm~50mm；
Preferably, Si target is in a target period with a thickness of 5mm~50mm.
8. VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3, it is characterized in that: sputtering function in sputtering process
Rate is 1000W~3000W；
Preferably, substrate bias is -30V~-70V；
Preferably, substrate temperature is 100 DEG C~400 DEG C.
9. VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3, it is characterized in that: the basis material includes
Stainless steel.
10. application of the VAlTiCrSi high-entropy alloy film as claimed in claim 1,2 or 3 under briny environment.
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| CN111074224A (en) * | 2020-01-06 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | Corrosion-resistant high-entropy alloy nitride coating, and preparation method and application thereof |
| CN111074223A (en) * | 2020-01-06 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | Physical vapor deposition preparation method of high-entropy alloy film with uniform and controllable components |
| CN111218657A (en) * | 2020-01-03 | 2020-06-02 | 北京工业大学 | Amorphous tungsten-based high-entropy alloy thin film material and preparation method thereof |
| CN112921267A (en) * | 2020-06-08 | 2021-06-08 | 自贡市量子金属制造有限公司 | TiVZrCrAl high-entropy alloy coating on round-head surface of ball valve and preparation method thereof |
| CN113789503A (en) * | 2021-09-15 | 2021-12-14 | 郑州大学 | In-situ synthesis method of high-entropy silicide film with anti-oxidation characteristic |
| CN114574827A (en) * | 2022-03-03 | 2022-06-03 | 中国科学院宁波材料技术与工程研究所 | Carbon-containing high-entropy alloy film and preparation method and application thereof |
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| CN111218657A (en) * | 2020-01-03 | 2020-06-02 | 北京工业大学 | Amorphous tungsten-based high-entropy alloy thin film material and preparation method thereof |
| CN111218657B (en) * | 2020-01-03 | 2021-07-30 | 北京工业大学 | Amorphous tungsten-based high-entropy alloy thin film material and preparation method thereof |
| CN111074224A (en) * | 2020-01-06 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | Corrosion-resistant high-entropy alloy nitride coating, and preparation method and application thereof |
| CN111074223A (en) * | 2020-01-06 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | Physical vapor deposition preparation method of high-entropy alloy film with uniform and controllable components |
| CN112921267A (en) * | 2020-06-08 | 2021-06-08 | 自贡市量子金属制造有限公司 | TiVZrCrAl high-entropy alloy coating on round-head surface of ball valve and preparation method thereof |
| CN113789503A (en) * | 2021-09-15 | 2021-12-14 | 郑州大学 | In-situ synthesis method of high-entropy silicide film with anti-oxidation characteristic |
| CN113789503B (en) * | 2021-09-15 | 2023-08-22 | 郑州大学 | In-situ synthesis method of high-entropy silicide film with antioxidant property |
| CN114574827A (en) * | 2022-03-03 | 2022-06-03 | 中国科学院宁波材料技术与工程研究所 | Carbon-containing high-entropy alloy film and preparation method and application thereof |
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