CN104862748B - A kind of crystal particle scale graded metal nickel and its controllable method for preparing - Google Patents
A kind of crystal particle scale graded metal nickel and its controllable method for preparing Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 11
- 239000002184 metal Substances 0.000 title claims abstract description 11
- 239000013078 crystal Substances 0.000 title claims description 8
- 239000002245 particle Substances 0.000 title description 2
- 239000000654 additive Substances 0.000 claims abstract description 22
- 230000000996 additive effect Effects 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000009826 distribution Methods 0.000 claims abstract description 10
- 238000000151 deposition Methods 0.000 claims abstract description 9
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 230000000694 effects Effects 0.000 claims abstract description 3
- 238000009713 electroplating Methods 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 10
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical group OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 229940085605 saccharin sodium Drugs 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 claims description 2
- LKNLEKUNTUVOML-UHFFFAOYSA-L nickel(2+);sulfate;hydrate Chemical compound O.[Ni+2].[O-]S([O-])(=O)=O LKNLEKUNTUVOML-UHFFFAOYSA-L 0.000 claims description 2
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 1
- 235000011152 sodium sulphate Nutrition 0.000 claims 1
- 239000007769 metal material Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000011734 sodium Substances 0.000 description 7
- 239000003814 drug Substances 0.000 description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 6
- XSXHWVKGUXMUQE-UHFFFAOYSA-N osmium dioxide Inorganic materials O=[Os]=O XSXHWVKGUXMUQE-UHFFFAOYSA-N 0.000 description 6
- 229940081974 saccharin Drugs 0.000 description 6
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 6
- 235000019204 saccharin Nutrition 0.000 description 6
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000035772 mutation Effects 0.000 description 2
- -1 Sodium dialkyl sulfate Chemical class 0.000 description 1
- 229910000937 TWIP steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Abstract
For the shortage of the current effective preparation method of gradient-structure metal material, the invention provides a kind of low cost, more easily graded metal nickel of industrialized production and preparation method thereof, it is characterised in that：Prepared using electro-plating method, with nickel as consumable anode, according to diverse microcosmic structure or mechanical property requirements, changed with time using computer controls current density and additive concentration, deposition forms grain size gradient metallic nickel under DC current effect.This gradient-structure metallic nickel size is almost unrestricted, and gradient distribution form is controllable, and crystallite dimension progressively increases to 1 30 μm by 10 100nm, and each hierarchical structure part exists without interface；The gradient-structure metallic nickel good mechanical performance, its yield strength >=750MPa is 34 times of traditional coarse-grain, and stretching plastic deformation reaches more than 10%, bulk sample consistency >=99.5%.
Description
Technical field
The present invention relates to grain size gradient metallic nickel and its controllable method for preparing with excellent mechanical performance.
Background technology
Gradient-structure is gradually to another composition, tissue or phase (or constituent element) from a kind of composition, tissue or phase (or constituent element)
Transitional structure material, such as be gradually transitions fine grain, or even amorphous structure by coarse-grain.It is different from traditional uniform pure metals
Or uniform single-stage composite, the heterogeneity of the feature exhibit tissue of functionally gradient material (FGM) and multiple dimensioned property, and structure is more
Level property.Because tissue and phase in version are gentle, interface is broadened even and disappear.Different from traditional composite, this structure ladder
Degree can not only be prevented effectively from the performance mutation that size mutation causes, moreover it is possible to make the structure with different characteristic size mutually coordinated,
The multiple action mechanism corresponding to each characteristic size is shown simultaneously, obtains the overall performance of material and usage performance greatly excellent
Change and lifted, realize the perfect matching and multifunctionality of Fracture of Material.Exactly this unique structure is gradient-structure metal
Material brings the performance of uniqueness：Such as high intensity, high rigidity, high-wearing feature, highly corrosion resistant etc..These excellent performances
For gradient-structure metal material brings in fields such as Aero-Space, communications and transportation, energy facilities, machine-building, electronic information
Vast potential for future development.
The preparation method of existing gradient-structure metal material is mainly by mechanically deform acquisition, this top-down system
Preparation Method is primarily present three limitation of aspect：(1) the method prepares functionally gradient material (FGM) limited types, is only limitted to have good modeling
The preparation of property metal material, such as Cu, IF steel, TWIP steel etc.；(2) sample that prepared by the method is generally surface graded, gradient layer
Thickness is hundreds of microns, it is impossible to meet the demand of industrial applications；(3) gradient type that prepared by the method is limited, and not
Gradient type and distribution can accurately be regulated and controled, quantify gradient structure relation between structure and property, thus can not developed with optimal ladder
Degree structure and the research for carrying out gradient-structure metal material related scientific issues in a deep going way.Therefore, in gradient-structure metal material
In industrialization process, effective preparation method of gradient-structure how is developed, optimization gradient-structure is the matter of utmost importance for facing at present.
The content of the invention
For the shortage of the current effective preparation method of gradient-structure metal material, the invention provides a kind of low cost, more
Plus it is easy to graded metal nickel of industrialized production and preparation method thereof, this gradient-structure metallic nickel size is almost unrestricted
(>=5mm, such as Fig. 1), gradient distribution form is controllable, and crystallite dimension progressively increases to 1-30 μm, and each level knot by 10-100nm
There is (as shown in Figure 2) without interface in component；The gradient-structure metallic nickel good mechanical performance, its yield strength >=750MPa is
3-4 times of traditional coarse-grain, and stretching plastic deformation reaches more than 10%, bulk sample consistency >=99.5%.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of preparation method of crystal grain graded metal nickel, it is characterised in that：Prepared using electro-plating method, be consumption sun with nickel
Pole, according to diverse microcosmic structure or mechanical property requirements, using computer controls current density and additive concentration with the time
Change, deposition forms grain size gradient metallic nickel under DC current effect.
Preparation method of the present invention, it is characterised in that：It is addition with saccharin sodium with titanium, copper, steel or nickel as negative electrode
Agent.Changed with time using computer controls current density and additive concentration, current density is from 5-10mA/cm2Gradually increase
Add to 100-150mA/cm2, the concentration of additive saccharin sodium progressively increases to 8g/L from 0.5g/L.
Concrete technology step is as follows：
1), matrix polishing, surface degreasing；
2), plating solution configuration：Weigh seven water nickel sulfate 300g/L of requirement, six water nickel chloride 45g/L, boric acid 40g/L, ten
Sodium dialkyl sulfate 0.01-0.1g/L, is dissolved in distilled water, stirring and dissolving；Adjust pH value to 4 ± 0.2；
3), current density and solution composition regulate and control：According to required grain size gradient distribution form and thickness of sample will
Ask, continuously adjust current density using computer and additive concentration changes over time form, current density is from 5-10mA/cm2
It is gradually increased to 100-150mA/cm2, additive concentration progressively increases to 5-8g/L from 0.5-1.0g/L.
Wherein, the purpose of matrix polishing be in order to eliminate the trickle uneven, oxide skin of matrix surface and various gross imperfections, with
Surface smoothness is improved, 600#, 800#, 1000#, 2000# can be followed successively by, be gone forward side by side using the method for sand papering, grinding turn
One step is polished to matrix, makes it have bright luster.
Matrix surface oil removing removes matrix surface greasy dirt using organic solvent (such as acetone) in order to the implementation of plating
Remove.
All reagents used of the invention are analyzes pure, and plating solution is configured using distilled water, and it is 99% that anode uses purity
Nickel sheet.The method has simple to operate, and sample size is almost unrestricted, and sample quality is good, and microstructure and mechanical property can
The advantages of control.
Brief description of the drawings
Fig. 1 multi-form grain size distributions schematic diagram (by taking three kinds of crystallite dimensions of different distributions as an example).
The crystal grain distribution of the typically different distribution grain size gradient metallic nickel of three kinds of Fig. 2 electro-deposition.
The close-up view (a) and coarse-grain side (b) of Fig. 3 electro-deposition grain size gradients structural metal nickel and the shape of nanocrystalline side
Looks figure (c).
The tensile stress-strain curve of Fig. 4 various grain sizes gradient distribution metallic nickel (I-V)
Specific embodiment
Embodiment 1
With nickel as consumable anode, with Ti cathode, 800ml plating solutions are configured on request, solution composition is：
NiSO4·7H2O:300g/L, NiCl2·6H2O:45g/L, H3BO3:40g/L, C12H25OSO2Na:0.05g/L.With
Balance weighs above medicine, is dissolved in beaker, makes 3/4ths of liquor capacity no more than beaker nominal volume, by what is configured
Plating solution magnetic stirrer, pH value is adjusted to 4 ± 0.2 with sodium hydroxide solution, and bath temperature is controlled to 55 ± 1 DEG C.
Computer controls current density and additive concentration：
Current density：(1), start current density in 47.5h and keep constant 10mA/cm2, electric current in (2), afterwards 0.75h
Density is by 10mA/cm2Gradually increase to 20mA/cm2, (3) and then current density gradually increases to 30mA/cm in 0.75h2,
(4), continue that current density is gradually increased into 50mA/cm in 0.25h2, current density gradually increases in (5), afterwards 0.25h
To 120mA/cm2, (6), last current density are maintained at 120mA/cm2Deposition 1h.
Control additive concentration at the same time：(1), start saccharin na concn and keep constant 0.5g/L about 10h, (2), afterwards
25h in 2g/L is gradually increased to by 0.5g/L, (3) and then 3g/L is gradually increased in 5h, (4), again in 7.5h gradually
6g/L is increased to, (5), its constant concentration is finally kept in 6g/L.
As shown in figure 3, sample crystallite dimension is from 20nm to 5 μm, and maximum intensity >=850MPa, plastic deformation >=10% is (such as
Fig. 4 curve IV).
Embodiment 2
With nickel as consumable anode, with titanium as negative electrode, 800ml plating solutions are configured on request, solution composition is：
NiSO4·7H2O:300g/L, NiCl2·6H2O:45g/L, H3BO3:40g/L, C12H25OSO2Na:0.05g/L.With
Balance weighs above medicine, is dissolved in beaker, makes 3/4ths of liquor capacity no more than beaker nominal volume, by what is configured
Plating solution magnetic stirrer, pH value is adjusted to 4 ± 0.2 with sodium hydroxide solution, and bath temperature is controlled to 55 ± 1 DEG C.
Computer controls current density and additive concentration：
Control electric current density mainly divides six stages：(1), start current density in 25h and keep constant 5mA/cm2, (2),
Afterwards in 3h current density by 5mA/cm2Gradually increase to 20mA/cm2, (3) and then 30mA/ is gradually increased in 2.5h
cm2, current density is gradually increased to 50mA/cm by (4), continuation in 2.5h2, current density gradually increases in (5), afterwards 2h
To 120mA/cm2, (6) finally current density is maintained at 120mA/cm2Deposition 1h.
Control additive concentration at the same time：(1), saccharin na concn keeps constant 0.7g/L about 10h, the 15h after (2)
5g/L is gradually inside increased to by 0.7g/L, (3), its constant concentration is finally kept in 5g/L.
Plating obtains sample crystallite dimension from 20nm to 10 μm, maximum intensity >=750MPa, and plastic deformation >=15% is (as schemed
4 curve V).
Embodiment 3
With nickel as consumable anode, with steel as negative electrode, 800ml plating solutions are configured on request, solution composition is：
NiSO4·7H2O:300g/L, NiCl2·6H2O:45g/L, H3BO3:40g/L, C12H25OSO2Na:0.06g/L.With
Balance weighs above medicine, is dissolved in beaker, makes 3/4ths of liquor capacity no more than beaker nominal volume, by what is configured
Plating solution magnetic stirrer, pH value is adjusted to 4 ± 0.2 with sodium hydroxide solution, and bath temperature is controlled to 55 ± 1 DEG C.
Computer controls current density and additive concentration：
Current density：(1), constant 7mA/cm is kept in 18h current densities first2, (2) and then the current density in 3h
By 7mA/cm2Gradually increase to 20mA/cm2, current density gradually increases to 30mA/cm in (3), 3h afterwards2, (4), continue
Current density is gradually increased into 50mA/cm in 5h2, (5) and then current density gradually increases to 120mA/cm in 4h2,
(6), last current density is maintained at 120mA/cm2Deposition 1h.
Control additive concentration at the same time：(1), start saccharin na concn and keep constant 0.5g/L about 10h, (2), afterwards
8h in be gradually increased to 6g/L, (3), finally keep its constant concentration in 6g/L.
Plating obtains sample crystallite dimension from 18nm to 10 μm, maximum intensity >=1100MPa, and plastic deformation >=9% is (as schemed
4 curve II).
Embodiment 4
With nickel as consumable anode, with nickel as negative electrode, 800ml plating solutions are configured on request, solution composition is：
NiSO4·7H2O:300g/L, NiCl2·6H2O:45g/L, H3BO3:40g/L, C12H25OSO2Na:0.07g/L.With
Balance weighs above medicine, is dissolved in beaker, makes 3/4ths of liquor capacity no more than beaker nominal volume, by what is configured
Plating solution magnetic stirrer, pH value is adjusted to 4 ± 0.2 with sodium hydroxide solution, and bath temperature is controlled to 55 ± 1 DEG C.
Computer controls current density and additive concentration：
Current density：(1), constant 8mA/cm is kept in 14h current densities first2, current density in (2), 3h afterwards
By 8mA/cm2Gradually increase to 20mA/cm2, (3) and then current density is gradually increased into 30mA/cm in 4h2, (4), after
Continue and current density is gradually increased into 50mA/cm in 6h2, current density gradually increases to 150mA/cm in (5), afterwards 4h2,
(6), last current density is maintained at 150mA/cm2Deposition 1h.
Control additive concentration at the same time：(1), start saccharin na concn and keep constant 1g/L about 10h, (2), afterwards
8g/L is gradually increased to by 1g/L in 4h, (3), its constant concentration is finally kept in 8g/L.
Plating obtains sample crystallite dimension from 15nm to 5 μm, maximum intensity >=1250MPa, is plastically deformed >=8% (such as Fig. 4
Curve I).
Embodiment 5
With nickel as consumable anode, with cathode, 800ml plating solutions are configured on request, solution composition is：
NiSO4·7H2O:300g/L, NiCl2·6H2O:45g/L, H3BO3:40g/L, C12H25OSO2Na:0.1g/L.With day
It is flat to weigh above medicine, dissolved in beaker, make 3/4ths of liquor capacity no more than beaker nominal volume, the plating that will be configured
Liquid magnetic stirrer, pH value is adjusted to 4 ± 0.2 with sodium hydroxide solution, and bath temperature is controlled to 55 ± 1 DEG C.
Computer controls current density and additive concentration：
Current density：(1), constant 10mA/cm is kept in 30h current densities first2, (2) and then electric current is close in 2.5h
Degree is by 10mA/cm2Gradually increase to 20mA/cm2, current density gradually increases to 30mA/cm in (3), 2.5h afterwards2, (4),
Current density is gradually increased to 50mA/cm by continuation in 2.5h2, current density is gradually increased in (5), 2h afterwards
100mA/cm2, (6), last current density are maintained at 100mA/cm2Deposition 1h.
Control additive concentration at the same time：(1), start saccharin na concn and keep constant 1g/L about 10h, (2), afterwards
5g/L is gradually increased in 20h, (3), its constant concentration is finally kept in 5g/L.
Plating obtains sample crystallite dimension from 25nm to 5 μm, maximum intensity >=800MPa, is plastically deformed >=10% (such as Fig. 4
Curve III).
Embodiment 6
With nickel as consumable anode, with titanium as negative electrode, 800ml plating solutions are configured on request, solution composition is：
NiSO4·7H2O:300g/L, NiCl2·6H2O:45g/L, H3BO3:40g/L, C12H25OSO2Na:0.05g/L.With
Balance weighs above medicine, is dissolved in beaker, makes 3/4ths of liquor capacity no more than beaker nominal volume, by what is configured
Plating solution magnetic stirrer, pH value is adjusted to 4 ± 0.2 with sodium hydroxide solution, and bath temperature is controlled to 55 ± 1 DEG C.
Computer controls current density and additive concentration：
Current density：(1), constant 5mA/cm is kept in 36h current densities first2, electric current is close in (2), 2.5h afterwards
Degree is by 5mA/cm2Gradually increase to 20mA/cm2, (3) and then current density is gradually increased into 30mA/cm in 2h2, (4),
Current density is gradually increased to 50mA/cm by continuation in 1.25h2, current density is gradually increased in (5), afterwards 0.5h
120mA/cm2, (6), last current density are maintained at 120mA/cm2Deposition 1h.
Control additive concentration at the same time：(1), start saccharin na concn and keep constant 0.5g/L about 10h, (2), afterwards
26h in be gradually increased to 7g/L, (3), finally keep its constant concentration in 7g/L.
Plating obtains sample crystallite dimension from 15nm to 6 μm, maximum intensity >=800MPa, plastic deformation >=12%.
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of crystal grain graded metal nickel, it is characterised in that：Prepared using electro-plating method, be consumption sun with nickel
Pole, according to diverse microcosmic structure or mechanical property requirements, using computer controls current density and additive concentration with the time
Change, current density is from 5-10mA/cm2It is gradually increased to 100-150mA/cm2, additive is saccharin sodium, and concentration is from 0.5-
1.0g/L progressively increases to 5-8g/L, and finally deposition forms grain size gradient metallic nickel under DC current effect.
2. according to the preparation method described in claim 1, it is characterised in that：With titanium, copper, steel or nickel as negative electrode.
3. according to any described preparation method of claim 1~2, it is characterised in that processing step is：
1), matrix polishing, surface degreasing；
2), plating solution configuration：Weigh seven water nickel sulfate 300g/L, six water nickel chloride 45g/L, boric acid 40g/L, dodecane of requirement
Base sodium sulphate 0.01-0.1g/L, is dissolved in distilled water, stirring and dissolving；Adjust pH value to 4 ± 0.2；
3), current density and solution composition regulate and control：According to the requirement of required grain size gradient distribution form and thickness of sample, profit
Current density being continuously adjusted with computer and additive concentration changing over time form, current density is from 5-10mA/cm2Gradually increase
Add to 100-150mA/cm2, additive concentration progressively increases to 5-8g/L from 0.5-1.0g/L.
4. the crystal grain graded metal nickel that prepared by a kind of claim 1 methods described.
5. according to crystal grain graded metal nickel described in claim 4, it is characterised in that：The metallic nickel crystallite dimension is by 10-100nm
1-30 μm is progressively increased to, and each hierarchical structure part exists without interface.
6. according to crystal grain graded metal nickel described in claim 4, it is characterised in that：The metallic nickel bulk sample consistency >=
99.5%.
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| CN105506693A (en) * | 2015-12-28 | 2016-04-20 | 上海交通大学 | Surface nickel coating grain size regulating method capable of improving corrosion resistance |
| CN106929888B (en) * | 2017-05-03 | 2018-12-14 | 上海电力学院 | A kind of preparation method of lamellar composite nanostructure nickel |
| CN109338288B (en) * | 2018-09-17 | 2020-09-18 | 中国科学院金属研究所 | Gas turbine blade tip protective coating and preparation method and application thereof |
| CN111254467B (en) * | 2020-01-20 | 2021-03-02 | 广东省科学院中乌焊接研究所 | Nickel-tungsten alloy with gradient structure, preparation method and novel layered structure |
| CN111266593B (en) * | 2020-03-31 | 2022-11-08 | 燕山大学 | High-toughness metal material with gradient structural units and preparation method thereof |
| CN111411377B (en) * | 2020-05-07 | 2021-02-02 | 广东省科学院中乌焊接研究所 | Novel nickel-phosphorus alloy with gradient structure and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS62202094A (en) * | 1986-02-28 | 1987-09-05 | Sumitomo Metal Ind Ltd | Production of gradient plating |
| US6524461B2 (en) * | 1998-10-14 | 2003-02-25 | Faraday Technology Marketing Group, Llc | Electrodeposition of metals in small recesses using modulated electric fields |
| DE10259362A1 (en) * | 2002-12-18 | 2004-07-08 | Siemens Ag | Process for depositing an alloy on a substrate |
| CN101165219A (en) * | 2007-08-08 | 2008-04-23 | 北京科技大学 | Method for control size of electroforming nickel crystal in nickel sulphate electroforming liquid |
| CN102400194A (en) * | 2011-12-06 | 2012-04-04 | 淮海工学院 | Method for preparing gradient nano crystal coating |
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2015
- 2015-05-29 CN CN201510290567.1A patent/CN104862748B/en active Active
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