CN111254467B - Nickel-tungsten alloy with gradient structure, preparation method and novel layered structure - Google Patents
Nickel-tungsten alloy with gradient structure, preparation method and novel layered structure Download PDFInfo
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Abstract
The invention discloses a nickel-tungsten alloy with a gradient structure, a preparation method and a novel layered structure, and relates to the technical field of metal materials. The preparation method provided by the invention can prepare different distribution forms of grain size gradient gradually transiting from micron-sized coarse crystals to nano crystals and component gradient gradually increasing in tungsten content in the nickel-tungsten alloy by utilizing an electrochemical deposition technology and regulating and controlling electrodeposition parameters through a computer. The method is favorable for regulating and controlling the comprehensive performance of the whole material in a larger scale space, thereby avoiding the defect of poor plasticity/toughness of the homogeneous nano structure. The nickel-tungsten alloy with the gradient structure prepared by the method can further widen the application range of the nickel-tungsten alloy and provide technical reserve for future engineering application. The novel layered structure comprises a base body and a nickel-tungsten alloy coating with a gradient structure.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a nickel-tungsten alloy with a gradient structure, a preparation method and a novel layered structure.
Background
Inspired by gradient materials commonly existing in nature, a gradient structure is widely introduced into the design and development of novel metal structure materials so as to improve the overall mechanical performance of the novel metal structure materials. At present, the gradient structure metal material is mainly obtained by a plastic deformation method, and the preparation technology has some inevitable limitations, such as that the distribution form of the gradient structure is difficult to control accurately. Patent document CN104862748A discloses a grain size gradient metal nickel and a controllable preparation method thereof, which realizes controllable preparation of the grain size gradient metal nickel by continuously regulating and controlling current density and additive (saccharin sodium) concentration. However, the method only focuses on the grain size gradient, and the preparation and control of the chemical composition gradient are not involved.
Nickel-based alloys have a broader background for industrial applications than pure metallic nickel. For example, homogeneous nanostructured nickel-tungsten alloys have attracted considerable attention for their excellent corrosion resistance, high hardness and high wear resistance, and have found relevant applications in electronics, chemical, mechanical and other industries. However, under severe working conditions such as high speed and heavy load, the homogeneous nanostructure nickel-tungsten alloy is easy to crack in the whole thickness direction due to the brittleness, and is very unfavorable for the service life of a structural member, thereby limiting the application range of the nickel-tungsten alloy. The preparation process is limited, continuous change of grain size and chemical components in the nickel-tungsten alloy is not realized at present, the whole change interval of the grain size is narrow and is still in the nanometer level, and the plasticity/toughness of the whole material is still poor. Therefore, it can be assumed that if a grain gradient (wider grain size variation range) gradually transitioning from micron-sized coarse grains to nano-sized grains and a component gradient with gradually rising tungsten content are prepared in the nickel-tungsten alloy, and the gradient distribution form is accurate and controllable, the performance of the whole material can be regulated and controlled in a larger scale space, so that the defect of poor plasticity/toughness of the nickel-tungsten alloy is avoided, and the application range of the nickel-tungsten alloy is further expanded.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a nickel-tungsten alloy with a gradient structure, a preparation method and a novel layered structure to solve the technical problems.
The invention is realized by the following steps:
a preparation method of a nickel-tungsten alloy with a gradient structure comprises the following steps: adopting an electrochemical deposition technology, taking nickel as a consumable anode, and controlling the current density and the additive concentration in the electroplating solution to change along with time by using a computer to deposit and form the nickel-tungsten alloy with a gradient structure with chemical composition gradient and grain size gradient under the action of direct current; the additive comprises tungstate and saccharin sodium, wherein the tungstate provides a tungsten element in the nickel-tungsten alloy coating, and the saccharin sodium can optimize the internal stress of the coating.
The anode is selected from nickel plates with the purity of 99%. The cathode is selected from titanium, copper, steel or nickel.
The preparation method provided by the invention utilizes an electrochemical deposition technology, and the electrodeposition parameters are regulated and controlled by a computer, so that the grain size gradient and the component gradient with gradually rising tungsten content in different distribution forms, which are transited from micron-sized coarse crystals to nano crystals, can be prepared in the nickel-tungsten alloy, and the double composition of the grain size gradient and the chemical component gradient is realized.
In the preferred embodiment of the present invention, the current density is from 10 to 20mA/cm2Gradually increasing to 50-100mA/cm2。
In other embodiments, the current density is controlled to be between 10 and 20mA/cm2Keeping for 1-1.5h, and uniformly increasing the current density to 30mA/cm within 1.5-2h2Then increasing the current density to 50-55mA/cm at a constant speed within 1-1.2h2Then the current density is increased to 80-85mA/cm at a constant speed within 1.6-1.7h2Keeping the current density at 80-85mA/cm2Depositing for 0.5-0.6 h.
In a preferred embodiment of the present invention, the tungstate is sodium tungstate or ammonium tungstate.
In the preferred embodiment of the invention, the concentration of sodium tungstate controlled by the computer is gradually increased from 0-1g/L to 10-50 g/L.
In other embodiment modes, the concentration of the sodium tungstate is kept at 0g/L within 4.5h after the electrochemical deposition, the concentration of the sodium tungstate is gradually increased from 0g/L to 20g/L within 1.6h after the electrochemical deposition, and finally the concentration of the sodium tungstate is kept at 20 g/L.
In addition, in other embodiments, sodium tungstate may also be added to the plating solution at the beginning of the electrochemical deposition.
Sodium tungstate is a strong alkali weak acid salt, and if the concentration of sodium tungstate is excessive, precipitation can be generated under an acidic electroplating solution, so that the electrochemical deposition efficiency and the surface quality of an alloy coating are influenced.
In other embodiments, the concentration of saccharin sodium is gradually increased from 0.5-0.6g/L to 15-15.5g/L using computer control.
In other embodiments, the concentration of sodium saccharin is controlled by a computer to be constant at 0.5-0.6g/L over the first 1-1.5h of electrochemical deposition, then the concentration of sodium saccharin is controlled to gradually increase to 5.0-5.5g/L over 1.5-2h, then kept for 1-1.5h, and then the concentration of sodium saccharin is gradually increased to 15-15.5g/L over the subsequent 1.6-1.7 h.
In other embodiments, the electrochemical deposition parameters can be adaptively controlled according to the gradient alloy material to be prepared.
In a preferred embodiment of the present invention, before performing the electrochemical deposition, a plating solution is prepared, such that the plating solution contains the following components: the concentration of the nickel sulfate hexahydrate is 50-300g/L, the concentration of the nickel chloride hexahydrate is 43-45g/L, the concentration of the boric acid is 40-42g/L, and the concentration of the sodium dodecyl sulfate is 0.05-0.5 g/L.
In other embodiments, the pH of the plating solution is adjusted to 3.5 ± 0.2.
In other embodiments, the temperature of the plating solution is adjusted to 55. + -. 1 ℃.
Under the conditions of the plating solution components, pH and temperature, the high-efficiency codeposition of the metal nickel and the metal tungsten can be realized on the cathode.
In a preferred embodiment of the present invention, the preparation method further comprises pre-treating the substrate before plating.
In other embodiments, the pretreatment comprises mechanical polishing and degreasing of the substrate.
The mechanical grinding and polishing can eliminate the fine unevenness, oxide skin and various macroscopic defects of the surface of the substrate, thereby improving the flatness of the surface of the substrate. The substrate surface is polished to have a mirror surface gloss.
In other embodiments, mechanical polishing is performed by sanding the surface of the substrate with 200#, 400# and 800# sandpaper in sequence.
In other embodiments, the surface degreasing is cleaning the substrate surface with an organic solvent; the organic solvent is preferably acetone or ethanol.
The surface is degreased to facilitate the implementation of electroplating, and the greasy dirt on the surface of the substrate can be removed by utilizing the similar compatible principle of organic solvents.
The nickel-tungsten alloy with the gradient structure prepared by the preparation method.
The grain size of the nickel-tungsten alloy with the gradient structure is gradually increased from 10nm to 10 mu m.
The preparation method provided by the invention realizes the controllable preparation of the nickel-tungsten alloy with the gradient structure by controlling the current density and the change of the additive concentration through a computer, and the prepared nickel-tungsten alloy with the gradient structure has good quality and controllable microstructure and mechanical structure.
In a preferred embodiment of the present invention, the content of tungsten in the nickel-tungsten alloy with gradient structure is 1-20% by mass.
A novel layered structure comprises a matrix and a plating layer made of nickel-tungsten alloy with a gradient structure, wherein the matrix is any one of pure copper, pure nickel, copper alloy, nickel alloy, aluminum alloy, carbon steel and alloy steel.
The invention has the following beneficial effects:
the invention provides a nickel-tungsten alloy with a gradient structure, a preparation method and a novel layered structure, wherein the electrochemical deposition technology is utilized, the electrodeposition parameters are regulated and controlled by a computer, the grain gradient gradually transited from micron-sized coarse crystals to nano crystals and the component gradient of tungsten content can be prepared in the nickel-tungsten alloy, and the corresponding gradient distribution form is accurate and controllable. The method is favorable for regulating and controlling the comprehensive performance of the whole material in a larger scale space, thereby avoiding the defect of poor plasticity/toughness of the homogeneous nano structure. The nickel-tungsten alloy with the gradient structure prepared by the method can further widen the application range of the nickel-tungsten alloy and provide technical reserve for future engineering application.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a cross-sectional microstructure morphology and surface energy spectrum analysis of electrochemically deposited 3 typical gradient structure nickel-tungsten alloys;
FIG. 2 is X-ray diffraction (XRD) spectra of nickel-tungsten alloy with 3 typical gradient structures at different positions in the thickness direction;
FIG. 3 shows the grain size distribution and corresponding surface tungsten content of electrochemically deposited 3 typical gradient structure nickel-tungsten alloys;
FIG. 4 is a sectional hardness value distribution of the nickel-tungsten alloy with the gradient structure.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a nickel-tungsten alloy with a gradient structure. Which comprises the following steps:
(1) in this example, a metallic nickel plate with a purity of 99.6% is used as a consumable anode, and a metallic nickel plate is used as a cathode.
500ml of plating solution was prepared, the base plating solution comprising the following concentrations of chemicals: NiSO4·6H2O：100g/L，NiCl2·6H2O：45g/L，H3BO3：40g/L，C12H25OSO2Na: 0.1 g/L. Weighing the above chemical reagents, dissolving in 500ml beaker with ultrapure water, stirring the solution with magnetic stirrer to clear state, adjusting pH to 3.5 + -0.2 with dilute sulfuric acid solution or sodium hydroxide solution, and controlling the temperature of the plating solution to 55 + -1 deg.C with heating device.
(2) The current density and the concentration of the additive were controlled with a computer:
current density: electrochemical sinkThe current density is kept constant at 20mA/cm within 1.5h after the product is started2Then the current density is controlled to be 20mA/cm within 2h2Gradually increased to 30mA/cm2Then the current density was gradually increased to 50mA/cm within 1h2The current density was gradually increased to 80mA/cm in the following 1.6h2Finally, the current density was kept at 80mA/cm2The deposition is carried out for 0.5 h.
And simultaneously regulating and controlling the concentration of saccharin sodium as an additive: the concentration of the saccharin sodium is kept constant at 0.5g/L within 1.5h after the beginning of the electrochemical deposition, the concentration of the saccharin sodium is gradually increased from 0.5g/L to 5.5g/L within 2h later, and finally the concentration of the saccharin sodium is kept at 5.5 g/L.
And simultaneously regulating and controlling the concentration of the additive sodium tungstate: the concentration of sodium tungstate is kept at 0g/L within 4.5h after the electrochemical deposition, the concentration of sodium tungstate is gradually increased from 0g/L to 10g/L within 1.6h later, and finally the concentration of sodium tungstate is kept at 10 g/L.
In this embodiment, a nickel-tungsten alloy sample i with a gradient structure is prepared, and as shown in a and d in fig. 1, the grain size of the sample i is gradually refined from micron to nanometer, and no obvious macroscopic interface exists. Referring to a graph a in fig. 2, it can be seen that the XRD curves at different positions in the thickness direction of the gradient-structured nickel-tungsten alloy sample i are clearly different from those in fig. 2 in the grain size and crystallographic orientation at different thickness positions of the gradient layer.
The grain size distribution and the maximum tungsten content of the nickel-tungsten alloy sample i with the electrochemical deposition gradient structure are shown in fig. 3, and it can be seen from fig. 3 that the grain size variation ranges are as follows: from-30 nm to-4 μm, with a maximum tungsten content of 1.82 wt.%.
The sectional hardness distribution of the nickel-tungsten alloy with the gradient structure is shown in FIG. 4, and the hardness is gradually increased from 2.4GPa to 4.6 GPa.
Example 2
The embodiment provides a preparation method of a nickel-tungsten alloy with a gradient structure. Which comprises the following steps:
(1) in this example, a metallic nickel plate with a purity of 99.6% is used as a consumable anode, and a metallic nickel plate is used as a cathode.
500ml of plating solution was prepared, and the base plating solution was composed ofChemical reagents: NiSO4·6H2O：100g/L，NiCl2·6H2O：45g/L，H3BO3：40g/L，C12H25OSO2Na: 0.1 g/L. Weighing the above chemical reagents, dissolving in 500ml beaker with ultrapure water, stirring the solution with magnetic stirrer to clear state, adjusting pH to 3.5 + -0.2 with dilute sulfuric acid solution or sodium hydroxide solution, and controlling the temperature of the plating solution to 55 + -1 deg.C with heating device.
(2) The current density and the concentration of the additive were controlled with a computer:
current density: the current density remained constant at 20mA/cm for 1.5h after the start of electrochemical deposition2Then the current density is controlled to be 20mA/cm within 2h2Gradually increased to 30mA/cm2Then the current density was gradually increased to 50mA/cm within 1h2The current density was gradually increased to 80mA/cm in the following 1.6h2Finally, the current density was kept at 80mA/cm2The deposition is carried out for 0.5 h.
And simultaneously regulating and controlling the concentration of saccharin sodium as an additive: the concentration of the saccharin sodium is kept constant at 0.5g/L within 1.5h after the beginning of the electrochemical deposition, the concentration of the saccharin sodium is gradually increased from 0.5g/L to 5.5g/L within 2h later, then the concentration of the saccharin sodium is kept at 5.5g/L within 1h, the concentration of the saccharin sodium is gradually increased from 5.5g/L to 10.5g/L within 1.6h later, and finally the concentration of the saccharin sodium is kept at 10.5 g/L.
And simultaneously regulating and controlling the concentration of the additive sodium tungstate: the concentration of sodium tungstate is kept at 0g/L within 4.5h after the electrochemical deposition, the concentration of sodium tungstate is gradually increased from 0g/L to 20g/L within 1.6h later, and finally the concentration of sodium tungstate is kept at 20 g/L.
The sample ii of the nickel-tungsten alloy with the gradient structure is prepared in the embodiment, and as shown in a diagram b and a diagram e in a figure 1, the grain size of the sample ii is gradually thinned from a micron level to a nanometer level without any obvious macroscopic interface. Referring to the graph b in fig. 2, it can be seen that the XRD curves at different positions in the thickness direction of the gradient-structured nickel-tungsten alloy sample ii are shown, and the grain size and crystallographic orientation of the gradient layer vary with the position as shown in fig. 2.
The grain size distribution and the maximum tungsten content of the electrochemical deposition gradient structure nickel-tungsten alloy sample ii are shown in fig. 3, and it can be seen from fig. 3 that the grain size variation range is: from-20 nm to 3 μm, with a maximum tungsten content of 3.54 wt.%.
The sectional hardness distribution of the nickel-tungsten alloy sample ii having a gradient structure is shown in FIG. 4, in which the hardness gradually increases from 2.4GPa to 4.75 GPa.
Example 3
The embodiment provides a preparation method of a nickel-tungsten alloy with a gradient structure. Which comprises the following steps:
(1) in this example, a metallic nickel plate with a purity of 99.6% is used as a consumable anode, and a metallic nickel plate is used as a cathode.
500ml of plating solution was prepared, the base plating solution comprising the following concentrations of chemicals: NiSO4·6H2O：100g/L，NiCl2·6H2O：45g/L，H3BO3：40g/L，C12H25OSO2Na: 0.1 g/L. Weighing the above chemical reagents, dissolving in 500ml beaker with ultrapure water, stirring the solution with magnetic stirrer to clear state, adjusting pH to 3.5 + -0.2 with dilute sulfuric acid solution or sodium hydroxide solution, and controlling the temperature of the plating solution to 55 + -1 deg.C with heating device.
(2) The current density and the concentration of the additive were controlled with a computer:
current density: the current density remained constant at 20mA/cm for 1.5h after the start of electrochemical deposition2Then the current density is controlled to be 20mA/cm within 2h2Gradually increased to 30mA/cm2Then the current density was gradually increased to 50mA/cm within 1h2The current density was gradually increased to 80mA/cm in the following 1.6h2Finally, the current density was kept at 80mA/cm2The deposition is carried out for 0.5 h.
And simultaneously regulating and controlling the concentration of saccharin sodium as an additive: the concentration of the saccharin sodium is kept constant at 0.5g/L within 1.5h after the beginning of the electrochemical deposition, the concentration of the saccharin sodium is gradually increased from 0.5g/L to 5.5g/L within 2h later, then the concentration of the saccharin sodium is kept at 5.5g/L within 1h, the concentration of the saccharin sodium is gradually increased from 5.5g/L to 15.5g/L within 1.6h later, and finally the concentration of the saccharin sodium is kept at 15.5 g/L.
And simultaneously regulating and controlling the concentration of the additive sodium tungstate: the concentration of sodium tungstate is kept at 0g/L within 4.5h after the electrochemical deposition, the concentration of sodium tungstate is gradually increased from 0g/L to 50g/L within 1.6h later, and finally the concentration of sodium tungstate is kept at 50 g/L.
In this embodiment, a nickel-tungsten alloy sample iii with a gradient structure is prepared, and as shown in fig. c and f in fig. 1, the grain size of the sample iii is gradually refined from micron to nanometer, and no obvious macroscopic interface exists. Referring to the XRD curves in the thickness direction of the gradient-structured nickel-tungsten alloy sample iii shown in fig. 2 c, it can be seen from fig. 2 that the grain size and crystallographic orientation are significantly different at different thickness positions of the gradient layer.
The grain size distribution and the maximum tungsten content of the electrochemical deposition gradient structure nickel-tungsten alloy sample iii are shown in fig. 3, and it can be seen from fig. 3 that the grain size variation ranges are: from-10 nm to-1.5 μm, with a maximum tungsten content of 6.67 wt.%.
The sectional hardness distribution of the nickel-tungsten alloy with the gradient structure is shown in FIG. 4, and the hardness is gradually increased from 2.6GPa to 5.5 GPa.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of a nickel-tungsten alloy with a gradient structure is characterized by comprising the following steps: adopting an electrochemical deposition technology, taking nickel as a consumable anode, and controlling the current density and the additive concentration in the electroplating solution to change along with time by using a computer to deposit and form the nickel-tungsten alloy with a gradient structure with chemical composition gradient and grain size gradient under the action of direct current; the additive comprises tungstate and saccharin sodium;
the current density is from 10 to 20mA/cm2Gradually increasing to 50-100mA/cm2；
Controlling the current density to be 10-20mA/cm2Keeping for 1-1.5h, and increasing the current density to 30mA/cm within 1.5-2h2Then increasing the current density to 50-55mA/cm at a constant speed within 1-1.2h2And then increasing the current density to 80-85mA/cm at a constant speed within 1.6-1.7h2Keeping the current density at 80-85mA/cm2Depositing for 0.5-0.6 h;
controlling the concentration of the saccharin sodium to gradually increase from 0.5-0.6g/L to 15-15.5g/L by using a computer;
controlling the concentration of the saccharin sodium to be constant at 0.5-0.6g/L within 1-1.5h after the beginning of electrochemical deposition by using a computer, then controlling the concentration of the saccharin sodium to be gradually increased to 5.0-5.5g/L within 1.5-2h, then keeping for 1-1.5h, and then gradually increasing the concentration of the saccharin sodium to be 15-15.5g/L within the subsequent 1.6-1.7 h;
the tungstate is sodium tungstate or ammonium tungstate; controlling the concentration of sodium tungstate to be gradually increased from 0-1g/L to 10-50g/L by using a computer;
the mass percentage range of the tungsten content in the nickel-tungsten alloy with the gradient structure is 1-20%;
the grain size of the nickel-tungsten alloy with the gradient structure is gradually increased from 10nm to 10 mu m.
2. The method according to claim 1, further comprising preparing a plating solution before performing the electrochemical deposition, such that the plating solution contains the following components: the concentration of the nickel sulfate hexahydrate is 50-300g/L, the concentration of the nickel chloride hexahydrate is 43-45g/L, the concentration of the boric acid is 40-42g/L, and the concentration of the sodium dodecyl sulfate is 0.05-0.5 g/L;
adjusting the pH of the plating solution to 3.5 +/-0.2;
the temperature of the plating solution is adjusted to be 55 +/-1 ℃.
3. The method of claim 2, further comprising pre-treating the substrate prior to plating;
the pretreatment comprises mechanical grinding and polishing and surface oil removal of a matrix;
the mechanical polishing is to polish the surface of the substrate by sequentially adopting 200#, 400# and 800# sandpaper;
the surface degreasing is to clean the surface of a matrix by using an organic solvent; the organic solvent is preferably acetone and ethanol.
4. A gradient structure nickel tungsten alloy prepared by the preparation method according to any one of claims 1 to 3.
5. A layered structure comprising a substrate and a coating layer made of the gradient structure nickel tungsten alloy according to claim 4, wherein the substrate is any one of pure copper, pure nickel, copper alloy, nickel alloy, aluminum alloy, carbon steel and alloy steel.
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| CN102321894A (en) * | 2011-09-19 | 2012-01-18 | 北京工业大学 | Method for preparing nickel-tungsten composite material with layered structure |
| CN104862748A (en) * | 2015-05-29 | 2015-08-26 | 中国科学院金属研究所 | Crystalline grain scale gradient metallic nickel and controllable preparation method thereof |
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| CN102321894A (en) * | 2011-09-19 | 2012-01-18 | 北京工业大学 | Method for preparing nickel-tungsten composite material with layered structure |
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