CN102677099A - Ni-w gradient material and preparation method thereof - Google Patents
Ni-w gradient material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000000034 method Methods 0.000 claims abstract description 32
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 23
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010937 tungsten Substances 0.000 claims abstract description 14
- 238000009826 distribution Methods 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 13
- 238000007254 oxidation reaction Methods 0.000 abstract description 13
- 238000009792 diffusion process Methods 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 8
- 238000004070 electrodeposition Methods 0.000 abstract description 6
- 230000005684 electric field Effects 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 229910001080 W alloy Inorganic materials 0.000 description 19
- 239000000956 alloy Substances 0.000 description 16
- 229910045601 alloy Inorganic materials 0.000 description 12
- 238000005245 sintering Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012611 container material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
The invention discloses a Ni-W gradient material and a preparation method thereof. A nickel layer is arranged at the middle of the Ni-W gradient material and tungsten layers are arranged at two sides of the Ni-W gradient material; gradient distribution layers are arranged between the nickel layer and the tungsten layers; and in the gradient distribution layers, the content of nickel reduces in a gradient way while the content of tungsten increases in a gradient way towards the tungsten layers. Different parts of the material are compactly combined, the surface structure of the material is compact and smooth, and the material has good abrasive resistance, corrosion resistance, acid resistance and high temperature oxidation resistance. When the material is disposed in air with temperature of 500-1300 DEG C, a stable WO3 protective film can be quickly formed on the surface of the material to effectively protect the base body of the material against oxidation, so the material has the characteristic that the surface of the material has strong oxidation resistance. In the preparation method disclosed by the invention, according to the properties of the conventional Ni-W gradient material and the basic theory of diffusion, electro-deposition of the W and the counterdiffusion of the Ni and the W under the action of an electric field are carried out at the same time so as to increase the thicknesses of the gradient layers. The preparation method has the characteristics that the forming speed of the gradient layers is fast, the time to prepare a thicker gradient layer is short, and the process is easy to control and is simple.
Description
Technical field
The present invention relates to a kind of gradient material and preparation method thereof, especially a kind of Ni-W gradient material and preparation method thereof.
Background technology
The Ni-W gradient material has good wear-resisting, anti-corrosion, acidproof and high temperature oxidation resistance, is widely used in the surface strengthening with screw rod etc. of casting mould, hot forged mould, bearing, injection moulding, also can be used as heat sink material and uses.
The preparation research of Ni-W gradient material does not still have report at present both at home and abroad, but domestic aspect the preparation of Ni-W alloy material less report is arranged.At present, the preparation method of Ni-W alloy material mainly contains electrodip process, vaccum sintering process and vacuum melting method both at home and abroad.
The apply pulse electro-deposition techniques can weaken evolving hydrogen reaction, helps elimination of hydrogen embrittlement, spot corrosion, reduction stress, and can improve current efficiency effectively." Southern Yangtze University's journal (natural science edition) " 03 phase in 2006 has been reported the friction and wear behavior of pulse electrodeposition Ni-W alloy layer, and it utilizes the pulse electrodeposition mode to prepare the Ni-W alloy layer at 45 steel.Research shows that the wear resistance at elevated temperature of alloy layer obviously is superior to 45 steel.Reason is, the adding refinement of W crystal grain, improved the microhardness of alloy layer, played the effect of solution strengthening and grain-boundary strengthening.Simultaneously,, stoped the moulding distortion and heat adhesion that cause by high temperature oxidation, improved the wear resisting property of coating because W has high heat conductance, high temperature red hardness and characteristics such as anti-oxidant.But; Adopt in the Ni-W alloy layer of this method preparation; W content content is lower, generally remains on below the 60wt%, can not prepare alloy surface and have high W content; W, Ni content demonstrate the gradient layer of graded in the alloy, have influenced the comprehensive mechanical property and the high-temperature oxidation resistance of coating to a certain extent.
One Chinese patent application numbers 201110273196.8 discloses and has a kind ofly prepared the method for Ni-W alloy with vacuum sintering, and it utilizes the method for vacuum sintering successfully to prepare the Ni-W alloy.This method is not less than 99% Ni powder and purity with purity and is not less than 99% W powder, under the condition of different time and different ball milling ratios, is carrying out ball milling through two kinds of powder of Different Weight proportioning; Suppress then, the technology pressed compact being carried out vacuum sintering and furnace cooling is machined to finished product with the Ni-W alloy at last and gets final product.Adopting this method to prepare the Ni-W alloy, to have technology simple, and production cost is low, can prepare comparatively fine and close Ni-W alloy.But in the Ni-W alloy of this method preparation, W content is relatively low, generally between 25～30%wt, if further improve the W content in the alloy, will influence the density of alloy, reduces the mechanical property and the high-temperature oxidation resistance of alloy.Simultaneously, this employing method can not prepare the material that Ni, W content have graded.
In addition; One Chinese patent application numbers 201110280220.0 discloses a kind of method of smelting method for preparing Ni-W alloy; It prepares at vaccum sintering process on the basis of Ni-W alloy, and the Ni-W alloy behind the sintering is put into high temperature melting furnace, earlier to vacuumizing in the stove; In stove, pour protective gas then and heat melting, carry out machining at last and be prepared into Ni-W target finished product.To prepare the Ni-W alloy as broad as long with vaccum sintering process in essence for the Ni-W alloy that adopts the preparation of this melting method; Just improved smelting temperature; Improved the density of Ni-W alloy to a certain extent; Reduced component segregation, the mechanical property and the high-temperature oxidation resistance of alloy material increased.But, adopt this method to handle after, still can not prepare alloy surface and have high W content, the material that Ni, W content have graded in the alloy.
Top analysis revealed; Still there is not Ni-W gradient material and preparation method thereof at present, even on preparing the Ni-W alloy material of materials similar therewith, have following deficiency: can not prepare the gradient material that alloy surface has high W content in (1) preparation process yet.(2) if the too high composition that improves W in the Ni-W alloy will reduce the density of alloy, reduce wear-resisting, anti-corrosion, the acidproof and high temperature oxidation resistance of alloy.(3) can not prepare and both had well wear-resisting, anti-corrosion, acidproof and resistance to high temperature oxidation, have the material that Ni, W concentration gradients change again.
Summary of the invention
The technical problem that the present invention will solve provides a kind of Ni-W gradient material with graded layer; The present invention also provides the preparation method of this Ni-W gradient material.
For solving the problems of the technologies described above, the technical scheme that the present invention taked is: be nickel dam wherein, both sides are tungsten layer; The Gradient distribution layer is arranged between said nickel dam and the tungsten layer, and said Gradient distribution course tungsten layer direction nickel concentration gradients reduces, the W content gradient raises.
The thickness of Gradient distribution layer according to the invention is 110 μ m～360 μ m.
Preparing method of the present invention is at NaCl-KCl-NaF-WO
3In the molten salt system, be negative electrode with metal Ni, metal W is an anode, galvanic deposit under the effect of dc pulse current, and described Ni negative electrode can be deposited as the Ni-W gradient material.
The described fused salt of the inventive method disposes by following x: NaCl 0.25～0.36, KCl 0.25～0.36, NaF 0.17～0.3, WO
30.1～0.20.
The process step of the inventive method is: NaCl, KCl, NaF and WO will be equipped with in (1)
3The crystal vessel of miscellany is heated to 700 ℃～900 ℃, and insulation makes fused salt reach stable;
(2) negative electrode Ni plate and anode W plate are inserted in the fused salt simultaneously, then at current density 50mAcm
-2～100mAcm
-2Condition under galvanic deposit 20min～40min;
(3) the negative electrode Ni plate after galvanic deposit finishes is removed the fused salt dirt settling, uses ultrasonic cleaning again, can obtain the Ni-W gradient material.
In the said step of the inventive method (1), be incubated 120min so that fused salt reaches stable at 700 ℃～900 ℃.
In the said described step of the inventive method (3), the negative electrode Ni plate after galvanic deposit finishes boils 10～30min to remove the fused salt dirt settling in boiling water.
Adopt the beneficial effect that technique scheme produced to be: to the invention solves the deficiency of still not having Ni-W gradient material and preparation method at present.
Material each several part of the present invention combines closely, and material surface compact structure, smooth has good wear-resisting, anti-corrosion, acidproof and high temperature oxidation resistance; This material in 500 ℃～1300 ℃ air, the stable WO of formation that the surface can be very fast
3Protective membrane protects matrix not oxidized effectively, has the strong characteristics of surface oxidation-resistant property.
The inventive method is to the characteristic of existing Ni-W gradient material; According to the diffusion basic theories; Adopt galvanic deposit W and under effect of electric field Ni, W mutual diffusion (electric field can quicken the diffusion of solid metal; The multielement diffusion time also can improve the other side's velocity of diffusion each other in the solid-state diffusion) method of carrying out simultaneously, the thickening of accelerating gradient layer.Characteristics such as present method has gradient layer, and to form the gradient layer required time that speed is fast, preparation is thicker short, and control easily, technology are simple.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Fig. 1, Fig. 2, Fig. 3 are respectively tungsten, the nickel distribution plans of gradient layer in the embodiment 1-3 gradient material.
Embodiment
The preparation method of this Ni-W gradient material is with NaCl-KCl-KF-WO
3Fused salt is an ionogen, is negative electrode with metal Ni, and metal W is an anode, and under the effect of dc pulse current, through the related parameter that has of control electrodeposition process, galvanic deposit W and Ni, W ooze mutually simultaneously and carry out on the Ni matrix, finally form the Ni-W gradient material.Contain NaCl-KCl-KF-WO
3The container material of fused salt is a high purity graphite, 700 ℃～900 ℃ of temperature, electrodeposition time 20min～40min, current density 50mAcm
-2～100mAcm
-2, obtaining the material both side surface is metal W, the middle layer is metal Ni, is the Ni-W gradient material layer to W direction Ni content reduces gradually, W content raises gradually between W layer and the Ni layer.Present method principle of work is following: because the mutual diffusion of electric field, W concentration gradient and Ni, W improves the effect of velocity of diffusion; W passes through physical diffusion in negative electrode Ni matrix; Thereby form the phase change rule fast is the gradient material of W
Ni
W
Ni
W
Ni
W structure; The formation time of gradient layer, the speed that thickens of accelerating gradient layer have been shortened in three kinds of measures of quickening to spread.Through check, this gradient material has good wear-resisting, anti-corrosion, acidproof and high temperature oxidation resistance, surperficial W in 500 ℃～1300 ℃ air, the fine and close smooth WO of formation that can be very fast
3Protective membrane, its reason is following: concerning the Ni-W gradient material, the pure W part of its material has wear-resisting, anti-corrosion, acidproof and high temperature oxidation resistance, in middle high temperature atmosphere environment, can form fine and close relatively WO
3Protective membrane has improved the oxidation-resistance of material, and prolong the work-ing life of material.
Embodiment 1: this Ni-W gradient material adopts following prepared to form.
By mole mark 0.25mol NaCl, 0.25mol KCl, 0.3mol NaF, 0.2mol WO
3Ratio preparation fused salt, above-mentioned fused salt is contained into carbon crucible, put into electric furnace and be warming up to 700 ℃, constant temperature 120min; Put into fused NaCl-KCl-KF-WO to the cathode nickel plate
3In the fused salt, apply dc pulse current, current density is 50mAcm
-2The time, behind the galvanic deposit 20min, from fusion NaCl-KCl-KF-WO
3Take out cathode material in the fused salt, put into boiling water and boil 10min, make no tangible fused salt dirt settling on the nickel board substrate, use the ultrasonic cleaning sample again.Coating surface morphology, section thickness and tungsten, nickel content distribution, surperficial X-ray diffraction analysis result are shown that the specimen surface densification that obtains is smooth; Shown in Figure 1, with the GDA750 glow discharge spectrometry material analysis is shown: the material both side surface is metal W, and the middle layer is metal Ni, is along the gradient layer that W direction Ni content reduces gradually, W content raises gradually in the middle of W, the Ni layer, the about 110 μ m of gradient layer thickness.
Embodiment 2: this Ni-W gradient material adopts following prepared to form.
By mole mark 0.3mol NaCl, 0.3mol KCl, 0.25mol NaF, 0.15mol WO
3Ratio preparation fused salt, above-mentioned fused salt is contained into carbon crucible, put into electric furnace and be warming up to 800 ℃, constant temperature 120min; Put into fused NaCl-KCl-KF-WO to the cathode nickel plate
3In the fused salt, apply dc pulse current, current density is 75mAcm
-2The time, behind the galvanic deposit 30min, from fusion NaCl-KCl-KF-WO
3Take out cathode material in the fused salt, put into boiling water and boil 20min, make no tangible fused salt dirt settling on the nickel board substrate, use the ultrasonic cleaning sample again.Coating surface morphology, section thickness and tungsten, nickel content distribution, surperficial X-ray diffraction analysis result are shown that the specimen surface densification that obtains is smooth; Shown in Figure 2, with the GDA750 glow discharge spectrometry material analysis is shown: the material both side surface is metal W, and the middle layer is metal Ni, is along the gradient layer that W direction Ni content reduces gradually, W content raises gradually in the middle of W, the Ni layer, the about 230 μ m of gradient layer thickness.
Embodiment 3: this Ni-W gradient material adopts following prepared to form.
By mole mark 0.36 NaCl, 0.36mol KCl, 0.17mol NaF, 0.1mol WO
3Ratio preparation fused salt, above-mentioned fused salt is contained into carbon crucible, put into electric furnace and be warming up to 900 ℃, constant temperature 120min; Put into fused NaCl-KCl-KF-WO to the cathode nickel plate
3In the fused salt, apply dc pulse current, current density is 100mAcm
-2The time, behind the galvanic deposit 40min, from fusion NaCl-KCl-KF-WO
3Take out cathode material in the fused salt, put into boiling water and boil about 30min, make no tangible fused salt dirt settling on the nickel board substrate, use the ultrasonic cleaning sample again.Coating surface morphology, section thickness and tungsten, nickel content distribution, surperficial X-ray diffraction analysis result are shown that the specimen surface densification that obtains is smooth; Shown in Figure 3, with the GDA750 glow discharge spectrometry material analysis is shown: the material both side surface is metal W, and the middle layer is metal Ni, is along the gradient layer that W direction Ni content reduces gradually, W content raises gradually in the middle of W, the Ni layer, the about 360 μ m of gradient layer thickness.
Claims (7)
1. Ni-W gradient material is characterized in that: be nickel dam wherein, both sides are tungsten layer; The Gradient distribution layer is arranged between said nickel dam and the tungsten layer, and said Gradient distribution course tungsten layer direction nickel concentration gradients reduces, the W content gradient raises.
2. Ni-W gradient material according to claim 1 is characterized in that: the thickness of said Gradient distribution layer is 110 μ m～360 μ m.
3. the preparation method of claim 1 or 2 said Ni-W gradient materials, it is characterized in that: it is at NaCl-KCl-NaF-WO
3In the molten salt system, be negative electrode with metal Ni, metal W is an anode, galvanic deposit under the effect of dc pulse current, and described Ni negative electrode can be deposited as the Ni-W gradient material.
4. the preparation method of Ni-W gradient material according to claim 3 is characterized in that: described fused salt disposes by following x: NaCl 0.25～0.36, KCl 0.25～0.36, NaF 0.17～0.3, WO
30.1～0.20.
5. according to the preparation method of claim 3 or 4 described Ni-W gradient materials, it is characterized in that the process step of this method is: NaCl, KCl, NaF and WO will be equipped with in (1)
3The crystal vessel of miscellany is heated to 700 ℃～900 ℃, and insulation makes fused salt reach stable;
(2) negative electrode Ni plate and anode W plate are inserted in the fused salt simultaneously, then at current density 50mAcm
-2～100mAcm
-2Condition under galvanic deposit 20min～40min;
(3) the negative electrode Ni plate after galvanic deposit finishes is removed the fused salt dirt settling, uses ultrasonic cleaning again, can obtain the Ni-W gradient material.
6. the preparation method of Ni-W gradient material according to claim 5 is characterized in that: in the said step (1), be incubated 120min so that fused salt reaches stable at 700 ℃～900 ℃.
7. the preparation method of Ni-W gradient material according to claim 5 is characterized in that: in the said described step (3), the negative electrode Ni plate after galvanic deposit finishes boils 10～30min to remove the fused salt dirt settling in boiling water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719846A (en) * | 2011-03-31 | 2012-10-10 | 北京化工大学 | Alkaline water electrolysis Ni-based three-dimensional network gradient alloy hydrogen evolution cathode |
| CN105177633A (en) * | 2015-09-09 | 2015-12-23 | 华北理工大学 | W-Ni-Cu gradient material and preparation method thereof |
| CN113897642A (en) * | 2021-09-29 | 2022-01-07 | 内蒙金属材料研究所 | Tungsten cathode for molten salt electrolysis, preparation method thereof and application of laser cladding technology |
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| US20040195296A1 (en) * | 2003-04-02 | 2004-10-07 | Bertram Schedler | Composite component for fusion reactors |
| EP1644549A2 (en) * | 2003-05-20 | 2006-04-12 | ExxonMobil Research and Engineering Company | Composition gradient cermets and reactive heat treatment process for preparing same |
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2012
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| CN1451505A (en) * | 2002-04-16 | 2003-10-29 | 西北有色金属研究院 | Carbon based composite material and titanium alloy soldering method |
| US20040195296A1 (en) * | 2003-04-02 | 2004-10-07 | Bertram Schedler | Composite component for fusion reactors |
| EP1644549A2 (en) * | 2003-05-20 | 2006-04-12 | ExxonMobil Research and Engineering Company | Composition gradient cermets and reactive heat treatment process for preparing same |
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| 姚素薇等: "电沉积Ni-W纳米梯度镀层", 《天津大学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719846A (en) * | 2011-03-31 | 2012-10-10 | 北京化工大学 | Alkaline water electrolysis Ni-based three-dimensional network gradient alloy hydrogen evolution cathode |
| CN105177633A (en) * | 2015-09-09 | 2015-12-23 | 华北理工大学 | W-Ni-Cu gradient material and preparation method thereof |
| CN113897642A (en) * | 2021-09-29 | 2022-01-07 | 内蒙金属材料研究所 | Tungsten cathode for molten salt electrolysis, preparation method thereof and application of laser cladding technology |
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Application publication date: 20120919 |