CN1834291A - Ni-CrN hard composite coating, its prepn. process and application - Google Patents
Ni-CrN hard composite coating, its prepn. process and application Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims description 62
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- 229910018487 Ni—Cr Inorganic materials 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims 1
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Abstract
This invention discloses the manufacture and application of Ni-CrN composite hard coating layer, which is composed of 70-90 wt.% of Ni matrix and 10-30 wt.% of CrN hard particles formed when Cr reacts with implanted N2. The coating layer is manufactured by: performing composite electroplating on metal or alloy matrix to obtain Ni-Cr composie coating layer, and performing nitrogen ion implantation to obtain Ni-CrN composite hard coating layer that has a strong adhesion to the coated matrix. The method has such advantages as simple and mature process, and high hardness of the coating layer.
Description
Technical field
The present invention relates to coat preparing technology, specifically a kind of Ni-CrN hard composite coating and preparation method and application.
Background technology
Ni base alloy is used under the hot environment usually, but their hardness and wear resistance all fail well to solve all the time.Nitride obtains widespread use owing to have higher hardness and wear resistance, and the method that obtains nitride at present mainly realizes by methods such as physical vapor deposition (for example magnetron sputtering), chemical vapour deposition, gas nitriding and ion nitridings.Advantages such as ion nitriding is owing to having technical maturity, and is with low cost, and nitriding temperature is low, the time is short are used widely.Consider that the affine of Ni and nitrogen can be very little, be difficult to, and Cr easily generates the CrN hard mutually with N chemical combination, can improve Ni base alloy rigidity directly with the Ni nitrogenize.But at present the problem that exists is: after the Ni base alloy that the method that adopts ion nitriding contains Cr to tradition carried out modification, the nitride layer that obtains was thin, is difficult to satisfy actual requirement.
Summary of the invention
At above-mentioned deficiency, the purpose of this invention is to provide a kind of Ni-CrN hard composite coating and preparation method and application.It passes through composite plating in advance, and the two-stage process of ionitriding is incorporated into CrN among the metal Ni then, thereby significantly improves its hardness and wear resistance.
Technical scheme of the present invention is as follows:
The Ni-CrN hard composite coating, its composition is by the nitrogen that infiltrates and the Cr reaction generates the CrN particle and composite deposite metal Ni forms; By mass percentage, CrN content is 10～30% in the coating, and all the other are Ni.
The preparation method of described Ni-CrN hard composite coating is to be base material with metal Ni or alloy material, at first, adopts routine techniques, realizes the coelectrodeposition of Ni and nanometer Cr powder, prepares nano-composite plate, i.e. the Ni-Cr nano-composite plate.The plating bath of composite plating is a citrate system, stirs up and down with 50～120rpm by porous plate in the coelectrodeposition process to make nanometer Cr particle suspension in plating bath, and uniform deposition is at specimen surface; Bath temperature is 25～35 ℃, and current density is 1～4A/dm
2, electroplating time is 1.5～2 hours, the Cr content in the coating is 10～30% mass percents.Secondly, NH is adopted in ionitriding
3Be nitriding atmosphere, pressure is 900～1100Pa in the stove, NH
3Flow is 400～600ml/min, 450 ℃～600 ℃ of temperature, and nitriding time is 7～20 hours.
The present invention is by the different Cr content of control, the coating structure difference that obtains; By mass percentage, when Cr content was 10%, the Ni-CrN hard composite coating that obtains (being called for short type i, down together) has following " bilayer structure ": outer for the CrN particle dispersion is distributed in the metallic matrix, internal layer was one deck successive CrN film; When Cr content is 30%, the Ni-CrN hard composite coating that obtains (being called for short Type II, down together) also is to have " bilayer structure ", but its result is just opposite with the type i situation, be that skin is one deck successive CrN film, internal layer is the double-layer structure of CrN particle dispersion in metallic matrix; When Cr content was between 10～30%, Ni-CrN hard composite coating structure and the Cr content that obtains was that 10% o'clock structure is identical, but the position of the continuous CrN film of one deck compare than 10%, more outer.
Ultimate principle of the present invention is as follows:
Because nitride has very high hardness, wear resistance, so can be used for strengthening Ni base hardness of alloy and wear resistance.The ultimate principle that forms CrN is as follows: the present invention at first makes the Ni-Cr nano-composite plate by the method for coelectrodeposition, nanometer Cr powder is dispersed in the nanometer Ni crystal grain uniformly, method by ion nitriding is diffused into nitrogen in the coating then, with wherein than the particle that is easier to nitrogenize--Cr powder reaction, generate CrN, and owing to Ni does not react with nitrogen under the condition of being controlled basically, so obtain the Ni-CrN hard coat.Because prepared Ni base composite cladding is a nanostructure, so nitrogen inwardly increases greatly along the velocity of diffusion of crystal boundary, has so also just overcome the very thin shortcoming of nitride layer; Again because the Cr powder is a nano particle, and activity is very high, can with the nitrogen rapid reaction, accelerate to form the speed of continuous CrN layer, improve hardness and wear resistance.
Advantage of the present invention is as follows:
1. nitride layer can be controlled.The present invention can pass through time, the temperature of control ion nitriding, and the nano composite plating layer thickness is controlled the degree of depth of nitride layer; Cr content by in the control composite deposite can obtain all different various coatings of hardness, structure.Two Cr content with the embodiment of the invention are example, type i is the outer CrN particle dispersion distribution that is, internal layer is the double-layer structure of continuous CrN layer, wherein outer field hardness is that (50g loads metal Ni, its Vickers' hardness is approximately 200Hv) 3～4 times, internal layer hardness ratio skin is significantly improved, and approximately 1200Hv (50 load) is more than 6 times of metal Ni hardness; The Type II skin is the continuous CrN film of the about 3～4um of one deck, internal layer is the double-layer structure of CrN hard point disperse discrete distribution, its mesectoderm hardness can reach 1500Hv (50g loading), and this hardness is more than 7 times of metal Ni, and internal layer hardness also can reach 900～1000Hv (50g loading).
2. technical maturity, cost is low.The present invention prepares the Ni-CrN hard composite coating by a kind of new " two step process ".Step 1-prepares the Ni-Cr nano-composite plate: utilize composite plating technology that certain amount of nano Cr particle is introduced in the Ni base coating, and for to make this coating have good nitriding, prepared Ni base composite cladding is a nanostructure; Step 2--ion nitriding: (＜600 ℃) at a certain temperature by ionitriding, make the nanometer Cr particle nitrogenize in the Ni-Cr nano-composite plate, thereby form the Ni-CrN rigid composite material.The present invention adopts ion nitriding method, and cost is lower, and is very low to the requirement of workpiece shape, therefore, is of wide application.
Description of drawings
Fig. 1-1 is the cross section pattern of Ni-Cr coating after rotten quarter in the prior art.
Fig. 1-2 is the TEM pattern of Ni-Cr coating in the prior art.
Fig. 2-1 is the surface topography of Ni-10Cr coating in the prior art.
Fig. 2-2 is the surface topography of Ni-30Cr coating in the prior art.
Fig. 3-1 is the surface topography of type i of the present invention.
Fig. 3-2 is the surface topography of Type II of the present invention.
Fig. 4 is the XRD result of type i of the present invention and two embodiment of Type II.
Fig. 5-1 is the cross section pattern of one embodiment of the invention type i.
Fig. 5-2 is the cross section pattern of one embodiment of the invention Type II.
Fig. 6-1 is that the face of the pairing N element of Fig. 5-1 distributes.
Fig. 6-2 is that the face of the pairing Cr element of Fig. 5-1 distributes.
Fig. 6-3 is that the face of the pairing Ni element of Fig. 5-1 distributes.
Fig. 6-4 is the pairing N of Fig. 5-1, Cr, the line sweep result of Ni.
Fig. 7-1 is that the face of the pairing N element of Fig. 5-2 distributes.
Fig. 7-2 is that the face of the pairing Cr element of Fig. 5-2 distributes.
Fig. 7-3 is that the face of the pairing Ni element of Fig. 5-2 distributes.
Fig. 7-4 is the pairing N of Fig. 5-2, Cr, the line sweep result of Ni.
Fig. 8 is type i and Type II changes in hardness curve on the different positions of cross section among the present invention.
Embodiment
Below in conjunction with drawings and Examples in detail the present invention is described in detail.
Embodiment
Present embodiment is with first Ni-Cr composite plating on Ni, and to prepare the Ni-CrN compound coating be example in ion nitriding then:
Its preparation method is: adopt conventional composite plating technology to prepare the Ni-Cr compound coating.Body material is metal_based materials such as Fe, Ni, Co, steel (carbon steel, low alloy steel, stainless steel), and other alloys.Plating bath is a citrate system.Present embodiment is selected Ni Citrate trianion plating bath for use, preparation Ni-Cr nano-composite coating, and the Ni-CrN compound coating is prepared in ion nitriding thereon then.Its flow process is as follows:
Substrate metal → surface finish to 800
#Waterproof abrasive paper → surperficial ultrasonic cleaning → in the nickel plating bath that contains nanometer Cr powder, carry out composite plating → acquisition Ni-Cr composite deposite → ion nitriding → acquisition Ni-CrN compound coating.
When being plating, key of the present invention keep the Cr particle suspension in tank liquor, control process parameters during nitriding.Present embodiment adopts traditional composite plating facility and ionitriding equipment to prepare.Specific as follows:
1) getting pure Ni is base material, is processed into the sample of 15 * 10 * 2mm size, is milled to 800 through silicon carbide paper
#Sand paper, ultrasonic cleaning in acetone;
2) the Cr powder of selecting for use is a nano-scale, 20～100 nanometers.Particle is immersed in the bath soln earlier, so that particles dispersed is avoided reuniting;
3) electroplate liquid adopts Ni Citrate trianion plating bath, and composition is as follows: 150g/l NiSO
47H
2O, 12g/l NaCl, 35g/l H
3BO
3, the 180g/l Trisodium Citrate; The solution of configuration was placed 24 hours through fully stirring after-filtration; The pH value of solution value can be used in 5.4～5.6 scopes;
4) electrodeposition process adopts plate pump formula device to stir plating bath, is suspended in the plating bath to guarantee plating bath middle-weight rare earths oxide particle, and uniform deposition is at specimen surface; Bath temperature is 30 ℃, and current density is 3A/dm
2, stirring velocity is 75rpm.Electroplating time is 1.5 hours, and the sample mean thickness of coating is 50 μ m, and the Cr compounding quantity is 10～30% mass percents;
5) ionitriding then.Nitriding gas adopts NH
3Be nitriding atmosphere, pressure is 900～1100Pa in the stove, NH
3Flow is 400～600ml/min, 560 ℃ of temperature, and nitriding time is 10 hours.
Be the result of type i of the present invention and two embodiment of Type II below:
1) Ni-Cr nano-composite plate structure
Fig. 1-the 1st, the cross section pattern of Ni-Cr nano-composite plate can see that particle is evenly distributed in the Ni base after corruption is carved.The crystal grain plating of Ni base detects through XRD, and calculates average out to 30nm according to the Scherrer formula.Fig. 1-2 is the TEM pattern of Ni-Cr nano-composite plate, and as can be seen, equally distributed nanometer Cr particle is circular, the maximum about 100nm of particle, minimum about 20nm, and the median size size is approximately 40nm.
2) tissue of coating and constitutional features
The coating surface morphology of Ni-10Cr and Ni-30Cr such as Fig. 2-1 and 2-2.Because the difference of Cr content, both surface topographies are different: the Ni-10Cr surface ratio is more smooth, and by contrast, there are many little thrusts on the Ni-30Cr surface.Surface topography after the process ion nitriding is respectively as Fig. 3-1 and 3-2.As can be seen, sample surfaces becomes more coarse after the nitrogenize, and this is the generation owing to CrN, what volumetric expansion caused.Its surperficial X light analysis result such as Fig. 4, (a) and (b) are respectively the results of type i and Type II coating.As seen for the type i coating, three apparent in view CrN peaks are arranged, but because the restriction of Cr content, the CrN peak is more weak; And Type II coating situation is obviously different, except three three weak peaks the same with type i occurring, apparent in view (a 200) CrN peak occurred near matrix (111) peak.Because the CrN peak is more intense, (111) of matrix, (200) and (220) peak-to-peak signal have obviously been suppressed.
The cross section pattern of the Ni-CrN compound coating that obtains shown in Fig. 5-1 and 5-2, its N, Cr, the distribution of Ni element is respectively shown in Fig. 6-1～6-3 and 7-1～7-3.As can be seen, through 560 ℃, after 10 hours the ion nitriding, the nitriding coat-thickness of two kinds of different Cr content is all greatly about about 50um, thickness and Cr relation with contents that nitrided case is described are little, only relevant with the grain-size size of Ni, both Ni crystal particle scales are approximate, so also basically identical of the nitride layer thickness that obtains.Through after the nitrogenize, different is the nitride layer structure difference that obtains.(Cr content is 10%, and by mass percentage) the Ni-CrN hard composite coating has following " bilayer structure ": outer for the CrN particle dispersion is distributed in the metallic matrix, internal layer is one deck successive CrN film to type i; Type II (Cr content is 30%) Ni-CrN hard composite coating also is to have " bilayer structure ", but its result is just opposite with type i, and promptly skin is one deck successive CrN film, and internal layer is the double-layer structure of CrN particle dispersion in metallic matrix.The difference of this explanation Cr content has influenced the structure of nitride layer.Fig. 6-4 and 7-4 are respectively the N of type i and Type II, and Cr, three kinds of elements of Ni be at coating center line scanning result, and as can be seen, in coating, the content of N is to be consistent with the content of Cr.
Experiment of hardness:
Adopt SHIMADZU microhardness machine, each different positions carries out the microhardness experiment in the cross section.Experiment load is chosen 50g deadweight counterweight, and the loading time is 10 seconds.Each specimen surface keeps at a certain distance away and measures 4 points, gets its mean value, obtains comparative microhardness experimental result, as shown in Figure 8.For a well contrast is arranged, before carrying out nitriding treatment, the microhardness of Ni-Cr nano-composite plate to be measured, its Vickers' hardness is approximately 240Hv.Experimental result from Fig. 8 as can be seen, the top layer of Type II coating is because what generate is successive CrN film, so hardness is the highest, greatly about 1500Hv, what generate below this film is that the CrN particle dispersion is distributed in the structure in the Ni matrix, hardness descends to some extent, and how much directly related hardness value is with the distribution of CrN content, greatly between 900Hv～1200Hv.For type i, though its skin and Type II endothecium structure all are that the CrN particle dispersion is distributed in the Ni matrix, but because the difference of CrN content, some reduction of hardness, greatly between 600Hv～700Hv, and internal layer hardness is owing to there is the generation of continuous CrN, and hardness value greatly improves, greatly about about 1200Hv.
By top result as can be seen, the hardness of rigid composite coating of the present invention obtains greatly to improve.Since the nitrogenize bed thickness that obtains, and can form one deck successive CrN film, can greatly improve the hardness and the wear resistance of coating like this.Its mechanism mainly is that the Ni crystal grain by control Ni-Cr nano-deposit is nanocrystalline, and the Cr particle that adds is that nanoparticle is realized.For Ni-30Cr nano-composite plate among the present invention, in nitridation process, because the Cr particle is a nanoparticle, active high, so can be rapidly and the N atomic reaction, generate the CrN particle, but form one deck successive CrN film if desired, need enough Cr content, generally in common coarse-grain Ni-Cr alloy, to reach 40% at least, and coating Cr content of the present invention has only 30%, and this just needs enough Cr and is diffused into the surface from below, contains quantity not sufficient to remedy top layer Cr, because the Ni crystal grain among the present invention is nanocrystalline, provide a large amount of passages to external diffusion so for Cr, improved the speed of Cr greatly, make N to external diffusion
ND
N＜＜N
CrD
Cr, like this, the very fast formation one deck of skin CrN film.For Ni-10Cr nano-composite plate among the present invention, in nitridation process, though the Cr particle is similarly nanoparticle, but because content is low excessively, just form continuous CrN film so be difficult in the initial stage, the N atom can be by nanometer Ni crystal boundary rapid permeability in matrix, generate the CrN particle with the Cr particle, but carrying out along with nitridation process, N slows down gradually to the speed of internal diffusion, increase with the time of the Cr particle reaction that runs into, meanwhile a large amount of Cr make and satisfy N in the inner somewhere of coating to external diffusion
ND
N＜＜N
CrD
Cr, generate successive CrN layer at internal layer at last.When Cr content circle is between 10% and 30%, owing to do not reach the critical content that forms outer CrN, so that the coating structure that obtains and Cr content are 10% o'clock structure is identical, still owing to Cr content＞10%, generate continuous CrN film and speed up, so its position is more outer.
Ni-CrN hard composite coating of the present invention can be used as hard, wear-resistant coating, is used for the relatively poor metal_based material of wear resistance.And this coating is expected to be used as on the working part of related industrieies such as petrochemical complex, machinofacture.
Claims (9)
1, a kind of Ni-CrN hard composite coating is characterized in that: its composition is by the nitrogen that infiltrates and the Cr reaction generates the CrN hard particles and composite deposite metal Ni forms; By mass percentage, CrN content is 10～30% in the coating, and all the other are Ni.
2, by the described Ni-CrN hard composite coating of claim 1, it is characterized in that: control different Cr content, the coating structure difference that obtains; By mass percentage, when Cr content was 10%, the Ni-CrN hard composite coating that obtains had following " bilayer structure ": outer for the CrN particle dispersion is distributed in the metallic matrix, internal layer is one deck successive CrN film; When Cr content was 30%, the Ni-CrN hard composite coating that obtains also was to have " bilayer structure ", and skin is one deck successive CrN film, and internal layer is the double-layer structure of CrN particle dispersion in metallic matrix; When Cr content was between 10～30%, Ni-CrN hard composite coating structure and the Cr content that obtains was that 10% o'clock structure is identical.
3, a kind of preparation method of Ni-CrN hard composite coating is characterized in that the preparation of coating is divided into latter two flow process earlier: be base material with the metal 1), pass through to add nanometer Cr powder with the method for coelectrodeposition in advance on base material, preparation Ni-Cr nano-composite plate; 2) with method nitriding on the Ni-Cr nano-composite plate of ionitriding, make the Ni-CrN hard composite coating.
4, according to the preparation method of the described Ni-CrN hard composite coating of claim 3, it is characterized in that: wherein flow process 1) the Ni-Cr nano-composite plate in, by mass percentage, Cr is 10～30%, all the other are Ni.
5, according to the preparation method of the described Ni-CrN hard composite coating of claim 3, it is characterized in that: make nanometer Cr particle suspension in plating bath by stirring in the electrodeposition process, uniform deposition is at specimen surface; Bath temperature is 25～35 ℃, and current density is 1～4A/dm
2, electroplating time is 1.5～4 hours.
6, according to the preparation method of the described Ni-CrN hard composite coating of claim 3, it is characterized in that: wherein flow process 2) after nitriding on the Ni-Cr nano-composite plate, obtain the Ni-CrN hard composite coating, by mass percentage, wherein CrN content 10～30%.
7, according to the preparation method of claim 3 or 6 described Ni-CrN hard composite coatings, it is characterized in that:, adopt NH by the method for ion nitriding
3Be nitriding atmosphere, pressure is 900～1100Pa in the stove, NH
3Flow is 400～600ml/min, 450 ℃～600 ℃ of temperature, 7～20 hours time.
8, according to the preparation method of the described Ni-CrN hard composite coating of claim 3, it is characterized in that: metal base comprises Fe, Ni, Co, and carbon steel, low alloy steel, stainless steel, and other alloys.
9, a kind of application of Ni-CrN hard composite coating is characterized in that: described Ni-CrN hard composite coating is as carbon steel, low alloy steel or stainless hard, wear-resistant coating.
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|---|---|---|---|---|
| CN1010148B (en) * | 1987-09-22 | 1990-10-24 | 斯奎尔·D·强电股份有限公司 | Contactor |
| US5445683A (en) * | 1992-05-13 | 1995-08-29 | Daidousanso Co., Ltd. | Nickel alloy products with their surfaces nitrided and hardened |
-
2005
- 2005-03-15 CN CNB2005100460241A patent/CN100406615C/en not_active Expired - Fee Related
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| CN101625056B (en) * | 2008-07-11 | 2011-07-20 | 中国科学院金属研究所 | Double-ferrule type pipe joint of double-sealing and double-fastening support and using method thereof |
| TWI400357B (en) * | 2010-05-05 | 2013-07-01 | Hon Hai Prec Ind Co Ltd | Surface hardening substrate and method making the same |
| CN111826654A (en) * | 2020-07-06 | 2020-10-27 | 安徽省赛威输送设备有限公司 | Processing method for improving corrosion resistance of elevator shell |
| CN113328111A (en) * | 2021-05-25 | 2021-08-31 | 上海电力大学 | Stainless steel bipolar plate with chromium-based nitride composite coating and preparation method thereof |
| CN113319654A (en) * | 2021-05-31 | 2021-08-31 | 江苏鑫泽不锈钢制品有限公司 | Grinding process for stainless steel workpiece with honeycomb structure |
| CN117144447A (en) * | 2023-10-30 | 2023-12-01 | 北矿新材科技有限公司 | High-temperature-resistant active cutting coating and preparation method thereof |
| CN117144447B (en) * | 2023-10-30 | 2024-02-02 | 北矿新材科技有限公司 | High-temperature-resistant active cutting coating and preparation method thereof |
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