CN105714339B - Zr doping Ni Al bonding layer materials with Ni Zr diffusion barrier layers and preparation method thereof - Google Patents
Zr doping Ni Al bonding layer materials with Ni Zr diffusion barrier layers and preparation method thereof Download PDFInfo
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- CN105714339B CN105714339B CN201610202735.1A CN201610202735A CN105714339B CN 105714339 B CN105714339 B CN 105714339B CN 201610202735 A CN201610202735 A CN 201610202735A CN 105714339 B CN105714339 B CN 105714339B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
- C23C10/48—Aluminising
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
- C25D5/40—Nickel; Chromium
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Abstract
The present invention relates to doping Ni Al bonding layer materials of the Zr with Ni Zr diffusion barrier layers and preparation method thereof, this method is to be combined galvanoplastic with the method for pack cementation aluminizing, the different nickel aluminum metal tack coat of Zr contents is prepared, it is main to include surface treatment, prepare the steps such as electroplating solution, coating Ni Zr coating and pack cementation aluminizing.Compared with prior art, cost of the present invention is low and process conditions are simple, due to during aluminising, there is the presence of one layer of unreacted Ni Zr barrier layer, so that the nickel aluminium tack coat for the Zr doping being prepared is not influenceed by substrate composition, and by the addition of Zr metal powders in electroplating process and the mixing speed in electroplating process, the content and distribution that can make the Zr in Zr doping Ni Al tack coats are controlled.
Description
Technical field
The invention belongs to Thermal Barrier Coating Technologies field, is related to a kind of Zr doping nickel aluminium with Ni-Zr diffusion barrier layers and glues
Tie layer material and preparation method thereof.
Background technology
Doping Pt β-NiAl and γ/γ ' coating obtains as the tack coat of thermal barrier coating in civilian and military domain
It is widely applied, such as aviation and rocket engine, the nickel-base alloy high-temperature component such as blade of ships engine.So
And during the military service of blade, fold, creep can be produced by adulterating Pt β-NiAl tack coats so that oxide layer with
The interface of tack coat cracks, and the extension of crackle can further result in the failure that comes off of coating with merging；Doping Pt γ/
For γ ' although fold, creep will not be produced, its aluminum content is low, the brittlement phases such as spinelle can be produced in oxidizing process, no
The growth rate of oxide layer is only accelerated, while also reduces boundary strength.Answered in addition, cost high Pt also limit it
With.Therefore, domestic and international researchers attempt to develop a kind of new tack coat, and and can makes its performance not low while cost is reduced
In the tack coat of existing Pt doping.
Research finds that some active elements are expected to substitute Pt to be doped in the tack coat of thermal barrier coating.Include active element
The preparation method of nickel aluminium tack coat typically have pack cementation method, chemical vapour deposition technique, magnetron sputtering method and electron-beam qi-regulating
Phase sedimentation etc..Wherein, chemical vapour deposition technique, magnetron sputtering method and electro beam physics vapour deposition method need to use special
Equipment, and these equipment prices are expensive.By contrast, pack cementation method cost is low, simple to operate, can carry out large-batch industrial
Production, thus be widely accepted.But because pack cementation method is by diffuseing to form coating, so the alloying element in matrix
It can be diffused into coating preparation process in coating, the presence of these alloying elements can be disturbed grinds to active element Influencing Mechanism
Study carefully.In addition, the solubility limit of active element all very littles (typically in 0.05at.%), on the one hand cause active element in tack coat
In content and distribution be difficult control, on the other hand after active element content exceedes solubility limit, substantial amounts of inside can be produced
Oxidation, has a negative impact to the performance of coating.
Application publication number is that the A of CN 101914774 Chinese invention patent discloses one kind with the expansion of Re-Ni-Cr alloys
Dissipate bonding layer material of barrier layer and preparation method thereof.Re-Ni-Cr alloy diffusion barrier layer is applied and is plated on matrix material, matrix
Material is Ni, Al, Ti, Fe or Nb base alloy material, the mass percent group of each element in Re-Cr-Ni alloy diffusion barrier layers
As 20-65% Re, 30-50% Cr and 5-30% Ni.Its preparation method is i.e. by electric plating method in matrix high temperature
The material of Re-Cr-Ni alloy diffusion barrier layers is formed on superalloy.In the technical scheme of above-mentioned patent disclosure, there is Re-Ni-
The bonding layer material overlay coating of Cr alloy diffusion barrier layers is smooth, is evenly distributed, and can keep stable in the case of a high temperature, can
Oxygen of the alloying element into external diffusion, air is prevented in matrix to alloy substrate diffusion inside.However, the bonding layer material composition
Complexity, and Re is rare metal, the content in the earth's crust is few, in addition, the preparation process of the bonding layer material is relatively complicated, no
Beneficial to further industrialized production.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind can effectively control Zr
Content and distribution in tack coat and prepare Zr doping nickel aluminium bonding layer materials simply with Ni-Zr diffusion barrier layers and
Its preparation method.
The purpose of the present invention can be achieved through the following technical solutions：
With Ni-Zr diffusion barrier layers Zr doping Ni-Al bonding layer materials preparation method, this method specifically include with
Lower step：
(1) it is surface-treated：
(1-1) by Wire EDM by nickel-base alloy cut into length be 25-35mm, width 15-25mm, height
For 2-4mm nickel-base alloy sheet metal；
(1-2) by Wire EDM by the nickel plate of purity >=99% cut into length be 25-35mm, width 15-
25mm, it is highly 2-4mm nickel plate sheet metal；
(1-3) cleaning nickel-base alloy sheet metal, nickel plate sheet metal, polishing derusting, then clean except degreasing；
(1-4) carries out electrolytic anode activation process using acid solution to nickel-base alloy sheet metal at room temperature, then uses
Clear water cleaning is flowed, is cleaned by ultrasonic in deionized water, drying is stand-by；
(2) electroplating solution is prepared；
(3) coating Ni-Zr coating：
Using nickel plate sheet metal as anode, nickel-base alloy sheet metal is negative electrode, and nickel plate sheet metal, nickel-base alloy sheet metal are put
In the electroplating solution of step (2), at 50-60 DEG C, electroplated while stirring, Ni-Zr needed for the basis of time of plating is plated
Depending on the thickness of layer, after end to be electroplated, cleaning, drying is stand-by, obtained to apply the nickel-base alloy for being coated with Ni-Zr coating；
(4) pack cementation aluminizing：
(4-1) grinds elemental metals Al powder together with ammonium salt powder, is well mixed, and mixed-powder is made, then will mixing
Powder is placed in crucible；
The nickel-base alloy that the painting that step (3) obtains is coated with Ni-Zr coating by (4-2) is embedded into mixed-powder, and crucible is put
In tube furnace, 550-650 DEG C is heated to, constant temperature processing 10-12h, room temperature is then cooled to, takes out sample, through being cleaned by ultrasonic
Afterwards, dry, that is, the described doping Ni-Al bonding layer materials of the Zr with Ni-Zr diffusion barrier layers are made.
As preferable technical scheme, in step (1-1), nickel-base alloy is cut into length by Wire EDM is
25mm, width 20mm, be highly 4mm nickel-base alloy sheet metal.
As preferable technical scheme, in step (1-2), by Wire EDM by nickel plate that purity is 99.99%
Cut into length be 30mm, width 20mm, be highly 2mm nickel plate sheet metal.
As preferable technical scheme, the treatment conditions of the polishing described in step (1-3) are：Using from No. 240 to No. 600
Aluminum oxide sandpaper the surface of nickel-base alloy sheet metal, nickel plate sheet metal is polished.
As preferable technical scheme, the condition of the cleaning described in step (1-3) is：Carried out using alcohol or acetone clear
Wash.
The condition of electrolytic anode activation process described in step (1-4) is：It is 25-30 DEG C to control temperature, current density
For 100-200mA/cm2, processing time 1-5min.
As preferable technical scheme, the acid solution described in step (1-4) is hydrochloric acid solution, and the hydrochloric acid solution is 10-
15vol% hydrochloric acid and the mixed solution of the water nickel chlorides of 20-30g/L six.
The method of preparation electroplating solution described in step (2) specifically includes following steps：
Nickel salt and acidic electrolyte bath are dissolved in 50-70 DEG C of deionized water by (2-1), and mixed solution is made；
Anion surfactant is dissolved in the deionized water boiled by (2-2), is then added in mixed solution, and
Alkaline solution is used to adjust pH value as 4-4.5；
(2-3) adds metal Zr powder, is sufficiently stirred, and makes metal Zr powder dispersed in mixed solution, that is, institute is made
The electroplating solution stated.
As preferable technical scheme, the nickel salt described in step (2-1) is nickel sulfate hexahydrate and six water nickel chlorides, described
Acidic electrolyte bath is boric acid, and the mass concentration of described nickel sulfate hexahydrate, six water nickel chlorides and boric acid in mixed solution
Respectively 100~300g/L, 10~30g/L, 20~40g/L.
As preferable technical scheme, quality of the anion surfactant in mixed solution described in step (2-2)
Concentration is 0.2-1g/L, and described anion surfactant is lauryl sodium sulfate.
In actual electroplating process, a small amount of H in plating solution+Electronics is obtained in negative electrode, is separated out in the form of hydrogen.Although institute
Caused hydrogen largely escapes from plating solution in gaseous form, but still has a small amount of bubble hydrogen absorption in cathode surface, so that
The pin hole of nickel coating is produced in the position that bubble hydrogen is detained.As wetting agent, (be also called pin hole prevents lauryl sodium sulfate
Agent), after adding this wetting agent, plating solution is added to piece surface wetting action, so that bubble is difficult to remain in negative electrode
Surface, so as to reduce and eliminate pin hole, improve the compactness of coating.
As preferable technical scheme, the alkaline solution described in step (2-2) is the NaOH solution that mass fraction is 5%.
As preferable technical scheme, mass concentration of the metal Zr powder in mixed solution described in step (2-3) is
0.1-1g/L, and the particle diameter of described metal Zr powder is 1-3 μm.
When contents of the Zr in coating or alloy is near its solubility limit, i.e. during 0.05-0.1at.%, its oxidation susceptibility
It is best.Zr too high levels or the too low raising for being all unfavorable for oxidation susceptibility.Therefore, the quality that the present invention gradually changes Zr powder is dense
Degree, and then change the Zr contents in actual coating, it is therefore an objective to prepare the coating containing Zr with optimal oxidation susceptibility.According to
The reaction mechanism of composite plating, metal Zr powder as dispersing solid particles in Ni electroplate liquid, with the progress of electroplating process
It is co-deposited to form Ni-Zr composite coatings with Ni matrix metals.When the mass concentration of Zr powder is too small, Zr content is relative in coating
Diminish, situation when being added similar to the 0.1g/L Zr powder in the present invention, on the one hand cause the skewness of Zr in the coating
It is even, only Zr, the oxidation susceptibility that on the other hand so few Zr contents can not bring into play be present in the local location of coating；With
The increase of Zr mass concentration, the content of the Zr in coating gradually increase, and distributions of the Zr in whole coating gradually becomes uniform,
Situation when being added similar to the 0.5-0.7g/L Zr powder in the present invention.When the quality for the solia particle being dispersed in electroplate liquid
When concentration increases to finite concentration, it will not also make solia particle in coating even if the mass concentration for continuing to increase solia particle
Content increase.The mass concentration of 0.5-0.7g/L Zr powder in the present invention has made Zr be uniformly distributed in whole coating, if
On the one hand it is waste of materials when the mass concentration of Zr powder is excessive, from the aspect of oxidation susceptibility, excessive Zr contents can cause
Coating produces substantial amounts of internal oxidation in high-temperature oxidation process, is unfavorable for the raising of oxidation susceptibility.
In composite plating, the fairly small particulate of generally use particle diameter, the selection of the particle diameter of metal Zr powder is mainly from Zr's
Chemical property and cost consideration.Metal Zr powder is as active element, and very strong to the affinity of oxygen, its surface easily forms oxidation
Film.If the particle diameter of metal Zr powder is too small, such as nanometer scale, the cost produced first is high, and particle diameter is too small, surface area
Increase, during use or preservation, is more prone to so that Zr is oxidized, so that the simple substance Zr's included in Zr powder contains
Amount reduces, if in addition, particle diameter is meticulous, easy conglomeration is blocking, and particulate is unable to even suspension.If particle diameter is excessive, particulate is easy to
Precipitate and be not easy to be deposited metallic cover, coating is coarse, and particle diameter is excessive in addition, the metal of unit area in obtained composite deposite
Particle number is reduced, and causes its skewness in the coating.Therefore, the size controlling of heretofore described metal Zr powder
It is most appropriate for 1-3 μm.
Electroplating technique condition described in step (3) is：It is 250-350r/min to control mixing speed, and current density is
50-100mA/cm2。
In actual fabrication process, current density influences the crystalline condition and sedimentation rate of coating.When current density is smaller
When, the speed of one side coating deposition is slower, and another aspect nucleation rate is low, and only a small amount of crystal is grown up, the knot of coating
It is brilliant thick.And as the increase of current density, nucleus formation speed increase, coating crystallization are careful.So suitably improve electric current
Density, the crystallization of coating can not only be made careful, and sedimentation rate can be improved, improve production efficiency.But if current density mistake
Greatly, because liberation of hydrogen raises the pH value in cathodic region, basic salt or hydroxide are formed, the absorption of these materials exists in negative electrode or folder matter
In coating, spongy sediment is formed, is now referred to as " burning ".
In the electroplating process of reality, each plating solution has its suitable current density range, and used electric current
The factors such as density and composition, temperature, pH value and the stirring of electroplate liquid are relevant.Generally, the concentration increase of plating solution, temperature liter
Height, stirring intensity increase, when pH value is relatively low, can use larger current density.Electroplating technique condition of the present invention controls：
Mixing speed is 250-350r/min, current density 50-100mA/cm2, it is most appropriate.
The mass ratio of elemental metals Al powder and ammonium salt powder described in step (4-1) is 92-97:3-8, and it is described
Ammonium salt powder is NH4Cl powder.Using NH4Cl powder is as activator, and in coating high-temp preparation process, it can be analyzed to NH3
With HCl gases, the chloride of HCl gases and Al powder reaction generation aluminium, the chloride of aluminium is diffused into alloy surface, and in Ni-based conjunction
Gold surface occurs chemical reaction and forms nickel aluminium coating.
As preferable technical scheme, in step (4-1), elemental metals Al powder and ammonium salt powder are placed in agate mortar
Grind 5-10min.
As preferable technical scheme, described crucible is corundum crucible, and described tube furnace is horizontal pipe furnace.
Described nickel-base alloy includes one in polycrystalline nickel-base alloy, directionally solidified superalloy or single crystal nickel base alloy
Kind.
As preferable technical scheme, described nickel-base alloy is polycrystalline Hastelloy X nickel-base alloys.
When step (4-2) is heated, it is 550-650 DEG C to control temperature, and this is due to used in pack cementation method of the present invention
The comparision contents of aluminium are high, and the fusing point of aluminium is close to 660 DEG C, if temperature is too high, aluminium powder will be dissolved in metal surface.Therefore, it is warm
Degree control is most appropriate for 550-650 DEG C.
As preferable technical scheme, the condition of the ultrasonic cleaning described in step (4-2) is：, will under room temperature condition
Sample is placed in acetone soln, and it is 40-60KHz to control frequency size, is cleaned by ultrasonic 0.5-2 hours.
The Zr with Ni-Zr diffusion barrier layers being prepared using described method adulterates Ni-Al tack coats.
For the present invention in plating, the temperature for controlling electroplating solution is 50-60 DEG C；This is due to electric at a lower temperature
Plating, the internal stress of coating can increase, and raise the temperature of plating solution, and the internal stress of coating reduces；And higher electroplating temperature, then can be with
Increase the solution degree and electrical conductivity of each composition in plating solution, improve diffusion rate of the nickel ion to negative electrode, accelerate the deposition effect of coating
Rate, but if temperature is too high, coating crystallization is thick, and the increase of the evaporation capacity of plating solution, energy expenditure is larger, while nickel salt also easy water
Solution, nickel hydroxide precipitate is generated, this can make coating easily produce pin hole.
With the technology of the existing nickel aluminium tack coat for preparing Zr doping, such as electro beam physics vapour deposition, magnetron sputtering
Being compared with CVD etc., the present invention prepares the different nickel aluminum metal tack coat of Zr contents using the method for galvanoplastic combination pack cementation aluminizing,
Due to during aluminising, there is the presence of one layer of unreacted Ni-Zr barrier layer so that the nickel aluminium tack coat of the Zr doping of preparation
Do not influenceed by substrate composition, and the stirring in the dosage and electroplating process for passing through the Zr metal powders added in electroplating process makes
The content of Zr in tack coat and distribution are controlled.The invention has the characteristics that：
1) there are Ni-Zr Diffusion Barrier Rotating fields so that tack coat can not be influenceed by matrix composition；
2) compound electric plating method combination pack cementation aluminizing method is used, avoids preparation of the alloying element in matrix in tack coat
It is diffused into journey in tack coat；
3) amount of Zr powder and the stir speed (S.S.) of electroplating reaction that can be added by changing in electroplating solution are viscous to control
Tie Zr content and distribution in layer；
4) preparation process is simple, and cost is low, is advantageous to further industrialized production.
Brief description of the drawings
Fig. 1 is the SEM spectrograms for the Ni-Zr composite deposites that plating obtains；
Wherein, the Zr that (a) is 0.1g/L adulterates obtained Ni-Zr coating, and the Zr that (b) is 0.3g/L adulterates obtained Ni-
Zr coating, the Zr that (c) is 0.5g/L adulterate obtained Ni-Zr coating, and the Zr that (d) is 0.7g/L adulterates obtained Ni-Zr coating.
Fig. 2 is the content of metal Zr particles in Zr metallics percent by volume shared in Ni-Zr coatings and plating solution
Graph of a relation.
Fig. 3 is the XRD spectra of the nickel aluminium tack coat for the Zr doping for obtaining Ni-Zr coating in 650 DEG C/10h pack cementation aluminizings.
Fig. 4 is the SEM spectrograms for the nickel aluminium tack coat that the Zr for obtaining Ni-Zr coating 650 DEG C/10h pack cementation aluminizings is adulterated；
Wherein, the nickel aluminium tack coat that the Zr that (a) is 0.1g/L is adulterated, the nickel aluminium tack coat that the Zr that (b) is 0.3g/L is adulterated,
(c) the nickel aluminium tack coat adulterated for 0.5g/L Zr, the nickel aluminium tack coat that the Zr that (d) is 0.7g/L is adulterated.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
The first step：It is from polycrystalline Hastelloy X nickel-base alloys as alloy substrate, polycrystalline Hastelloy X is Ni-based
Alloy cuts into 20mm × 25mm × 4mm sheet metal, is that 99.99% nickel plate cuts into 20mm × 30mm × 2mm's by purity
Sheet metal, then clean 10min with acetone respectively；
Second step：Polished with aluminum oxide sandpaper from No. 240 to No. 600 to alloy-based body surface face, remove alloy substrate
The debris such as the corrosion on surface, the greasy dirt on alloy substrate surface is then removed with ethanol and acetone, then existed with the hydrochloric acid solution of dilution
Electrolytic anode activation process is carried out to alloy-based body surface face at room temperature, cleans 10min with the clear water of flowing afterwards, then use deionization
Water is cleaned by ultrasonic 10min；
3rd step：Electrolytic solution is prepared by the following method：
(1) by nickel sulfate hexahydrate (200g/L), six water nickel chlorides (20g/L) and boric acid (30g/L) with 60 DEG C of deionization
Water dissolves；
(2) lauryl sodium sulfate (0.5g/L) is added into the solution of (1) with after the deionized water dissolving boiled,
Deionized water is added to 200mL；
(3) with the NaOH solution that mass fraction is 5%, the pH value of solution is adjusted to 4；
(4) the metal Zr powder that 0.1g/L, 0.3g/L, 0.5g/L and 0.7g/L particle diameter are 2 microns is added to respectively
State in solution, with 300 rpms of rotating speed, stir 2 hours, that is, electrolytic solution is made；
4th step：Electroplated Ni-Zr coating, the technological parameter of electroplating process are as follows：
(1) temperature of plating is 55 DEG C；
(2) mixing speed is 300 turns per minute
(3) current density of plating is 80mA/cm2；
(4) depending on electroplating time is according to the thickness needed for plating；
5th step：Sample after plating is subjected to pack cementation aluminizing.Weigh elemental metals 97%Al powder and 3%NH4Cl powder,
Two kinds of powder are ground into nearly 5min in agate mortar, powder is uniformly mixed, and uniform mixed powder is put into just
Beautiful crucible, sample is embedded into mixed-powder, and with corundum lid sealed crucible, crucible is put into the heating of horizontal pipe furnace
Area, 10h is incubated at a temperature of 650 DEG C, after being cooled to room temperature, sample is taken out, be cleaned by ultrasonic 1 hour in acetone soln；
Step prepares the Ni-Zr coating of different content Zr doping as described above, as shown in Figure 1.It can be seen by Fig. 1
Go out, the bright particle being distributed in Ni-Zr coating is metal Zr, and the average thickness of Ni-Zr coating is 65.98 ± 1.22 μm.
When the Zr in electroplating solution is 0.1g/L, skewness of the Zr in Ni-Zr coating, only exist in local location；Work as electricity
When Zr in plating liquor is increased to by 0.3g/L during 0.7g/L, distribution of the Zr particles in Ni-Zr coating is gradually uniform.
From Figure 2 it can be seen that volume fractions of the Zr in Ni-Zr coating with electroplating solution in Zr particle additions increase and
Increase.
Fig. 3 is the XRD of the nickel aluminium tack coat for the Zr doping for obtaining Ni-Zr coating in 650 DEG C/10h pack cementation aluminizings, from
The thing of the nickel aluminium tack coat of Zr doping in figure after visible aluminising is mutually δ-Ni2Al3。
Fig. 4 is in the SEM sections of the Zr that 650 DEG C/10h pack cementation aluminizings the obtain nickel aluminium tack coats adulterated by Ni-Zr coating
Scheme, visible obtained tack coat divides two layers in figure, and one layer of outside is by δ-Ni2Al3Composition, one layer of the inside are not by aluminising
Ni-Zr coating, diffusion barrier layer can be used as.
Embodiment 2：
The present embodiment has the preparation method of the Zr doping Ni-Al bonding layer materials of Ni-Zr diffusion barrier layers, specifically includes
Following steps：
(1) it is surface-treated：
Nickel-base alloy is cut into length by Wire EDM and is 25mm, width 15mm, is highly 4mm by (1-1)
Nickel-base alloy sheet metal；
(1-2) by Wire EDM by the nickel plate of purity >=99% cut into length be 25mm, width 15mm, height
For 4mm nickel plate sheet metal；
(1-3) cleaning nickel-base alloy sheet metal, nickel plate sheet metal, polishing derusting, then clean except degreasing；
(1-4) carries out electrolytic anode activation process using acid solution to nickel-base alloy sheet metal at room temperature, then uses
Clear water cleaning is flowed, is cleaned by ultrasonic in deionized water, drying is stand-by；
(2) electroplating solution is prepared；
(3) coating Ni-Zr coating：
Using nickel plate sheet metal as anode, nickel-base alloy sheet metal is negative electrode, and nickel plate sheet metal, nickel-base alloy sheet metal are put
In the electroplating solution of step (2), at 50 DEG C, electroplated while stirring, Ni-Zr coating needed for the basis of time of plating
Depending on thickness, after end to be electroplated, cleaning, drying is stand-by, obtained to apply the nickel-base alloy for being coated with Ni-Zr coating；
(4) pack cementation aluminizing：
(4-1) grinds elemental metals Al powder together with ammonium salt powder, is well mixed, and mixed-powder is made, then will mixing
Powder is placed in crucible；
The nickel-base alloy that the obtained painting of step (3) is coated with Ni-Zr coating is embedded into mixed-powder by (4-2), by crucible
It is placed in tube furnace, is heated to 600 DEG C, constant temperature processing 11h, is then cooled to room temperature, takes out sample, after ultrasonic cleaning, do
It is dry, that is, the Zr doping Ni-Al bonding layer materials with Ni-Zr diffusion barrier layers are made.
Wherein, in step (1-4), the condition of electrolytic anode activation process is：It is 25 DEG C to control temperature, and current density is
100mA/cm2, processing time 5min.
The method that step (2) prepares electroplating solution specifically includes following steps：
Nickel salt and acidic electrolyte bath are dissolved in 50 DEG C of deionized water by (2-1), and mixed solution is made；
Anion surfactant is dissolved in the deionized water boiled by (2-2), is then added in mixed solution, and
Alkaline solution is used to adjust pH value as 4；
(2-3) adds metal Zr powder, is sufficiently stirred, and makes metal Zr powder dispersed in mixed solution, that is, electricity is made
Plating liquor.
In step (2-1), nickel salt is nickel sulfate hexahydrate and six water nickel chlorides, and acidic electrolyte bath is boric acid, and six water sulphur
The mass concentration of sour nickel, six water nickel chlorides and boric acid in mixed solution is respectively 100g/L, 10g/L, 20g/L.
Mass concentration of the anion surfactant in mixed solution is 0.2g/L in step (2-2), and anion
Surfactant is lauryl sodium sulfate.Alkaline solution is the NaOH solution that mass fraction is 5%.
Mass concentration of the metal Zr powder in mixed solution is 0.1g/L in step (2-3), and the particle diameter of metal Zr powder
For 1 μm.
Electroplating technique condition is in step (3)：It is 250r/min, current density 50mA/cm to control mixing speed2。
The mass ratio of elemental metals Al powder and ammonium salt powder is 92 in step (4-1):8, and ammonium salt powder is NH4Cl
Powder.
In the present embodiment, nickel-base alloy is Inconel nickel-base alloys.
The Zr with Ni-Zr diffusion barrier layers being prepared using the present embodiment method adulterates Ni-Al tack coats.
Embodiment 3：
The present embodiment has the preparation method of the Zr doping Ni-Al bonding layer materials of Ni-Zr diffusion barrier layers, specifically includes
Following steps：
(1) it is surface-treated：
Nickel-base alloy is cut into length by Wire EDM and is 35mm, width 25mm, is highly 2mm by (1-1)
Nickel-base alloy sheet metal；
(1-2) by Wire EDM by the nickel plate of purity >=99% cut into length be 35mm, width 25mm, height
For 2mm nickel plate sheet metal；
(1-3) cleaning nickel-base alloy sheet metal, nickel plate sheet metal, polishing derusting, then clean except degreasing；
(1-4) carries out electrolytic anode activation process using acid solution to nickel-base alloy sheet metal at room temperature, then uses
Clear water cleaning is flowed, is cleaned by ultrasonic in deionized water, drying is stand-by；
(2) electroplating solution is prepared；
(3) coating Ni-Zr coating：
Using nickel plate sheet metal as anode, nickel-base alloy sheet metal is negative electrode, and nickel plate sheet metal, nickel-base alloy sheet metal are put
In the electroplating solution of step (2), at 60 DEG C, electroplated while stirring, Ni-Zr coating needed for the basis of time of plating
Depending on thickness, after end to be electroplated, cleaning, drying is stand-by, obtained to apply the nickel-base alloy for being coated with Ni-Zr coating；
(4) pack cementation aluminizing：
(4-1) grinds elemental metals Al powder together with ammonium salt powder, is well mixed, and mixed-powder is made, then will mixing
Powder is placed in crucible；
The nickel-base alloy that the obtained painting of step (3) is coated with Ni-Zr coating is embedded into mixed-powder by (4-2), by crucible
It is placed in tube furnace, is heated to 550 DEG C, constant temperature processing 12h, is then cooled to room temperature, takes out sample, after ultrasonic cleaning, do
It is dry, that is, the Zr doping Ni-Al bonding layer materials with Ni-Zr diffusion barrier layers are made.
Wherein, in step (1-4), the condition of electrolytic anode activation process is：It is 25 DEG C to control temperature, and current density is
200mA/cm2, processing time 1min.
The method that step (2) prepares electroplating solution specifically includes following steps：
Nickel salt and acidic electrolyte bath are dissolved in 70 DEG C of deionized water by (2-1), and mixed solution is made；
Anion surfactant is dissolved in the deionized water boiled by (2-2), is then added in mixed solution, and
Alkaline solution is used to adjust pH value as 4.5；
(2-3) adds metal Zr powder, is sufficiently stirred, and makes metal Zr powder dispersed in mixed solution, that is, electricity is made
Plating liquor.
In step (2-1), nickel salt is nickel sulfate hexahydrate and six water nickel chlorides, and acidic electrolyte bath is boric acid, and six water sulphur
The mass concentration of sour nickel, six water nickel chlorides and boric acid in mixed solution is respectively 300g/L, 30g/L, 40g/L.
Mass concentration of the anion surfactant in mixed solution is 1g/L in step (2-2), and anion table
Face activating agent is lauryl sodium sulfate.Alkaline solution is the NaOH solution that mass fraction is 5%.
Mass concentration of the metal Zr powder in mixed solution is 1g/L in step (2-3), and the particle diameter of metal Zr powder is 3
μm。
Electroplating technique condition is in step (3)：It is 350r/min, current density 100mA/cm to control mixing speed2。
The mass ratio of elemental metals Al powder and ammonium salt powder is 95 in step (4-1):5, and ammonium salt powder is NH4Cl
Powder.
In the present embodiment, nickel-base alloy is Monel nickel-base alloys.
The Zr with Ni-Zr diffusion barrier layers being prepared using the present embodiment method adulterates Ni-Al tack coats.
Embodiment 4：
The present embodiment has the preparation method of the Zr doping Ni-Al bonding layer materials of Ni-Zr diffusion barrier layers, specifically includes
Following steps：
(1) it is surface-treated：
Nickel-base alloy is cut into length by Wire EDM and is 30mm, width 20mm, is highly 3mm by (1-1)
Nickel-base alloy sheet metal；
(1-2) by Wire EDM by the nickel plate of purity >=99% cut into length be 32mm, width 18mm, height
For 3mm nickel plate sheet metal；
(1-3) cleaning nickel-base alloy sheet metal, nickel plate sheet metal, polishing derusting, then clean except degreasing；
(1-4) carries out electrolytic anode activation process using acid solution to nickel-base alloy sheet metal at room temperature, then uses
Clear water cleaning is flowed, is cleaned by ultrasonic in deionized water, drying is stand-by；
(2) electroplating solution is prepared；
(3) coating Ni-Zr coating：
Using nickel plate sheet metal as anode, nickel-base alloy sheet metal is negative electrode, and nickel plate sheet metal, nickel-base alloy sheet metal are put
In the electroplating solution of step (2), at 58 DEG C, electroplated while stirring, Ni-Zr coating needed for the basis of time of plating
Depending on thickness, after end to be electroplated, cleaning, drying is stand-by, obtained to apply the nickel-base alloy for being coated with Ni-Zr coating；
(4) pack cementation aluminizing：
(4-1) grinds elemental metals Al powder together with ammonium salt powder, is well mixed, and mixed-powder is made, then will mixing
Powder is placed in crucible；
The nickel-base alloy that the obtained painting of step (3) is coated with Ni-Zr coating is embedded into mixed-powder by (4-2), by crucible
It is placed in tube furnace, is heated to 640 DEG C, constant temperature processing 10.5h, is then cooled to room temperature, takes out sample, after ultrasonic cleaning,
Dry, that is, the Zr doping Ni-Al bonding layer materials with Ni-Zr diffusion barrier layers are made.
Wherein, in step (1-4), the condition of electrolytic anode activation process is：It is 30 DEG C to control temperature, and current density is
120mA/cm2, processing time 3min.
The method that step (2) prepares electroplating solution specifically includes following steps：
Nickel salt and acidic electrolyte bath are dissolved in 65 DEG C of deionized water by (2-1), and mixed solution is made；
Anion surfactant is dissolved in the deionized water boiled by (2-2), is then added in mixed solution, and
Alkaline solution is used to adjust pH value as 4.2；
(2-3) adds metal Zr powder, is sufficiently stirred, and makes metal Zr powder dispersed in mixed solution, that is, electricity is made
Plating liquor.
In step (2-1), nickel salt is nickel sulfate hexahydrate and six water nickel chlorides, and acidic electrolyte bath is boric acid, and six water sulphur
The mass concentration of sour nickel, six water nickel chlorides and boric acid in mixed solution is respectively 200g/L, 20g/L, 30g/L.
Mass concentration of the anion surfactant in mixed solution is 0.6g/L in step (2-2), and anion
Surfactant is lauryl sodium sulfate.
Mass concentration of the metal Zr powder in mixed solution is 0.8g/L in step (2-3), and the particle diameter of metal Zr powder
For 2 μm.
Electroplating technique condition is in step (3)：It is 300r/min, current density 80mA/cm to control mixing speed2。
The mass ratio of elemental metals Al powder and ammonium salt powder is 96 in step (4-1):4, and ammonium salt powder is NH4Cl
Powder.
In the present embodiment, nickel-base alloy is directionally solidified superalloy.
The Zr with Ni-Zr diffusion barrier layers being prepared using the present embodiment method adulterates Ni-Al tack coats.
Embodiment 5：
The present embodiment has the preparation method of the Zr doping Ni-Al bonding layer materials of Ni-Zr diffusion barrier layers, specifically includes
Following steps：
(1) it is surface-treated：
Nickel-base alloy is cut into length by Wire EDM and is 32mm, width 24mm, is highly 2mm by (1-1)
Nickel-base alloy sheet metal；
(1-2) by Wire EDM by the nickel plate of purity >=99% cut into length be 35mm, width 20mm, height
For 2mm nickel plate sheet metal；
(1-3) cleaning nickel-base alloy sheet metal, nickel plate sheet metal, polishing derusting, then clean except degreasing；
(1-4) carries out electrolytic anode activation process using acid solution to nickel-base alloy sheet metal at room temperature, then uses
Clear water cleaning is flowed, is cleaned by ultrasonic in deionized water, drying is stand-by；
(2) electroplating solution is prepared；
(3) coating Ni-Zr coating：
Using nickel plate sheet metal as anode, nickel-base alloy sheet metal is negative electrode, and nickel plate sheet metal, nickel-base alloy sheet metal are put
In the electroplating solution of step (2), at 52 DEG C, electroplated while stirring, Ni-Zr coating needed for the basis of time of plating
Depending on thickness, after end to be electroplated, cleaning, drying is stand-by, obtained to apply the nickel-base alloy for being coated with Ni-Zr coating；
(4) pack cementation aluminizing：
(4-1) grinds elemental metals Al powder together with ammonium salt powder, is well mixed, and mixed-powder is made, then will mixing
Powder is placed in crucible；
The nickel-base alloy that the obtained painting of step (3) is coated with Ni-Zr coating is embedded into mixed-powder by (4-2), by crucible
It is placed in tube furnace, is heated to 580 DEG C, constant temperature processing 11.5h, is then cooled to room temperature, takes out sample, after ultrasonic cleaning,
Dry, that is, the Zr doping Ni-Al bonding layer materials with Ni-Zr diffusion barrier layers are made.
Wherein, in step (1-4), the condition of electrolytic anode activation process is：It is 30 DEG C to control temperature, and current density is
160mA/cm2, processing time 4min.
The method that step (2) prepares electroplating solution specifically includes following steps：
Nickel salt and acidic electrolyte bath are dissolved in 56 DEG C of deionized water by (2-1), and mixed solution is made；
Anion surfactant is dissolved in the deionized water boiled by (2-2), is then added in mixed solution, and
Alkaline solution is used to adjust pH value as 4；
(2-3) adds metal Zr powder, is sufficiently stirred, and makes metal Zr powder dispersed in mixed solution, that is, electricity is made
Plating liquor.
In step (2-1), nickel salt is nickel sulfate hexahydrate and six water nickel chlorides, and acidic electrolyte bath is boric acid, and six water sulphur
The mass concentration of sour nickel, six water nickel chlorides and boric acid in mixed solution is respectively 150g/L, 20g/L, 35g/L.
Mass concentration of the anion surfactant in mixed solution is 0.4g/L in step (2-2), and anion
Surfactant is lauryl sodium sulfate.
Mass concentration of the metal Zr powder in mixed solution is 0.6g/L in step (2-3), and the particle diameter of metal Zr powder
For 2 μm.
Electroplating technique condition is in step (3)：It is 320r/min, current density 95mA/cm to control mixing speed2。
The mass ratio of elemental metals Al powder and ammonium salt powder is 93 in step (4-1):7, and ammonium salt powder is NH4Cl
Powder.
In the present embodiment, nickel-base alloy is single crystal nickel base alloy.
The Zr with Ni-Zr diffusion barrier layers being prepared using the present embodiment method adulterates Ni-Al tack coats.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel do not depart from improvement that scope made and modification all should be the present invention's according to the announcement of the present invention
Within protection domain.
Claims (6)
1. the preparation method of the Zr doping Ni-Al bonding layer materials with Ni-Zr diffusion barrier layers, it is characterised in that this method
Specifically include following steps：
(1) it is surface-treated：
Nickel-base alloy is cut into length by Wire EDM and is 25-35mm, width 15-25mm, is highly 2- by (1-1)
4mm nickel-base alloy sheet metal；
(1-2) by Wire EDM by the nickel plate of purity >=99% cut into length be 25-35mm, width 15-25mm, height
Spend the nickel plate sheet metal for 2-4mm；
(1-3) cleaning nickel-base alloy sheet metal, nickel plate sheet metal, polishing derusting, then clean except degreasing；
(1-4) carries out electrolytic anode activation process to nickel-base alloy sheet metal using acid solution at room temperature, then with flowing
Clear water cleans, and is cleaned by ultrasonic in deionized water, and drying is stand-by；
(2) electroplating solution is prepared；
(3) coating Ni-Zr coating：
Using nickel plate sheet metal as anode, nickel-base alloy sheet metal is negative electrode, and nickel plate sheet metal, nickel-base alloy sheet metal are placed in into step
Suddenly in the electroplating solution of (2), at 50-60 DEG C, electroplated while stirring, Ni-Zr coating needed for the basis of time of plating
Depending on thickness, after end to be electroplated, cleaning, drying is stand-by, obtained to apply the nickel-base alloy for being coated with Ni-Zr coating；
(4) pack cementation aluminizing：
(4-1) grinds elemental metals Al powder together with ammonium salt powder, is well mixed, and mixed-powder is made, then by mixed-powder
It is placed in crucible；
The nickel-base alloy that the obtained painting of step (3) is coated with Ni-Zr coating is embedded into mixed-powder by (4-2), and crucible is placed in
In tube furnace, 550-650 DEG C is heated to, constant temperature processing 10-12h, room temperature is then cooled to, takes out sample, after ultrasonic cleaning,
Dry, that is, the described doping Ni-Al bonding layer materials of the Zr with Ni-Zr diffusion barrier layers are made；
The method of preparation electroplating solution described in step (2) specifically includes following steps：
Nickel salt and acidic electrolyte bath are dissolved in 50-70 DEG C of deionized water by (2-1), and mixed solution is made；
Anion surfactant is dissolved in the deionized water boiled by (2-2), is then added in mixed solution, and is used
Alkaline solution regulation pH value is 4-4.5；
(2-3) adds metal Zr powder, is sufficiently stirred, and makes metal Zr powder dispersed in mixed solution, that is, is made described
Electroplating solution；
Mass concentration of the metal Zr powder in mixed solution described in step (2-3) is 0.1-1g/L, and described metal Zr
The particle diameter of powder is 1-3 μm；
Electroplating technique condition described in step (3) is：It is 250-350r/min, current density 50- to control mixing speed
100mA/cm2；
The mass ratio of elemental metals Al powder and ammonium salt powder described in step (4-1) is 92-97:3-8, and described ammonium salt
Powder is NH4Cl powder.
2. the preparation method of the Zr doping Ni-Al tack coats according to claim 1 with Ni-Zr diffusion barrier layers, its
It is characterised by, the condition of the electrolytic anode activation process described in step (1-4) is：It is 25-30 DEG C to control temperature, current density
For 100-200mA/cm2, processing time 1-5min.
3. the preparation method of the Zr doping Ni-Al tack coats according to claim 1 with Ni-Zr diffusion barrier layers, its
It is characterised by, the nickel salt described in step (2-1) is nickel sulfate hexahydrate and six water nickel chlorides, and described acidic electrolyte bath is boric acid,
And mass concentration of the described nickel sulfate hexahydrate, six water nickel chlorides and boric acid in mixed solution be respectively 100~300g/L,
10~30g/L, 20~40g/L.
4. the preparation method of the Zr doping Ni-Al tack coats according to claim 1 with Ni-Zr diffusion barrier layers, its
It is characterised by, mass concentration of the anion surfactant described in step (2-2) in mixed solution is 0.2-1g/L, and
Described anion surfactant is lauryl sodium sulfate.
5. the preparation method of the Zr doping Ni-Al tack coats according to claim 1 with Ni-Zr diffusion barrier layers, its
It is characterised by, described nickel-base alloy includes one in polycrystalline nickel-base alloy, directionally solidified superalloy or single crystal nickel base alloy
Kind.
6. the doping of the Zr with the Ni-Zr diffusion barrier layers Ni- that the method as described in any one of claim 1 to 5 is prepared
Al tack coats.
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