CN108998816A - A kind of ammonium chloride helps Cr/ Nitriding Compound coating of infiltration and preparation method thereof - Google Patents
A kind of ammonium chloride helps Cr/ Nitriding Compound coating of infiltration and preparation method thereof Download PDFInfo
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- CN108998816A CN108998816A CN201810961024.1A CN201810961024A CN108998816A CN 108998816 A CN108998816 A CN 108998816A CN 201810961024 A CN201810961024 A CN 201810961024A CN 108998816 A CN108998816 A CN 108998816A
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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
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
-
- 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
- C25D5/48—After-treatment of electroplated surfaces
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- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Electroplating Methods And Accessories (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention discloses the Cr/ Nitriding Compound coating and preparation method thereof that a kind of ammonium chloride helps infiltration, the composite coating successively include from outside to inside the CrNx hardened layer of surface plating Cr, secondary surface layer diffusion layer, center portion matrix；The CrNx hardened layer is mainly by the CrNx phase composition of face-centred cubic structure；The secondary surface layer diffusion layer is mainly by nitrogenous oversaturated α-Fe phase, carbide, nanoscale alloy nitride and needle-shaped or band-like γ '-Fe4N phase composition；The matrix is mainly made of α-Fe phase and carbide.The present invention have the advantage that compared with prior art the coating in the present invention using ammonium chloride help infiltration method remove Cr layer surface densification passivating film, subsequent Nitrizing Treatment make Cr layers to be transformed into hardness is higher, wearability is higher, fracture toughness is stronger, corrosion resistance is CrNx layers better.Meanwhile activated nitrogen atom is spread from surface layer to center portion, change of gradient is presented in composite coating cross-sectional compositional and structure, improves interfacial stress and concentrates situation, improves composite coating interface binding power.
Description
Technical field
The present invention relates to a kind of composite coating more particularly to a kind of ammonium chloride help infiltration Cr/ Nitriding Compound coating and
Preparation method.
Background technique
With the development of the industry technologies such as modern space flight and aviation, automotive light weight technology, more and more products are light using aluminium, magnesium etc.
Matter alloy replaces steel material.Therefore, the hot-working process of the alloys such as aluminium, magnesium is of crucial importance, such as: injection molding, die casting, hot extrusion
Pressure etc..In the alloys hot procedure such as aluminium, magnesium, work metal is directly contacted with mold, contact surface temperature up to 300 DEG C~
800 DEG C, there are elements diffusion and interfacial reactions for metal and mould contact surface under high temperature, produce intermetallic compound object, cause by
Metal and die bonds are processed, adhesion wear and abrasive wear are caused, accelerate mould invalidation, such as: Fe reacts production with Al
Fe3Al、FeAl、FeAl2Or FeAl3Etc. weld metal zone brittle intermetallic things.The hot-working of the alloys such as aluminium, magnesium proposes die surface high resistance to
The demand of mill property, chemical stability and thermal stability；In addition, mold bears hot and cold alternation operating condition for a long time, die surface is mentioned
The requirement of high fatigue resistance is gone out.In addition, die surface and the performance requirement of center portion are different, it is difficult through material itself
Or the bulk heat treatmet of mold is realized.Therefore, surface of hot working die processing technique is paid close attention to by die industry.
Currently, hot die steel mainstream process for treating surface is nitriding or nitrocarburizing.Hot die steel nitriding or nitrogen carbon are total
During infiltration, mold steel surface forms certain thickness, nitrogenous oversaturated tempered martensite, with higher hard
Degree, wearability and anti-fatigue performance.Nevertheless, often sending out die surface in production is stained with some aluminum alloy granules, cause
Adhesion wear and abrasive wear occur for mold.The main reason is that Fe and Al form FeAl intermetallic at a certain temperature
Object, such as: Fe3Al、FeAl、FeAl2Or FeAl3Deng.As it can be seen that by nitriding or nitrocarburizing processing to surface of hot working die
The raising of energy is limited.
Physical vapour deposition (PVD) (PVD) CrN metal-cermic coating is because of its high rigidity, high-wearing feature, high thermal stability and chemistry
Inertia and be concerned, be used widely in cold working mold, the industries such as cutter.Therefore, there is part worker that PVD sinks
Product CrN coating technology set is on hot die steel, but its effect is limited.Al has very high solid solubility in CrN, is easy to lead
Cause adhesion wear.In addition, PVD coating internal stress is big, coating layer thickness is limited (usually less than 5 μm), coating and basal body binding force compared with
It is low.Disadvantages mentioned above causes PVD coating to be unable to satisfy the high abrasion proposed in the alloys hot procedure such as aluminium, magnesium to mold coating
The requirement of the performances such as property, high bearing capacity, high-fracture toughness, high thermal fatigue resistance.
Cr layers of plating has the characteristics that high rigidity, wear-resisting, stable and be widely used in the industrial production.Plate Cr thickness
Degree can control within 1.0mm, between 400~900HV of hardness.Cr layers of intermediate gap of plating are dissolved a small amount of hydrogen, lead to lattice dilatation,
Play solution strengthening effect.When being up to 500 DEG C using temperature, solid solution hydrogen is precipitated, and it is hard that coating hardness reduces 500HV or even lower
Degree.Cr layer directly progress Nitrizing Treatment will be plated and be difficult to obtain CrNx layers high performance, main cause is the cause easy to form of the surface Cr
Close passivating film hinders activated nitrogen atom to Cr layers of diffusion of plating.
Summary of the invention
Technical problem to be solved by the present invention lies in: existing nitriding or nitrocarburizing processing will cause mold and occur to glue
Attached abrasion and abrasive wear, PVD deposition CrN coating technology set on hot die steel with being easy to cause adhesion wear, and coating
It is lower with basal body binding force, and plating the solid solution hydrogen that Cr is chromatographed out can make coating hardness reduce, it provides a kind of ammonium chloride and helps infiltration
Cr/ Nitriding Compound coating and preparation method thereof.
The present invention is that solution above-mentioned technical problem, a kind of ammonium chloride of the invention help infiltration by the following technical programs
Cr/ Nitriding Compound coating, the composite coating successively include the CrNx hardened layer of surface plating Cr, the diffusion of secondary surface layer from outside to inside
The matrix of layer, center portion；The CrNx hardened layer is mainly by the CrNx phase composition of face-centred cubic structure；The secondary surface layer diffusion
Layer is mainly by nitrogenous oversaturated α-Fe phase, carbide, nanoscale alloy nitride and needle-shaped or band-like γ '-Fe4N phase composition；
The matrix is mainly made of α-Fe phase and carbide.Further, described matrix also contains a certain amount of carbide, or
Described matrix is other metals or noncrystal substrate.
Further, also contain a small amount of Cr and Cr in the CrNx hardened layer of the surface plating Cr2N phase.Further, institute
State the CrNx hardened layer of surface plating Cr with a thickness of 0.005~1.0mm, secondary surface layer thickness of diffusion layer is 0.01~0.5mm, compound
Total coating thickness is 0.015~1.5mm.
A kind of ammonium chloride helps the preparation method of the Cr/ Nitriding Compound coating of infiltration, comprising the following steps: first to steel matrix into
Row chromium plating process prepares certain thickness metal Cr layers.Then in the certain thickness ammonium chloride powder of Cr layer surface tiling, in advance
Heat removes Cr layer surface passivating film, is and then passed through ammonia nitriding, so that Cr layers are transformed into CrNx layers, closes on CrNx layers of steel
Matrix is then transformed into nitrogenous oversaturated diffusion layer.
Specific step is as follows:
(1) steel sample is polished to roughness≤0.1 μm, it, will be clear after carrying out prewashing, intermediate cleaning, electrolytic cleaned, drying
It washes dry sample to be electroplated, plating Cr sample is made；
(2) plating Cr sample is placed in nitriding furnace, is less than the ammonium chloride powder of 5mm in plating Cr layer surface pre-set thickness,
After preheating and keeping the temperature, it is passed through ammonia, hydrogen and nitrogen, composite coating is prepared in adjusting.Further, by plating Cr processing
Afterwards, electroplated layer with a thickness of 0.005~1.0mm, hardness is 400~900HV.
Further, Cr layers are electroplated and are transformed into CrNx layers through nitriding, CrNx layers are with a thickness of 0.005~1.0mm, hardness
1000HV~2000HV.After plating Cr processing, electroplated layer with a thickness of 0.005~1.0mm, hardness is 400~900HV.
In the step (1), electrolyte includes 200~250g/L chromic anhydride, 2.0~2.5g/L sulfuric acid and 3.0~6.0g/L tri- in plating
Valence chromium, current density are 50~90A/dm2, electroplating temperature is 50~70 DEG C.
In the step (2), preheating temperature is 350~500 DEG C, and soaking time is less than 5h, and nitriding temperature is 450~750
DEG C, nitridation time 1h~40h.
Although PVD coating hardness, wearability are high, its internal stress is big, and coating layer thickness is relatively thin (usually less than 5 μm), film base
Binding force is limited, is unable to satisfy the hot-working such as aluminium, magnesium and proposes that high film-base junction resultant force, bearing capacity, heat resistanceheat resistant are tired to mold coating
The requirement of labor and wearability.And PVD equipment cost and maintenance cost are high, it is more demanding to worker operation.Plating metal Cr, plating
For Cr thickness degree up to 1.0mm, thickness is easy to control, but electroplated metal layer hardness and wearability are low.Plating Cr layer surface is easily formed cause
Close oxide passivation film hinders activated nitrogen atom to Cr layers of diffusion of plating, Cr layers of plating is caused usually can not directly to carry out nitriding
Processing.
Since Cr layer surface forms fine and close passivating film, nitrogen-atoms is hindered to spread to matrix.It is thermally decomposed, is gone using ammonium chloride
Except Cr layer surface densification passivating film, and the ammonia that ammonium chloride is decomposed thermally to form then becomes nitridation source gas；Meanwhile Cr layers exist greatly
Born of the same parents' shape substructure of amount provides quick diffusion admittance for the diffusion of nitrogen.As a result, make Cr layers be transformed into hardness it is higher,
Wearability is higher, fracture toughness is stronger, corrosion resistance is CrNx layers better.Meanwhile secondary surface layer is formed due to nitrogen-atoms infiltration
The gradient layer that hardness changes in gradient improves the distribution of composite coating transverse section hardness, improves composite coating film-base junction resultant force.
The present invention has the advantage that the present invention by optimization plating and nitridation process, successively to steel compared with prior art
And other metal materials carry out plating Cr+ Nitrizing Treatment, prepare one layer of hardened layer in workpiece surface.The hardened layer is by secondary surface layer
Nitriding diffusion layer and surface layer CrNx layers of composition.The composite coating just has high hardness, film-substrate cohesion, bearing capacity, fracture tough
Property, fretting wear and thermal fatigue resistance, subsequent Nitrizing Treatment make Cr layers to be transformed into hardness is higher, wearability is higher, fracture
Toughness is stronger, corrosion resistance is CrNx layers better.Meanwhile activated nitrogen atom is spread from surface layer to center portion, composite coating is transversal
Change of gradient is presented in face ingredient and structure, improves interfacial stress and concentrates situation, improves composite coating interface binding power.
Detailed description of the invention
Fig. 1 is the XRD spectrum of 2 prepares coating of embodiment 1 and embodiment；
Fig. 2 is plating Cr and plating Cr/ Nitriding Compound coatings cross-section metallographic microscope；
Fig. 3 is hardness schematic diagram under Examples 1 and 2 different loads；
Fig. 4 is Examples 1 and 2 film-base junction resultant force and fracture toughness test figure.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
The H13 hot-work die steel sample that market is bought is mechanically polished to surface roughness roughness≤0.1 μm, so
Acetone, dehydrated alcohol ultrasonic cleaning are carried out afterwards, are then placed in alcohol and acetone, are first used ultrasonic cleaning 30 minutes, then use gas
Sample drying after cleaning is placed in the intracorporal substrate frame of furnace chamber by rifle.It will after cleaning be that print is put into electroplating bath, electricity
Plate Cr technique: electrolyte is by chromic anhydride (200~250g/L), sulfuric acid (2.0~2.5g/L) and trivalent chromium (3.0~6.0g/L) group
At；Current density is 50~90A/dm2；Electroplating temperature is 50~70 DEG C.Complete the preparation of plating Cr sample.
Embodiment 2
The H13 hot-work die steel sample that market is bought is mechanically polished to surface roughness roughness≤0.1 μm, so
Acetone, dehydrated alcohol ultrasonic cleaning are carried out afterwards, are then placed in alcohol and acetone, are first used ultrasonic cleaning 30 minutes, then use gas
Sample drying after cleaning is placed in the intracorporal substrate frame of furnace chamber by rifle.It will after cleaning be that print is put into electroplating bath, electricity
Plate Cr technique: electrolyte is by chromic anhydride (200~250g/L), sulfuric acid (2.0~2.5g/L) and trivalent chromium (3.0~6.0g/L) group
At；Current density is 50~90A/dm2；Electroplating temperature is 50~70 DEG C.Complete the preparation of plating Cr sample.Nitridation sample is put
Enter in nitriding furnace, plates the ammonium chloride powder of the preset high-purity of Cr layer surface, be then heated to 300~500 using furnace internal resistance wire
DEG C, soaking time is less than 5h.Then pass to ammonia, hydrogen and argon gas, 520~590 DEG C of nitriding temperature, 400~800V of back bias voltage,
1~40h of nitridation time, preparation nitridation sample.
As shown in Figure 1, the nitridation of Fig. 1 intermediate ion is sample prepared by embodiment 1 and embodiment 2, plating Cr processing is done to H13,
Then Nitrizing Treatment is carried out.
From figure 1 it appears that Cr layers of plating mainly has bcc-Cr phase composition.After nitrogen treatment, bcc-Cr is transformed into fcc-
CrNx phase.
Various coating samples in above-described embodiment are subjected to ultrasonic cleaning, then carry out hardness, bearing capacity, combination
Power, fracture toughness test, test result such as Fig. 2 and Fig. 3.Plating Cr indicates in embodiment 1 that H13 mould steel only deposits Cr coating；Plating
Cr/ nitriding indicates in embodiment 2 that H3 steel surface plates Cr, then Nitrizing Treatment.
Fig. 2 indicates plating Cr and plating Cr/ Nitriding Compound coatings cross-section metallographic microscope.As it can be seen that composite coating steel matrix is deposited
In certain thickness nitriding layer.
Fig. 3 indicates hardness number of the various coatings under different loads.It can be seen from the figure that with the increase of load, coating
Surface hardness gradually decreases.Under 50g power, plating Cr layer surface hard value is about 820HV, plates Cr/ nitriding composite coating surface hardness
About 1500HV；Under identical outer plus survey load, it is hard that plating Cr/ nitriding composite coating surface hardness is always above plating Cr layer surface
Degree, this, which is CrNx layers, has higher hard compared with Cr layers.Meanwhile also illustrating that plate Cr/ nitriding composite coating has more compared with Cr layers of plating
High bearing capacity.
Fig. 4 is various coated films-base junction resultant force and fracture toughness test.It can be seen from the figure that Cr layers of plating is in≤300g
It is not cracked around plating Cr layer surface impression under load, as additional test load >=500g, occur around impression
Circumferential crack.However, for plating Cr/ nitriding composite coating, even if not occurred around impression when adding 1000g load outside
Crackle, these illustrate that plating relatively Cr layers of plating of Cr/ nitriding composite coating has higher film-base junction resultant force and fracture toughness.So chlorine
Infiltration Cr layer surface hardness, bearing capacity, film-base junction resultant force and fracture toughness can be significantly improved by changing ammonium auxiliary nitriding.
The foregoing is merely illustrative of the preferred embodiments of the present invention, not to limit invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.
Claims (10)
1. the Cr/ Nitriding Compound coating that a kind of ammonium chloride helps infiltration, which is characterized in that the composite coating successively includes from outside to inside
Surface plate the CrNx hardened layer of Cr, secondary surface layer diffusion layer, center portion matrix；The CrNx hardened layer is mainly by face-centered cubic knot
The CrNx phase composition of structure；The secondary surface layer diffusion layer is mainly by nitrogenous oversaturated α-Fe phase, carbide, nanoscale alloy nitrogen
Compound and needle-shaped or band-like γ '-Fe4N phase composition；The matrix is mainly made of α-Fe phase and carbide.
2. the Cr/ Nitriding Compound coating that a kind of ammonium chloride according to claim 1 helps infiltration, which is characterized in that described matrix
It is also other metals or noncrystal substrate containing a certain amount of carbide or described matrix.
3. the Cr/ Nitriding Compound coating that a kind of ammonium chloride according to claim 1 helps infiltration, which is characterized in that the surface
It plates and also contains a small amount of Cr and Cr in the CrNx hardened layer of Cr2N phase.
4. the Cr/ Nitriding Compound coating that a kind of ammonium chloride according to claim 1 helps infiltration, which is characterized in that the surface
Plate the CrNx hardened layer of Cr with a thickness of 0.005~1.0mm, secondary surface layer thickness of diffusion layer is 0.01~0.5mm, and composite coating is total
With a thickness of 0.015~1.5mm.
5. a kind of ammonium chloride as described in any one of claims 1 to 4 helps the preparation method of the Cr/ Nitriding Compound coating of infiltration,
It is characterized in that, carrying out chromium plating process to steel matrix first, certain thickness metal Cr layers are prepared, is then tiled in Cr layer surface
Certain thickness ammonium chloride powder, preheating remove Cr layer surface passivating film, are and then passed through ammonia nitriding, so that Cr layers of transformation
At CrNx layers, closes on CrNx layers of steel matrix and be transformed into nitrogenous oversaturated diffusion layer.
6. a kind of ammonium chloride according to claim 5 helps the preparation method of the Cr/ Nitriding Compound coating of infiltration, feature exists
In, the specific steps are as follows:
(1) steel sample is polished to roughness≤0.1 μm, it is after carrying out prewashing, intermediate cleaning, electrolytic cleaned, drying, cleaning is dry
Dry sample is electroplated, and plating Cr sample is made；
(2) plating Cr sample is placed in nitriding furnace, is less than the ammonium chloride powder of 5mm, preheating in plating Cr layer surface pre-set thickness
And after keeping the temperature, it is passed through ammonia, hydrogen and nitrogen, composite coating is prepared in adjusting.
7. a kind of ammonium chloride according to claim 6 helps the preparation method of the Cr/ Nitriding Compound coating of infiltration, feature exists
In, after plating Cr processing, electroplated layer with a thickness of 0.005~1.0mm, hardness is 400~900HV.
8. a kind of ammonium chloride according to claim 6 helps the preparation method of the Cr/ Nitriding Compound coating of infiltration, feature exists
In, Cr layer of plating are transformed into CrNx layers through nitriding, CrNx layers with a thickness of 0.005~1.0mm, hardness is 1000HV~2000HV.
9. a kind of ammonium chloride according to claim 6 helps the preparation method of the Cr/ Nitriding Compound coating of infiltration, feature exists
In in the step (1), electrolyte includes 200~250g/L chromic anhydride, 2.0~2.5g/L sulfuric acid and 3.0~6.0g/L in plating
Trivalent chromium, current density are 50~90A/dm2, electroplating temperature is 50~70 DEG C.
10. a kind of ammonium chloride according to claim 6 helps the preparation method of the Cr/ Nitriding Compound coating of infiltration, feature exists
In in the step (2), preheating temperature is 350~500 DEG C, and soaking time is less than 5h, and nitriding temperature is 450~750 DEG C, nitrogen
Change time 1h~40h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210756A (en) * | 2020-10-13 | 2021-01-12 | 辽宁科技大学 | Preparation method of iron-based alloy surface strong-corrosion-resistance high-chromium composite nitriding layer |
| CN112899733A (en) * | 2021-01-20 | 2021-06-04 | 华中科技大学 | Compact chromium oxynitride hydrogen permeation-resistant coating and preparation method thereof |
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| CN104480478A (en) * | 2014-12-31 | 2015-04-01 | 马鞍山市安工大工业技术研究院有限公司 | Nitriding PVD composite coating and preparation method thereof |
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- 2018-08-22 CN CN201810961024.1A patent/CN108998816A/en active Pending
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| CN104480478A (en) * | 2014-12-31 | 2015-04-01 | 马鞍山市安工大工业技术研究院有限公司 | Nitriding PVD composite coating and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210756A (en) * | 2020-10-13 | 2021-01-12 | 辽宁科技大学 | Preparation method of iron-based alloy surface strong-corrosion-resistance high-chromium composite nitriding layer |
| CN112899733A (en) * | 2021-01-20 | 2021-06-04 | 华中科技大学 | Compact chromium oxynitride hydrogen permeation-resistant coating and preparation method thereof |
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