CN107268039A - A kind of Cr Fe graded composite anti-corrosion materials and preparation method thereof - Google Patents
A kind of Cr Fe graded composite anti-corrosion materials and preparation method thereof Download PDFInfo
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- CN107268039A CN107268039A CN201710457144.3A CN201710457144A CN107268039A CN 107268039 A CN107268039 A CN 107268039A CN 201710457144 A CN201710457144 A CN 201710457144A CN 107268039 A CN107268039 A CN 107268039A
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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
- C25D3/08—Deposition of black chromium, e.g. hexavalent chromium, CrVI
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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
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Abstract
The invention discloses a kind of Cr Fe graded composite anti-corrosion materials, the step of by carbon steel coupon through polishing, NaOH solution immersion, hydrochloric acid solution immersion, alcohol-pickled, cleaning, the clean steel disc of cathode material is obtained；Chromic anhybride, the concentrated sulfuric acid, auxiliary agent and water are mixed with out electrolyte, then make anode with chromium plate, and clean steel disc is made negative electrode, is electrolysed；Cleaning, annealing obtain Cr Fe graded composite anti-corrosion materials after electrolysis terminates.The preparation method of present invention deposit and spread substance C r on carbon steel material by the method for electrolysis, then chromium is made to diffuse into carbon steel by the method for high temperature diffusion annealing, so as to form carbon steel/stainless steel FGM, the functionally gradient material (FGM) has good corrosion resistance, there is low cost, high rigidity simultaneously and have the outward appearance of fineness, it is adaptable to every field.
Description
Technical field
The invention belongs to anti-corrosion material technical field, and in particular to a kind of Cr-Fe graded composites anti-corrosion material and its preparation
Method.
Background technology
In the application of ferrous materials, carbon steel material is simple due to cheap, manufacturing process, while have well again
The combination properties such as plasticity, toughness, workability, as the ferrous materials that number of applications in engineering is maximum, widest in area.However,
The perishable weakness of various carbon steel materials all generally existings in engineer applied.In order to solve this problem, domestic and foreign scholars are opened
Sent out many steel grades to improve the corrosion resistance of ferrous materials, stainless steel is exactly one kind therein, its have excellent corrosion resistance, into
The features such as outward appearance of type, compatibility, the obdurability in very wide temperature range and fineness, obtain wide in all trades and professions
General application.
But, the research for preparing carbon steel/stainless steel FGM by matrix of carbon steel material at present also there is no report,
The research for preparing the FGMs such as metal/metal, metal/ceramic, metal/carbon compound, ceramics/plastics is a lot, involved
Preparation method mainly have vapour deposition process, powder metallurgic method, plasma spraying method, self-propagating combustion high-temperature synthesis, laser
Melt the method for covering and melt metallurgical method etc..But each method has respective limitation, and these methods satisfaction can not prepare carbon simultaneously
Cost required for steel/stainless steel FGM is low, size is big, quantity is more, process is continuously required.Must in consideration of it, having
Want new FGM preparation method.
The content of the invention
It is an object of the invention to provide a kind of Cr-Fe graded composites anti-corrosion material and preparation method thereof, system can be met simultaneously
The requirement such as cost required for standby carbon steel/stainless steel FGM is low, size is big, quantity is more, process is continuous.
First purpose of the present invention is to provide a kind of preparation method of Cr-Fe graded composites anti-corrosion material, specifically includes
Following steps
Step 1, carbon steel coupon is polishing to surfacing light, obtains smooth steel disc；
Step 2, smooth steel disc is put into 5g/100ml NaOH solution and soaked, then taken out, obtain alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5% and soaked, then taken out, obtain sour place
Manage steel disc；
Step 4, acid treatment steel disc is placed in 70% alcohol, cleans, then take out, dry up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after, and electrolyte
The concentration of middle chromic anhybride is 150-400g/L, and the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent
For water；
Step 6, the preparation electrolyte of step 5 rises to design temperature, is passed through argon gas and is protected, anode is made with chromium plate, does
Net steel disc makees negative electrode, is electrolysed；
Step 7, after electrolysis terminates, carbon steel coupon is taken out, is put into ultrasonic washing instrument and cleans, then rushed with distilled water
Wash, dry after it is standby, obtain being electrolysed sample after heavy chromium；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at a temperature of 660-940 DEG C, argon gas-hydrogen is used during annealing
It is mixed gas protected, obtain Cr-Fe graded composite anti-corrosion materials.
It is preferred that, the preparation method of above-mentioned Cr-Fe graded composites anti-corrosion material, in step 5, the auxiliary agent be potassium chloride,
One kind in dipotassium hydrogen phosphate or citric acid.
It is preferred that, the preparation method of above-mentioned Cr-Fe graded composites anti-corrosion material, in step 6, design temperature is 50 DEG C, electricity
Using the current density of 35-65 amperes/square decimeter during solution.
It is preferred that, the preparation method of above-mentioned Cr-Fe graded composites anti-corrosion material, in step 8, the volume ratio of argon gas and hydrogen
Example is 100:1.
Second object of the present invention is the Cr-Fe graded composite anti-corrosion materials that the above method is prepared from.
Compared with prior art, Cr-Fe graded composite anti-corrosion materials of the invention have the advantages that：
The present invention method be made up of two big processing steps, first by the method for electrolysis on carbon steel material deposit and spread
Substance C r, secondly be exactly chromium is diffused into carbon steel by the method for high temperature diffusion annealing under atmospheric condition so that formed carbon steel/
Stainless steel FGM.The Cr-Fe graded composite anti-corrosion materials being prepared from have good corrosion resistance, have simultaneously
Cost is low, high rigidity and have the advantages that fineness outward appearance, it is adaptable to every field.
Brief description of the drawings
Chromium content is measured in Fig. 1 difference anti-corrosion materials；
Wherein, Fig. 1 (a), Fig. 1 (b), Fig. 1 (c), Fig. 1 (d), Fig. 1 (e) correspond to embodiment 1, embodiment 2, embodiment respectively
3rd, the anti-corrosion material of embodiment 4 and embodiment 5；
Fig. 2 is the ESEM view on the anti-corrosion material surface of embodiment 1；
Fig. 3 is the ESEM view of the anti-corrosion material section of embodiment 1；
Fig. 4 is the polarization curve of matrix and different anti-corrosion materials.
Embodiment
The embodiment and accompanying drawing to invention are described in detail below, it is to be understood that protection scope of the present invention
Do not limited by embodiment.The test method of unreceipted actual conditions in the following example, generally according to conventional strip
Part, or according to the condition proposed by each manufacturer.
All technologies used when embodiment provides number range, it should be appreciated that unless otherwise defined in the present invention and section
Technics is identical with the meaning that those skilled in the art of the present technique are generally understood that.Except the specific method used in embodiment, equipment, material
Material is outer, according to those skilled in the art to the grasp of prior art and the record of the present invention, can also use and this hair
Any method, equipment and the material of the similar or equivalent prior art of method, equipment described in bright embodiment, material is realized
The present invention.
Embodiment 1
A kind of Cr-Fe graded composites anti-corrosion material, is specifically prepared according to following steps：
Step 1,320# carbon steel coupons are polishing to surfacing light on sand paper, obtain smooth steel disc；
Step 2, smooth steel disc is put into the NaOH solution that concentration is 5g/100ml and soaks 5min, then taken out, obtain
Alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5%, soaks 5min, then take out, obtain
To acid treatment steel disc；
Step 4, acid treatment steel disc is placed in 70% alcohol, be then put into together with 70% alcohol in ultrasonic cleaning instrument
Concussion cleaning 5min, then takes out, dries up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after；Chromic anhybride it is dense
Spend for 150g/L, the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent is water；
Step 6, the preparation electrolyte of step 5 rises to 50 DEG C of design temperature, is passed through argon gas and is protected, and argon gas flow velocity is
6L/min, anode is made with chromium plate, and clean steel disc is made negative electrode, is electrolysed, and electric current during electrolysis using 35 amperes/square decimeter is close
Degree；
Step 7, after electrolysis terminates, carbon steel coupon is taken out rapidly, cleaning in ultrasonic washing instrument (power 400W) is put into
After 10min, then rinsed repeatedly with distilled water, dry after it is standby；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at 660 DEG C, protected during annealing using argon gas-hydrogen gas mixture
Shield, flow velocity is 6L/min, anti-oxidation, and hydrogen is anti-oxidation for aiding in, and the volume ratio of argon gas and hydrogen is 100:1, obtain Cr-
Fe graded composite anti-corrosion materials, Cr-Fe gradients are formed after electrolysis diffusion on anti-corrosion material.
Embodiment 2
A kind of Cr-Fe graded composites anti-corrosion material, is specifically prepared according to following steps：
Step 1,500# carbon steel coupons are polishing to surfacing light on sand paper, obtain smooth steel disc；
Step 2, smooth steel disc is put into the NaOH solution that concentration is 5g/100ml and soaks 5min, then taken out, obtain
Alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5%, soaks 5min, then take out, obtain
To acid treatment steel disc；
Step 4, acid treatment steel disc is placed in 70% alcohol, be then put into together with 70% alcohol in ultrasonic cleaning instrument
Concussion cleaning 5min, then takes out, dries up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after, chromic anhybride it is dense
Spend for 400g/L, the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent is water；
Step 6, the preparation electrolyte of step 5 rises to 50 DEG C of design temperature, is passed through argon gas and is protected, and argon gas flow velocity is
6L/min, anode is made with chromium plate, and clean steel disc is made negative electrode, is electrolysed, and electric current during electrolysis using 65 amperes/square decimeter is close
Degree；
Step 7, after electrolysis terminates, carbon steel coupon is taken out rapidly, cleaning in ultrasonic washing instrument (power 400W) is put into
After 10min, then rinsed repeatedly with distilled water, dry after it is standby；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at 700 DEG C, protected during annealing using argon gas-hydrogen gas mixture
Shield, flow velocity is 6L/min, anti-oxidation, and hydrogen is anti-oxidation for aiding in, and the volume ratio of argon gas and hydrogen is 100:1, obtain Cr-
Fe graded composite anti-corrosion materials.
Embodiment 3
A kind of Cr-Fe graded composites anti-corrosion material, is specifically prepared according to following steps：
Step 1,1000# carbon steel coupons are polishing to surfacing light on sand paper, obtain smooth steel disc；
Step 2, smooth steel disc is put into the NaOH solution that concentration is 5g/100ml and soaks 5min, then taken out, obtain
Alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5%, soaks 5min, then take out, obtain
To acid treatment steel disc；
Step 4, acid treatment steel disc is placed in 70% alcohol, be then put into together with 70% alcohol in ultrasonic cleaning instrument
Concussion cleaning 5min, then takes out, dries up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after, chromic anhybride it is dense
Spend for 200g/L, the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent is water；
Step 6, the preparation electrolyte of step 5 rises to 50 DEG C of design temperature, is passed through argon gas and is protected, and argon gas flow velocity is
6L/min, anode is made with chromium plate, and clean steel disc is made negative electrode, is electrolysed, and electric current during electrolysis using 50 amperes/square decimeter is close
Degree；
Step 7, after electrolysis terminates, carbon steel coupon is taken out rapidly, cleaning in ultrasonic washing instrument (power 400W) is put into
After 10min, then rinsed repeatedly with distilled water, dry after it is standby；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at 760 DEG C, protected during annealing using argon gas-hydrogen gas mixture
Shield, flow velocity is 5L/min, anti-oxidation, and hydrogen is anti-oxidation for aiding in, and the volume ratio of argon gas and hydrogen is 100:1, obtain Cr-
Fe graded composite anti-corrosion materials.
Embodiment 4
A kind of Cr-Fe graded composites anti-corrosion material, is specifically prepared according to following steps：
Step 1,1500# carbon steel coupons are polishing to surfacing light on sand paper, obtain smooth steel disc；
Step 2, smooth steel disc is put into the NaOH solution that concentration is 5g/100ml and soaks 5min, then taken out, obtain
Alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5%, soaks 5min, then take out, obtain
To acid treatment steel disc；
Step 4, acid treatment steel disc is placed in 70% alcohol, be then put into together with 70% alcohol in ultrasonic cleaning instrument
Concussion cleaning 5min, then takes out, dries up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after, chromic anhybride it is dense
Spend for 250g/L, the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent is water；
Step 6, the preparation electrolyte of step 5 rises to 50 DEG C of design temperature, is passed through argon gas and is protected, and argon gas flow velocity is
6L/min, anode is made with chromium plate, and clean steel disc is made negative electrode, is electrolysed, and electric current during electrolysis using 55 amperes/square decimeter is close
Degree；
Step 7, after electrolysis terminates, carbon steel coupon is taken out rapidly, cleaning in ultrasonic washing instrument (power 400W) is put into
After 10min, then rinsed repeatedly with distilled water, dry after it is standby；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at 800 DEG C, protected during annealing using argon gas-hydrogen gas mixture
Shield, flow velocity is 5L/min, anti-oxidation, and hydrogen is anti-oxidation for aiding in, and the volume ratio of argon gas and hydrogen is 100:1, obtain Cr-
Fe graded composite anti-corrosion materials.
Embodiment 5
A kind of Cr-Fe graded composites anti-corrosion material, is specifically prepared according to following steps：
Step 1,2000# carbon steel coupons are polishing to surfacing light on sand paper, obtain smooth steel disc；
Step 2, smooth steel disc is put into the NaOH solution that concentration is 5g/100ml and soaks 5min, then taken out, obtain
Alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5%, soaks 5min, then take out, obtain
To acid treatment steel disc；
Step 4, acid treatment steel disc is placed in 70% alcohol, be then put into together with 70% alcohol in ultrasonic cleaning instrument
Concussion cleaning 5min, then takes out, dries up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after, chromic anhybride it is dense
Spend for 350g/L, the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent is water；
Step 6, the preparation electrolyte of step 5 rises to 50 DEG C of design temperature, is passed through argon gas and is protected, and argon gas flow velocity is
6L/min, anode is made with chromium plate, and clean steel disc makees negative electrode, carries out electrolysis diffusion experiment, and 60 amperes/square decimeter are used during electrolysis
Current density；
Step 7, after electrolysis terminates, steel disc is taken out rapidly, cleaning 10min in ultrasonic washing instrument (power 400W) is put into
Afterwards, then rinsed repeatedly with distilled water, dry after it is standby；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at 900 DEG C respectively, argon gas-hydrogen mixed gas is used during annealing
Body is protected, and flow velocity is 4L/min, anti-oxidation, and hydrogen is anti-oxidation for aiding in, and the volume ratio of argon gas and hydrogen is 100:1, obtain
To Cr-Fe graded composite anti-corrosion materials.
Chromium content in embodiment 1-5 anti-corrosion material is measured respectively, as a result respectively as shown in figure 1, Fig. 1 (a), figure
1 (b), Fig. 1 (c), Fig. 1 (d), Fig. 1 (e) correspond to the anti-of embodiment 1, embodiment 2, embodiment 3, embodiment 4 and embodiment 5 respectively
Rotten material.As a result show to can be seen that with the increase of annealing temperature in preparation method from embodiment 1-5, chromium in anti-corrosion material
Content gradually increases.
Fig. 2 is the ESEM view on the anti-corrosion material surface of embodiment 1, and Fig. 3 is the anti-corrosion material section of embodiment 1
ESEM view, can be seen that clearly layers of chrome from Fig. 2 and Fig. 3.
We are tested the embodiment 1-4 anti-corrosion materials prepared respectively, the corrosion potential of test sample, wherein matrix
Using 320# carbon steel coupons, as a result as shown in figure 4, Fig. 4 is the polarization curve of matrix and different anti-corrosion materials, 1#-4# curves difference
Correspondence embodiment 1-4 anti-corrosion material.
Curve in Fig. 4 is fitted, the result shown in table 1 is obtained.As shown in Table 1, from matrix to embodiment 1-4's
Anti-corrosion material, corrosion potential increases successively, and corrosion electric current density is sequentially reduced, and polarization resistance increases successively.Commented according to corrosion resistance
Price card is accurate：In general, corrosion potential is higher, and corrosion electric current density is smaller, and polarization resistance is bigger, then sample decay resistance is got over
It is good.The corrosion resistance of this explanation embodiment 1-4 method material is higher than matrix, and with the increase functionally gradient material (FGM) of chrome content
Corrosion resistance strengthens successively.
The parameter fitting result of the matrix of table 1 and functionally gradient material (FGM)
, but those skilled in the art once know basic creation although preferred embodiments of the present invention have been described
Property concept, then can make other change and modification to these embodiments.So, appended claims are intended to be construed to include excellent
Select embodiment and fall into having altered and changing for the scope of the invention.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.So, if these modifications and variations of the present invention belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these changes and modification.
Claims (5)
1. a kind of preparation method of Cr-Fe graded composites anti-corrosion material, it is characterised in that specifically include following steps
Step 1, carbon steel coupon is polishing to surfacing light, obtains smooth steel disc；
Step 2, smooth steel disc is put into 5g/100ml NaOH solution and soaked, then taken out, obtain alkali process steel disc；
Step 3, alkali process steel disc is placed in the hydrochloric acid solution that volume fraction is 5% and soaked, then taken out, obtain acid treatment steel
Piece；
Step 4, acid treatment steel disc is placed in 70% alcohol, cleans, then take out, dry up, obtain clean steel disc；
Step 5, electrolyte is prepared：Electrolyte by water, auxiliary agent, the concentrated sulfuric acid mixed with chromic anhybride after, and chromium in electrolyte
The concentration of acid anhydrides is 150-400g/L, and the mass ratio of auxiliary agent, the concentrated sulfuric acid and chromic anhybride is 0.5g:1ml:100g, solvent is water；
Step 6, the preparation electrolyte of step 5 rises to design temperature, is passed through argon gas and is protected, and anode, clean steel are made with chromium plate
Piece makees negative electrode, is electrolysed；
Step 7, after electrolysis terminates, carbon steel coupon is taken out, is put into ultrasonic washing instrument and cleans, then with distilled water flushing, baking
It is standby after dry, obtain being electrolysed sample after heavy chromium；
Step 8, sample after the heavy chromium of electrolysis is annealed 4 hours at a temperature of 660-940 DEG C, using argon gas-hydrogen mixing during annealing
Gas shield, obtains Cr-Fe graded composite anti-corrosion materials.
2. the preparation method of Cr-Fe graded composites anti-corrosion material according to claim 1, it is characterised in that in step 5,
The auxiliary agent is one kind in potassium chloride, dipotassium hydrogen phosphate or citric acid.
3. the preparation method of Cr-Fe graded composites anti-corrosion material according to claim 1, it is characterised in that in step 6,
Design temperature is 50 DEG C, using the current density of 35-65 amperes/square decimeter during electrolysis.
4. the preparation method of Cr-Fe graded composites anti-corrosion material according to claim 1, it is characterised in that in step 8,
The volume ratio of argon gas and hydrogen is 100:1.
5. the Cr-Fe graded composite anti-corrosion materials being prepared from according to any one of claim 1-4 methods described.
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Cited By (1)
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| CN112695362A (en) * | 2020-12-17 | 2021-04-23 | 桂林理工大学 | Preparation method of porous metal zinc material |
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