CN109778105A - A kind of amorphous composite coating and preparation method thereof - Google Patents
A kind of amorphous composite coating and preparation method thereof Download PDFInfo
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- CN109778105A CN109778105A CN201910172412.6A CN201910172412A CN109778105A CN 109778105 A CN109778105 A CN 109778105A CN 201910172412 A CN201910172412 A CN 201910172412A CN 109778105 A CN109778105 A CN 109778105A
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Abstract
The invention discloses a kind of amorphous composite coatings and preparation method thereof, it include: that the composite granule being made of graphene oxide powder and metal powder is added in the mixed liquor being made of binder, dispersing agent and deionized water, mixed slurry is obtained through sonic oscillation, mechanical stirring, again by mixed slurry mist projection granulating, graphene-metal composite powder is heat-treated to obtain, matrix surface is pre-processed into even application nickel alclad bond coating；Using graphene-metal composite powder and Fe-based amorphous alloy powder as feeding powder, thermal spraying is carried out in matrix surface through multichannel powder feeding, obtains the Fe-based amorphous composite coating of graphene-metal-of abrasion resistant and corrosion resistant, more single amorphous coating, its abrasion loss reduces by 73%, and corrosion potential amplitude improves.
Description
Technical field
The invention belongs to technical field of surface coating, and in particular to a kind of amorphous composite coating and preparation method thereof.
Background technique
Amorphous alloy is by the super longrange disorder structure being quenched and solidified, and the crystal grain of crystal alloy, crystal boundary do not exist,
The special construction of amorphous alloy determines it with unique magnetic property, mechanical property, electrical property, corrosion resistance etc., by amorphous
Alloy is used for material surface technical field as coating material, can play good protective action.Wherein, Fe-based amorphous alloy
Typical feature is (such as B, P, C) containing a large amount of metalloids, can promote amorphous formation, and form passivating film to a certain extent, add
The corrosion resistance of strong amorphous alloy.Chu Zhenhua et al. (Surface and Coatings Technology, 2016,292
(25): 44-48.) research points out that iron-based amorphous coating can increase substantially the wear-resisting property of steel matrix.
But amorphous alloy, because its brittleness problems influences to apply, especially Fe-based amorphous toughness is poor, causes Fe-based amorphous
Coating is under abrasive wear conditions in use, the case where being especially easy to appear localized delamination under impact stress, seriously affects its use
Effect, under abrasive conditions caused by influence more serious because once part is peeled off, corrosive liquid enters matrix, coating with
The potential difference of matrix, the corrosion of matrix can be accelerated by forming galvanic interaction.
The Chinese invention patent of Publication No. CN104861760A discloses graphene composite coating, to be coated on matrix
Surface, graphene uniform dispersion are added and improve the interface bond strength of coating, effectively promote the mechanical property of composite material, make
Strengthen the anti-oxidant of the substrate, acid and alkali-resistance and mechanical strength etc. for strengthened coat.It can be seen that graphene is introduced Fe-based amorphous
In coating, the mechanical performance of amorphous coating, anti-oxidant and acid-alkali-corrosive-resisting can be improved.However, graphene density is smaller, it is non-
Crystalline flour density is larger, how the big graphene of density variation and non-crystalline flour is deposited on matrix surface simultaneously, obtains graphene/iron
Base amorphous composite coating is still problem.Metallic nickel materials are hard and ductility is good, while having good ferromagnetism and corrosion-proof wear
Property, stainless steel prepared therefrom and various steel alloys are widely used in aircraft, tank, submarine, radar, guided missile, spaceship
Machine manufacture, ceramic paint, permanent-magnet material, electronic telecontrol etc. in the fields such as civilian industry, are used in graphite as carrier
Alkene has not been reported with Fe-based amorphous co-deposition in the research of matrix surface.
Summary of the invention
The main purpose of the present invention is to provide a kind of preparation methods of amorphous composite coating, mainly solve graphene density
Smaller rather than crystalline flour density is larger to lead to that graphene and non-crystalline flour are difficult to while uniform deposition is in matrix surface, and directly prepares
The problem of graphene coating needs height and low efficiency.Specifically:
(1) using spray granulation that nickel powder and the progress of graphene oxide powder is compound, then stone will be aoxidized by thermal reduction
Black alkene is reduced into graphene, using nickel metal as the carrier of graphene, solve graphene density it is small be difficult to direct spraying and its with
Metal powder is difficult to evenly dispersed problem.
(2) plasma spraying technology high by gas ionization degree, that temperature is high, energy is concentrated guarantees graphene spray coated
It is not oxidized and modified in journey.
(3) multichannel powder feeding technology is used, it is by the difference of powder feeding air-flow in different channels that composite powder is common with amorphous
It is deposited on matrix surface, solves the problems, such as that graphene ratio regulates and controls and is uniformly distributed in composite coating.
Another object of the present invention is to provide the amorphous as made from the preparation method of above-mentioned amorphous composite coating is compound
Coating, wearability and corrosion resistance are high.
Above-mentioned purpose of the invention is achieved through the following technical solutions:
In a first aspect, the preparation method of amorphous composite coating, specifically, comprising the following steps:
(1) by be 0.1~10wt.% by mass percent graphene oxide powder and mass percent be 90~
The composite granule of the metal powder composition of 99.9wt.% is added to the mixed solution being made of binder, dispersing agent and deionized water
In, it is uniformly mixed after 0.2~0.5h of sonic oscillation, 0.5~3h of mechanical stirring, mixed slurry is made；Again by above-mentioned mixing slurry
Expect mist projection granulating, graphene-metal composite powder is made in thermal reduction；
(2) by matrix successively after surface polishing, the pretreatment of dehydrated alcohol ultrasonic cleaning and surface sand-blasting, in its table
Face even application is with a thickness of 80~120 μm of nickel alclad bond coating；Wherein, in the nickel alclad bond coating Ni/Al grain
Degree is 140~320 mesh；
(3) conduct after mixing graphene-metal composite powder described in step (1) and Fe-based amorphous alloy powder arbitrary proportion
Feeding powder carries out thermal spraying in the matrix surface that step (2) is handled well through multichannel powder feeding, is made with a thickness of 50~500 μm
The Fe-based amorphous composite coating of graphene-metal-.
In step (1), the graphene oxide powder is single-layer or multi-layer graphene oxide, with a thickness of 0.1~10 μm, lamella
Diameter is 5~100 μm；
The metal powder is metallic nickel and/or its alloy, and partial size is 0.5~50 μm；
The binder is sodium carboxymethylcellulose, and dosage accounts for the 30%~70% of the composite granule gross mass；
The dispersing agent is sodium polyphosphate, and dosage accounts for the 0.5%~3% of the composite granule gross mass；
The dosage of the deionized water accounts for the 100%~300% of the composite granule gross mass.
In step (1), the mist projection granulating carries out in spray drying tower, and inlet temperature is 150~300 DEG C, outlet
Temperature is 100~140 DEG C, and pressure is 0.5~1MPa, and the revolving speed of atomizing disk is 15000~30000r/min in spray drying tower,
The mixed slurry is shrunk to the compound feeding ball that partial size is 20~70 μm under surface tension effects；
The thermal reduction carries out in vacuum heat treatment furnace, and protective gas is at least one of hydrogen, argon gas and nitrogen,
Gas flow is 600mL/min, and reduction temperature is 300~500 DEG C, and soaking time is 30~120min, cools to room temperature with the furnace.
In step (2), described matrix is stainless steel, carbon steel or alloy material.
In step (3), the thermal spraying be selected from plasma spraying, Supersonic Plasma Spraying, the steady plasma spraying of water or
One of high speed plasma spraying.
Further, the thermal jet is painted with plasma spraying, technique are as follows: compound feeding powder gun internal powder conveying, spray gun speed
Degree is 10~15m/min, and rifle is away from being 80~110mm, and spray power is 30~35kW, and the powder feeding gas in powder feeder is N2, gas
Body flow is 30~130L/h.
In step (3), for the Fe-based amorphous alloy powder through outer tunnel powder feeding, powder feeding gas is N2, powder feeding gas flow is
50~200L/min；Graphene-the metal composite powder is Ar gas through internal channel powder feeding, powder feeding gas, and powder feeding gas flow is
20~100L/min；The Fe-based amorphous alloy powder, include: by mass percentage Cr 25%~27%, C 2%~
2.5%, Mo 16%~18%, B 2%~2.2%, surplus Fe；The Fe-based amorphous alloy powder is spherical, subsphaeroidal or class
Spherical powder, average particle size are 49~50 μm.
Second aspect, amorphous composite coating are made by the preparation method of above-mentioned amorphous composite coating, with a thickness of 50~
500μm。
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention is carried out nickel powder and graphene by mist projection granulating compound, is solved graphene light weight and is difficult to directly send
Enter to spray the problems in flame stream, the defect relatively high to equipment requirement when overcoming graphene for coating, production efficiency is low.
2, the composite coating of abrasion resistant and corrosion resistant is made by the nickel of high-intensitive graphene and high corrosion-resistant in the present invention,
The more single amorphous coating of abrasion loss reduces by 73%, and corrosion potential amplitude improves.
Detailed description of the invention
Fig. 1 is the scanning figure in embodiment 1 under 1000 times of graphene-nickel composite powder.
Fig. 2 is the Raman curve graph of the Fe-based amorphous composite coating of graphene-nickel-in embodiment 4.
Fig. 3 is the surface topography map of the Fe-based amorphous composite coating of graphene-nickel-in embodiment 4.
Fig. 4 is the abrasion spirogram of the Fe-based amorphous composite coating of graphene-nickel-, iron-based amorphous coating in embodiment 4 and 5.
Fig. 5 is the polarization curve of the Fe-based amorphous composite coating of graphene-nickel-, iron-based amorphous coating in embodiment 4 and 5.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
In following instance, Fe-based amorphous alloy powder used is spherical, subsphaeroidal or spherical powder, average particle size 49
~50 μm, include: by mass percentage Cr 25%~27%, C 2%~2.5%, Mo 16%~18%, B 2%~
2.2%, surplus Fe.
Binder used is by mixing sodium carboxymethylcellulose and deionized water 1:100 in mass ratio, and heating water bath is extremely
Mechanical stirring 1h after 95 DEG C and obtain.
Dispersing agent used is sodium polyphosphate.
Embodiment 1
(1) it weighs and is with a thickness of 0.1~10 μm, the single-layer graphene oxide powder that lamella diameter is 5~100 μm and partial size
Composite granule is formed after the mixing of 0.5~50 μm of metal nickel powder, in mass ratio 1:49, is added to by binder, dispersing agent and goes
Ionized water account for respectively composite granule gross mass 38%, 1.3% and 180% composition mixed solution in, through sonic oscillation 0.5h,
After mechanical stirring 0.5h, mixed slurry is made.
(2) above-mentioned mixed slurry is subjected to mist projection granulating in spray drying tower, inlet temperature is 150 DEG C, outlet temperature
Degree is 100 DEG C, pressure 0.5MPa, and the revolving speed of atomizing disk is 15000r/min in spray drying tower, under surface tension effects
Mixed slurry is shrunk to the compound feeding ball that partial size is 20~40 μm.
(3) above-mentioned compound feeding ball is heat-treated in vacuum heat treatment furnace, protective gas is hydrogen, gas stream
Amount is 600mL/min, is warming up to 300 DEG C with 5 DEG C/min, keeps the temperature 120min, cool to room temperature with the furnace, it is multiple to obtain graphene-metal
Close powder.
After tested, the pattern observed under scanning electron microscope under its 1000 times is as shown in Figure 1, it can be seen that the group of the composite powder
Poly- effect is good, and powder is spherical in shape or subsphaeroidal.
Embodiment 2
(1) it weighs and is with a thickness of 0.1~10 μm, the multilayer graphene oxide powder that lamella diameter is 5~100 μm and partial size
0.5~50 μm of nickel alloy powder, in mass ratio 1:9 mixing after form composite granule, be added to by binder, dispersing agent and go from
Sub- water is accounted for respectively in the mixed solution of 30%, 0.5% and 100% composition of composite granule gross mass, through sonic oscillation 0.2h, machine
After tool stirs 3h, mixed slurry is made.
(2) above-mentioned mixed slurry is subjected to mist projection granulating in spray drying tower, inlet temperature is 300 DEG C, outlet temperature
Degree is 140 DEG C, pressure 1MPa, and the revolving speed of atomizing disk is 30000r/min in spray drying tower, is mixed under surface tension effects
It closes slurry and is shrunk to the compound feeding ball that partial size is 40~70 μm.
(3) above-mentioned compound feeding ball is heat-treated in vacuum heat treatment furnace, protective gas is argon gas, gas stream
Amount is 600mL/min, is warming up to 500 DEG C with 5 DEG C/min, keeps the temperature 30min, cool to room temperature with the furnace, obtain graphene-metal composite
Powder.
Embodiment 3
(1) it weighs and is with a thickness of 0.1~10 μm, the single-layer graphene oxide powder that lamella diameter is 5~100 μm and partial size
Composite granule is formed after the mixing of 0.5~50 μm of nickel alloy powder, in mass ratio 1:99, is added to by binder, dispersing agent and goes
Ionized water is accounted for respectively in the mixed solution of 70%, 3% and 300% composition of composite granule gross mass, through sonic oscillation 0.3h, machine
After tool stirs 1h, mixed slurry is made.
(2) above-mentioned mixed slurry is subjected to mist projection granulating in spray drying tower, inlet temperature is 200 DEG C, outlet temperature
Degree is 120 DEG C, pressure 0.8MPa, and the revolving speed of atomizing disk is 20000r/min in spray drying tower, under surface tension effects
Mixed slurry is shrunk to the compound feeding ball that partial size is 40~70 μm.
(3) above-mentioned compound feeding ball is heat-treated in vacuum heat treatment furnace, protective gas is nitrogen, gas stream
Amount is 600mL/min, is warming up to 400 DEG C with 5 DEG C/min, keeps the temperature 60min, cool to room temperature with the furnace, obtain graphene-metal composite
Powder.
Embodiment 4
Matrix uses 45# steel, prepares the Fe-based amorphous composite coating of graphene-nickel-using plasma spraying technology, specific to walk
Suddenly are as follows:
(1) by 45# steel successively after surface polishing, the pretreatment of dehydrated alcohol ultrasonic cleaning and surface sand-blasting, at it
Surface even application is with a thickness of 80~120 μm of nickel alclad bond coating, and the granularity of Ni/Al is 140 in nickel alclad bond coating
~320 mesh.
(2) using 1 gained graphene of embodiment-metal composite powder and Fe-based amorphous alloy powder 1:19 in mass ratio as feeding
Powder, the matrix surface through multichannel powder feeding after treatment carry out plasma spraying, and spraying power is 35kw, and spray gun speed is 10m/
min；Wherein, for Fe-based amorphous alloy powder through outer tunnel powder feeding, powder feeding gas is N2, powder feeding gas flow is 50~200L/min,
For graphene-metal composite powder through internal channel powder feeding, powder feeding gas is Ar gas, and powder feeding gas flow is 20~100L/min, is obtained thick
The Fe-based amorphous composite coating of graphene-metal-that degree is 50~500 μm.
Raman spectrum detection will be carried out after the Fe-based amorphous composite coating sanding and polishing of the resulting graphene-nickel-of embodiment 4,
In 1350cm-1Left and right and 1580cm-1The position of left and right can obviously see the peak D and the peak G of graphene, it was demonstrated that graphene has succeeded
Be deposited on matrix surface, it is as shown in Figure 3 which observes its pattern under scanning electron microscope, it can be seen that composite powder be uniformly distributed and
Compact structure.
Embodiment 5
Matrix is 45# steel, prepares the Fe-based amorphous composite coating of graphene-nickel-, preparation method using plasma spraying technology
It is same as Example 4, the difference is that the mass ratio of graphene-nickel composite powder and Fe-based amorphous powder is 3:17.
Using state's production and marketing disc type SFT-2M friction wear testing machine respectively to iron-based amorphous coating, embodiment 4 and embodiment 5
The Fe-based amorphous composite coating of graphene-nickel-carry out friction and wear test, abrading-ball uses diameter for the Si of 4mm3N4Ceramic Balls carry
Lotus is 30N.
Referring to fig. 4, the Fe-based amorphous composite coating friction of the graphene-nickel-of iron-based amorphous coating, embodiment 4 and embodiment 5
Amount is it is found that the wearability of the Fe-based amorphous composite coating of graphene-nickel-has to be mentioned greatly very much compared with single coating iron-based amorphous coating
Height, abrasion loss reduce about 73%.
Using Gamry electrochemical workstation respectively to the graphene-nickel-of iron-based amorphous coating, embodiment 4 and embodiment 5
Fe-based amorphous composite coating carries out electro-chemical test, the NaCl solution that etchant solution is 3.5%.
Referring to Fig. 5, the Fe-based amorphous composite coating tower of the graphene-nickel-of iron-based amorphous coating, embodiment 4 and embodiment 5 is luxuriant and rich with fragrance
For that polarization curve it is found that compared with single coating iron-based amorphous coating, the corrosion of the Fe-based amorphous composite coating of graphene-nickel-is electric
Position greatly improves.
In conclusion be added in iron-based amorphous coating graphene and metal component can effectively improve coating wearability and
Corrosion resistance.
Claims (10)
1. a kind of preparation method of amorphous composite coating, which comprises the following steps:
(1) by be 0.1~10wt.% by mass percent graphene oxide powder and mass percent be 90~99.9wt.%
Metal powder composition composite granule be added to by account for the composite granule gross mass respectively 30%~70%, 0.5%~3%
With 100%~300% binder, dispersing agent and deionized water form mixed solution in, through 0.2~0.5h of sonic oscillation,
Mixed slurry is obtained after 0.5~3h of mechanical stirring, then by above-mentioned mixed slurry mist projection granulating, it is multiple that graphene-metal is made in thermal reduction
Close powder；
(2) after pre-processing matrix surface, in its surface even application with a thickness of 80~120 μm of nickel alclad bond coating；
(3) feeding is used as after mixing gained graphene-metal composite powder in step (1) and Fe-based amorphous alloy powder arbitrary proportion
Powder carries out thermal spraying in the matrix surface that step (2) is handled well through multichannel powder feeding, the graphite with a thickness of 50~500 μm is made
The Fe-based amorphous composite coating of alkene-metal-.
2. the preparation method of amorphous composite coating according to claim 1, which is characterized in that in step (1), the oxidation
Graphene powder is single-layer graphene oxide or multilayer graphene oxide, and with a thickness of 0.1~10 μm, lamella diameter is 5~100 μm；
The metal powder is metallic nickel or its alloy, and partial size is 0.5~50 μm；
The binder is sodium carboxymethylcellulose；
The dispersing agent is sodium polyphosphate.
3. the preparation method of amorphous composite coating according to claim 1, which is characterized in that described spraying in step (1)
Granulation carries out in spray drying tower, and inlet temperature is 150~300 DEG C, and outlet temperature is 100~140 DEG C, pressure 0.5
~1MPa, the revolving speed of atomizing disk is 15000~30000r/min, the mixing slurry under surface tension effects in spray drying tower
Material is shrunk to the compound feeding ball that partial size is 20~70 μm.
4. the preparation method of amorphous composite coating according to claim 1, which is characterized in that the thermal reduction is in Vacuum Heat
It is carried out in treatment furnace, protective gas is at least one of hydrogen, argon gas and nitrogen, gas flow 600mL/min, reduction temperature
Degree is 300~500 DEG C, and soaking time is 30~120min, cools to room temperature with the furnace.
5. the preparation method of amorphous composite coating according to claim 1, which is characterized in that in step (2), described matrix
For stainless steel, carbon steel or alloy material, surface preparation include surface polishing, and/or dehydrated alcohol ultrasonic cleaning and/
Or surface sand-blasting；
The granularity of Ni/Al is 140~320 mesh in the nickel alclad bond coating.
6. the preparation method of amorphous composite coating according to claim 1, which is characterized in that in step (3), the thermal jet
It applies selected from one of plasma spraying, Supersonic Plasma Spraying, the steady plasma spraying of water or high speed plasma spraying.
7. the preparation method of amorphous composite coating according to claim 1 or 6, which is characterized in that described in step (3)
Thermal jet be painted with plasma spraying, technique are as follows: compound feeding powder gun internal powder conveying, spray gun speed be 10~15m/min, rifle away from for
80~110mm, spray power are 30~35kW, and the powder feeding gas in powder feeder is N2, gas flow is 30~130L/h.
8. the preparation method of amorphous composite coating according to claim 1, which is characterized in that in step (3),
For the Fe-based amorphous alloy powder through outer tunnel powder feeding, powder feeding gas is N2, the flow of powder feeding gas is 50~200L/min；
For the graphene-metal composite powder through internal channel powder feeding, powder feeding gas is Ar gas, the flow of powder feeding gas is 20~
100L/min。
9. the preparation method of amorphous composite coating according to claim 1, which is characterized in that the Fe-based amorphous alloy powder
For spherical, subsphaeroidal or spherical powder, average particle size is 49~50 μm, include: by mass percentage Cr 25%~
27%, C 2%~2.5%, Mo 16%~18%, B 2%~2.2%, surplus Fe.
10. amorphous composite coating is made by the preparation method of any one of the claim 1~9 amorphous composite coating, thick
Degree is 50~500 μm.
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| CN110629153A (en) * | 2019-10-18 | 2019-12-31 | 常州大学 | Preparation method of graphene nanosheet/amorphous iron-based composite coating |
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Application publication date: 20190521 |