CN107400843A - The graphene of temperature indicating thermal barrier coating is modified hot spray powder preparation method - Google Patents
The graphene of temperature indicating thermal barrier coating is modified hot spray powder preparation method Download PDFInfo
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- CN107400843A CN107400843A CN201710507596.8A CN201710507596A CN107400843A CN 107400843 A CN107400843 A CN 107400843A CN 201710507596 A CN201710507596 A CN 201710507596A CN 107400843 A CN107400843 A CN 107400843A
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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Abstract
The present invention provides a kind of dusty spray of tungsten carbide containing modified graphene for being used to prepare self-lubricating wear-resistant coating, comprises the following steps：1）Weigh a certain amount of modified graphene/nano silicon carbide composite tungsten material.Mixed with a certain amount of absolute ethyl alcohol, the mixed solution of graphene/nanometer tungsten carbide composite is obtained after ultrasonic disperse.2）A certain amount of tungsten carbide/cobalt dusty spray is weighed, is added in the mixed solution of graphene nano tungsten carbide composite.3）The tungsten carbide/cobalt dusty spray for being compounded with modified graphene is obtained using the method for vacuum freeze drying.4）The tungsten carbide/cobalt self-lubricating wear-resistant coating for being compounded with modified graphene is prepared using piece surface of the hot-spraying technique after cleaning, sandblasting.The present invention had both remained with the stratiform individual layer carbonaceous architectural characteristic of graphene, and the nano silicon carbide composition granule of growth improves the proportion of graphene again, using the method for freeze-drying ball milling or other blending processes of powders can be avoided to cause the loss of graphene in addition.
Description
Technical field
The invention belongs to graphene/nanometer tungsten carbide composite technical field, more particularly to one kind to be used to prepare
The dusty spray of tungsten carbide containing modified graphene of self-lubricating wear-resistant coating.
Background technology
Thermal spraying tungsten carbide coating has higher microhardness, and preferable wearability, oxide content are low, and coating combines
The advantages such as intensity height, it is conventional wear-resistant coating, is widely used to the equipment of the industrial circles such as Aeronautics and Astronautics, nuclear energy, machinery
Crucial fricting movement pair component surface wear Protection.But in actual working environment, due to the higher hardness of tungsten carbide coating,
The coefficient of friction of friction system is larger, can pair friction pair coordinated with it produce more serious abrasion, or even influence wear Protection
The service life of coating.In addition, with scientific and technological progress, industrial production increasingly develops to increasingly automated, high speed direction, many
Part (such as bearing, bushing, sealing ring, piston rod) is usually severe in heavy duty, high speed, high temperature, low temperature, high vacuum, deep-etching etc.
Carve and worked under environmental condition, such environment has not only surmounted the operating limit of lubricating oil or fat, also makes answering for tungsten carbide coating
With being limited to, it is therefore necessary to the tungsten carbide coating with self-lubricating property is developed, to meet to take under extreme friction condition
Labour.
Tungsten carbide dusty spray is the basis that thermal spraying prepares tungsten carbide wear-resistant coating, to be prepared with self-lubricating property
Tungsten carbide wear-resistant coating, it is necessary to self-lubricating additive is added in tungsten carbide dusty spray, is added at present into dusty spray
Self-lubricating agent mainly include soft metal (Au, Ag etc.), fluoride (LiF2, CaF2 etc.), disulphide (MoS2, WS2 etc.) and
Metal oxide (Zr2O3, Cr2O3 etc.), prior art mutually have been carried out much grinding to these lubricants as the lubrication of coating
Study carefully.But these additives there are some limitations, such as the rise in friction process with temperature, sulfide in the coating is added
Lubrication is mutually oxidized easily, and tribological property seriously reduces, especially serious in wet environment；Although alkaline-earth metal and rare gold
The fluoride of category has high-temperature self-lubrication performance, but its tribological property is very poor during low temperature, and fragility is presented.
Through studying for a long period of time, analyzing, it is found that graphene is that carbon atom is tightly packed into individual layer bi-dimensional cellular shape lattice structure
A kind of carbonaceous new material, it is the elementary cell of the most frequently used kollag-graphite of structure, there is the friction system lower than graphite
Number, is a kind of new self-lubricant anti-friction coating additive.But graphene is the carbon material of nanoscale single layer structure, quality compared with
Gently, ceramic-like tungsten carbide dusty spray quality is big, if graphene is directly appended in tungsten carbide dusty spray, graphene exists
It can be blown in spraying process by high speed flame stream and fly and lose, it is difficult to retain graphene composition in resurfacing.In addition, graphene compares surface
Product is larger, and activity is high, easily reunites with tungsten carbide dusty spray compound tense, it is difficult to ensure that uniformly mixed in dusty spray,
So as to be difficult to ensure for preparing coating has self-lubricating abrasion-resistant characteristic.Therefore, graphene how is improved in tungsten carbide dusty spray
Proportion, ensure the uniform mixing in dusty spray, turn into current urgent problem.
Therefore, in surface of graphene oxide growth in situ nano silicon carbide tungsten particle, by controlling reaction condition to be received to realize
Rice tungsten carbide particle regulates and controls in the yardstick, pattern, distribution of surface of graphene oxide, prepares with certain weight proportion, and energy
Preferably reach the modified graphene oxide of preferable com-patibilising effect with tungsten-carbide powder, carbon is compounded in as self-lubricating additive application
Change in tungsten dusty spray, to improve the coefficient of friction for reducing thermal spraying tungsten carbide coating, expanded and be applied to empty day field
The harsher part self-lubricating abrasion-resistant protection of middle friction duty.
The content of the invention
The technical problems to be solved by the invention are in view of the shortcomings of the prior art, there is provided a kind of carbon containing modified graphene
Change the preparation method of tungsten self-lubricating wear-resistant coating.
Technical scheme is as follows：
A kind of dusty spray of tungsten carbide containing modified graphene for being used to prepare self-lubricating wear-resistant coating, comprises the following steps：
Step 1：A certain amount of modified graphene/nano silicon carbide composite tungsten material is weighed, is ultrasonically treated with a certain amount of absolute ethyl alcohol
The mixed solution of graphene/nanometer tungsten carbide composite is obtained after scattered；
Step 2：A certain amount of tungsten carbide/cobalt dusty spray is weighed, the graphene nano tungsten carbide obtained is added in above-mentioned steps 1 and answers
In the mixed solution of condensation material, using vertical mixer, obtain being modified stone with certain rotating speed stirring certain time under normal temperature condition
The mixed solution of black alkene/nano silicon carbide composite tungsten material and tungsten carbide/cobalt；
Step 3：The mixing of the modified graphene obtained in above-mentioned steps 2/nano silicon carbide composite tungsten material and tungsten carbide/cobalt is molten
Liquid obtains the tungsten carbide/cobalt dusty spray for being compounded with modified graphene using the method for vacuum freeze drying；
Step 4：The tungsten carbide/cobalt dusty spray for being compounded with modified graphene that will be obtained in above-mentioned steps 3, using thermal spraying work
Piece surface of the skill after cleaning, sandblasting prepares the tungsten carbide/cobalt self-lubricating wear-resistant coating for being compounded with modified graphene.
In above-mentioned, in the step 1, in the modified graphene/nano silicon carbide composite tungsten material preparation process before tungstenic
Drive body compound be tungsten carbonyl and ammonium metatungstate mixture in tungsten carbonyl account for ammonium metatungstate and weight/mass percentage composition be 1-5%.
In above-mentioned, in the step 1, graphene is commercial graphene oxide, tungstenic precursor mixture and graphite oxide
The mass ratio of alkene is 1:1-6.
In above-mentioned, in the step 1, graphene weight/mass percentage composition is 0.1- in absolute ethyl alcohol wetting graphene solution
0.5%, deionized water mass percent in graphene solution is 5-8%.
In above-mentioned, in the step 1, sonication treatment time 30-180min, supersonic frequency 10-15Hz.Vibration amplitude arm selects
Use 10mm.Tungstenic precursor compound is added to graphene solution after decentralized processing and the mixed solution formed in whipping process
Absolute ethyl alcohol is constantly instilled, absolute ethyl alcohol amount is instilled and accounts for mixed liquor volume ratio as 1:10-18, stir 30-60min.It will obtain
Solution precipitation filter, it is 70 DEG C -100 DEG C, drying time 10-60min to be placed in baking oven drying temperature, obtains graphene
With the compounding substances of tungstenic precursor mixture, reduction is then passed through with 5-70 DEG C/min heating rates in tubular reduction furnace
Gas H2 flows are 100 sccm, and wherein holding temperature is 700-900 DEG C, soaking time 1-3h, and fully after reaction, it is cold to lead to H2
But to room temperature.Obtaining nano-lamellar structure graphenic surface growth in situ has modified graphene/nano silicon carbide of nanometer tungsten carbide
Composite tungsten material, modified graphene/nano silicon carbide composite tungsten material is mixed with absolute ethyl alcohol, wherein modified graphene/nanometer
The mass ratio that tungsten carbide composite accounts for absolute ethyl alcohol is 1-5%, and sonication treatment time is 30-60min, and supersonic frequency is
15Hz.Vibration amplitude arm selects 10mm, finally obtains dispersed modified graphene/nano silicon carbide composite tungsten material mixed solution.
In above-mentioned, in the step 2, by a certain amount of tungsten carbide/cobalt dusty spray, the modification stone after ultrasonic disperse is added to
Black alkene/nano silicon carbide composite tungsten material mixed solution, wherein modified graphene/nano silicon carbide composite tungsten material and tungsten carbide/cobalt
Dusty spray mass percent is 1-5%, stirs 120min-150min, while heating-up temperature is maintained at 30-40 DEG C, is modified
The solution that graphene/nanometer tungsten carbide composite mixes with tungsten carbide/cobalt dusty spray.
In above-mentioned, in the step 3, processing modified graphene/nanometer tungsten carbide of being sublimated in vacuum freeze-drying system
The solution that composite mixes with tungsten carbide/cobalt dusty spray, its process are that liquid nitrogen constantly instills modified graphene/nano-sized carbon
Change the solution that composite tungsten material mixes with tungsten carbide/cobalt dusty spray, wherein cryogenic temperature is maintained at 0-5 DEG C, and final liquid nitrogen adds
It is 60- to enter amount to account for the solution quality ratio that modified graphene/nano silicon carbide composite tungsten material mixes with tungsten carbide/cobalt dusty spray
70%, the whole process operating time is 20-40min, will then freeze modified graphene/nano silicon carbide composite tungsten material of mixing
The solution mixed with tungsten carbide/cobalt dusty spray is placed in vacuum freeze, vacuumizes 0.1MPa, freezes 30-
40min, then take out and be placed in freeze drying box the 10-15min that thaws, temperature control finally obtains modified graphite at 25-30 DEG C
Alkene/nano silicon carbide composite tungsten material and tungsten carbide/cobalt mixing dusty spray.
In above-mentioned, in the step 4, acquisition is compounded with modified graphene/nano silicon carbide composite tungsten material and carbonization
Tungsten/cobalt dusty spray use detonation flame spraying technique prepare process for self-lubricating wear-resistant coating parameter for：Oxygen and acetylene are thermal source gas
The gas flow ratio of body, oxygen and acetylene is 1.0-1.5, and it is 60-90% that gas, which fills rifle amount, and regulation detonation frequency is 3-7 times/second,
Spray distance is 250-300mm, and powder feeding rate is 0.2-0.7g/s.
The present invention is advantageous in that tungsten carbide is modified using graphene first, acquisition modified graphene/receive
Rice tungsten carbide composite, nano-lamellar structure graphenic surface growth in situ, deposition is set to have the tungsten carbide particle of nanoscale,
Both uniform, Dispersed precipitate of the tungsten carbide in graphene had been served, has served and improves graphene weight, in addition, adopting
Modified graphene/nano silicon carbide composite tungsten material is mixed into spray with the compound acquisition of tungsten carbide/cobalt with the technique of vacuum freeze drying
Powder is applied, the technique can ensure modified graphene/nano silicon carbide composite tungsten material graphite with tungsten carbide/cobalt powder in vacuum bar
Under part, low temperature, which is directly sublimated from liquid to solid-state, obtains dry mixing dusty spray, avoids traditional handicraft powder（Sintering is broken
Broken, vacuum atomizing）Hot conditions oxidative deformation to caused by graphene, it also avoid ball milling and mix lighter weight graphite during powder
Alkene is easily layered with heavier mass tungsten carbide/cobalt solution and can not realize mixed uniformly problem, finally, based on plasma spray technology
Prepare and be compounded with graphene and be modified the graphene uniform of nanoscale twins in the wear-resistant coating of tungsten carbide self-lubricating additive, disperse
Coat inside is distributed in, in friction process, graphene is constantly exposed and forms graphene self-lubricating transfer membrane in wear surface,
Coating coefficient of friction is reduced so as to play, coating abrasion performance is improved, can apply to existing wear part, it is wear-resistant to play anti-attrition
Effect, hydraulic drive component in undercarriage piston rod or engineering machinery can also be applied to（Plunger, piston, connecting rod）
On, current plating hard chrome component is substituted, this can not only be avoided the environmental pollution of Cr VI particle, and substantially reduce coating
Coefficient of friction and wear rate in friction process, improve the service life of part.It can expand accordingly applied in empty day field
The harsher part self-lubricating abrasion-resistant protection of friction duty.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of modified graphene.
Fig. 2 is the scanning electron microscope (SEM) photograph of modified graphene.
Fig. 3 is the high power scanning electron microscope (SEM) photograph of modified graphene.
Fig. 4 is the transmission electron microscope picture for the tungsten carbide self-lubricating wear-resistant coating that thermal spraying is compounded with modified graphene.（In Fig. 4
Arrow show modified graphene）
The tungsten carbide for being compounded with modified graphene prepared by the tungsten carbide coating and the present invention that Fig. 5 is prepared for detonation flame spraying technique is certainly
Lubricating and wear-resisting coating friction coefficient curve.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
In the present invention, the preparation of graphene is modified first（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）Prepared
Journey is as follows：
1g graphene oxides are weighed, 1000g absolute ethyl alcohols is added, uniform stirring mixing, is mixed adding 50g deionized waters
Close, in ultrasonic disperse instrument, from 10mm vibration amplitude arms, sonication treatment time 30min, supersonic frequency 10Hz, obtain graphite
The scattered mixed liquor of alkene, the forerunner that mass percent is mixed into tungstenic for 99% ammonium metatungstate and 1% tungsten carbonyl is weighed respectively
Body mixture, weigh 1g tungstenic precursor mixtures and be added in graphene dispersion solution, stir 30min, in whipping process not
It is disconnected to instill absolute ethyl alcohol, infusion volume 18g, then obtained precipitation is filtered, heat 70 DEG C in an oven, dry 10min, will
Obtained drying powder, is placed in alumina crucible, a certain amount of H2 is led in tubular reduction furnace, H2 flows are l00sccm, with 5
DEG C/min heating rate, 700 DEG C, soaking time 1h are heated to, finally leads to H2 and is cooled to room temperature, obtain modified graphene
（Graphene is modified the self-lubricating abrasion-resistant additive of tungsten carbide）.
Thermal spraying prepares the tungsten-cobalt carbide that the graphene prepared containing the present invention is modified tungsten carbide self-lubricating abrasion-resistant additive
Wear-resistant coating process is as follows：
Modified graphene prepared by the present invention（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）2g is weighed, adds 200g
Absolute ethyl alcohol sonication treatment time is 30min, supersonic frequency 15Hz, and vibration amplitude arm selects 10mm, obtains dispersed modification
Graphene（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）Mixed solution.200gWC-12Co dusty sprays are added to
In modified graphene mixed solution, 120min is stirred, while heating-up temperature is maintained at 35 DEG C, obtains modified graphene/nano-sized carbon
Change the solution that composite tungsten material mixes with tungsten carbide/cobalt dusty spray.Mixed solution is constantly instilled and is placed in the oxygen for filling liquid nitrogen
To change in aluminium crucible, ensure that liquid nitrogen and mixed solution uniformly freeze mixing, wherein liquid nitrogen accounts for mixed solution mass percent 50%,
Whole process 30min, it will then mix solution and be placed in vacuum freeze, and vacuumize 0.1MPa, and freeze 30min,
Then take out and be placed in freeze drying box the 10min that thaws, temperature control finally obtains modified graphene/nano-sized carbon at 25 ~ 30 DEG C
Change composite tungsten material and tungsten carbide/cobalt mixing dusty spray.
Graphene modified coating is prepared using detonation flame spraying, technological parameter is：Oxygen and acetylene flow-rate ratio are 1.2, gas
It is 68% to fill rifle amount, and regulation detonation frequency is 3 times/second, and spray distance 250mm, powder feeding rate is 0.3g/s.Friction test exists
Carried out in CETR micro-moving frictional wear experimental machines, using ball-face way of contact, load 10N, upper sample is diameter 6.5mm's
GCrl5 steel balls, lower sample are 24.9 mm × 7.8mm disc surfaces spray-on coatings, and coating final thickness is 0.2 mm after polishing.
Test parameters is：Wearing- in period 10min, frequency 30 Hz, displacement amplitude D are 2 mm.
It is 0.72 that this example, which prepares tungsten carbide coating average friction coefficient, wear weight loss 4.2mg.Prepare graphene modification
The average friction coefficient of WC-Co coatings is 0.44, wear weight loss 3.1mg.Result of study shows：Graphene modified coating rubs
Wipe coefficient and be less than WC-12Co coatings, illustrate that graphene prepared by the present invention is modified self-lubricating abrasion-resistant additive to tungsten carbide coating
Play preferable self-lubricating property.In addition, graphene, which is modified self-lubricating wear-resistant coating wear extent, is less than original silicon carbide tungsten coating, say
Graphene prepared by the bright present invention is modified self-lubricating abrasion-resistant additive and the wear-resistant effect of anti-attrition is played to tungsten carbide coating.
The modified graphene prepared as shown in Figure 1 for the example, wherein graphene are modified the addition of tungsten carbide self-lubricating abrasion-resistant
The XRD of agent, it can be seen that all characteristic peaks are mutually fitted like a glove with WC thing in figure, and surface graphenic surface is loaded with
WC thing phases.
Fig. 2 show the modified graphene of example preparation, and graphenic surface growth in situ tungsten carbide nano particle is swept
Retouch electron microscope, it can be seen that the tungsten carbide particle of white nanoscale is evenly distributed in graphenic surface, and does not destroy graphite
The original lamellar structure characteristic of alkene.
Fig. 3 is modified graphene prepared by the example, wherein, the high power of graphenic surface growth in situ tungsten carbide particle is swept
Retouch electron microscope, it can be seen that the size of tungsten carbide particle is between 10-20nm, it was demonstrated that tungsten carbide particle yardstick is small, is evenly distributed.
Fig. 4 is modified graphene prepared by the present invention, wherein, graphene is modified tungsten carbide self-lubricating abrasion-resistant additive in carbon
Change the scanning electron microscope (SEM) photograph of uniform powder in tungsten dusty spray, it can be seen that graphene is closely adhered to spraying shown in Fig. 4 arrows
Powder surface, reach preferably compatible.
Fig. 5 is tungsten carbide coating prepared by the example and the tungsten carbide for being compounded with composite modified graphene prepared by the present invention
The wear-resistant coating friction coefficient curve of self-lubricating abrasion-resistant additive.
Embodiment 2：
On the basis of above-described embodiment, further, in the present embodiment, modified graphene（I.e. graphene is modified tungsten carbide from profit
Sliding anti-wear additive）Preparation process is as follows：
2g graphene oxides are weighed, 1000g absolute ethyl alcohols is added, uniform stirring mixing, is mixed adding 60g deionized waters
Close, in ultrasonic disperse instrument, from 10mm vibration amplitude arms, sonication treatment time 60min, supersonic frequency 12Hz, obtain graphite
The scattered mixed liquor of alkene, the forerunner that mass percent is mixed into tungstenic for 99% ammonium metatungstate and 1% tungsten carbonyl is weighed respectively
Body mixture, weigh 1g tungstenic precursor mixtures and be added in graphene dispersion solution, stir 40min, in whipping process not
It is disconnected to instill absolute ethyl alcohol, infusion volume 84g, then obtained precipitation is filtered, heat 80 DEG C in an oven, dry 20min, will
Obtained drying powder, is placed in alumina crucible, a certain amount of H2 is led in tubular reduction furnace, H2 flows are l00sccm, with 20
DEG C/min heating rate, 700 DEG C, soaking time 1h are heated to, finally leads to H2 and is cooled to room temperature, obtain graphene carbon modified
Change the self-lubricating abrasion-resistant additive of tungsten.
Thermal spraying prepares the tungsten-cobalt carbide that the graphene prepared containing the present invention is modified tungsten carbide self-lubricating abrasion-resistant additive
Wear-resistant coating process is as follows：
Modified graphene prepared by the present invention（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）4g is weighed, adds 200g
Absolute ethyl alcohol sonication treatment time is 40min, supersonic frequency 15Hz, and vibration amplitude arm selects 10mm, obtains dispersed modification
Graphene（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）Mixed solution.200gWC-12Co dusty sprays are added to
In modified graphene mixed solution, 140min is stirred, while heating-up temperature is maintained at 35 DEG C, obtains modified graphene/nano-sized carbon
Change the solution that composite tungsten material mixes with tungsten carbide/cobalt dusty spray.Mixed solution is constantly instilled and is placed in the oxygen for filling liquid nitrogen
To change in aluminium crucible, ensure that liquid nitrogen and mixed solution uniformly freeze mixing, wherein liquid nitrogen accounts for mixed solution mass percent 50%,
Whole process 30min, it will then mix solution and be placed in vacuum freeze, and vacuumize 0.1MPa, and freeze 30min,
Then take out and be placed in freeze drying box the 10min that thaws, temperature control finally obtains modified graphene/nano-sized carbon at 25 ~ 30 DEG C
Change composite tungsten material and tungsten carbide/cobalt mixing dusty spray.
Graphene modified coating is prepared using detonation flame spraying, technological parameter is：Oxygen and acetylene flow-rate ratio are 1.3, gas
It is 72%, spray distance 265mm to fill rifle amount, and regulation detonation frequency is 3 times/second, and powder feeding rate is 0.3g/s.Friction test exists
Carried out in CETR micro-moving frictional wear experimental machines, using ball-face way of contact, load 10N, upper sample is diameter 6.5mm's
GCrl5 steel balls, lower sample are 24.9 mm × 7.8mm disc surfaces spray-on coatings, and coating final thickness is 0.2 mm after polishing.
Test parameters is：Wearing- in period 10min, frequency 30 Hz, displacement amplitude D are 2 mm.
It is 0.67 that this example, which prepares tungsten carbide coating average friction coefficient, wear weight loss 3.4mg.Prepare graphene modification
The average friction coefficient of WC-Co coatings is 0.45, wear weight loss 2.7mg.Result of study shows：Graphene modified coating rubs
Wipe coefficient and be less than WC-12Co coatings, illustrate that graphene prepared by the present invention is modified self-lubricating abrasion-resistant additive to tungsten carbide coating
Play preferable self-lubricating property.In addition, graphene, which is modified self-lubricating wear-resistant coating wear extent, is less than original silicon carbide tungsten coating, say
Graphene prepared by the bright present invention is modified self-lubricating abrasion-resistant additive and the wear-resistant effect of anti-attrition is played to tungsten carbide coating.
Embodiment 3：
On the basis of above-described embodiment, further, in the present embodiment, modified graphene（Graphene is modified tungsten carbide self-lubricating
Anti-wear additive）Preparation process is as follows：
3g graphene oxides are weighed, 1000g absolute ethyl alcohols is added, uniform stirring mixing, is mixed adding 700g deionized waters
Close, in ultrasonic disperse instrument, from 10mm vibration amplitude arms, sonication treatment time 120min, supersonic frequency 12Hz, obtain graphite
The scattered mixed liquor of alkene, the forerunner that mass percent is mixed into tungstenic for 99% ammonium metatungstate and 1% tungsten carbonyl is weighed respectively
Body mixture, weigh 1g tungstenic precursor mixtures and be added in graphene dispersion solution, stir 50min, in whipping process not
It is disconnected to instill absolute ethyl alcohol, infusion volume 168g, then obtained precipitation is filtered, heat 80 DEG C in an oven, dry 20min,
The drying powder that will be obtained, is placed in alumina crucible, and a certain amount of H2 is led in tubular reduction furnace, and H2 flows are l00sccm, with
30 DEG C/min heating rate, 800 DEG C, soaking time 2h are heated to, finally lead to H2 and be cooled to room temperature, obtained graphene and be modified
The self-lubricating abrasion-resistant additive of tungsten carbide.
Thermal spraying prepares the tungsten-cobalt carbide that the graphene prepared containing the present invention is modified tungsten carbide self-lubricating abrasion-resistant additive
Wear-resistant coating process is as follows：
Modified graphene prepared by the present invention（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）6g is weighed, adds 200g
Absolute ethyl alcohol sonication treatment time is 40min, supersonic frequency 15Hz, and vibration amplitude arm selects 10mm, obtains dispersed modification
Graphene（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）Mixed solution.200gWC-12Co dusty sprays are added to
In modified graphene mixed solution, 140min is stirred, while heating-up temperature is maintained at 35 DEG C, obtains modified graphene/nano-sized carbon
Change the solution that composite tungsten material mixes with tungsten carbide/cobalt dusty spray.Mixed solution is constantly instilled and is placed in the oxygen for filling liquid nitrogen
To change in aluminium crucible, ensure that liquid nitrogen and mixed solution uniformly freeze mixing, wherein liquid nitrogen accounts for mixed solution mass percent 50%,
Whole process 30min, it will then mix solution and be placed in vacuum freeze, and vacuumize 0.1MPa, and freeze 30min,
Then take out and be placed in freeze drying box the 10min that thaws, temperature control finally obtains modified graphene/nano-sized carbon at 25 ~ 30 DEG C
Change composite tungsten material and tungsten carbide/cobalt mixing dusty spray.
Graphene modified coating is prepared using detonation flame spraying, technological parameter is：Oxygen and acetylene flow-rate ratio are 1.4, gas
It is 68%, spray distance 270mm to fill rifle amount, and regulation detonation frequency is 3 times/second, and powder feeding rate is 0.3g/s.Friction test exists
Carried out in CETR micro-moving frictional wear experimental machines, using ball-face way of contact, load 10N, upper sample is diameter 6.5mm's
GCrl5 steel balls, lower sample are 24.9 mm × 7.8mm disc surfaces spray-on coatings, and coating final thickness is 0.2 mm after polishing.
Test parameters is：Wearing- in period 10min, frequency 30 Hz, displacement amplitude D are 2 mm.
It is 0.62 that this example, which prepares tungsten carbide coating average friction coefficient, wear weight loss 3.5mg.Prepare graphene modification
The average friction coefficient of WC-Co coatings is 0.40, wear weight loss 2.2mg.Result of study shows：Graphene modified coating rubs
Wipe coefficient and be less than WC-12Co coatings, increase as graphene is modified content of the self-lubricating abrasion-resistant additive in tungsten-carbide powder,
The graphene of preparation, which is modified self-lubricating wear-resistant coating coefficient of friction, reduction trend.
Example 4：
On the basis of above-described embodiment, further, in the present embodiment, modified graphene（Graphene is modified tungsten carbide self-lubricating
Anti-wear additive）Preparation process is as follows：
4g graphene oxides are weighed, 1000g absolute ethyl alcohols is added, uniform stirring mixing, is mixed adding 800g deionized waters
Close, in ultrasonic disperse instrument, from 10mm vibration amplitude arms, sonication treatment time 150min, supersonic frequency 15Hz, obtain graphite
The scattered mixed liquor of alkene, the forerunner that mass percent is mixed into tungstenic for 99% ammonium metatungstate and 1% tungsten carbonyl is weighed respectively
Body mixture, weigh 1g tungstenic precursor mixtures and be added in graphene dispersion solution, stir 60min, in whipping process not
It is disconnected to instill absolute ethyl alcohol, infusion volume 228g, then obtained precipitation is filtered, heat 90 DEG C in an oven, dry 40min,
The drying powder that will be obtained, is placed in alumina crucible, and a certain amount of H2 is led in tubular reduction furnace, and H2 flows are l00sccm, with
50 DEG C/min heating rate, 900 DEG C, soaking time 2h are heated to, finally lead to H2 and be cooled to room temperature, obtained graphene and be modified
The self-lubricating abrasion-resistant additive of tungsten carbide.
Thermal spraying prepares the tungsten-cobalt carbide that the graphene prepared containing the present invention is modified tungsten carbide self-lubricating abrasion-resistant additive
Wear-resistant coating process is as follows：
Modified graphene prepared by the present invention（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）8g is weighed, adds 200g
Absolute ethyl alcohol sonication treatment time is 40min, supersonic frequency 15Hz, and vibration amplitude arm selects 10mm, obtains dispersed modification
Graphene（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）Mixed solution.200gWC-12Co dusty sprays are added to
In modified graphene mixed solution, 140min is stirred, while heating-up temperature is maintained at 35 DEG C, obtains modified graphene/nano-sized carbon
Change the solution that composite tungsten material mixes with tungsten carbide/cobalt dusty spray.Mixed solution is constantly instilled and is placed in the oxygen for filling liquid nitrogen
To change in aluminium crucible, ensure that liquid nitrogen and mixed solution uniformly freeze mixing, wherein liquid nitrogen accounts for mixed solution mass percent 50%,
Whole process 30min, it will then mix solution and be placed in vacuum freeze, and vacuumize 0.1MPa, and freeze 30min,
Then take out and be placed in freeze drying box the 10min that thaws, temperature control finally obtains modified graphene/nano-sized carbon at 25 ~ 30 DEG C
Change composite tungsten material and tungsten carbide/cobalt mixing dusty spray.
Graphene modified coating is prepared using detonation flame spraying, technological parameter is：Oxygen and acetylene flow-rate ratio are 1.2, gas
It is 68%, spray distance 260mm to fill rifle amount, and regulation detonation frequency is 3 times/second, spray distance 250mm, and powder feeding rate is
0.3g/s.Friction test is carried out in CETR micro-moving frictional wear experimental machines, using ball-face way of contact, load 10N, on
Sample is diameter 6.5mm GCrl5 steel balls, and lower sample is 24.9 mm × 7.8mm disc surfaces spray-on coatings, coating after polishing
Final thickness is 0.2 mm.
Test parameters is：Wearing- in period 10min, frequency 30 Hz, displacement amplitude D are 2 mm.
It is 0.65 that this example, which prepares tungsten carbide coating average friction coefficient, and wear weight loss is 3.9 mg.Graphene is prepared to change
Property WC-Co coatings average friction coefficient be 0.42, wear weight loss 2.4mg.Result of study shows：Graphene modified coating
Coefficient of friction is less than WC-12Co coatings, illustrates that graphene prepared by the present invention is modified self-lubricating abrasion-resistant additive to tungsten carbide painting
Layer plays preferable self-lubricating property.
Example 5：
On the basis of above-described embodiment, further, in the present embodiment, modified graphene（Graphene is modified tungsten carbide self-lubricating
Anti-wear additive）Preparation process is as follows：
5g graphene oxides are weighed, 1000g absolute ethyl alcohols is added, uniform stirring mixing, is mixed adding 800g deionized waters
Close, in ultrasonic disperse instrument, from 10mm vibration amplitude arms, sonication treatment time 150min, supersonic frequency 15Hz, obtain graphite
The scattered mixed liquor of alkene, the forerunner that mass percent is mixed into tungstenic for 99% ammonium metatungstate and 1% tungsten carbonyl is weighed respectively
Body mixture, weigh 1g tungstenic precursor mixtures and be added in graphene dispersion solution, stir 60min, in whipping process not
It is disconnected to instill absolute ethyl alcohol, infusion volume 286g, then obtained precipitation is filtered, heat 90 DEG C in an oven, dry 40min,
The drying powder that will be obtained, is placed in alumina crucible, and a certain amount of H2 is led in tubular reduction furnace, and H2 flows are l00sccm, with
50 DEG C/min heating rate, 900 DEG C, soaking time 2h are heated to, finally lead to H2 and be cooled to room temperature, obtained graphene and be modified
The self-lubricating abrasion-resistant additive of tungsten carbide.
Thermal spraying prepares the tungsten-cobalt carbide that the graphene prepared containing the present invention is modified tungsten carbide self-lubricating abrasion-resistant additive
Wear-resistant coating process is as follows：
Modified graphene prepared by the present invention（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）4g is weighed, adds 200g
Absolute ethyl alcohol sonication treatment time is 40min, supersonic frequency 15Hz, and vibration amplitude arm selects 10mm, obtains dispersed modification
Graphene（Graphene is modified tungsten carbide self-lubricating abrasion-resistant additive）Mixed solution.200gWC-12Co dusty sprays are added to
In modified graphene mixed solution, 140min is stirred, while heating-up temperature is maintained at 35 DEG C, obtains modified graphene/nano-sized carbon
Change the solution that composite tungsten material mixes with tungsten carbide/cobalt dusty spray.Mixed solution is constantly instilled and is placed in the oxygen for filling liquid nitrogen
To change in aluminium crucible, ensure that liquid nitrogen and mixed solution uniformly freeze mixing, wherein liquid nitrogen accounts for mixed solution mass percent 50%,
Whole process 30min, it will then mix solution and be placed in vacuum freeze, and vacuumize 0.1MPa, and freeze 30min,
Then take out and be placed in freeze drying box the 10min that thaws, temperature control finally obtains modified graphene/nano-sized carbon at 25 ~ 30 DEG C
Change composite tungsten material and tungsten carbide/cobalt mixing dusty spray.
Graphene modified coating is prepared using detonation flame spraying, technological parameter is：Oxygen and acetylene flow-rate ratio are 1.4, gas
It is 80%, spray distance 300mm to fill rifle amount, and regulation detonation frequency is 3 times/second, and powder feeding rate is 0.5g/s.Friction test exists
Carried out in CETR micro-moving frictional wear experimental machines, using ball-face way of contact, load 10N, upper sample is diameter 6.5mm's
GCrl5 steel balls, lower sample are 24.9 mm × 7.8mm disc surfaces spray-on coatings, and coating final thickness is 0.2 mm after polishing.
Test parameters is：Wearing- in period 10min, frequency 30 Hz, displacement amplitude D are 2 mm.
It is 0.68 that this example, which prepares tungsten carbide coating average friction coefficient, and wear weight loss is 3.6 mg.Graphene is prepared to change
Property WC-Co coatings average friction coefficient be 0.44, wear weight loss 2.6mg.Result of study shows：Graphene modified coating
Coefficient of friction is less than WC-12Co coatings, illustrates that graphene prepared by the present invention is modified self-lubricating abrasion-resistant additive to tungsten carbide painting
Layer plays preferable self-lubricating property.
Example 6：
On the basis of above-described embodiment, further, in the present embodiment, modified graphene（Graphene is modified tungsten carbide self-lubricating
Anti-wear additive）Preparation process is as follows：
6g graphene oxides are weighed, 1000g absolute ethyl alcohols is added, uniform stirring mixing, is mixed adding 800g deionized waters
Close, in ultrasonic disperse instrument, from 10mm vibration amplitude arms, sonication treatment time 180min, supersonic frequency 15Hz, obtain graphite
The scattered mixed liquor of alkene, the forerunner that mass percent is mixed into tungstenic for 99% ammonium metatungstate and 1% tungsten carbonyl is weighed respectively
Body mixture, weigh 1g tungstenic precursor mixtures and be added in graphene dispersion solution, stir 60min, in whipping process not
It is disconnected to instill absolute ethyl alcohol, infusion volume 324g, then obtained precipitation is filtered, heat 90 DEG C in an oven, dry 40min,
The drying powder that will be obtained, is placed in alumina crucible, and a certain amount of H2 is led in tubular reduction furnace, and H2 flows are l00sccm, with
70 DEG C/min heating rate, 900 DEG C, soaking time 3h are heated to, finally lead to H2 and be cooled to room temperature, obtained graphene and be modified
The self-lubricating abrasion-resistant additive of tungsten carbide.
Thermal spraying prepares the tungsten-cobalt carbide that the graphene prepared containing the present invention is modified tungsten carbide self-lubricating abrasion-resistant additive
Wear-resistant coating process is as follows：
Weigh graphene prepared by the 10g present invention and be modified tungsten carbide self-lubricating abrasion-resistant additive addition 200gWC-12Co spray coating powders
In end, ball milling 10 hours in anhydrous ethanol medium, drum's speed of rotation is 3 rpm/s, will be mixed containing liquid medium after ball milling
Close powder ultrasonic decentralized processing 2 hours, it is 25 ~ 45 μm that powder, which screens out granularity, after supersound process after being dried 2 hours at 40 DEG C
Dusty spray.
Graphene modified coating is prepared using detonation flame spraying, technological parameter is：Oxygen and acetylene flow-rate ratio are 1.2, gas
It is 90%, spray distance 270mm to fill rifle amount, and regulation detonation frequency is 7 times/second, and powder feeding rate is 0.7g/s.Friction test exists
Carried out in CETR micro-moving frictional wear experimental machines, using ball-face way of contact, load 50N, upper sample is diameter 6.5mm's
GCrl5 steel balls, lower sample are 24.9 mm × 7.8mm disc surfaces spray-on coatings, and coating final thickness is 0.2 mm after polishing.
Test parameters is：Wearing- in period 10min, frequency 30 Hz, displacement amplitude D are 2 mm.
It is 0.65 that this example, which prepares tungsten carbide coating average friction coefficient, and wear weight loss is 3.5 mg.Graphene is prepared to change
Property WC-Co coatings average friction coefficient be 0.39, wear weight loss 2.1mg.Result of study shows：Graphene modified coating
Coefficient of friction is less than WC-12Co coatings, illustrates that graphene prepared by the present invention is modified self-lubricating abrasion-resistant additive to tungsten carbide painting
Layer plays preferable self-lubricating property.
Compared with immediate prior art, the invention has the advantages that：
1）Technical scheme provided by the invention can obtain modified graphene, make nano-lamellar structure graphenic surface in situ raw
Long, deposition has the tungsten carbide particle of nanoscale, by controlling the content ratio between reactant, and reaction condition, it is possible to achieve
The size of graphenic surface growth in situ nano silicon carbide composition granule, pattern, content regulation and control.
2）Compared to graphene tungsten carbide dusty spray, modified graphite prepared by the present invention are directly appended to as self-lubricating agent
Alkene had not both changed the characteristic of graphene sheet layer carbon structure unit, and graphene still has larger specific surface area and greater activity etc. excellent
Point, greatly enhances the weight of graphene again, and the nanometer tungsten carbide that area load has growth in situ improves and is carbonized
The compatibility of tungsten dusty spray and uniformly mixing.
3）The tungsten carbide coating for being directly appended to the preparation of tungsten carbide dusty spray not modified compared to graphene, institute of the present invention
The graphene of acquisition, which is modified tungsten carbide self-lubricating agent and will not blown in spraying process by the spraying flame stream of high speed, high temperature, to fly and loses
Fall, be effectively kept the component content of graphene in the coating and be uniformly distributed.
4）Modified graphene/nano silicon carbide composite tungsten material is answered with tungsten carbide/cobalt using the technique of vacuum freeze drying
Close and obtain mixing dusty spray, the technique can ensure modified graphene/nano silicon carbide composite tungsten material graphite and tungsten carbide/cobalt
Under vacuum, low temperature is directly sublimated from liquid to solid-state obtains dry mixing dusty spray to powder, avoids traditional work
Skill powder（Sintering crushing, vacuum atomizing）Hot conditions oxidative deformation to caused by graphene, it also avoid ball milling and mix powder process
Middle lighter weight graphene is easily layered with heavier mass tungsten carbide/cobalt solution and can not realize mixed uniformly problem.
5）The graphene that the present invention obtains is modified tungsten carbide self-lubricating abrasion-resistant additive application in wear-resistant coating, graphene
On the one hand the intensity and toughness of coating can be improved, the shearing force of graphene film interlayer is minimum in addition, the graphite in friction process
The relative relative slip slided, surface of friction pair metalwork can be replaced occurs between alkene lamella, realizes abrasive dust and friction subtabulation
The separation in face, greatly reduces coefficient of friction, reduces abrasion.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted, and institute
There is the protection domain that these modifications and variations should all belong to appended claims of the present invention.
Claims (13)
- A kind of 1. dusty spray of tungsten carbide containing modified graphene for being used to prepare self-lubricating wear-resistant coating, it is characterised in that including Following steps：Step 1：A certain amount of modified graphene/nano silicon carbide composite tungsten material is weighed, is ultrasonically treated with a certain amount of absolute ethyl alcohol The mixed solution of graphene/nanometer tungsten carbide composite is obtained after scattered；Step 2：A certain amount of tungsten carbide/cobalt dusty spray is weighed, the graphene nano tungsten carbide obtained is added in above-mentioned steps 1 and answers In the mixed solution of condensation material, using vertical mixer, obtain being modified stone with certain rotating speed stirring certain time under normal temperature condition The mixed solution of black alkene/nano silicon carbide composite tungsten material and tungsten carbide/cobalt；Step 3：The mixing of the modified graphene obtained in above-mentioned steps 2/nano silicon carbide composite tungsten material and tungsten carbide/cobalt is molten Liquid obtains the tungsten carbide/cobalt dusty spray for being compounded with modified graphene using the method for vacuum freeze drying；Step 4：The tungsten carbide/cobalt dusty spray for being compounded with modified graphene that will be obtained in above-mentioned steps 3, using thermal spraying work Piece surface of the skill after cleaning, sandblasting prepares the tungsten carbide/cobalt self-lubricating wear-resistant coating for being compounded with modified graphene.
- 2. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that described in the step 1 Tungstenic precursor compound is the mixed of tungsten carbonyl and ammonium metatungstate in modified graphene/nano silicon carbide composite tungsten material preparation process In compound tungsten carbonyl account for ammonium metatungstate and weight/mass percentage composition be 1-5%.
- 3. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that in the step 1, graphite Alkene is commercial graphene oxide, and the mass ratio of tungstenic precursor mixture and graphene oxide is 1:1-6.
- 4. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that anhydrous in the step 1 Graphene weight/mass percentage composition is 0.1-0.5% in ethanol wet graphene solution, deionized water quality hundred in graphene solution It is 5-8% to divide ratio.
- 5. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that in the step 1, ultrasound Processing time is 30-180min, supersonic frequency 10-15Hz.
- 6. vibration amplitude arm selects 10mm.
- 7. tungstenic precursor compound is added to graphene solution after decentralized processing and the mixed solution formed in whipping process Absolute ethyl alcohol is constantly instilled, absolute ethyl alcohol amount is instilled and accounts for mixed liquor volume ratio as 1:10-18, stir 30-60min.
- Filtered 8. obtained solution is precipitated, it is 70 DEG C -100 DEG C to be placed in drying temperature in baking oven, drying time 10- 60min, the compounding substances of graphene and tungstenic precursor mixture are obtained, then with 5-70 DEG C/min liters in tubular reduction furnace Warm speed, it is 100 sccm to be passed through reducing gas H2 flows, and wherein holding temperature is 700-900 DEG C, soaking time 1-3h, is filled After dividing reaction, logical H2 is cooled to room temperature.
- There is modified graphene/nanometer tungsten carbide of nanometer tungsten carbide multiple 9. obtaining nano-lamellar structure graphenic surface growth in situ Condensation material, modified graphene/nano silicon carbide composite tungsten material is mixed with absolute ethyl alcohol, wherein modified graphene/nano silicon carbide The mass ratio that composite tungsten material accounts for absolute ethyl alcohol is 1-5%, and sonication treatment time is 30-60min, supersonic frequency 15Hz.
- 10. vibration amplitude arm selects 10mm, it is molten finally to obtain dispersed modified graphene/nano silicon carbide composite tungsten material mixing Liquid.
- 11. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that, will in the step 2 A certain amount of tungsten carbide/cobalt dusty spray, it is molten to be added to the modified graphene after ultrasonic disperse/nano silicon carbide composite tungsten material mixing Liquid, wherein modified graphene/nano silicon carbide composite tungsten material and tungsten carbide/cobalt dusty spray mass percent are 1-5%, stirring 120min-150min, while heating-up temperature is maintained at 30-40 DEG C, obtains modified graphene/nano silicon carbide composite tungsten material and carbon Change the solution of tungsten/cobalt dusty spray mixing.
- 12. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that in the step 3, Processing modified graphene/nano silicon carbide composite tungsten material of being sublimated in vacuum freeze-drying system mixes with tungsten carbide/cobalt dusty spray The solution of conjunction, its process are that liquid nitrogen constantly instills modified graphene/nano silicon carbide composite tungsten material and tungsten carbide/cobalt spray coating powder The solution of end mixing, wherein cryogenic temperature are maintained at 0-5 DEG C, and it is multiple that final liquid nitrogen addition accounts for modified graphene/nanometer tungsten carbide The solution quality ratio that condensation material mixes with tungsten carbide/cobalt dusty spray is 60-70%, and the whole process operating time is 20-40min, Then the solution that the modified graphene/nano silicon carbide composite tungsten material for freezing mixing mixes with tungsten carbide/cobalt dusty spray is put In vacuum freeze, 0.1MPa is vacuumized, freezes 30-40min, then takes out to be placed in freeze drying box and thaws 10-15min, temperature control finally obtain modified graphene/nano silicon carbide composite tungsten material and mixed with tungsten carbide/cobalt at 25-30 DEG C Close dusty spray.
- 13. the dusty spray of tungsten carbide containing modified graphene as claimed in claim 1, it is characterised in that, will in the step 4 Modified graphene/nano silicon carbide the composite tungsten material that is compounded with obtained uses detonation flame spraying technique with tungsten carbide/cobalt dusty spray Preparing process for self-lubricating wear-resistant coating parameter is：Oxygen and acetylene are heat source gas, and the gas flow ratio of oxygen and acetylene is 1.0-1.5, it is 60-90% that gas, which fills rifle amount, and regulation detonation frequency is 3-7 times/second, spray distance 250-300mm, powder feeding rate For 0.2-0.7g/s.
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