CN106917059B - A kind of thermal spraying composite granule and its preparation method and application - Google Patents
A kind of thermal spraying composite granule and its preparation method and application Download PDFInfo
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- CN106917059B CN106917059B CN201511001006.1A CN201511001006A CN106917059B CN 106917059 B CN106917059 B CN 106917059B CN 201511001006 A CN201511001006 A CN 201511001006A CN 106917059 B CN106917059 B CN 106917059B
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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Abstract
The present invention provides a kind of thermal spraying composite granule and its preparation method and application, the thermal spraying composite granule includes mainly following component by mass percentage：NiCrAlY powder 74.5~81.5%；Cr2O3Powder 13.5~16.5%；Ag powder 5~9%；Wherein, NiCrAlY powder, Cr2O3The average grain diameter of powder and Ag powder must be independently less than 5 μm.The thermal spraying composite granule is obtained using ball mill grinding and two step composite granule preparation processes of spray drying.Each component is uniformly dispersed in the thermal spraying composite granule, can avoid the burning problems of Ag in spraying process.It can be used for the preparation of wear-resisting composite solid lubricant coating in thermal spraying, especially suitable for the surfacecti proteon of the mechanical equipment and component that are operated under the extreme harsh operating mode such as high temperature, high speed and heavy duty.
Description
Technical field
The invention belongs to technical field of hot more particularly to a kind of thermal spraying composite granule and preparation method thereof and use
On the way.
Background technology
A kind of dispersion that hot spray powder is made of a large amount of powder particles.The preparation method of hot spray powder is a variety of
It is various, include mainly following six kinds：Gas atomization, water atomization, melting flour method, sintering crush hair, polymerization powder method processed and
Cladding process.The preparation method of the hot spray powder can be used for manufacturing all kinds of powder systems such as metal (alloy) or ceramics.Usually
Need the preparation method according to the structure and purposes of powder reasonable selection hot spray powder.
As hot-spraying coating is in the extensive use of every field, traditional single or simple component hot spray powder material
Material cannot meet coating multiple demands under certain special military service operating modes.Therefore, often by two or more powder
End is prepared into thermal spraying mixed powder or thermal spraying composite granule.Thermal spraying mixed powder refers to directly by various one-components
Powder is put into agitating ball mill, under the process conditions of certain rotating speed and ratio of grinding media to material, carries out the powder prepared by mixed powder；Thermal jet
It is certain by the solid matter particle of different nature warp of two or more submicron order (or nanoscale) to apply composite granule
The powder particle that technique is prepared.The ingredient for forming composite powder can be that metal (alloy) (is closed with metal (alloy), metal
Gold) and ceramics, ceramic and ceramics, metal (alloy) and plastics etc., range is very extensive, almost including all solid-state engineering materials
Material.The preparation method of common thermal spraying composite granule has spray drying process, sintering crushing method, the damaged method of melting and co-deposition
Method.
For the component of machine operated under the harsh working condition such as high temperature, high speed and heavy duty, its fretting wear
Problem of Failure is very serious, often requires that surface protection coating while having high temperature resistance, wear-resistant and solid lubrication performance.
The powder preparation process of composite solid lubricant coating wear-resisting in general is by Binder Phase powder (to improve coating
Bond strength, example NiAl, NiMoAl, NiCrAlY powder etc.), hard phase powder is (to improve the wearability of coating, example Cr3C2、
Al2O3、Cr2O3Deng) and solid lubrication phase powder (example MoS2, graphite, Ag etc.) directly carry out powder mixing machine, then carry out spraying and apply
Work.Mostly between 15-105 μm, the granularity between mixing constituent element may differ by larger the grain size of various powders.
PS families of coatings prepared by the research centers NASA NASA is typical wear-resisting composite solid lubricant
Coating (table 1 show the composition of PS100, PS200, PS300 and PS400 families of coatings).Their powder preparation process is
Using powder mixing machine method.
The table 1PS series plasma spraying coating component tables of comparisons
| Apply layer name | Binder Phase | Hard phase | Solid lubrication phase |
| PS 100 | NiCr | Glass | Ag and BaF2/CaF2Eutectic |
| PS 200 | NiCo | Cr3C2 | Ag and BaF2/CaF2Eutectic |
| PS 300 | NiCr | Cr2O3 | Ag and BaF2/CaF2Eutectic |
| PS 400 | NiMoAl | Cr2O3 | Ag and BaF2/CaF2Eutectic |
104278226 A of CN disclose a kind of technology of preparing of the wide temperature range self-lubricating coat in use of all-metal phase, and coating is using big
Prepared by gas plasma spraying technology, dusty spray is by NiCrAlY, Cr2O3, Ag and CaF2/BaF2Four kinds of powder of eutectic pass through machine
Tool is mixed with to obtain；NiCrAlY powder accounts for 60~80wt%, Cr in dusty spray2O3Powder accounts for 10~20wt%, and Ag powder accounts for 5
~10wt%, CaF2/BaF2Eutectic powder accounts for 5~10wt%；NiCrAlY powder diameters are 30~100 μm, in NiCrAlY powder
Ni contents are that 67%, Cr contents are 22%, and Al content 10%, remaining is Y；Cr2O3Powder is Mechanical Crushing powder, grain size
It is 20~80 μm；Ag powder is spherical shape, and grain size is 80~120 μm；CaF2/BaF2Eutectic powder grain size is 20~150 μm.
However, the hot spraying powder prepared with powder mixing machine method has disadvantages that, include mainly following two aspects：(1)
Powder mixing is uneven：Due to NiCrAlY, Cr2O3Density with Ag is respectively 2.96g/cm3、5.2g/cm3And 10.5g/cm3,
Proportion great disparity is larger.Therefore, the evenly dispersed effect of the different larger powder systems of powder mixing machine comparison resuspension is poor, and then influences
Prepared coating composition distributing homogeneity, enables coating integrity to reduce；(2) distillation of Ag：The fusing point of Ag is 961.78 DEG C,
Also only 2262 DEG C of boiling point, and Cr2O3Fusing point be 2266 DEG C；It means that being mixed by thermal spraying prepared by powder mixing machine method
Powder is when carrying out thermal spraying, it is necessary to adjust spraying parameter, make Cr2O3Powder is close to or up to molten condition, but Ag at this time
Powder is then vaporized because of excessively high temperature；It is formed by the significant decrease of coating silver content, to make the solid lubrication of coating
Effect is deteriorated.Therefore, in recent years, gradually by plasma spraying, (heat source temperature is up to hot-spraying technique of the preparation containing silver coating
10000 DEG C) it is transitioned into supersonic flame spraying (flame stream temperature is at 1000-2000 DEG C)；
In addition, compared with spraying mixed-powder, the coating performance prepared by spraying composite powder is excellent, spray rate and heavy
Product efficiency is much higher, and component and proportioning are easier to adjust, and performance is easier to control.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of thermal spraying composite granule and its preparation
The uniformity coefficient of method and purposes, the thermal spraying composite granule is high, and good dispersion can dramatically reduce spraying process
The loss of middle Ag makes the solid lubrication performance of coating be not fully exerted, especially suitable for extreme in high temperature, high speed and heavy duty etc.
The surfacecti proteon of the mechanical equipment and component that are operated under harsh operating mode.
For this purpose, the present invention uses following technical scheme：
One of the objects of the present invention is to provide a kind of thermal spraying composite granule, the thermal spraying composite granule presses quality hundred
It includes following component to divide content mainly：
NiCrAlY powder 74.5~81.5%
Cr2O3Powder 13.5~16.5%
Ag powder 5~9%；
Wherein, NiCrAlY powder, Cr2O3The average grain diameter of powder and Ag powder is independently less than 5 μm, such as 4.5 μm, 4 μm, 3 μm, 2 μ
M, 1 μm, 900nm, 800nm, 600nm, 300nm, 200nm, 100nm, 80nm, 60nm, 40nm or 20nm etc..
The thermal spraying composite granule includes mainly following component by mass percentage：NiCrAlY powder 74.5~
81.5%, such as 75%, 76%, 78%, 80% or 81%；Cr2O3Powder 13.5~16.5%, such as 14%, 14.2%, 14.5%,
14.8%, 15%, 15.2%, 15.8%, 16% or 16.3% etc.；Ag powder 5~9%, such as 5.5%, 6.8%, 7.0%,
7.2%, 8.3% or 8.5% etc..
The mass percentage of each metal is all higher than 0, and the sum of the mass percentage of each metal in the NiCrAlY powder
It is 100%, the ratio between mass percentage of each metal object is specifically limited, and the average grain diameter of the NiCrAlY powder is 800~
1000nm, such as 820nm, 850nm, 880nm, 900nm, 920nm, 950nm or 980nm.
Preferably, the Cr2O3The average grain diameter of powder is 60~100nm, such as 65,70,75,80,85,90 or 95.
Preferably, the average grain diameter of the Ag powder be 800nm~1.2 μm, as 850nm, 900nm, 950nm, 1.0 μm or
1.1 μm etc..
The NiCrAlY powder is prepared by ball-milling method.
Preferably, the NiCrAlY powder is obtained by high energy ball mill ball milling.
The particle size of the composite granule is 15~45 μm, such as 20 μm, 25 μm, 30 μm, 35 μm, 40 μm or 42 μm.
Preferably, the composite granule is prepared by spray drying process.
Preferably, the composite granule is prepared by centrifugal spray dryer.
The second object of the present invention is to provide a kind of preparation method of thermal spraying composite granule, and the preparation method includes
Following steps：
(1) NiCrAlY powder is subjected to ball milling, obtains the NiCrAlY powder that average grain diameter is less than 5 μm；
(2) the NiCrAlY powder of formula ratio and average grain diameter are independently less than to 5 μm of Cr2O3Powder and the mixing of Ag powder, obtain
Mixed powder is spray-dried by mixed powder, obtains thermal spraying composite granule.
Practicality spray drying process of the invention prepares NiCrAlY, Cr2O3With the composite granule of Ag, make (or to receive with sub-micron
Rice) rank NiCrAlY, Cr2O3With Ag uniformly dispersings in each powder；The composite powder uniformity coefficient being prepared out is high,
Good dispersion；Meanwhile the other Ag of submicron order is uniformly distributed in single composite granule, and in spraying process, only composite powder
The Ag particles in body surface face are easy to be distilled by high temperature, and the Ag inside powder is then protected because the gradient of temperature reduces well；
The loss for reducing Ag in spraying process of high degree in this way, makes the solid lubrication performance of coating be not fully exerted.
Step (1) described ball milling uses wet-milling；
Preferably, stainless steel ball in the wet-milling, NiCrAlY powder and deionized water is 22.5~27.5 in mass ratio:
1:1.35~1.65 mixing are such as 23 according to mass ratio:1:1.40、24:1:1.45、25:1:1.50、26:1:1.55 or 27:1:
1.60 etc., obtain slurry.
Preferably, in 10~20min after step (1) described ball milling starts, as 12min, 13min, 14min, 15min,
When 16min or 18min, antifoaming agent is added into ball milling system, the loss of powder is caused to prevent a large amount of bubbles from emerging.
Preferably, the addition of the antifoaming agent accounts for the 0.049~0.060% of slurry gross mass, such as the antifoaming agent
Addition is 0.050%, 0.052%, 0.053%, 0.055%, 0.056% or 0.058% etc. of slurry gross mass.
Preferably, the antifoaming agent is tbp.
Preferably, step (1) described ball milling carries out in an inert atmosphere, and the inert atmosphere can avoid sample oxidation.
The inert atmosphere can be selected from argon gas etc..
In mechanical milling process, if it find that the grain size reduction speed of powder is slower, a small amount of grinding aid can be added.Preferably, it walks
Suddenly in 2~3h before (1) described ball milling terminates, 2h, 2.1h, 2.3h, 2.4h, 2.5h, 2.8h or 2.9h before terminating such as ball milling
When, grinding aid is added into ball milling system, to effectively reduce Ball-milling Time.
Preferably, the addition of the grinding aid is the 0.018% of slurry gross mass.
Preferably, the grinding aid is OP-10 (condensation product of alkyl phenol and ethylene oxide).
Preferably, the rotating speed of step (1) described ball milling be 450~650rpm, as 480rpm, 500rpm, 520rpm,
550rpm, 580rpm, 600rpm, 620rpm or 640rpm etc..
Preferably, the time of step (1) described ball milling be 13~15h, as 13.2h, 13.5h, 13.8h, 14h, 14.2h,
14.5h or 14.8h etc..
Preferably, step (1) the ball milling interval carries out：Ball milling 0.5h, be spaced 0.5h after be further continued for ball milling, with prevent compared with
High rotational speed of ball-mill can make in mechanical milling process that powder local temperature is excessively high, cause the variation to powder structure and quality,.
Preferably, step (1) described ball milling carries out on high energy ball mill.
Before step (2) described spray drying, by mixed powder, deionized water and binder according to weight ratio be 28~32:
66~70:1.8~2.2 are mixed into slurry, are such as 29 according to weight ratio:67:1.9、30:68:2.0、31:69:2.1 or 31.5:
69.5:2.2 mixing.
Preferably, the binder is polyvinyl alcohol.
Preferably, the slurry is first subjected to ball milling mixing, then is spray-dried, each component distributing in slurry is made to obtain
More uniformly.
Preferably, the rotating speed of the ball milling be 108~132r/min, as 109r/min, 110r/min, 112r/min,
115r/min, 118r/min, 120r/min, 122r/min, 125r/min or 130r/min etc., ratio of grinding media to material are 9~11:1, such as 9:
1、10:1 or 11:1 etc..
Preferably, dispersant is added in the mechanical milling process, the addition of the dispersant accounts for the 0.009 of slurry gross mass
~0.011wt%, such as 0.009wt%, 0.010wt% or 0.011wt% prevent nano-scale particle from agglomeration occurs.
Preferably, the dispersant is SND6800 (anionic polycarboxylate's salt electrolyte)；
Step (2) spray drying carries out on centrifugal spray dryer.
Preferably, the temperature of inlet air of step (2) described spray drying be 220~240 DEG C, such as 222 DEG C, 225 DEG C,
228 DEG C, 230 DEG C, 232 DEG C, 235 DEG C or 238 DEG C etc., cavity air themperature be 135~165 DEG C, such as 138 DEG C, 140 DEG C, 142
DEG C, 145 DEG C, 148 DEG C, 150 DEG C, 152 DEG C, 155 DEG C, 160 DEG C or 163 DEG C etc., air exit temp is 112.5~136.5 DEG C,
Such as 113 DEG C, 114 DEG C, 115 DEG C, 120 DEG C, 125 DEG C, 130 DEG C, 132 DEG C or 135 DEG C.
Preferably, the nozzle rotary speed of step (2) described spray drying is 12870~13130r/min, such as 12880r/
Min, 13000r/min, 13100r/min, 13110r/min or 13120r/min etc..
Preferably, it is 54~66g/min that the slurry of step (2) described spray drying, which gives rate, such as 55g/min, 56g/
Min, 57g/min, 58g/min, 60g/min, 62g/min or 65g/min etc..
Preferably, the atomization air flow of step (2) described spray drying is 10.8~13.2m3/ h, such as 11m3/h、
11.2m3/h、11.5m3/h、11.8m3/h、12.0m3/h、12.3m3/h、12.5m3/h、12.8m3/ h or 13.0m3/ h etc..
Preferably, the high-pressure air pressure of step (2) described spray drying be 0.36~0.44MPa, as 0.37MPa,
0.38MPa, 0.40MPa, 0.41MPa, 0.42MPa or 0.43MPa etc..
The preparation method of the thermal spraying composite granule includes the following steps as a preferred technical solution,：
(1) by stainless steel ball, NiCrAlY powder and deionized water in mass ratio be 22.5~27.5:1:1.35~1.65
Mixing, is put into ball grinder；The inert gas that flow velocity air pressure is 0.2MPa is passed through in ball grinder, it is 20 minutes to be passed through the time；
Drum's speed of rotation is set as 450~650rpm, 13~15h of ball milling, ball milling start after 10~20min in into ball milling system plus
Enter to account for the tbp of slurry gross mass 0.049~0.060%, ball milling terminate before 2~3h in, be added into ball milling system
The grinding aid for accounting for slurry gross mass 0.018% obtains the NiCrAlY powder that average grain diameter is less than 5 μm；
(2) the NiCrAlY powder of formula ratio and average grain diameter are independently less than to 5 μm of Cr2O3Powder and the mixing of Ag powder, obtain
Mixed powder, by mixed powder, deionized water and polyvinyl alcohol according to mass ratio 28~32:66~70:1.8~2.2 are mixed into
Slurry is carried out ball milling by slurry, and rotational speed of ball-mill is 108~132r/min, and ratio of grinding media to material is 9~11:1, it is added in mechanical milling process point
Powder, the dispersant account for 0.009~0.011wt% of slurry gross weight, and the slurry after ball milling is spray-dried, spraying
Dry parameter is：Temperature of inlet air is 220~240 DEG C, and cavity air themperature is 135~165 DEG C, and air exit temp is
112.5~136.5 DEG C, nozzle rotary speed is 12870~13130r/min, and it is 54~66g/min that slurry, which gives rate,；Atomization
Air mass flow is 10.8~13.2m3/ h, high-pressure air pressure are 0.36~0.44MPa, obtain thermal spraying composite granule.
Composite granule provided by the invention specific additive formula (ball milling antifoaming agent be tbp 0.049~
0.060%, grinding aid is OP-10 agent 0.018%, and dispersant is SND6800 agent 0.009~0.011%) and technological parameter (ball
Time consuming will reach 13~15h, and the slurry of spray drying gives rate 54~66g/min, and atomization air flow 10.8~
13.2m3/h, 0.36~0.44MPa of high-pressure air pressure) under, it can be achieved that in powder each component it is evenly dispersed, and avoid spraying
The burning problems of Ag in the process.
The preparation method of thermal spraying composite granule provided by the invention uses the compound flouring technology of two steps, overcomes direct machine
The shortcomings that tool powder mixing method, i.e., powder mixing is uneven fine with part low melting point caused by proportion great disparity is larger between hybrid particles
Constituent element, can be by the size controlling of whole constituent elements similar as long as selecting technological parameter appropriate in spraying the problem of scaling loss
Grade, and the spraying feedstock of specified particle diameter can be synthesized as required.
The three of the object of the invention are to provide a kind of purposes of the thermal spraying composite granule, be used to prepare wear-resisting compound
Solid lubricant coating.
The wear-resisting composite solid lubricant coating using the NiCrAlY powder of submicron order as Binder Phase, with Cr2O3Particle is hard
Matter hardening constituent, using soft metal Ag as solid lubrication phase.Especially suitable for being transported under the extreme harsh operating mode such as high temperature, high speed and heavy duty
The surfacecti proteon of the mechanical equipment and component that turn.
Compared with prior art, beneficial effects of the present invention are：
Thermal spraying composite powder uniformity coefficient provided by the invention is high, the good dispersion of each component, the other Ag of submicron order
It is uniformly distributed in single composite granule, in spraying process, only the Ag particles on composite granule surface are easy to be distilled by high temperature,
Ag inside powder is then protected because the gradient of temperature reduces well, dramatically reduces the damage of Ag in spraying process
It loses, the solid lubrication performance of coating is made to be not fully exerted；
The preparation method of thermal spraying composite granule provided by the invention uses the compound flouring technology of two steps, overcomes direct machine
The shortcomings that tool powder mixing method, i.e., the uneven and Ag powder of powder mixing is burnt in spraying caused by proportion great disparity is larger between hybrid particles
The problem of damage, selects technological parameter appropriate, can be by the size controlling of each component in similar levels, and can synthesize spy as required
Determine the hot spray powder of grain size；
Using coating made from thermal spraying composite powder provided by the invention especially suitable in high temperature, high speed and heavy duty etc.
The surfacecti proteon of the mechanical equipment and component that are operated under extreme harshness operating mode.
Description of the drawings
Fig. 1 is the schematic diagram of thermal spraying composite granule prepared by powder mixing machine method.
Fig. 2 is the schematic diagram of thermal spraying composite granule prepared by spray granulation.
Fig. 3 is the preparation flow figure for the thermal spraying composite granule that embodiment 1 provides.
Fig. 4 be embodiment 1 provide ball milling 7h after, with the volume distribution map for the NiCrAlY powder that laser particle analyzer measures.
Fig. 5 be embodiment 1 provide ball milling 13h after, with the volume distribution map for the NiCrAlY powder that laser particle analyzer measures.
Fig. 6 be embodiment 1 provide ball milling before and ball milling 13h after NiCrAlY powder SEM figure, wherein a be ball milling before
The SEM of NiCrAlY powder schemes；The SEM figures of NiCrAlY powder after b is ball milling 13h.
Fig. 7 is the SEM figures of thermal spraying composite granule made from embodiment 1.
Fig. 8 is the backscattered electron scanning electron microscope (SEM) photograph inside the thermal spraying composite granule that embodiment 1 provides, wherein a, b, c
It is respectively the backscattered electron scanning electron microscope (SEM) photograph for the four typical composite granule particles chosen with d.
Fig. 9 be embodiment 1 provide thermal spraying composite granule made from coating backscattered electron scanning electron microscope (SEM) photograph and
EDS schemes, wherein a is the scanning electron microscope (SEM) photograph of backscattered electron, and b schemes for EDS.
Figure 10 is the SEM figures for the coating that comparative example 2 provides.
Figure 11 is the laser particle distribution map of NiCrAlY powder after the ball milling 13h that comparative example 5 provides.
Figure 12 is the SEM figures when NiCrAlY spheres of powder that comparative example 6 provides grind 4h.
Figure 13 is the SEM figures for the composite granule obtained that the preparation method 1 of comparative example 7 provides.
Figure 14 is the SEM figures for the composite granule obtained that the preparation method 2 of comparative example 7 provides
Specific implementation mode
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
Embodiment 1
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 78%
Cr2O3Powder 15%
Ag powder 7%；
Wherein, the average grain diameter of NiCrAlY powder is 900nm；The Cr2O3The average grain diameter of powder is 60nm；The Ag powder
Average grain diameter is 1 μm.
The preparation method of the thermal spraying composite granule is as shown in figure 3, the preparation method includes the following steps：
(1) by stainless steel ball, NiCrAlY powder and deionized water in mass ratio be 25:1:1.5 mixing, are put into ball grinder
In；The inert gas that flow velocity air pressure is 0.2MPa is passed through in ball grinder, it is 20 minutes to be passed through the time；Set drum's speed of rotation as
The tbp of 15g is added in 500rpm, ball milling 13h, ball milling initial stage, and the ball milling later stage is added 5g grinding aids, obtains average grain diameter
For the NiCrAlY powder of 900nm；
(2) it is 78 by mass ratio:1:7 NiCrAlY powder and Cr2O3Powder and the mixing of Ag powder, obtain mixed powder, will mix
Powder, deionized water and polyvinyl alcohol are according to mass ratio 30:68:2 are mixed into slurry, slurry are carried out ball milling, rotational speed of ball-mill is
120r/min, ratio of grinding media to material 10:1, dispersant is added in mechanical milling process, the dispersant accounts for the 0.01wt% of slurry gross weight, will
Slurry after ball milling is spray-dried, and the parameter of spray drying is：Temperature of inlet air is 230 DEG C, cavity air themperature
It it is 150 DEG C, air exit temp is 125 DEG C, and nozzle rotary speed is 13000r/min, and it is 60g/min that slurry, which gives rate,；Mist
Change air mass flow is 12m3/ h, high-pressure air pressure 0.4MPa obtain thermal spraying composite granule.
NiCrAlY powder and Cr in the thermal spraying composite granule2O3The distribution situation of powder and Ag powder is as shown in Fig. 2, with machinery
Thermal spraying composite granule (as shown in Figure 1) prepared by mixing method is compared, in thermal spraying composite granule prepared by spray drying process
NiCrAlY powder and Cr2O3The grain size of powder and Ag powder is less than the grain size of composite granule made from powder mixing machine method, and the big portion of Ag powder
It is distributed in the inside of single composite granule.
After Fig. 4 and Fig. 5 is ball milling 7h and 13h, with the volume distribution map for the NiCrAlY powder that laser particle analyzer measures.From figure
In as can be seen that after grinding 7h, the median of NiCrAlY powder is 5.62 μm, after grinding 13h, the median of NiCrAlY powder
For 890nm.
The SEM figures of NiCrAlY powder after Fig. 6 is before ball milling and ball milling 13h.The testing result of the SEM figures and Fig. 4 and Fig. 5
In testing result it is consistent.
Fig. 7 is NiCrAlY, Cr obtained2O3Scheme with the SEM of the composite granule of Ag, it can be seen from the figure that obtained multiple
Its particle size of conjunction powder is at 20~30 μm or so.
To carrying out backscattered electron sweep test inside the thermal spraying composite granule of preparation, testing result as shown in figure 8, from
It can be seen from the figure that, most Ag particles are covered by inside powder in composite granule, and only fraction Ag is exposed in powder
Surface, in this way in thermal spray process, Ag particles can be protected well, reduce the gasification of Ag to coating Ag contents and
The influence of self-lubricating property.
By composite granule hot spray process prepares coating, the scanning electron microscope (SEM) photograph of the backscattered electron of gained coating and
EDS images are as shown in Figure 9.
Comparative example 1
An Yulong etc. has studied another thermal spraying composite granule (including Ni-based Binder Phase, hard phase and lubrication phase
Ag), which includes mainly following component by mass percentage：
NiMoAl powder 76%
Cr3C2Powder 19%
Ag powder 5%；
Wherein, NiMoAl powder, Cr3C2The average grain diameter of powder and Ag powder is between 15~80 μm.
The composite granule is obtained using powder mixing machine method.
The SEM figures of gained composite granule hot spray process prepares coating, gained coating is as shown in Figure 10.
It is found by embodiment 1 and comparative example 1, the Ag particles in comparative example 1 can hold very much under the amplification factor under 400 times
It can easily find.And the Ag in embodiment 1 is due to smaller average grain diameter, even if being not easy to sweep in back scattering if 8 000 times
It retouches in Electronic Speculum and observes, and the Ag particles that only small part is reunited, grain size reach 2~3 μm, could find out in the picture；Knot
It closes its EDS image and can be seen that and uniformly scatter in the coating with the other Ag of submicron order, only small part Ag occurs
Reunite.
It can be seen that being prepared using powder mixing machine method, the coating Ag particles obtained by powder are other in the micron-scale, and dispersibility is poor.
And spray drying process prepares the other Ag of its internal submicron order of the coating obtained by powder and has more uniform dispersibility (in addition to few
A few micrometers grades of reunion Ag particles).
Embodiment 2
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 74.5%
Cr2O3Powder 16.5%
Ag powder 9%；
Wherein, the average grain diameter of NiCrAlY powder is 800nm；The Cr2O3The average grain diameter of powder is 100nm；The Ag powder
Average grain diameter be 800nm.
The preparation method of the thermal spraying composite granule is as shown in figure 3, the preparation method includes the following steps：
(1) by stainless steel ball, NiCrAlY powder and deionized water in mass ratio be 22.5:1:1.35 mixing, are put into ball milling
In tank；The inert gas that flow velocity air pressure is 0.2MPa is passed through in ball grinder, it is 20 minutes to be passed through the time；Set drum's speed of rotation
For 450rpm, ball milling 14h, the tbp for accounting for slurry gross mass 0.049% is added in ball milling initial stage, and the addition of ball milling later stage accounts for slurry
The grinding aid for expecting gross mass 0.018% obtains the NiCrAlY powder that average grain diameter is 800nm；
(2) by the NiCrAlY powder and Cr of formula ratio2O3Powder and Ag powder mixing, obtain mixed powder, by mixed powder, go from
Sub- water and polyvinyl alcohol are according to mass ratio 28:66:1.8 are mixed into slurry, and slurry is carried out ball milling, rotational speed of ball-mill 108r/
Min, ratio of grinding media to material 9:1, dispersant is added in mechanical milling process, the dispersant accounts for the 0.009wt% of slurry gross weight, by ball milling it
Slurry afterwards is spray-dried, and the parameter of spray drying is：Temperature of inlet air is 220 DEG C, and cavity air themperature is 135
DEG C, air exit temp is 112.5 DEG C, and nozzle rotary speed is 12870r/min, and it is 54g/min that slurry, which gives rate,；Atomization
Air mass flow is 10.8m3/ h, high-pressure air pressure 0.36MPa obtain thermal spraying composite granule.
It finds after tested, most Ag particles are covered by inside powder in gained composite granule, only fraction Ag
It is exposed in powder surface.
Embodiment 3
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 81.5%
Cr2O3Powder 13.5%
Ag powder 5%；
Wherein, the average grain diameter of NiCrAlY powder is 1000nm；The Cr2O3The average grain diameter of powder is 80nm；The Ag powder
Average grain diameter be 1200nm.
The preparation method of the thermal spraying composite granule is as shown in figure 3, the preparation method includes the following steps：
(1) by stainless steel ball, NiCrAlY powder and deionized water in mass ratio be 27.5:1:1.65 mixing, are put into ball milling
In tank；The inert gas that flow velocity air pressure is 0.2MPa is passed through in ball grinder, it is 20 minutes to be passed through the time；Set drum's speed of rotation
For 650rpm, ball milling 15h, the tbp for accounting for slurry gross mass 0.060% is added in ball milling initial stage, and the addition of ball milling later stage accounts for slurry
The grinding aid for expecting gross mass 0.018% obtains the NiCrAlY powder that average grain diameter is 1000nm；
(2) by the NiCrAlY powder and Cr of formula ratio2O3Powder and Ag powder mixing, obtain mixed powder, by mixed powder, go from
Sub- water and polyvinyl alcohol are according to mass ratio 32:70:2.2 are mixed into slurry, and slurry is carried out ball milling, rotational speed of ball-mill 132r/
Min, ratio of grinding media to material 11:1, dispersant is added in mechanical milling process, the dispersant accounts for the 0.011wt% of slurry gross weight, by ball milling
Slurry later is spray-dried, and the parameter of spray drying is：Temperature of inlet air is 240 DEG C, and cavity air themperature is 165
DEG C, air exit temp is 136.5 DEG C, and nozzle rotary speed is 13130r/min, and it is 66g/min that slurry, which gives rate,；Atomization
Air mass flow is 13.2m3/ h, high-pressure air pressure 0.44MPa obtain thermal spraying composite granule.
It finds after tested, most Ag particles are covered by inside powder in gained composite granule, only fraction Ag
It is exposed in powder surface.
Comparative example 2
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 73%
Cr2O3Powder 17%
Ag powder 10%；
Wherein, the average grain diameter of NiCrAlY powder is 900nm；The Cr2O3The average grain diameter of powder is 60nm；The Ag powder
Average grain diameter is 1 μm.
The preparation method of the thermal spraying composite granule is identical as the preparation method of embodiment 1.
Comparative example 3
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 84%
Cr2O3Powder 12%
Ag powder 4%；
Wherein, the average grain diameter of NiCrAlY powder is 900nm；The Cr2O3The average grain diameter of powder is 60nm；The Ag powder
Average grain diameter is 1 μm.
The preparation method of the thermal spraying composite granule is identical as the preparation method of embodiment 1.
Comparative example 4
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 78%
Cr2O3Powder 15%
Ag powder 7%；
Wherein, NiCrAlY powder, Cr2O3The average grain diameter of powder and Ag powder is 6 μm.
By composite granule hot spray process prepares coating made from comparative example 2-4, in gained coating Ag particle dispersions compared with
Difference, the surface of mechanical equipment and component for being operated under the extreme harsh operating mode such as high temperature, high speed and heavy duty, performance is obviously not
The coating as made from embodiment 1.
Comparative example 5：Antifoaming agent type it is preferred
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 73%
Cr2O3Powder 17%
Ag powder 10%.
The preparation method of the thermal spraying composite granule disappears except the tbp in step (1) is replaced with organic silicon
Outside infusion, remaining is identical as the preparation method in embodiment 1.
It is found in preparation process：Organic silicon antifoaming agent defoaming effect unobvious, so being needed in entire mechanical milling process
It is continuously added, 10g or so is added every about half an hour, but ball milling is to 13h always, can not still accomplish that NiCrAlY powder is averaged grain
Diameter is less than 5um, and the average particle size distribution figure of NiCrAlY powder is as shown in figure 11 after ball milling 13h, as can be seen from the figure ball milling 13h
The average grain diameter of NiCrAlY powder is at 10 μm or so afterwards.
Comparative example 6：Ball milling solvent it is preferred
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 73%
Cr2O3Powder 17%
Ag powder 10%.
The preparation method of the hot spraying powder by the deionized water in step (1) in addition to replacing with alcohol, remaining and reality
The preparation method applied described in example 1 is identical.
It is found in preparation process：With the extension of time, the gradual flattening of NiCrAlY powders, i.e. radius-thickness ratio gradually increase.
When Figure 12 is ball milling 4h, the SEM figures of NiCrAlY powders.It can be seen from the figure that flat substance is relatively more, sheet it is big and
It is relatively thin.Continue ball milling, the distribution of shapes of particle flattening does not mitigate, and more obvious.
Comparative example 7：Binder polyvinyl alcohol (PVA) content it is preferred
A kind of thermal spraying composite granule, the thermal spraying composite granule include following component by mass percentage：
NiCrAlY powder 73%
Cr2O3 powder 17%
Ag powder 10%.
Preparation method 1：
The preparation method 1 of the thermal spraying composite granule in addition in step (2) by mixed powder, deionized water and binder
According to mass ratio 30:68:1.5 mixing are outer, remaining is identical as preparation method described in embodiment 1.
It is found in preparation process, the content of binder is very few, causes the cohesive strength of prilling powder internal particle small and holds
It is easily loose so that the spheric granules being granulated out is seldom, has more powder drawout, as shown in figure 13.
Preparation method 2：
The preparation method 2 in addition in step (2) by mixed powder, deionized water and binder according to mass ratio 30:68:
2.5 mixing are outer, remaining is identical as preparation method described in embodiment 1.
It is found in preparation process, the too high levels of binder, the slurry viscosity being made into is excessive, therefore causes powder surface viscous
Conjunction property is excessive, and phenomenon mutually cohesive is serious between particle, and powder will appear flocculence, coarse or irregular shape, such as Figure 14
It is shown.
Applicant states, the foregoing is merely the specific implementation mode of the present invention, but protection scope of the present invention not office
It is limited to this, person of ordinary skill in the field is it will be clearly understood that any belong to those skilled in the art and taken off in the present invention
In the technical scope of dew, the change or replacement that can be readily occurred in are all fallen within protection scope of the present invention and the open scope.
Claims (12)
1. a kind of thermal spraying composite granule, which is characterized in that the thermal spraying composite granule includes mainly by mass percentage
Following component：
NiCrAlY powder 74.5 ~ 81.5%
Cr2O3Powder 13.5 ~ 16.5%
Ag powder 5 ~ 9%；
Wherein, NiCrAlY powder, Cr2O3The average grain diameter of powder and Ag powder is independently less than 5 μm；
The preparation method of the thermal spraying composite granule includes the following steps：
（1）What it is by stainless steel ball, NiCrAlY powder and deionized water is 22.5 ~ 27.5 in mass ratio:1:1.35 ~ 1.65 mixing, put
Enter in ball grinder；The inert gas that flow velocity air pressure is 0.2MPa is passed through in ball grinder, it is 20 minutes to be passed through the time；Set ball milling
Machine rotating speed is 450 ~ 650rpm, 13 ~ 15h of ball milling, ball milling start after 10 ~ 20min in be added that account for slurry total into ball milling system
The tbp of quality 0.049 ~ 0.060%, ball milling terminate before 2 ~ 3h in, into ball milling system be added account for slurry gross mass
0.018% grinding aid obtains the NiCrAlY powder that average grain diameter is less than 5 μm；
（2）The NiCrAlY powder of formula ratio and average grain diameter are independently less than to 5 μm of Cr2O3Powder and the mixing of Ag powder, are mixed
Powder, by mixed powder, deionized water and polyvinyl alcohol according to mass ratio 28 ~ 32:66~70:1.8 ~ 2.2 are mixed into slurry, will
Slurry carries out ball milling, and rotational speed of ball-mill is 108 ~ 132r/min, and ratio of grinding media to material is 9 ~ 11:1, dispersant is added in mechanical milling process, it is described
Dispersant accounts for 0.009 ~ 0.011wt% of slurry gross weight, and the slurry after ball milling is spray-dried, the parameter of spray drying
For：Temperature of inlet air is 220 ~ 240 DEG C, and cavity air themperature is 135 ~ 165 DEG C, and air exit temp is 112.5 ~ 136.5
DEG C, nozzle rotary speed is 12870 ~ 13130r/min, and it is 54 ~ 66g/min that slurry, which gives rate,；Atomization air flow is 10.8
~13.2m3/ h, high-pressure air pressure are 0.36 ~ 0.44MPa, obtain thermal spraying composite granule；
Wherein, grinding aid OP-10；Dispersant is SND6800 agent.
2. composite granule according to claim 1, which is characterized in that the average grain diameter of the NiCrAlY powder be 800nm ~
1000nm。
3. composite granule according to claim 1, which is characterized in that the Cr2O3The average grain diameter of powder be 60nm ~
100nm。
4. composite granule according to claim 1, which is characterized in that the average grain diameter of the Ag powder is 800nm ~ 1.2 μm.
5. composite granule according to claim 1, which is characterized in that the NiCrAlY powder is obtained by high energy ball mill ball milling
It arrives.
6. composite granule according to claim 1, which is characterized in that the particle size of the composite granule is 15 ~ 45 μm.
7. composite granule according to claim 1, which is characterized in that the composite granule passes through centrifugal spray dryer
It is prepared.
8. the preparation method of the composite granule according to one of claim 1-7, which is characterized in that the preparation method includes
Following steps：
（1）NiCrAlY powder is subjected to ball milling, obtains the NiCrAlY powder that average grain diameter is less than 5 μm；
（2）The NiCrAlY powder of formula ratio and average grain diameter are independently less than to 5 μm of Cr2O3Powder and the mixing of Ag powder, are mixed
Mixed powder is spray-dried by powder, obtains thermal spraying composite granule；
The preparation method specifically comprises the following steps：
（1）What it is by stainless steel ball, NiCrAlY powder and deionized water is 22.5 ~ 27.5 in mass ratio:1:1.35 ~ 1.65 mixing, put
Enter in ball grinder；The inert gas that flow velocity air pressure is 0.2MPa is passed through in ball grinder, it is 20 minutes to be passed through the time；Set ball milling
Machine rotating speed is 450 ~ 650rpm, 13 ~ 15h of ball milling, ball milling start after 10 ~ 20min in be added that account for slurry total into ball milling system
The tbp of quality 0.049 ~ 0.060%, ball milling terminate before 2 ~ 3h in, into ball milling system be added account for slurry gross mass
0.018% grinding aid obtains the NiCrAlY powder that average grain diameter is less than 5 μm；
（2）The NiCrAlY powder of formula ratio and average grain diameter are independently less than to 5 μm of Cr2O3Powder and the mixing of Ag powder, are mixed
Powder, by mixed powder, deionized water and polyvinyl alcohol according to mass ratio 28 ~ 32:66~70:1.8 ~ 2.2 are mixed into slurry, will
Slurry carries out ball milling, and rotational speed of ball-mill is 108 ~ 132r/min, and ratio of grinding media to material is 9 ~ 11:1, dispersant is added in mechanical milling process, it is described
Dispersant accounts for 0.009 ~ 0.011wt% of slurry gross weight, and the slurry after ball milling is spray-dried, the parameter of spray drying
For：Temperature of inlet air is 220 ~ 240 DEG C, and cavity air themperature is 135 ~ 165 DEG C, and air exit temp is 112.5 ~ 136.5
DEG C, nozzle rotary speed is 12870 ~ 13130r/min, and it is 54 ~ 66g/min that slurry, which gives rate,；Atomization air flow is 10.8
~13.2m3/ h, high-pressure air pressure are 0.36 ~ 0.44MPa, obtain thermal spraying composite granule；
Wherein, grinding aid OP-10；Dispersant is SND6800 agent.
9. preparation method according to claim 8, which is characterized in that step（1）The ball milling interval carries out：Ball milling
0.5h is further continued for ball milling after being spaced 0.5h.
10. preparation method according to claim 8, which is characterized in that step（1）The ball milling is enterprising in high energy ball mill
Row.
11. preparation method according to claim 8, which is characterized in that step（2）The spray drying is in atomizer
It is carried out on drying machine.
12. the purposes of the composite granule according to one of claim 1-7 is used to prepare wear-resisting composite solid lubricant and applies
Layer.
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| CN108716574B (en) * | 2018-06-19 | 2020-05-19 | 广汉华气防腐工程有限公司 | Production process of high-weather-resistance anticorrosive pipe |
| CN109504933A (en) * | 2019-01-16 | 2019-03-22 | 兰州城市学院 | A kind of NiAl-Cr2O3- Mo-Ag high temperature lubricating composite coating and preparation method |
| CN109868443B (en) * | 2019-03-12 | 2020-12-22 | 唐山学院 | Nickel-based aluminum oxide high-temperature self-lubricating wear-resistant coating and preparation method thereof |
| CN110230018A (en) * | 2019-04-26 | 2019-09-13 | 中国科学院兰州化学物理研究所 | A kind of preparation method of metal sound stage width temperature range self-lubricating coat in use |
| CN110607526B (en) * | 2019-09-06 | 2022-07-05 | 中国兵器科学研究院宁波分院 | Method for preparing nickel-based wide-temperature-range self-lubricating coating with nano structure by cold spraying |
| CN115522156B (en) * | 2022-09-29 | 2024-05-14 | 中国科学院兰州化学物理研究所 | Nickel-chromium carbide-based self-lubricating composite coating with wide temperature range and preparation method thereof |
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