CN102703850A - Ternary boride ceramic coating with cerium oxide and preparation method thereof - Google Patents
Ternary boride ceramic coating with cerium oxide and preparation method thereof Download PDFInfo
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- CN102703850A CN102703850A CN2012101952883A CN201210195288A CN102703850A CN 102703850 A CN102703850 A CN 102703850A CN 2012101952883 A CN2012101952883 A CN 2012101952883A CN 201210195288 A CN201210195288 A CN 201210195288A CN 102703850 A CN102703850 A CN 102703850A
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Abstract
The invention discloses a ternary boride ceramic coating with cerium oxide and a preparation method thereof, belonging to the technical field of coating preparation. The preparation method comprises the following steps of: adopting a thermal spraying technology, taking Mo powder, Fe powder and FeB powder as raw materials, and preparing the Mo2FeB2 ternary boride ceramic coating on a Q235 steel matrix; and adding CeO2 powder with a friction reducing effect on the ternary boride ceramic coating, and preparing the Mo2FeB2 ternary boride ceramic coating with CeO2 components by using the same technology. In comparison with the Q235 matrix, the abrasive wear resistance of the ternary boride ceramic coating disclosed by the invention is improved by 50%, and the adhesive wear resistance of the ternary boride ceramic coating is improved by 59%, so that the ternary boride ceramic coating has an excellent abrasion resistance and a higher friction coefficient ranging from 0.31 to 0.52.
Description
Technical field
The invention belongs to the coat preparing technology field, be specifically related to a kind of ternary boride ceramic coating that contains cerium oxide.
Background technology
At present, ternary boride (Mo
2FeB
2) preparation method of ceramic coating mainly concentrates on vacuum liquid-phase sintering method, reaction in synthesis method, but all there is certain deficiency in preparation technology.At present, domestic research for the ternary boride ceramic coating is less, and the research of self-lubricating ternary boride ceramic coating does not appear in the newspapers especially.REE has unique physicochemical property, in the application of lubricant, has obtained bigger achievement, and REE also has and manyly more do not awaited inquiring into by the mechanism of action of the special property, particularly its compound of people's understanding.It is added in the ternary boride ceramic coating, and the research that the expection acquisition has than the ternary boride cement coating of low-friction coefficient has never seen report.
The metal matrix ceramic composite coating material because of it has had the two-fold advantage of metal with pottery concurrently, has obtained using widely.In recent years, the ternary boride-based metal pottery enjoys the attention of Chinese scholars as a kind of novel mechanically resistant material of excellent property.At present, a few developed countries such as Japan, the U.S. after deliberation the ternary boride-based metal pottery of a plurality of systems, and be applied to make the cold and hot drawing-die of part, steel wire of a jar instrument, injection moulding machine, the protection part of boiler heat exchanger tube etc.And domestic research for ternary boride pottery is started late, and starts from recent years especially for the research of ternary boride ceramic coating.The ternary boride-based metal pottery has high firmness, HS, low density and high rigidity; And characteristics such as excellent chemicalstability and mechanical behavior under high temperature; But its rubbing factor generally reaches between the 0.7-0.8 generally all than higher, is difficult to realize the purpose of oil-free self lubrication.And not enough below traditional lubricating system exists: 1) additive in the lubricant is not had an effect with ceramic surface, thereby can not form the boundary film that can fully contact; 2) existing lubricant is owing to raise with temperature, and its viscosity is index decreased, is prone to cause micro-bulge directly to contact; 3) performance degradation of liquid lubricant takes place down in high temperature easily.Therefore, carry out relevant ceramic matric composite Study on Tribological Properties and come into one's own day by day, become one of advanced subject of present material science and tribological field.Cooperate the collaborative most important thing that addresses this problem that becomes between the resistance to abrasion that realizes coating and the frictional coefficient.
Summary of the invention
The present invention adopts hot-spraying techniques, is that raw material has prepared Mo on the Q235 steel matrix with Mo powder, Fe powder and FeB powder
2FeB
2The ternary boride ceramic coating, and add CeO on this basis with antifriction function
2Powder adopts the hot-spraying techniques preparation to contain CeO
2The ceramic coating of constituent element; The composition and the pattern of utilized X-ray diffractometer (XRD), ESEM equipment such as (SEM) and means analysis dusty spray and ceramic coating; And thermal shock performance, compactness, microhardness, the friction and wear behavior of coating tested, analyze CeO one by one
2Interpolation to ceramic coating weave construction and Effect on Performance.
The preparation method who contains the ternary boride ceramic coating of cerium oxide of the present invention comprises the steps:
The first step, substrate pretreated:
Select the Q235 steel board for use, roughening treatment is carried out on its surface after, at matrix surface spraying Ni-Al transition layer.
Second step, the preparation of spraying feeding:
Mo powder, FeB alloy powder and Fe powder are mixed, become metal-powder, in metal-powder, add the PVB sticker according to mass ratio ω (FeB): ω (Mo): ω (Fe)=32:48:20 mixes; The mass ratio of metal-powder and PVB sticker is 5:1, in 100 ℃ of drying bakers, dries 1.5 ~ 2h, and the reunion powder after the oven dry is broken; Cross 200 mesh sieves; Be 1%～5% rare earth cerium oxide to wherein adding mass percent then, mix, obtain spraying feeding.
The 3rd step, the preparation of ceramic coating:
Pretreated matrix is carried out preheating, and spraying preparation ceramic coating carries out remelting after the spraying then, cooling.Spraying parameter is: 70～85 ° of spray angles, spray distance 130～150mm, translational speed 60～90mms
-1, oxygen pressure 0.6～0.8Mpa, acetylene pressure 0.10～0.11Mpa.
The CeO that contains provided by the invention
2The ceramic coating of constituent element, the mass percent of in the ceramic coating preparation, adding cerium oxide is 1～5%, the microhardness Hv of ceramic coating
0.1Be 665～1405, porosity is 7.61～21.78%, and the thermal shock number of times is more than 40 times, and bond area is 225mm
2Under the condition, tensile strength is 15.99～19.8MPa, and the frictional coefficient of coating is between 0.31～0.52.
The mass percent of in the ceramic coating preparation, adding cerium oxide is 1～4%, the microhardness Hv of ceramic coating
0.1Be 817～1405, porosity is 7.61～15.58%, and the thermal shock number of times is more than 53 times, and bond area is 225mm
2Under the condition, tensile strength is 16.9～19.8MPa, and the frictional coefficient of coating is between 0.34～0.52.
Description of drawings
Fig. 1 is the ceramic coating preparation method schema that contains cerium oxide of the present invention;
Fig. 2 is the mensuration sketch of ceramic coating bonding force among the present invention;
Fig. 3 is the XRD diffractogram of the ternary boride ceramic coating for preparing among the comparative example of the present invention;
Fig. 4 (A), (B), (C) are respectively ceramic coating surface topography, cross section pattern, the cross section backscatter images for preparing among the comparative example, and Fig. 4 (D) is the EDS curve of corresponding points among Fig. 4 (C).
Fig. 5 A is the XRD diffractogram of the ceramic coating that contains cerium oxide 1% for preparing among the present invention;
Fig. 5 B is the XRD diffractogram of the ceramic coating that contains cerium oxide 5% for preparing among the present invention;
Among Fig. 6, (A) add 1%CeO
2The coatingsurface pattern; (B) add 3%CeO
2The coatingsurface pattern; (C) add 5%CeO
2The coatingsurface pattern; (D) add 3%CeO
2Be coated with the layer cross section pattern; (E) add 5%CeO
2Be coated with the layer cross section pattern.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
The present invention provides a kind of preparation method who contains the ternary boride ceramic coating of cerium oxide, and technical process is as shown in Figure 1, comprises that mainly matrix sample pretreatment, the preparation of spraying feeding and ceramic coating prepare three parts, and is specific as follows:
The first step, substrate pretreated:
(1) specimen surface alligatoring:
Body material is the Q235 steel board, and chemical ingredients is seen table 1:
Table 1Q235-A steel plate chemical ingredients (wt.%)
With thickness is that the Q235 steel plate line cutting of 6mm is cut into the sample that area is 25mm * 25mm; The surface through sandblasting to remove surface scale; Make specimen surface activation and alligatoring, with the contact area of increase workpiece and sprayed coating, and the alligatoring of coating can change the coating unrelieved stress; Help improving coating and high base strength, for the preparation of transition layer lays the foundation.The sandblasting processing parameter is: the sandblast abrasive particle is emergy (preferred 20 orders), spray distance 100～150mm, 90 ° of sandblast angles, compressed air pressure 0.6～0.8MPa.
(2) preparation of Ni-Al transition layer:
Buffer layer material is selected nickel alclad powdered alloy for use, Al contained Ni Ni-Al granularity 46.67 ~ 103.55 μ m, and the content of Al element is mass percent 10.24%, all the other are Ni.At first use flame spray gun (QH-2/h type) that the matrix sample of alligatoring is carried out (300～400 ℃ of preheatings; 5～7 minutes); To eliminate the moisture and the moisture on surface; Improve the temperature that spray material contacts with workpiece surface, reduce stress, thereby reduce disbonding because of its generation because of the thermal dilation difference generation of matrix and coating.Immediately at specimen surface spraying Ni-Al transition layer, alleviate the thermal stresses between coating and the matrix after the preheating, improve coating and high base strength.
Second step, the preparation of spraying feeding:
The preparation process of Mo-FeB-Fe system spraying feeding is: Mo powder, FeB alloy powder and Fe powder are mixed; Mix the formation metal-powder according to mass ratio ω (FeB): ω (Mo): ω (Fe)=32:48:20, in metal-powder, add the PVB sticker, the mass ratio of metal-powder and sticker is 5:1; In 100 ℃ of drying bakers, dry 1.5 ~ 2h; Reunion powder after the oven dry is broken, cross 200 mesh sieves, be 1% ~ 5% rare earth cerium oxide to wherein adding mass percent then; Mix, obtain spraying feeding.
Iron particle size 4.95 μ m, ferro-boron powder FeB granularity 6.47 μ m, cerium oxide is an analytical pure.Molybdenum powder particle diameter 300 orders, because granularity and Fe powder and FeB powder degree are close, each powder after the granulation mixes fully, each is evenly distributed mutually in the coating that after spraying, forms.
Described PVB adhesive preparation step is specific as follows:
(1) using graduated cylinder to measure 50ml concentration is that 98% absolute ethyl alcohol is poured in the 150ml beaker, is placed on and is heated to (PVB this moment solubleness in ethanol is maximum) about 60 ℃ on the time constant-temperature magnetic stirring apparatus; (2) take by weighing the PVB of 3.75g, join in the beaker slowly and constantly stir, make absolute ethyl alcohol and PVB thorough mixing, after PVB dissolves fully, stop to heat, finally obtain colourless, transparent PVB sticker with glass stick.
Ceramic powder must add sticker in the process of preparation spraying feeding, to increase the bonding strength between the particle in the powder.Sticker has played the adhesive effect between powder in the powder preparing process, divided particles is more closely bonded together, and discharges in the next meeting of the pyritous environment of thermospray, can not introduce new composition for coating.Because mostly the raw material of selecting for use in the experiment is metal-powder; For preventing that it from the preparation feeding procedure oxidation taking place; Elite is sticker (polyvinyl butyral acetal and absolute ethyl alcohol are analytical pure) with polyvinyl butyral acetal (PVB) ethanolic soln, and ethanolic soln selects absolute ethyl alcohol for use, guarantees not introduce in the preparation process moisture; If the aqueous solution of employing Z 150PH is sticker then can makes metal-powder generation oxidation, thereby influences the carrying out of subsequent experimental.
The 3rd step, the preparation of ceramic coating:
To pass through pretreated matrix sample and use acetone, and utilize spraying flame that it is carried out preheating, the spraying feeding that spraying immediately prepares after the preheating.After sample has sprayed,, utilize spraying flame for improving coating performance and compactness; It is carried out remelting handle, after the end, with tweezers it is sandwiched furnace cooling in 200 ℃ of baking ovens immediately; Avoid too fast, make the big thermal stresses of generation between coating and the matrix, and cause disbonding because of cooling off.The concrete processing parameter of spraying and remelting is following:
300～400 ℃ of substrate preheating temperature, time 5 ~ 7min, 700～800 ℃ of remelting temperatures, time 1～2min; 70～85 ° of spray angles, spray distance 130～150mm moves speed 60～90mms
-1, oxygen pressure 0.6～0.8Mpa, acetylene pressure 0.10～0.11Mpa.
The spraying method of being selected for use among the embodiment is oxyacetylene torch spraying (selecting the spray gun model for use is QH-2/H type flame spray gun); Flame temperature is with descending apart from increase apart from jet hole; Temperature can reach 3100 ℃; Temperature is higher in the jet hole 50mm scope, so selected spray distance is apart from about the jet hole 100mm among the embodiment.When oxygen was pressed to 0.7Mpa, the coating of formation is consolidation comparatively, and thickness is comparatively even, does not have peeling phenomenon.
Through the ternary boride ceramic coating that contains cerium oxide that method for preparing obtains, the microhardness Hv of ceramic coating
0.1Be 665～1405, porosity is 7.61～21.78%, and the thermal shock number of times is more than 40 times, and bond area is 225mm
2Under the condition, tensile strength is 15.99～19.8MPa, and the frictional coefficient of coating is between 0.31～0.52.
Embodiment 1:
Adopt preparing method's preparation provided by the invention to contain the ternary boride ceramic coating of cerium oxide, the adding mass percent is 1% cerium oxide in the dusty spray, and preparing method's step is following:
The first step, substrate pretreated:
Matrix is carried out surface coarsening, prepare the Ni-Al transition layer then above that.
Described matrix is selected the Q235 steel plate for use, and surface coarsening adopts blasting method, and the sandblasting processing parameter is: the sandblast abrasive particle is 20 order emergies, spray distance 150mm, 90 ° of sandblast angles, compressed air pressure 0.8MPa.
Carrying out can carrying out thermal pretreatment to matrix earlier before the transition layer preparation, preheating temperature is 300 ℃, and be 7min warm up time.Al contained Ni is selected in the transition layer preparation for use.
Second step, the preparation of spraying feeding:
Choose Mo powder, FeB alloy powder and Fe powder and be respectively 32g, 48g, 20g, add the PVB sticker, the mass ratio of metal-powder and sticker is 5:1; In 100 ℃ of drying bakers, dry 1.5h; Reunion powder after the oven dry is broken, cross 200 mesh sieves, be 1% rare earth cerium oxide to wherein adding mass percent then; Mix, obtain spraying feeding.Described PVB sticker is that to adopt 50ml concentration be that 98% absolute ethyl alcohol and the PVB of 3.75g are prepared from.
The 3rd step, the preparation of ceramic coating:
It is clear with acetone to pass through pretreated matrix sample, utilizes spraying flame that it is carried out preheating, 400 ℃ of substrate preheating temperature, the spraying feeding that spraying prepares on transition layer immediately after the preheating.After sample has sprayed, utilize spraying flame that it is carried out remelting (700 ℃ of temperature, time 2min) and handle, after the end, with tweezers it is sandwiched furnace cooling in 200 ℃ of baking ovens immediately.Adopt the concrete processing parameter of oxy-acetylene flame thermospray to be: 85 ° of spray angles, spray distance 150mm moves fast 90mms
-1, oxygen pressure 0.8Mpa, acetylene pressure 0.11Mpa.
In the ceramic coating that method for preparing obtains, see Fig. 5 A, except have hard reach mutually iron-based bonding mutually, also have FeMoO
4, B
2O
3Generate Deng mutually, the result does not have Fe
2O
3Produce, reduced the inclusion in the coating, help improving the compactness of coating; Shown in Fig. 6 A, coating has the characteristic feature in the hot spray coating in the atmosphere, mainly forms (being laminated structure) by flat particle not of uniform size; The coatingsurface hole is less, obviously is superior to not adding CeO
2Coating.Microhardness of coating Hv
0.1Be 817～1376, porosity is 15.58%, is lower than the comparative example's who does not add cerium oxide porosity (19.14%), and thermal shock number of times 53 times, bond area are 225mm
2Under the condition, tensile strength is 16.9MPa, and the coating frictional coefficient is between 0.47～0.49.
Embodiment 2:
Adopt preparing method's preparation provided by the invention to contain the ternary boride ceramic coating of cerium oxide, the adding mass percent is 2% cerium oxide in the dusty spray, and preparing method's step is following:
The first step, substrate pretreated:
Matrix Q235 steel is carried out surface coarsening, prepare the Ni-Al transition layer then above that.
Blasting method is adopted in described matrix surface alligatoring, and the sandblasting processing parameter is: the sandblast abrasive particle is 20 order emergies, spray distance 100mm, 90 ° of sandblast angles, compressed air pressure 0.6MPa.
Carrying out can carrying out thermal pretreatment to matrix earlier before the transition layer preparation, preheating temperature is 400 ℃, and be 5min warm up time.
Second step, the preparation of spraying feeding:
Choose Mo powder, FeB alloy powder and Fe powder and be respectively 32g, 48g, 20g, add the PVB sticker, the mass ratio of metal-powder and sticker is 5:1; In 100 ℃ of drying bakers, dry 2h; Reunion powder after the oven dry is broken, cross 200 mesh sieves, be 2% rare earth cerium oxide to wherein adding mass percent then; Mix, obtain spraying feeding.Described PVB sticker is that to adopt 50ml concentration be that 98% absolute ethyl alcohol and the PVB of 3.75g are prepared from.
The 3rd step, the preparation of ceramic coating:
It is clear with acetone to pass through pretreated matrix sample, utilizes spraying flame that it is carried out preheating, 400 ℃ of substrate preheating temperature, the spraying feeding that spraying immediately prepares after the preheating.After sample has sprayed, utilize spraying flame that it is carried out remelting and handle (800 ℃ of temperature, time 1min), after the end, with tweezers it is sandwiched furnace cooling in 200 ℃ of baking ovens immediately.Adopt the concrete processing parameter of oxy-acetylene flame thermospray to be: 70 ° of spray angles, spray distance 130mm moves fast 60mms
-1, oxygen pressure 0.6Mpa, acetylene is pressed 0.1Mpa.
Mainly be Mo in the coating that method for preparing obtains mutually
2FeB
2, Fe, FeMoO
4, B
2O
3And CeO
2, microhardness of coating Hv
0.1Be 817-1385, porosity is 10.61%, and the thermal shock number of times is more than 54 times, and bond area is 225mm
2Under the condition, tensile strength is 17.31MPa, and the coating frictional coefficient is between 0.49-0.52.
Embodiment 3:
Adopt preparing method's preparation provided by the invention to contain the ternary boride ceramic coating of cerium oxide, the adding mass percent is 3% cerium oxide in the dusty spray, and preparing method's step is following:
The first step, substrate pretreated:
Matrix is carried out surface coarsening, prepare the Ni-Al transition layer then above that, Al contained Ni Ni-Al granularity 103.55 μ m.
Described matrix is selected the Q235 steel plate for use, and surface coarsening adopts blasting method, and the sandblasting processing parameter is: the sandblast abrasive particle is 20 order emergies, spray distance 120mm, 90 ° of sandblast angles, compressed air pressure 0.7MPa.
Carrying out can carrying out thermal pretreatment to matrix earlier before the transition layer preparation, preheating temperature is 400 ℃, and be 6min warm up time.
Second step, the preparation of spraying feeding:
Choose Mo powder, FeB alloy powder and Fe powder and be respectively 32g, 48g, 20g; Add 20g PVB sticker, in 100 ℃ of drying bakers, dry 1.5h, the reunion powder after the oven dry is broken; Cross 200 mesh sieves; Be 3% rare earth cerium oxide to wherein adding mass percent then, mix, obtain spraying feeding.Described PVB sticker is that to adopt according to 50ml concentration be that the proportioning of the PVB of 98% absolute ethyl alcohol and 3.75g is prepared from.
The 3rd step, the preparation of ceramic coating:
To pass through pretreated matrix sample and use acetone, and utilize spraying flame that it is carried out preheating, 350 ℃ of substrate preheating temperature, the spraying feeding that spraying immediately prepares after the preheating.After sample has sprayed, utilize spraying flame that it is carried out remelting and handle (750 ℃ of temperature, time 2min), after the end, with tweezers it is sandwiched furnace cooling in 200 ℃ of baking ovens immediately.Adopt the concrete processing parameter of oxy-acetylene flame thermospray to be: 75 ° of spray angles, spray distance 140mm moves fast 80mms
-1, oxygen pressure 0.8Mpa, acetylene is pressed 0.11Mpa.
In the ceramic coating that method for preparing obtains, mainly be Mo mutually
2FeB
2, Fe, FeMoO
4, B
2O
3And CeO
2, shown in Fig. 6 B and 6D, show can see clearly in the pattern that drop melts after, the pattern that trickling is sprawled, visible CeO
2Interpolation can effectively improve the coatingsurface pattern, the hole and the fecula that reduce in the coating are mingled with, and combine closely between coating and the Ni-Al layer, the boundary line is not obvious, defective is less at the interface; Microhardness of coating Hv
0.1Be 879-1405, porosity is 7.61%, and the thermal shock number of times is more than 60 times, and bond area is 225mm
2Under the condition, tensile strength is 19.80MPa.When wearing-in period was 10min, the abrasion loss of comparative example's coating was 0.0274g, added 3%CeO
2The ceramic coating abrasion loss be 0.0072g, wear resistance is not add 3.81 times of CeO2 ceramic coating; When wearing-in period was 15min, the abrasion loss of starting powder ceramic coating was 0.0379g, added 3%CeO
2The ceramic coating abrasion loss be 0.0087g, wear resistance is not add CeO
24.37 times of ceramic coating; The abrasion loss of starting powder ceramic coating was 0.0494g when wearing-in period was 20min, added 3%CeO
2The ceramic coating abrasion loss be 0.0148g, wear resistance is not add CeO
23.34 times of ceramic coating.Under the load of 300N, do not add CeO
2The abrasion loss of ceramic coating is 0.0123g, adds 3%CeO
2The abrasion loss of ceramic coating be 0.0041g, wear resistance is not add CeO
23.00 times of ceramic coating; Under 400N load, do not add CeO
2The ceramic coating abrasion loss is 0.0274g, adds 3%CeO
2The abrasion loss of ceramic coating be 0.0072g, wear resistance is not add CeO
23.81 times of ceramic coating; Under 500N load, do not add CeO
2The ceramic coating abrasion loss is 0.0449g, adds 3%CeO
2The abrasion loss of ceramic coating be 0.0043g, wear resistance is not add CeO
210.44 times of ceramic coating.The frictional coefficient of coating is between 0.34-0.36.
Embodiment 4:
Adopt preparing method's preparation provided by the invention to contain the ternary boride ceramic coating of cerium oxide, the adding mass percent is 4% cerium oxide in the dusty spray, and preparing method's step is following:
The first step, matrix are carried out surface coarsening sandblasting processing parameter: the sandblast abrasive particle is 20 order emergies, spray distance 150mm, 90 ° of sandblast angles, compressed air pressure 0.8MPa.All the other are with embodiment 1.
In second step, the adding mass percent is 4% rare earth cerium oxide in the spraying feeding, and all the other are with embodiment 1.
In the 3rd step, the preparation of ceramic coating adopts the concrete processing parameter of oxy-acetylene flame thermospray to be: 85 ° of spray angles, spray distance 150mm moves fast 90mms
-1, oxygen pressure 0.8Mpa, acetylene is pressed 0.11Mpa, and all the other are with embodiment 1.
Mainly be Mo in the coating that method for preparing obtains mutually
2FeB
2, Fe, FeMoO
4, B
2O
3And CeO
2, the microhardness Hv of ceramic coating
0.1Be 862～1392, porosity is 9.13%, and the thermal shock number of times is more than 60 times, and bond area is 225mm
2Under the condition, tensile strength is 18.60MPa, and the frictional coefficient of coating is between 0.38～0.40.
Embodiment 5:
Adopt preparing method's preparation provided by the invention to contain the ternary boride ceramic coating of cerium oxide, the adding mass percent is 5% cerium oxide in the dusty spray, and preparing method's step is following:
The first step, substrate pretreated surface coarsening sandblasting processing parameter is: the sandblast abrasive particle is 20 order emergies, spray distance 120mm, 90 ° of sandblast angles, compressed air pressure 0.8MPa.All the other are with embodiment 2.
In second step, the adding mass percent is 5% rare earth cerium oxide in the spraying feeding, and all the other are with embodiment 2.
In the 3rd step, the preparation of ceramic coating adopts the concrete processing parameter of oxy-acetylene flame thermospray to be: 75 ° of spray angles, spray distance 150mm moves fast 90mms
-1, oxygen pressure 0.6Mpa, acetylene is pressed 0.1Mpa.
In the ceramic coating that method for preparing obtains, shown in Fig. 5 B, except hard phase Mo is arranged
2FeB
2And iron-based bonding mutually outside, also have FeMoO
4, B
2O
3Generate Deng mutually, almost detect in the coating less than Fe, but have FeO to generate, explain that oxidation has taken place coating in the preparation process, especially the oxidation of coating top layer is comparatively serious.Microhardness of coating Hv
0.1Be 665～1142, porosity is 21.78%, and thermal shock number of times 40 times, bond area are 225mm
2Under the condition, tensile strength is 15.99MPa, and the frictional coefficient of coating is between 0.31～0.33.Fig. 6 C is 5%CeO
2The coatingsurface pattern can be seen owing to the more short texture that forms of coatingsurface hole, and has and do not melt particulate inclusion on a small quantity.Fig. 6 E is the cross section shape appearance figure of coating, by the visible 5%CeO that adds of figure
2Coating interface place defective is more, and the coating internal void is more, and the stack of the drop that melts in the spraying process and partly melt, accumulation are not as adding 3%CeO
2Coating is fine and close.
The coating condition of experimentizing that the foregoing description is prepared is respectively:
1, adopt Japanese D/MAX-RB type x-ray diffractometer of science that the thing phase composite of powder and coating is analyzed.X-ray diffractometer adopts the Cu target, and wherein sweep velocity is: 2 °/min, sweep limit: 10 ~ 80 °, step-length is 0.02 °, and voltage is 40kV, and electric current is 30mA.
2, observe the pattern of spraying feeding and the surface and the cross section of ternary boride cement coating with the SSX-550 of Hitachi type ESEM (SEM) and QUANTA 200F field launch environment sem (ESEM), and the surface topography after the wearing and tearing of coating is carried out observation analysis.
3, the heat-shock resistance test adopts the rapid heat cycle method to measure, and during test sample is heated to 400 ℃, constant temperature insulation 10min.Take out in the room temperature water of quenching rapidly then, treat to take out after the water surface calmness, after drying naturally, whether the observation coatingsurface crackle occurs or peels off, if no above-mentioned phenomenon occurs, promptly as a heat shock cycling.And then sample put into stove, circulation successively crackle occurs or peels off until coating, writes down the changing conditions of coating after anti-thermal shock cycle index and the thermal cycling each time of sample respectively.For improving the accuracy of experimental data, each component is got 3 samples, and net result is the MV of 3 coupon results in each component.
4, judge the quality of coating compactness among the present invention with the porosity size.Adopt buoyancy method to measure, its concrete test process is following: at first, coating and matrix are peeled off and weighed, obtain dry mass m
0Again the test piece after the thorough drying is hung with fine rule, immerses in the zero(ppm) water, soak into exhaust, treat that bubble has been arranged after, measure the gravity of test piece in water with weight beam, obtain quality m in the water of test piece
1Test piece is taken out from water, rapidly dry the surface and weigh, obtain the aerial quality m of saturation water test piece with wet cloth
2Coating porosity is got by following formula:
In the formula: the p-porosity; m
0The dry mass of-water test piece (g); m
1The quality (g) of-saturation water test piece in water; m
2The aerial quality of-saturation water test piece (g).
5, Bond Strength of Coating adopts rendezvous method to measure, and adopts cyanoacrylate 2 to be bonded to together on two spraying samples 1, and is fixed on the self-control jig 3, and is as shown in Figure 2, so that on tensile testing machine, assemble.Carry out stretching experiment, the load during the record fracture is measured the bonding strength that its tensile strength is coating self.
The concrete processing parameter of rendezvous method is: the butt joint area of sample is about 15mm * 15mm, and draw speed≤25mm/min, each prescription get three groups of samples and stretch, and it is averaged is Bond Strength of Coating.Anchoring strength of coating σ (N/mm
2) can calculate according to σ=F/A, wherein A is coating area (mm
2), the ultimate load when F is sample fracture (N).
6, the microhardness of coating test is on HV-1000 microhardness appearance, to carry out.Testing used pressure head is rectangular pyramid shape brale, load 100g, loading time 10s.
7, the wear resisting property of ceramic coating test: the coating and the steel matrix of preparation have been carried out abrasive wear and adhesive wear test, and its wear resistance is compared analysis.
Embodiment 6:
Embodiment as a comparison, selecting Mo powder, Fe powder and FeB powder in the present embodiment for use is raw material, adopt the transition layer that hot-spraying techniques prepares on the Q235 steel matrix surface preparation Mo
2FeB
2The ternary boride ceramic coating, the preparation method is identical with the preparation method of the ceramic coating that contains cerium oxide.The fine and close hole of coating is less, mainly by Mo
2FeB
2With the phase composite of Fe base bonding, with a spot of Fe
2O
3Thermospray ternary boride ceramic coating porosity is 19.14%, and bonding strength is 16.05MPa, and the thermal shock resistance maximum can reach 40 times, and its abrasive wear behavior improves 50% than the Q235 matrix, and anti-adhesive wear performance improves 59% than the Q235 matrix.
As shown in Figure 3, the staple of coating is Mo
2FeB
2Hard phase, Fe base bonding phase.Powder does not have cenotype through mechanically mixing, granulation process and produces hard phase Mo
2FeB
2Formation be fully in spraying and reflow process, the pyroreaction that relies on oxy-acetylene flame to produce forms.Hard phase Mo
2FeB
2Hardness be equivalent to the hardness of wimet, its existence will help the abrasion property ability.In addition, because flame temperature is higher, powder particle passes through to fly to not have in the matrix process after oxy-acetylene flame heats and adds protective atmosphere, thereby the part iron powder is oxidized, contains a spot of Fe in the coating
2O
3
Fig. 4 (A) is the hot spray coating surface topography.Can see that by figure the surface is a grey black, be coralliform typical case pattern, there is a spot of hole in coatingsurface.Fig. 4 (B) is a hot spray coating cross section pattern, and is visible by figure, combines tight between coating and matrix; The interface totally, only there is defective in individual areas, combines closelyr between ceramic coating and the Ni-Al layer, do not have obvious boundary; Coating is piled up closely, and internal void is less.Fig. 4 (C) is for being coated with the layer cross section backscatter images, and Fig. 4 (D) is the energy spectrum analysis of corresponding points.Can know that in conjunction with EDS and XRD analysis the light gray zone is Mo among the figure
2FeB
2The hard phase, visible by figure, dividing some hard phases not of uniform size in the coating.
Testing used pressure head is rectangular pyramid shape brale, load 100g, loading time 10s.Test result shows: coating has the microhardness higher than matrix, and the matrix microhardness is Hv
0.1170, and the hardness of coating is at Hv
0.1Between 763～1363.
Abrasive wear experiment to the ceramic coating for preparing among the embodiment; Can know; The wear resistance that has the ceramic coating sample is superior to the matrix of uncoated Q235 steel; And when wearing-in period is 16min, two kinds of wear resistance difference maximums that sample shows, the unit surface abrasion loss of Q235 matrix is 114.22g/m
2, the unit surface abrasion loss of coating sample is 75.72g/m
2, wear resistance is 1.5 times of matrix.And the matrix wearing and tearing are comparatively serious, and polishing scratch is darker, the groove that the surface has tangible plough wrinkle to form; And the ceramic coating zone that is worn is less, and polishing scratch is less more shallow, and along with the carrying out of wearing and tearing, the bonding phase bleed that hardness is lower, hard comes out mutually gradually, when the mill material is moved each other, can peel off, and stays pit.
Under 300N, 400N, three load-up conditions of 500N, the wear resisting property of ceramic coating all is superior to the firm matrix of Q235, and the weight loss of coating and matrix all increases along with the increase of load.When load was 500N, matrix wear weight loss amount was 0.0712g, and the wear weight loss amount of coating is 0.0449g.Wear resistance has improved 59% than matrix.This is owing to Mo in the coating
2FeB
2The existence of hard phase has improved the hardness of coating, and this has improved the resistance to abrasion of coating self on the one hand; On the other hand, Mo
2FeB
2The existence of hard phase has reduced coated material and friction pair material mutual solubility to a certain extent, thereby has weakened the generation of adherent phenomenon.Add CeO
2After coating mainly by Mo
2FeB
2, Fe base bonding phase, MOFeO
4And B
2O
3Form; Add CeO
2Ceramic coating compactness, heat-shock resistance, bonding strength and microhardness with CeO
2The Changing Pattern basically identical of content is with the increase of its content and improves the trend that afterwards reduces earlier, wherein adds 3%CeO
2Ceramic coating performance optimum, porosity is merely 7.61%, thermal shock resistance can reach 60 times, bonding strength is 19.80Mpa, microhardness is Hv
0.1879～1405.The coating resistance to abrasion is with CeO
2The increase of content becomes the trend that raises and afterwards reduce earlier.3%CeO wherein
2The content coating abrasion performance is best.Abrasive wear behavior is not add CeO
21.7 times of coating; The adhesive wear performance is not add CeO
23.34～10.44 times of coating.
Claims (9)
1. ternary boride ceramic coating, it is characterized in that: selecting Mo powder, Fe powder and FeB powder for use is raw material, adopts the surface preparation of the transition layer that hot-spraying techniques prepares on the Q235 steel matrix, coating is mainly by Mo
2FeB
2With the phase composite of Fe base bonding, with Fe
2O
3
2. ternary boride ceramic coating that contains cerium oxide; It is characterized in that: selecting Mo powder, Fe powder and FeB powder for use is raw material; Adding mass percent is 1%～5% cerium oxide, the surface preparation of the transition layer that the employing hot-spraying techniques prepares on the Q235 steel matrix, and staple is Mo in the ceramic coating
2FeB
2Hard phase, Fe base bonding phase also have FeMoO
4, B
2O
3And CeO
2
3. a kind of ternary boride ceramic coating that contains cerium oxide according to claim 2 is characterized in that: the microhardness Hv of ceramic coating
0.1Be 665～1405, porosity is 7.61～21.78%, and the thermal shock number of times is more than 40 times, and bond area is 225mm
2Under the condition, tensile strength is 15.99～19.8MPa, and the frictional coefficient of coating is between 0.31～0.52.
4. a kind of ternary boride ceramic coating that contains cerium oxide according to claim 2 is characterized in that: if add the mass percent of cerium oxide in the ceramic coating preparation is 1～4%, the microhardness Hv of ceramic coating
0.1Be 817～1405, porosity is 7.61～15.58%, and the thermal shock number of times is more than 53 times, and bond area is 225mm
2Under the condition, tensile strength is 16.9～19.8MPa, and the frictional coefficient of coating is between 0.34～0.52.
5. preparation method who contains the ternary boride ceramic coating of cerium oxide is characterized in that:
The first step, substrate pretreated:
Select the Q235 steel board for use, roughening treatment is carried out on its surface after, at matrix surface spraying Ni-Al transition layer;
Second step, the preparation of spraying feeding:
Mo powder, FeB alloy powder and Fe powder are mixed, mix, add the PVB sticker according to mass ratio ω (Fe-B): ω (Mo): ω (Fe)=32:48:20; The mass ratio of metal-powder and sticker is 5:1, in 100 ℃ of drying bakers, dries 1.5 ~ 2h, and the reunion powder after the oven dry is broken; Cross 200 mesh sieves; Be 1%～5% rare earth cerium oxide to wherein adding mass percent then, mix, obtain spraying feeding;
The 3rd step, the preparation of ceramic coating:
Pretreated matrix is carried out preheating, and spraying preparation ceramic coating carries out remelting after the spraying then, cooling; Spraying parameter is: 70～85 ° of spray angles, spray distance 130～150mm, translational speed 60～90mms
-1, oxygen pressure 0.6～0.8Mpa, acetylene is pressed 0.10～0.11Mpa.
6. a kind of preparation method who contains the ternary boride ceramic coating of cerium oxide according to claim 5; It is characterized in that: sandblasting is adopted in described matrix surface alligatoring; Processing parameter is: the sandblast abrasive particle is an emergy; Spray distance 100～150mm, 90 ° of sandblast angles, compressed air pressure 0.6～0.8MPa; Nickel alclad powdered alloy is selected in the preparation of Ni-Al transition layer for use, granularity 46.67～103.55 μ m.
7. a kind of preparation method who contains the ternary boride ceramic coating of cerium oxide according to claim 5 is characterized in that: iron particle size 4.95 μ m in the said spraying feeding, and ferro-boron powder FeB granularity 6.47 μ m, cerium oxide is an analytical pure, molybdenum powder particle diameter 300 orders.
8. a kind of preparation method who contains the ternary boride ceramic coating of cerium oxide according to claim 5 is characterized in that: described PVB adhesive preparation step is specific as follows:
(1) using graduated cylinder to measure 50ml concentration is that 98% absolute ethyl alcohol is poured in the 150ml beaker, is placed on and is heated to 60 ℃ on the time constant-temperature magnetic stirring apparatus; (2) take by weighing the PVB of 3.75g, join in the beaker and constantly stir, make absolute ethyl alcohol and PVB thorough mixing, after PVB dissolves fully, stop to heat, finally obtain colourless, transparent PVB sticker with glass stick.
9. a kind of preparation method who contains the ternary boride ceramic coating of cerium oxide according to claim 5 is characterized in that: the substrate preheating temperature is 300～400 ℃ in the 3rd step, time 5～7min; 700～800 ℃ of remelting temperatures, time 1～2min.
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| CN105215365A (en) * | 2014-06-05 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | A kind of metal-cermic coating and preparation method thereof |
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| CN105603331A (en) * | 2016-01-12 | 2016-05-25 | 江苏千博机械科技有限公司 | Mo2FeB2-based hard alloy and preparation method thereof |
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