CN102581292A - Preparation method of coating containing TiB2 metal ceramic composite powder for thermal spraying piston ring - Google Patents
Preparation method of coating containing TiB2 metal ceramic composite powder for thermal spraying piston ring Download PDFInfo
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- CN102581292A CN102581292A CN2012100656280A CN201210065628A CN102581292A CN 102581292 A CN102581292 A CN 102581292A CN 2012100656280 A CN2012100656280 A CN 2012100656280A CN 201210065628 A CN201210065628 A CN 201210065628A CN 102581292 A CN102581292 A CN 102581292A
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Abstract
The invention relates to a preparation method of a coating containing TiB2 metal ceramic composite powder for a thermal spraying piston ring, belonging to the field of composite power body technology. The preparation method provided by the invention comprises the following steps: firstly, adopting a ball-milling method to perform mixing and wet grinding on 25-75wt.% TiB2 powder, 25-10wt.% NiCr alloy powder and 50-15wt.% Mo metal powder to obtain mixed powder with the particle size less than 3 micrometers; then mixing the mixed powder with adhesion agent PVA (Polyvinyl Alcohol), dispersing agent and deionized water in proportion in to slurry, performing atomization and granulation of the slurry at the drying temperature rang of 150-250 DEG C and under the atomizing disc frequency range of 140-190Hz through a spray drying device; and finally performing densification treatment on the powder through heat treatment technology and plasma balling technology. For the composite powder prepared by the preparation method of the invention, the particle size is uniformly distributed, the spherical degree, the densification degree and the mobility are good, the deposition efficiency of TiB2 can be improved, and the metal ceramic coating with good wear-resisting property can be prepared.
Description
Technical field
The present invention relates to a kind of TiB that contains that is used for the thermal spraying piston ring coating
2The preparation method at metal-ceramic composite powder end belongs to the composite granule technical field.
Background technology
Cermet composite coating is the composite coating that a kind of metallic matrix of ceramic phase and the high tenacity by high rigidity, high-wearing feature is formed; This coating is widely used in automobile (like piston ring); Aero-Space (like the aircraft undercarriage), metallurgical (like the sinking roller) and papermaking (like the corrugation roller) wait in the manufacturing and reparation of the industrial or civilian member that surface abrasion resistance and obdurability are had higher requirements.Conventional cermet composite coating material such as WC-Co, Cr
3C
2Reasons such as-NiCr etc. are owing to cost an arm and a leg, and density is big are dull gradually in the application prospect of industries such as automobile and Aero-Space in recent years.
TiB
2Have high rigidity, high chemical stability, low-friction coefficient, many characteristics such as low-density, itself and metal composite and the cermet composite coating through the thermal spraying preparation are the WC-Co that continues, Cr
3C
2The utmost point is hopeful in wear-resisting field after the systems such as-NiCr, especially the cermet composite coating material system of high-temperature wearable field (like the piston ring surface) application.
Research shows, NiCr alloy and TiB
2Wetability is best, and the NiCr alloy has well anti-oxygen etch resistant properties, is and TiB
2The best metal phase of coupling, and the Mo metal can further improve and contains TiB
2The fracture toughness of cermet composite coating and antifraying property.Different proportionings contain TiB
2The requirement of the multiple friction and wear behavior of thermal spraying piston ring face coat can be satisfied in the metal-ceramic composite powder end.
Nowadays be used for preparation and contain TiB
2The composite powder of cermet composite coating all is to adopt mechanical alloying method or synthetic (SHS) method preparation of self propagating high temperature, and powder shape is irregular, and is mobile poor, is difficult to reach the hot-spraying technique requirement.Literature search through to prior art is found; At the Chinese patent publication number is in the document of CN101280129A; Disclose a kind of Titanium that is directed against, the preparation method of cobalt and boron carbide-mixed thermal spraying powder adopts spray drying process that mixed-powder is carried out mist projection granulating; Carry out powder heat treatment after the granulation, final sizing obtains spherical or subglobose Conglobation type composite powder.Though adopt the powder of this method preparation to have good mobility, can satisfy the thermal spraying needs, this agglomerate type powder hole is more, and is closely knit inadequately, and the metal-ceramic composite powder end less for density (as contains TiB
2Metal-ceramic composite powder end), powder " unstable " easily in spraying process, the coating density that obtains is not high.
The inventive method preparation contain TiB
2It is irregular that the compound Conglobation type hot spray powder of cermet can overcome domestic and international this type of powder shape, the shortcoming of mobile difference, and can further improve powder densification degree and apparent density, thus prepare the TiB that contains of excellent wear-resisting property
2Cermet composite coating.
Summary of the invention
The present invention seeks to existing pure TiB
2The dusty material particle size is little, and density is little, and fragility is big, is difficult to directly be used for the present situation that thermal spraying prepares coating, and a kind of TiB is provided
2The Conglobation type hot spray powder preparation method compound with multiple metal or alloy realizes multiple metal or alloy and TiB
2Compound, and make the composite powder good sphericity through the method for heat treatment post plasma nodularization, density is high, good fluidity, apparent density is high, even particle size distribution can be applicable to thermal spraying and can improve TiB
2Deposition and coating abrasion performance.
A kind of TiB that contains that is used for the thermal spraying piston ring coating of the present invention
2The preparation method at metal-ceramic composite powder end specifically may further comprise the steps:
(1) at first according to the requirement of thermal spraying composite powder composition, with TiB
2Powder, NiCr powder and Mo powder add in the ball grinder, wherein TiB
2Powder 25～75wt.%, NiCr alloy powder 25～10wt.%, Mo powder 50～15wt.% add absolute ethyl alcohol simultaneously and carry out mixing and ball milling, suppress TiB
2The ball milling oxidation, and make metal phase and TiB
2Compound evenly the mixed powder granularity is less than 3 microns, and the powder oven dry that wet-milling is good is continued to employ after the dispersion of sieving;
(2) mixed-powder after above-mentioned the sieving and polyvinyl alcohol (PVA), dispersant and deionized water are mixed and made into slip by a certain percentage; Wherein the mixed-powder quality is 35～55% of a slip gross mass, and the PVA quality is 1%～5% of a mixed powder quality, and the dispersant quality is 0.3～1.5% of a mixed powder quality; The concrete steps of slurrying comprise: at first mixed-powder is dropped into fully to stir in the deionized water and be heated to and add dispersant after 75 ℃～85 ℃; Continue to stir and to add the solvent PVA aqueous solution after 10～15 minutes, and continue to stir each composition is uniformly dispersed, if there is bubble to produce; Drip the n-butanol antifoaming agent, obtain containing TiB
2Metal-ceramic composite powder end slip;
(3) utilize spray drying device that above-mentioned slip is carried out spray-drying process, the drying equipment inlet temperature is 150～250 ℃, and the atomizing disk frequency is 140～190Hz, obtains spray-dried powders;
(4) utilize Ar gas heat-treatment furnace that spray-dried powders is heat-treated, heat treatment temperature is 400～700 ℃, and temperature retention time is 0.5-1.5 hour; Powder after the heat treatment is sprayed in the deionized water through plasma spheroidization equipment; Plasma spheroidization power is 10KW～20KW; With the oven dry of the powder in the deionized water and the hierarchical processing of sieving, finally obtain particle diameter and be distributed in the compound reunion powder in 65 microns～85 micrometer ranges at last.
The consumption of the preferred absolute ethyl alcohol of above-mentioned steps (1) is 100%～120% of a powder gross mass, 10～15 hours ball milling time.
The preferred TiB of above-mentioned steps (1)
2The powder degree is 1～3 micron, and NiCr powder degree is 20～30 microns, and Mo powder degree is 1～2 micron.
For the better dispersion of powder, according to powder properties, dispersant is one or more in ammonium citrate, polyethylene glycol or ammonium polyacrylate preferably in the above-mentioned steps (2).
In the process of above-mentioned steps (2) slurrying, preferably add after the dispersant, accomplish up to the preparation of composite powder slip, temperature remains on 75 ℃～85 ℃ always.
Above-mentioned steps (2) is better peptizaiton for dispersant plays, and slip is not flocculated, and adds that the adjustment pH value is 8～11 behind the solvent PVA aqueous solution.
The preferred 500-600 of heat treatment temperature in the above-mentioned steps (4) ℃; Plasma spheroidization power is 12KW～16KW.
The main feature of the inventive method is:
When carrying out follow-up densification; Utilize the Ar atmosphere heat treatment to remove organic matters such as PVA, dispersant earlier, utilize plasma spheroidization to make powder densification fast again, and through regulation and control plasma spheroidization parameter; When making the powder quick densifying, reduce TiB under the high-temperature condition
2(reaction between Mo) guarantees the TiB in the powder for Ni, Cr with motlten metal
2Content.Handle through heat treatment of Ar gas and plasma spheroidization under the proper parameter, both can reduce TiB in the powder
2With metal Ni, Cr, the dephasign that the Mo reaction generates (comprises Ni
3B, Cr
2B, Mo
2B) content, can prepare again handle than ordinary sinter finer and close, sphericity, mobile better, apparent density is higher contains TiB
2Metal-ceramic composite powder end, when satisfying thermal spraying powder feeding demand, solve because " unstable " phenomenon of the little generation of powder density improves powder deposition efficiency, preparation have excellent wear can coating.
Description of drawings
Fig. 1 is 500 times of magnified sweep electromicroscopic photographs of embodiment 1 product pattern;
Fig. 2 is 1000 times of magnified sweep electromicroscopic photographs of single powder in embodiment 1 product.
The specific embodiment
Following examples have further been explained the present invention, but the present invention is not limited to following examples.
Embodiment 1
Get the TiB of 1～3 micron granularity
2Powder 128.1g; The Mo powder 46.3g of the NiCr powder 25.6g of 20～30 micron granularities and 1～2 micron granularity adds in the ball grinder, adds the 250g absolute ethyl alcohol again and carries out mixing and ball milling 15 hours, 60 ℃ of oven dry of the powder that wet-milling is good; Sieve to join less than 3 microns mixed-powder after disperseing and fully stir in the 300g deionized water and heat with electric furnace; Add 0.4g ammonium citrate and 0.7g polyethylene glycol after being heated to 80 ℃, keeping under 80 ℃ of temperature then, it is the aqueous solution of 3.2g that lasting again stirring added solvent PVA content after 10 minutes; Keeping under 80 ℃ of temperature at last, the adjustment pH value is that 9.5 also lasting stirrings after 60 minutes obtain containing TiB
2Metal-ceramic composite powder end slip.If have bubble to produce, drip the n-butanol antifoaming agent.After slip prepares, utilize spray drying device that slip is carried out spray-drying process, the drying equipment inlet temperature is 170 ℃, and the atomizing disk frequency is 165Hz, obtains spray-dried powders.Utilize Ar gas heat-treatment furnace that spray-dried powders is carried out Low Temperature Heat Treatment then, heat treatment temperature is 550 ℃, and temperature retention time is 1 hour.Powder after the heat treatment is sprayed in the deionized water through plasma spheroidization equipment, and plasma spheroidization power is 12KW.With the oven dry of the powder in the deionized water and the hierarchical processing of sieving, finally obtain particle diameter and be distributed in the compound reunion powder in 65 microns～85 micrometer ranges at last.
Under SEM, observe its pattern, the shape approximation of the powder of as can be seen from Figure 1 reuniting is spherical, and particle size distribution is between 45～75 microns; Can see that from Fig. 2 the powder surface metal melts better mutually; The powder densification degree is improved, thereby improve the apparent density and the flowability of powder, utilize standard funnel method (GB 1479-84) to measure the apparent density and the flowability of Conglobation type composite powder; Each sample in measurement is averaged for three times, and measurement result is seen table 1.
Embodiment 2
Get the TiB of 1～3 micron granularity
2Powder 108.1g; The Mo powder 56.3g of the NiCr powder 35.6g of 20～30 micron granularities and 1～2 micron granularity adds in the ball grinder; Add the 250g absolute ethyl alcohol again and carried out mixing and ball milling 13 hours; 60 ℃ of oven dry of the powder that wet-milling is good will join less than 3 microns mixed-powder after the dispersion of sieving and fully stir in the 250g deionized water and with the electric furnace heating, be heated to 80 ℃ and add 0.2g ammonium citrate, 0.3g ammonium polyacrylate and 1g polyethylene glycol afterwards; Keeping under 75 ℃ of temperature then; It is the aqueous solution of 2.6g that lasting again stirring added solvent PVA content after 10 minutes, is keeping under 75 ℃ of temperature at last, and the adjustment pH value is that 10.3 also lasting stirrings after 60 minutes obtain containing TiB
2Metal-ceramic composite powder end slip.If have bubble to produce, drip the n-butanol antifoaming agent.After slip prepares, utilize spray drying device that slip is carried out spray-drying process, the drying equipment inlet temperature is 160 ℃, and the atomizing disk frequency is 155Hz, obtains spray-dried powders.Utilize Ar atmosphere heat treatment stove that spray-dried powders is carried out Low Temperature Heat Treatment then, heat treatment temperature is 500 ℃, and temperature retention time is 1.2 hours.Powder after the heat treatment is sprayed in the deionized water through plasma spheroidization equipment, and plasma spheroidization power is 14KW.With the oven dry of the powder in the deionized water and the hierarchical processing of sieving, finally obtain particle diameter and be distributed in the compound reunion powder in 65 microns～85 micrometer ranges at last.
Utilize standard funnel method (GB 1479-84) to measure the apparent density and the flowability of Conglobation type composite powder, each sample in measurement is averaged for three times, and measurement result is seen table 1.
Embodiment 3
Get the TiB of 1～3 micron granularity
2Powder 88.1g; The Mo powder 66.3g of the NiCr powder 45.6g of 20～30 micron granularities and 1～2 micron granularity adds in the ball grinder, adds the 250g absolute ethyl alcohol again and carries out mixing and ball milling 11 hours, 60 ℃ of oven dry of the powder that wet-milling is good; Sieve to join less than 3 microns mixed-powder after disperseing and fully stir in the 200g deionized water and heat with electric furnace; Add 0.4g ammonium polyacrylate and 0.8g polyethylene glycol after being heated to 80 ℃, keeping under 85 ℃ of temperature then, it is the aqueous solution of 2.2g that lasting again stirring added solvent PVA content after 10 minutes; Keeping under 85 ℃ of temperature at last, the adjustment pH value is that 8.6 also lasting stirrings after 60 minutes obtain containing TiB
2Metal-ceramic composite powder end slip.If have bubble to produce, drip the n-butanol antifoaming agent.After slip prepares, utilize spray drying device that slip is carried out spray-drying process, the drying equipment inlet temperature is 150 ℃, and the atomizing disk frequency is 145Hz, obtains spray-dried powders.Utilize Ar atmosphere heat treatment stove that spray-dried powders is carried out Low Temperature Heat Treatment then, heat treatment temperature is 600 ℃, and temperature retention time is 0.8 hour.Powder after the heat treatment is sprayed in the deionized water through plasma spheroidization equipment, and plasma spheroidization power is 16KW.With the oven dry of the powder in the deionized water and the hierarchical processing of sieving, finally obtain particle diameter and be distributed in the compound agglomerate type powder in 65 microns～85 micrometer ranges at last.
Utilize standard funnel method (GB 1479-84) to measure the apparent density and the flowability of Conglobation type composite powder, each sample in measurement is averaged for three times, and measurement result is seen table 1.
Table 1 embodiment 1-3 prepares contains TiB
2The compound agglomerate type powder physical parameter of cermet
Claims (8)
1. a kind of TiB that contains that is used for the thermal spraying piston ring coating of the present invention
2The preparation method at metal-ceramic composite powder end specifically may further comprise the steps:
(1) at first according to the requirement of thermal spraying composite powder composition, with TiB
2Powder, NiCr powder and Mo powder add in the ball grinder, wherein TiB
2Powder 25～75wt.%, NiCr alloy powder 25～10wt.%, Mo powder 50～15wt.% add absolute ethyl alcohol simultaneously and carry out mixing and ball milling, suppress TiB
2The ball milling oxidation, and make metal phase and TiB
2Compound evenly the mixed powder granularity is less than 3 microns, and the powder oven dry that wet-milling is good is continued to employ after the dispersion of sieving;
(2) mixed-powder after above-mentioned the sieving and polyvinyl alcohol (PVA), dispersant and deionized water are mixed and made into slip by a certain percentage; Wherein the mixed-powder quality is 35～55% of a slip gross mass, and the PVA quality is 1%～5% of a mixed powder quality, and the dispersant quality is 0.3～1.5% of a mixed powder quality; The concrete steps of slurrying comprise: at first mixed-powder is dropped into fully to stir in the deionized water and be heated to and add dispersant after 75 ℃～85 ℃; Continue to stir and to add the solvent PVA aqueous solution after 10～15 minutes, lasting stirring makes that each composition is uniformly dispersed in the slip, if there is bubble to produce; Drip the n-butanol antifoaming agent, obtain containing TiB
2Metal-ceramic composite powder end slip;
(3) utilize spray drying device that above-mentioned slip is carried out spray-drying process, the drying equipment inlet temperature is 150～250 ℃, and the atomizing disk frequency is 140～190Hz, obtains spray-dried powders;
(4) utilize Ar gas heat-treatment furnace that spray-dried powders is heat-treated, heat treatment temperature is 400～700 ℃, and temperature retention time is 0.5-1.5 hour; Powder after the heat treatment is sprayed in the deionized water through plasma spheroidization equipment; Plasma spheroidization power is 10KW～20KW; With the oven dry of the powder in the deionized water and the hierarchical processing of sieving, finally obtain particle diameter and be distributed in the compound reunion powder in 65 microns～85 micrometer ranges at last.
2. according to the method for claim 1, it is characterized in that the consumption of the preferred absolute ethyl alcohol of step (1) is 100%～120% of a powder gross mass, 10～15 hours ball milling time.
3. according to the method for claim 1, it is characterized in that the preferred TiB of step (1)
2The powder degree is 1～3 micron, and NiCr powder degree is 20～30 microns, and Mo powder degree is 1～2 micron.
4. according to the method for claim 1, it is characterized in that, in the process of above-mentioned steps (2) slurrying, preferably add after the dispersant that accomplish up to the preparation of composite powder slip, temperature remains on 75 ℃～85 ℃ always.
5. according to the method for claim 1, it is characterized in that above-mentioned steps (2) dispersant is selected from one or more in ammonium citrate, polyethylene glycol or the ammonium polyacrylate.
6. according to the method for claim 1, it is characterized in that above-mentioned steps (2) adds that the adjustment pH value is 8～11 behind the solvent PVA aqueous solution.
7. according to the method for claim 1, it is characterized in that middle the preferred 500-600 of heat treatment temperature ℃ of step (4).
8. according to the method for claim 1, it is characterized in that step (4) ionic medium nodularization power is 12KW～16KW.
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| CN106498332A (en) * | 2016-11-18 | 2017-03-15 | 无锡明盛纺织机械有限公司 | A kind of preparation method of large granular spherical powder used for hot spraying |
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Application publication date: 20120718 |