CN101176920A - Method for preparing active metal titanium and boron carbide complex spherical hot spraying powder - Google Patents
Method for preparing active metal titanium and boron carbide complex spherical hot spraying powder Download PDFInfo
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- CN101176920A CN101176920A CNA2007101707664A CN200710170766A CN101176920A CN 101176920 A CN101176920 A CN 101176920A CN A2007101707664 A CNA2007101707664 A CN A2007101707664A CN 200710170766 A CN200710170766 A CN 200710170766A CN 101176920 A CN101176920 A CN 101176920A
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Abstract
The invention discloses a preparation method for compound spherical hot spray powder, comprising the active titanium and boron carbide. Firstly, in weight ratio, put Ti powder of 50% to 70% and B4C powder of 25% to 50% into a ball mill; after ethanol of 60% to 100% in weigh ratio being put, mill wetly the material powder until the particle size is 1 to 10 micron; with the ethanol taken as ball mill medium and polyvinyl alcohol as bonding agent of granulating, wetly mill the material powder to prepare a sizing agent, dry the powder with hot spray, sieve the dry powder and sinter under the argon atmosphere; then grade the sintering powder according to the requirements. The invention overcomes the difficulty of oxidation in titanium granulation due to big density difference, and has advantages of simple technological process, regulate powder shape, high degree of sphericity and fluidity, and improved productivity. The invention is applied in reactive spray, and the deposition efficiency and coating layer performance can be improved greatly.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of composite materials, specifically is the preparation method of bigger active metal titanium of a kind of density contrast and boron carbide complex spherical hot spraying powder.
Background technology
Composite coating, especially be that the metal and the ceramic composite coating of wild phase is a kind of wear-resisting, corrosion-resistant finishes with vast industry and civil applications prospect with special ceramics-boride, carbide, the manufacturing of the wear member in fields such as Aero-Space, metallurgy, mine, petrochemical industry, iron and steel, civil goods and repair in all be widely used.Traditional thermal spraying composite powder generally adopts mechanical mixing and sintering crushing method to produce.Yet, when being metal powder and ceramic powder for the reactive spray raw material, because the difference of aspects such as the density of metal powder and ceramic powder, granularity, metal powder and ceramic powder are directly sprayed after the mixing, or carry out simple sintering screening, and powder sphericity and granularity are mobile poor, and reaction can not be carried out fully in the spraying process often, coating performance is relatively poor, can not obtain needed coating.
Find through literature search prior art, at the Chinese patent publication number is in the patent documentation of CN101003092, disclose a kind of at high cobalt-tungsten carbide hot spray powder and technology of preparing thereof, metallic cobalt powder and tungsten-carbide powder are mixed according to a certain percentage, carry out granulation by the reunion method of granulating.Carry out after the granulation powder sintered, sintering temperature: 800-1400 ℃, 2～24 hours sintered heat insulating time, with the powder behind the sintering carry out fragmentation, the screening after, obtain non-sphere or class spherical powder.Carry out densification by the powder of high temperature heat source after again, finally obtain high cobalt content cobalt-tungsten carbide hot spray powder, comprise sphere, class sphere or aspherical particle sintering.Though the WC-Co hot spray powder function admirable of utilizing this method to produce, price is very expensive, and wherein because of very shortage of cobalt resource, it is very difficult to cause producing this product.The former raw material impurity content that has is higher, and the WC-Co hot spray powder performance of utilizing them to produce is also bad.Find also in the retrieval that United States Patent (USP) 5126104 discloses a kind of employing Ni-Cr-B-Si alloyed powder, Mo powder and Cr
3C
2/ NiCr alloyed powder; be mixed into stream juice slip through ball milling; adopting ammonium paramolybdate and polyvinyl alcohol is that binding agent causes granule; and under 800-950 ℃ reducing atmosphere the constant temperature sintering, its sinter places the plasma torch stove, and keeps the enough time in plasma flame stream; all powder particle in the sinter is melted substantially; become spheric granules, further make its metallization at last again, form through cooling.Can obtain comparatively ideal powder morphology, granularity though adopt this method to have, characteristics such as the hardness of its microscopic structure and powder, wearability are also better, required plasma torch stove is very expensive, equipment investment is big but exist, and nodularization output is very low, general productivity ratio is 5kg/h only, and production cost is high.Above-mentioned two kinds of methods all are at high temperature, and the expensive granulation of carrying out hot spray powder down is all inapplicable to the granulation of reactive spray powder.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, the preparation method of a kind of active metal and Ceramic Composite ball shaped thermal spray coating powder is provided, the oxidation of eliminating in the granulation process reaches because the powder feeding problem in the spraying process that density contrast brings, make it reach powder good sphericity, regular shape, can realize large-scale industrial production, enhance productivity and reduce production costs, be used to improve the deposition efficiency and the purposes such as abrasion property, corrosion resistance of hot spray powder.The present invention can realize fully compound between metal powder and the ceramic powder, and the preparation method is simple, the composite powder good fluidity, and sphericity and epigranular can satisfy the needs of subsequent reactions spraying.
The present invention is achieved by the following technical solutions, and the present invention cuts off the oxidation passage of active titanium valve by the control important technical parameter, reduces the titanium valve degree of oxidation.At first according to metal Ti powder and ceramic B
4The composition of C sphere of powder shape hot spray powder requires batching to carry out wet-milling to desired particle size, after the oven dry, add adhesive for granulating polyvinyl alcohol and deionized water again and make slip, the solid concentration of regulating slip reaches necessary requirement, be spray dried to spherical powder, then this spherical powder screening back direct sintering, last classified processing promptly got target product.
The present invention specifically may further comprise the steps:
(1) wet-milling preparation slip: at first according to the raw meal percentage by weight, with Ti powder 50%～75% and B
4C powder 25%～50% adds in the ball mill, add the absolute ethyl alcohol of raw meal gross weight 60%～100% simultaneously after, wet-milling, the granularity of raw meal reaches 1 micron～10 microns;
Described wet-milling, its time is 10 hours～20 hours, carries out the closed processes of ball grinder, cuts off the oxidation passage of titanium valve.
(2) wet-milling is good slurry is dried, and sieves then, and powder is fully disperseed;
Described oven dry, its temperature are 50 ℃-65 ℃.
Described oven dry, its time is 10 hours～20 hours.
(3) mixed powder after will sieving adds deionized water, solid phase weight content 30%～50%, the polyvinyl alcohol adhesive that under the effect of magnetic stirring apparatus, adds 0.5%～1.5% solid phase weight content, the dispersant of 0.2%～0.5% solid phase weight content, stir, polyvinyl alcohol is well dispersed in the slurry;
Described stirring, its time is 1 hour～3 hours, notes the rotating speed of control stirrer in the whipping process, slurry is not produced splash.
(4) spray drying granulation: the slurry for preparing is carried out mist projection granulating in the atmosphere spray dryer;
Described spray dryer, its inlet temperature are controlled at 200 ℃～250 ℃, and outlet temperature is controlled at 90 ℃～110 ℃, reduce oxidation in the titanium valve mist projection granulating process.
(5) screening: will cross double-deck reciprocating sieve by product requirement by the spherical mixed-powder of gained in the step (4), oversize powder and minus sieve powder all return the granulation again of step (4) operation, and the interior thing of sieve is packed in the corundum crucible;
(6) sintering: the corundum crucible of the powder of will packing into places continuous fritting furnace, behind sintering under argon gas (Ar) protection, is cooled to room temperature and comes out of the stove;
Described continuous fritting furnace is a vacuum carbon tube furnace, and the argon gas amount of charging into makes and keeps negative pressure in the stove.
Described sintering, its temperature are 650 ℃～800 ℃.
Described sintering, its time is 1 hour～3 hours.
(7) classification is handled: the granularity that above-mentioned gained sintered powder requires according to hot-spraying technique is carried out the classification processing, promptly get target product.
Described classification is handled, and is agglomerated powder to be adopted bilayer to revolve to shake sieve or the air draught sorting.
The present invention is because the employing absolute ethyl alcohol is made ball-milling medium, polyvinyl alcohol is made adhesive for granulating, after the spray-dried granulation, is sintered directly into spherical powder under argon shield, and last calibrate can get Ti and B
4The compound hot spray powder of C, it is simple to have technological process, the powder shape rule, good sphericity, productivity ratio can improve more than 5 times, and this product is used for reactive spray, and its powder deposition efficiency and coating performance will improve more than 3 times, detect by power spectrum (EDS), the oxygen mass percent that contains in the ball shaped thermal spray coating powder is lower than 2%.
Description of drawings
Fig. 1 is 300 times of stereoscan photographs of embodiment 1 product pattern;
Fig. 2 is 1000 times of stereoscan photographs of embodiment 1 product pattern.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(1) wet-milling preparation slip: at first with Ti powder 361.15g and B
4C powder 138.85g adds in the ball mill, add the absolute ethyl alcohol of 450g simultaneously after, wet-milling 12h reaches about 6 μ m the granularity of raw meal;
(2) wet-milling is good slurry sieves then 60 ℃ of oven dry 12 hours, and powder is fully disperseed;
(3) mixed powder after will sieving adds deionized water, and solid concentration 40% adds 1% solid concentration polyvinyl alcohol adhesive under the effect of magnetic stirring apparatus, and the dispersant magnetic agitation 2h of 0.3% solid concentration is well dispersed in the slurry polyvinyl alcohol;
(4) spray drying granulation: the slurry for preparing is carried out mist projection granulating in the atmosphere spray dryer, inlet temperature is controlled at 240 ℃, and outlet temperature is controlled at 110 ℃;
(5) screening: will cross 200 orders and the double-deck reciprocating sieve of 600 orders by the spherical mixed-powder of gained in (4), obtain≤75 μ m, the powder of 〉=23 μ m, on 200 mesh sieves under powder and 600 mesh sieves powder all return granulation again, thing is packed in the corundum crucible in the sieve;
(6) sintering: the corundum crucible of the powder of will packing into places continuous fritting furnace, behind argon gas (Ar) protection and 750 ℃ of following constant temperature sintering 1h, is cooled to room temperature and comes out of the stove;
(7) classification is handled: above-mentioned gained sintered powder is adopted 800 orders and the screening of 240 order double-deck screen shale shakers, and getting granularity is Ti and the B of 15～60 μ m
4The C complex spherical hot spraying powder.
The present embodiment powder is pressed GB1482-1984 and is detected: flow velocity＜20s/50g, and productivity ratio can improve more than 5 times, detects by power spectrum (EDS), and the oxygen mass percent that contains in the ball shaped thermal spray coating powder is lower than 2%.
Embodiment 2
(1) wet-milling preparation slip: at first with Ti powder 300g and B
4C powder 100g adds in the ball mill, add the absolute ethyl alcohol of 320g simultaneously after, wet-milling 10h reaches about 6 μ m the granularity of raw meal;
(2) wet-milling is good slurry sieves then 65 ℃ of oven dry 10 hours, and powder is fully disperseed;
(3) mixed powder after will sieving adds deionized water, and solid concentration 30% adds 1.5% solid concentration polyvinyl alcohol adhesive under the effect of magnetic stirring apparatus, and the dispersant magnetic agitation 3h of 0.5% solid concentration is well dispersed in the slurry polyvinyl alcohol;
(4) spray drying granulation: the slurry for preparing is carried out mist projection granulating in the atmosphere spray dryer, inlet temperature is controlled at 200 ℃, and outlet temperature is controlled at 100 ℃;
(5) screening: same with embodiment 1;
(6) sintering: the corundum crucible of the powder of will packing into places continuous fritting furnace, behind argon gas (Ar) protection and 650 ℃ of following constant temperature sintering 3h, is cooled to room temperature and comes out of the stove;
(7) classification is handled: same with embodiment 1.
The present embodiment powder is pressed GB1482-1984 and is detected: flow velocity＜22s/50g, and productivity ratio can improve more than 5 times, detects by power spectrum (EDS), and the oxygen mass percent that contains in the ball shaped thermal spray coating powder is lower than 2%.
Embodiment 3
(1) wet-milling preparation slip: at first with Ti powder 180g and B
4C powder 120g adds in the ball mill, add the absolute ethyl alcohol of 300g simultaneously after, wet-milling 20h reaches about 6 μ m the granularity of raw meal;
(2) wet-milling is good slurry sieves then 50 ℃ of oven dry 20 hours, and powder is fully disperseed;
(3) mixed powder after will sieving adds deionized water, and solid concentration 50% adds 1% solid concentration polyvinyl alcohol adhesive under the effect of magnetic stirring apparatus, and the dispersant magnetic agitation 1h of 0.4% solid concentration is well dispersed in the slurry polyvinyl alcohol;
(4) spray drying granulation: the slurry for preparing is carried out mist projection granulating in the atmosphere spray dryer, inlet temperature is controlled at 250 ℃, and outlet temperature is controlled at 90 ℃;
(5) screening: same with embodiment 1;
(6) sintering: the corundum crucible of the powder of will packing into places continuous fritting furnace, behind argon gas (Ar) protection and 800 ℃ of following constant temperature sintering 2h, is cooled to room temperature and comes out of the stove;
(7) classification is handled: same with embodiment 1.
The present embodiment powder is pressed GB1482-1984 and is detected: flow velocity＜24s/50g, productivity ratio can improve more than 5 times, this product is used for reactive spray, its powder deposition efficiency and coating performance will improve more than 3 times, detect by power spectrum (EDS), the oxygen mass percent that contains in the ball shaped thermal spray coating powder is lower than 2%.
Claims (9)
1. the preparation method of active metal titanium and boron carbide complex spherical hot spraying powder is characterized in that, may further comprise the steps:
(1) wet-milling preparation slip: at first according to the raw meal percentage by weight, with Ti powder 50%～75% and B
4C powder 25%～50% adds in the ball mill, add the absolute ethyl alcohol of raw meal gross weight 60%～100% simultaneously after, wet-milling keeps the airtight of ball grinder, cuts off the oxidation passage of titanium valve, the granularity of raw meal reaches 1 micron～10 microns;
(2) wet-milling is good slurry is dried, and sieves then, and powder is fully disperseed;
(3) mixed powder after will sieving adds deionized water, solid phase weight content 30%～50%, under the effect of magnetic stirring apparatus, add the polyvinyl alcohol adhesive of 0.5%～1.5% solid phase weight content, the dispersant of 0.2%～0.5% solid phase weight content, stir, polyvinyl alcohol is well dispersed in the slurry;
(4) spray drying granulation: the slurry for preparing is carried out mist projection granulating in the atmosphere spray dryer, strict control out temperature is at 200 ℃～250 ℃, and outlet temperature is at 90 ℃～110 ℃;
(5) screening: will cross double-deck reciprocating sieve by product requirement by the spherical mixed-powder of gained in the step (4), oversize powder and minus sieve powder all return the granulation again of step (4) operation, and the interior thing of sieve is packed in the corundum crucible;
(6) sintering: the corundum crucible of the powder of will packing into places continuous fritting furnace, behind sintering under the argon shield, is cooled to room temperature and comes out of the stove;
(7) classification is handled: the granularity that above-mentioned gained sintered powder requires according to hot-spraying technique is carried out the classification processing, promptly get target product.
2. the preparation method of active metal according to claim 1 titanium and boron carbide complex spherical hot spraying powder is characterized in that, described wet-milling, and its time is 10 hours～20 hours.
3. the preparation method of active metal according to claim 1 titanium and boron carbide complex spherical hot spraying powder is characterized in that, described oven dry, and its temperature is 50 ℃-65 ℃.
4. according to the preparation method of claim 1 or 3 described active metal titaniums and boron carbide complex spherical hot spraying powder, it is characterized in that, described oven dry, its time is 10 hours～20 hours.
5. the preparation method of active metal according to claim 1 titanium and boron carbide complex spherical hot spraying powder is characterized in that, described stirring, and its time is 1 hour～3 hours.
6. the preparation method of active metal according to claim 1 titanium and boron carbide complex spherical hot spraying powder is characterized in that, described continuous fritting furnace is a vacuum carbon tube furnace, and the argon gas amount of charging into makes and keeps negative pressure in the stove.
7. the preparation method of active metal according to claim 1 titanium and boron carbide complex spherical hot spraying powder is characterized in that, described sintering, and its temperature is 650 ℃～800 ℃.
8. according to the preparation method of claim 1 or 7 described active metal titaniums and boron carbide complex spherical hot spraying powder, it is characterized in that, described sintering, its time is 1 hour～3 hours.
9. the preparation method of active metal according to claim 1 titanium and boron carbide complex spherical hot spraying powder is characterized in that, described classification is handled, and is agglomerated powder to be adopted bilayer to revolve to shake sieve or the air draught sorting.
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| CN102503428A (en) * | 2011-10-17 | 2012-06-20 | 宁波伏尔肯机械密封件制造有限公司 | Spray drying granulation method of boron carbide powder |
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| CN108080625A (en) * | 2017-12-21 | 2018-05-29 | 洛阳名力科技开发有限公司 | A kind of preparation method at Hardmetal Dusting end |
| CN112981169A (en) * | 2021-02-05 | 2021-06-18 | 中国人民解放军陆军装甲兵学院 | Copper-based composite powder and preparation method thereof, and anti-corrosion wear-resistant composite coating and preparation method thereof |
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