CN108213411A - Coating spraying and 3D printing cermet material based on TiCN-MxC-Co and preparation method thereof - Google Patents

Coating spraying and 3D printing cermet material based on TiCN-MxC-Co and preparation method thereof Download PDF

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CN108213411A
CN108213411A CN201810162461.7A CN201810162461A CN108213411A CN 108213411 A CN108213411 A CN 108213411A CN 201810162461 A CN201810162461 A CN 201810162461A CN 108213411 A CN108213411 A CN 108213411A
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powder
cermet
spheroidization
ball milling
mxc
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CN108213411B (en
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赵明建
陈可
陈一可
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Chengdu Jintai Jinggong Technology Co Ltd
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Chengdu Jintai Jinggong Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • B22F9/10—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 using centrifugal force
    • 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
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/04—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbonitrides
    • 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
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention discloses a kind of coating spraying based on TiCN MxC Co and 3D printing cermet material and preparation method thereof, cermet material is spherical powder, and component composition includes by percentage to the quality：The content that the content of TiCN MxC Co and selected from least one of Ni, Mo and Fe, TiCN are 20~94%, MxC is 1~40%, Co and the content selected from least one of Ni, Mo and Fe is 5~40%；Carbide MxC is at least one of WC, MoC, Mo2C, TaC, Cr3C2, NbC, VC and ZrC.It is produced by batch mixing drying, spheroidization powder, sintering processes.Powder spheroidization may be used the methods of roller nodularization, radio frequency plasma nodularization or mist projection granulating nodularization and carry out.Cermet material provided by the invention improves the binding force between coating and matrix as coating material, as 3D printing material, can improve the quality of 3D printing product.

Description

Coating spraying and 3D printing cermet material and its system based on TiCN-MxC-Co Preparation Method
Technical field
The invention belongs to heat spray coating layer materials and 3D printing Material Field, are beaten more particularly to a kind of coating spraying and 3D Cermet composite alloy material of print and preparation method thereof.
Background technology
Caused by the failure mode of metal works is mainly worn.Although taking heat treatment, Metamorphism treatment, doping etc. means Its wearability can be improved, but extremely limited to the raising of case hardness, limit the performance of its potentiality.And then workpiece surface Coating technology come into being, and cermet is also taken as common coating material and uses.Usually cermet material is hard Degree it is higher, the ability of surface resistance to deformation is stronger, and wearability is better, when its as coating in use, be more conducive to raising workpiece The wearability on surface；And its obdurability (intensity and toughness) is higher, impact resistance is better.Therefore, hardness and obdurability have become To evaluate the important indicator of cermet performance.And traditional metal ceramic coating material, due to its main stock size and shape The raw material powder of shape, directly uses after being simply mixed.Its advantage is that cost is relatively low, but shortcoming is since powder size is distributed Range is big, and pattern is uneven, the associativity for leading to sprayed on material and matrix is deteriorated and complicated anti-in thermal spray process Should, the uniformity of ingredient is also a big problem.The degradation that these problems will lead to coating, used so as to cause workpiece Journey coating material cracks, and the generation for phenomena such as coming off influences the use of product.
It is essentially a kind of rapid shaping technique for the 3D printing of cermet material.Some are complicated The cermet workpiece of shape is difficult to realize one using traditional PM technique and prepares molding, and used traditional powder Last metallurgical raw material, and it is relatively inaccessible to requirement of the 3D printing technique to its raw material.In 3D printing Rapid Prototyping Process, conventional powder Metallurgical raw material is extremely difficult to the high compactness and strong mechanical performance of prior powder metallurgy product.So metal as 3D printing Ceramic raw material generally requires uniform spherical powder, and the method (such as air-flow spheroidization) of existing frequently-used powder spheroidization powder Cost is higher, and commercial applications are limited by larger.
Invention content
It is an object of the invention to be directed to the present situation of the prior art and deficiency, a kind of painting based on TiCN-MxC-Co is provided Layer spraying and 3D printing cermet material and preparation method thereof, to improve the combination between the performance of coating and coating and matrix Power meets requirement of the 3D printing to cermet raw material, improves the quality of 3D printing product, reduces cost of material.
Coating spraying and 3D printing cermet material provided by the invention based on TiCN-MxC-Co are spherical powder, Component composition includes by percentage to the quality：TiCN-MxC-Co and selected from least one of Ni, Mo and Fe, the content of TiCN Content for 20~94%, MxC is 1~40%, Co and the content selected from least one of Ni, Mo and Fe is 5~40%；Carbon Compound MxC is at least one of WC, MoC, Mo2C, TaC, Cr3C2, NbC, VC and ZrC.
The preparation method of above-mentioned cermet material, comprises the following steps that：
(1) batch mixing is dried, and each raw material powder and ball milling agent of formula ratio are added to abundant ball milling in ball milling mixing equipment Mixture is mixed to get, obtained mixture is placed in drying equipment fully dries, and obtains drying mixture；
(2) the drying mixture that step (1) obtains was crushed 300~600 mesh sieve, by the powder that is sieved by spheroidization powder Material is sent into roller spheroidization equipment by powder spheroidization, and then sieving removes grain size more than 30 mesh and the spherical powder less than 120 mesh End is to get to the spherical powder of even particle size distribution；
And forming agent is added in before pelletizing；
(3) spherical powder made from step (2) is put into vacuum sintering furnace, is evacuated to 1 × 10-1Pa by sintering processes Below or be continually fed into Ar gas keep vacuum sintering furnace in air pressure be 500~1200Pa, be warming up to 350~600 DEG C heat preservation 2~ 8 hours forming agents with removal addition, then in 1 × 10-1Pa of vacuum hereinafter, be warming up to 800~1300 DEG C fire it is 0.5~4 small When, then furnace cooling is to get to the spherical powder of cermet composite alloy；
Or it comprises the following steps that：
(1) batch mixing is dried, and each raw material powder and ball milling agent of formula ratio are added to abundant ball milling in ball milling mixing equipment Mixture is mixed to get, obtained mixture is placed in drying equipment fully dries, and obtains drying mixture；
(2) green compact is molded, and the sieve of 30~80 mesh of mixture made from step (1) is sieved and is granulated, then will sieving Pellet green compact is molded；
And forming agent is added in before pelletizing；
(3) fire broken, step (2) obtained in shaping blank merging vacuum sintering furnace, be evacuated to 1 × 10-1Pa with It is 500~1200Pa to descend or be continually fed into Ar gas and keep air pressure in vacuum sintering furnace, is warming up to 350~600 DEG C of heat preservations 2~8 Hour to remove forming agent, then in 1 × 10-1Pa of vacuum hereinafter, being warming up to 800~1300 DEG C fires 0.5~4 hour, then Sintered shaping blank is broken into 30-100 microns of particulate material by furnace cooling；
(4) radio frequency plasma nodularization, the grain size that step (3) is obtained be 30-100 microns of particulate material be placed in radio frequency etc. from Lower progress nodularization is protected in argon gas in sub- spheroidization device, obtains the spherical powder of cermet composite alloy；
Or it comprises the following steps that：
(1) batch mixing is dried, and each raw material powder, ball milling agent and the forming agent of formula ratio are added in ball milling mixing equipment and filled Bulb separation mill is mixed to get mixed slurry；
(2) mist projection granulating, the slurry that step (1) is obtained are sent into centrifugal spray granulation drying machine and carry out mist projection granulating, obtain To spherical powder；
(3) sintering heat treatment, the spherical powder that step (2) obtains is placed in vacuum sintering furnace, with 3~10 DEG C/min's Heating rate is warming up to 800~1300 DEG C of 0.5~5h of sintering, then cools to room temperature with the furnace to get to the compound conjunction of cermet The spherical powder of gold.
In above-mentioned cermet composite alloy spherical powder preparation method technical solution, ball milling mixing produces mixture mistake The ball milling agent that journey adds in preferentially selects alcohol or acetone；The forming agent added in mixing process or forming process, preferentially One kind in polyethylene glycol, paraffin, buna and SD glue is selected, the addition priority acccess control of forming agent is in the total matter of raw material powder The range of amount 0.5~5%.
In the preparation method of above-mentioned cermet composite alloy spherical powder, the spheroidization that powder spheroidization uses rolls Cylinder, preferentially uses cylinder wall as jacket structured drum apparatus, and during spheroidization, it is 50~80 DEG C that temperature is passed through in chuck Circulating water flow, drum rotation speed are 15~45r/min, and the spheroidization time is 10~20min.
In the preparation method of above-mentioned cermet composite alloy spherical powder, the operation of radio frequency plasma spheroidization device is excellent It first controls and is：30~100KW of power, argon gas 15~40slpm of working flow, argon gas protection 100~200slpm of flow, system are born Press 0.1~0.5atm, powder feeding 2~8slpm of throughput, 20~60g/min of powder feed rate；The electric discharge of radio frequency plasma spheroidization device The temperature of plasma is preferably controlled not less than 3200 DEG C.
In the preparation method of above-mentioned cermet composite alloy spherical powder, the centrifugal spray granulation drying machine operation Priority acccess control is：100~350 DEG C of inlet temperature, outlet temperature set 80~250 DEG C, 10~25kr/min of rotating speed, and slurry is sent into speed Spend 5~22ml/min.
Compared with prior art, the invention has the advantages that：
1st, the cermet composite alloy spherical powder prepared using the method for the invention, spherical powder ingredient can basis It needs to adjust, simultaneously as the sintering after spheroidization belongs to solid-state diffusion sintering, component segregation is small, and high uniformity makes spraying Or the microstructure of the product after 3D printing is evenly, properties of product consistency higher.
2nd, cermet composite alloy spherical powder provided by the invention for 3D printing material, solves carbon nitrogen Compound material is the porosity height under conditions of 3D printing rapid shaping and poor mechanical property the shortcomings that.
3rd, cermet composite alloy spherical powder provided by the invention since it is solid-solution powder, can improve coating With the binding property of matrix, effectively reduce the stress between coating and matrix and improve the performance of coating.It can also adjust simultaneously The mechanical properties such as the toughness of coating
4th, cermet composite alloy spherical powder preparation method provided by the invention, it is simple for process, it is low for equipment requirements, The manufacturing cost of spherical powder substantially reduces, and is particularly suitable for industrialized production.
Description of the drawings
Fig. 1 is the spherical powder that embodiment 2 prepares gained
Specific embodiment
Cermet composite alloy spherical powder of the present invention and preparation method thereof is made into one by the following examples Walk explanation.
In following embodiment, the percentage in the chemical formula of the composite alloy containing cermet before each component represents the group Divide the mass percent in nitrogenous master alloy, that does not write percentage before component exactly represents it as surplus.
Embodiment 1
1. dispensing batch mixing is dried
Weigh 4kg Co powder and 6kg Ti (C0.7,N0.3) powder, polyethylene glycol 500g is added in, each raw material is passed through into ball mill mixing Method is uniformly mixed, and ball milling agent alcohol, then vacuum drying obtain mixture；
2. spheroidization
By step, 1. mixture obtained crushes sieving powdered, and the sieving sieve mesh number is 300 mesh；Then using rolling The method of cylinder spheroidization is sieved by powder spheroidization, and with the sieve of 30 mesh, takes the powder by sieve；Again with the sieve of 50 mesh Net sieving is taken not by the powder of sieve to get to the spherical powder of even particle size distribution；
3. slough forming agent and heat treatment
By step 2. in spherical powder obtained be put into vacuum sintering furnace, be evacuated to 1 × 10-1Pa hereinafter, being warming up to 600 DEG C of heat preservations, 2 hours forming agents with removal addition；Then 1 × 10-1Pa is down in air pressure hereinafter, be warming up to again 800 DEG C into Row is fired 4 hours；Then furnace cooling is to get to the spherical powder of cermet composite alloy；
The spheroidization process, using roller spheroidization, equipment cylinder wall is jacket structured, the flowing water being passed through in chuck, At 50 DEG C, drum rotation speed 15r/min, the spheroidization time is 10min for water temperature control.
Embodiment 2
1. dispensing batch mixing is dried
Weigh TiC0.5N0.5 powder：9.5kg；Co powder:0.4kg；Fe powder：0.1kg adds in polyethylene glycol 50g, by each raw material It is uniformly mixed by ball mill mixing method, ball milling agent is alcohol, then vacuum drying obtains mixture；
2. it is molded
It is sieved and is granulated with the sieve of 30 mesh, be then molded the pellet green compact after granulation；
3. pre-burned and broken
By step 2. in green compact obtained be put into vacuum sintering furnace, be evacuated to 1 × 10-1Pa hereinafter, being warming up to 350 8 hours forming agents with removal addition of heat preservation；Then 1 × 10-1Pa is down in air pressure hereinafter, being warming up to 800 again is fired 4 Hour；Then furnace cooling will be broken into 30 microns of particle with sintered green compact.
4. plasma discharging nodularization
By step 3. in composite cermet particle obtained be placed in ball in the radio frequency plasma spheroidization device of stable operation Change and obtain composite cermet spherical powder.Plasma discharging spheroidizing process parameter is：Power is 30KW, argon gas working flow For 15slpm, argon gas protection flow is 100slpm, and system negative pressure is 0.1atm, and powder feeding throughput is 2slpm, and powder feed rate is 20g/min.The temperature of wherein described plasma discharging nodularization plasma is
3400℃。
Embodiment 3
1. dispensing batch mixing is dried
Weigh (Ti, 20W, 15Mo, 5Ta) C0.7N0.3 powder：6kg；Co powder：2.5kg；Ni powder:1kg；Mo powder
Each raw material is uniformly mixed by 0.5kg, paraffin 200g by ball mill mixing method, and ball milling agent is acetone, then vacuum drying Obtain mixture；
2. it is molded
It is sieved and is granulated with the sieve of 80 mesh, be then molded the pellet green compact after granulation；
3. pre-burned and broken
By step 2. in green compact obtained be put into vacuum sintering furnace, be then continually fed into and keep the air pressure in vacuum drying oven to be The flowing Ar gas of 500pa is warming up to 600 DEG C of heat preservations, 2 hours forming agents with removal addition；Then 1 × 10- is down in air pressure 1Pa is fired 0.5 hour hereinafter, being warming up to 1350 DEG C again；It is micro- to be broken into 100 by then furnace cooling for sintered green compact The particle of rice.
4. plasma discharging nodularization
By step 3. in composite cermet particle obtained be placed in ball in the radio frequency plasma spheroidization device of stable operation Change and obtain composite cermet spherical powder.Plasma discharging spheroidizing process parameter is：Operation power is 100KW, and argon gas works Flow is 40slpm, and argon gas protection flow is 200slpm, and system negative pressure is 0.5atm, and powder feeding throughput is 8slpm, and powder feeding is fast It spends for 60g/min.The temperature of wherein described plasma discharging nodularization plasma is 3600 DEG C.
Embodiment 4
1. dispensing batch mixing is dried
Weigh TiC0.7N0.3 powder：2kg；WC：3kg；Mo2C：1kg；Co powder:2.7kg；Ni powder：1.3kg adds in fourth and receives rubber Each raw material is uniformly mixed by glue 100g by ball mill mixing method, and ball milling agent is acetone, then vacuum drying obtains mixture；
2. it is molded
It is sieved and is granulated with the sieve of 60 mesh, be then molded the pellet green compact after granulation；
3. pre-burned and broken
By step 2. in green compact obtained be put into vacuum sintering furnace, be then continually fed into keep vacuum drying oven in air pressure be, The flowing Ar gas of 1200Pa is warming up to 400 DEG C of heat preservations, 6 hours forming agents with removal addition；Then 1 × 10- is down in air pressure 1Pa is fired 3 hours hereinafter, being warming up to 1200 DEG C again；Then furnace cooling will be broken into 60 microns with sintered green compact Particle.
4. plasma discharging nodularization
By step 3. in composite cermet particle obtained be placed in ball in the radio frequency plasma spheroidization device of stable operation Change and obtain composite cermet spherical powder.Operation power is 60KW, and argon gas working flow is 30slpm, and argon gas protection flow is 120slpm, system negative pressure are 0.3atm, and powder feeding throughput is 6slpm, and powder feed rate is
30g/min.The temperature of wherein described plasma discharging nodularization plasma is 3900 DEG C.
Embodiment 5
1. dispensing batch mixing is dried
Weigh TiC0.7N0.3 powder：9.4kg；MoC：0.1kg；Co powder:0.5kg adds in SD glue 300g, each raw material is passed through Ball mill mixing method is uniformly mixed, and ball milling agent is acetone, then vacuum drying obtains mixture；
2. spheroidization
By step, 1. mixture obtained crushes sieving powdered, and the sieving sieve mesh number is 300 mesh；Then using rolling The method of cylinder spheroidization is sieved by powder spheroidization, and with the sieve of 30 mesh, takes the powder by sieve；Again with the sieve of 50 mesh Net sieving is taken not by the powder of sieve to get to the spherical powder of even particle size distribution；
3. slough forming agent and heat treatment
By step 2. in spherical powder obtained be put into vacuum sintering furnace, be evacuated to 1 × 10-1Pa hereinafter, being warming up to 350 DEG C of heat preservations, 8 hours forming agents with removal addition；Then 1 × 10-1Pa is down in air pressure hereinafter, be warming up to again 800 DEG C into Row is fired 4 hours；Then furnace cooling is to get to the spherical powder of cermet composite alloy；
The spheroidization process is using roller spheroidization, and cylinder wall is double-layer structure, hollow, and hollow space can Circulation water is passed through, at 50 DEG C, drum rotation speed 15r/min, the spheroidization time is 10min for water temperature control.
Embodiment 6
1. dispensing batch mixing is dried
Weigh (Ti, 5W) C0.7N0.3 powder：9.5kg；Ni powder:0.5kg adds in paraffin 400g, each raw material is passed through ball milling Batch mixing method is uniformly mixed, and ball milling agent is alcohol, then vacuum drying obtains mixture；
2. spheroidization
By step, 1. mixture obtained crushes sieving powdered, and the sieving sieve mesh number is 600 mesh；Then using rolling The method of cylinder spheroidization is sieved by powder spheroidization, and with the sieve of 100 mesh, takes the powder by sieve；Again with 120 purposes Sieve is sieved, and takes not by the powder of sieve to get to the spherical powder of even particle size distribution；
3. slough forming agent and heat treatment
By step 2. in spherical powder obtained be put into vacuum sintering furnace, be then continually fed into keep vacuum drying oven in air pressure be The flowing Ar gas of 500Pa is warming up to 600 DEG C of heat preservations, 2 hours forming agents with removal addition；Then 1 × 10- is down in air pressure 1Pa is fired 0.5 hour hereinafter, being warming up to 1300 DEG C again；Then furnace cooling is to get to the ball of cermet composite alloy Shape powder；
The spheroidization process is using roller spheroidization, and cylinder wall is double-layer structure, hollow, and hollow space can Circulation water is passed through, at 80 DEG C, drum rotation speed 45r/min, the spheroidization time is 20min for water temperature control.
Embodiment 7
1. dispensing batch mixing is dried
Weigh (Ti, 20W, 15Mo, 5Ta) C0.5N0.5 powder：4.65kg；TiCN:0.25kg；WC:2kg；MoC：
1kg；TaC:1kg；NbC:0.1kg；Mo powder:1kg；Polyethylene glycol 350g is added in, each raw material is passed through into ball mill mixing Method is uniformly mixed, and ball milling agent is alcohol, then vacuum drying obtains mixture；
2. spheroidization
By step, 1. mixture obtained crushes sieving powdered, and the sieving sieve mesh number is 600 mesh；Then using rolling The method of cylinder spheroidization is sieved by powder spheroidization, and with the sieve of 100 mesh, takes the powder by sieve；Again with 120 purposes Sieve is sieved, and takes not by the powder of sieve to get to the spherical powder of even particle size distribution；
3. slough forming agent and heat treatment
By step 2. in spherical powder obtained be put into vacuum sintering furnace, be then continually fed into keep vacuum drying oven in air pressure be The flowing Ar gas of 1200Pa is warming up to 600 DEG C of heat preservations, 2 hours forming agents with removal addition；Then 1 × 10- is down in air pressure 1Pa is fired 0.5 hour hereinafter, being warming up to 1300 DEG C again；Then furnace cooling is to get to the ball of cermet composite alloy Shape powder；
The spheroidization process is using roller spheroidization, and cylinder wall is double-layer structure, hollow, and hollow space can Circulation water is passed through, at 80 DEG C, drum rotation speed 45r/min, the spheroidization time is 20min for water temperature control.
Embodiment 8
1. dispensing batch mixing is dried
Weigh (Ti, 5Cr, 2V, 0.2Nb) C0.3N0.7 powder:2kg；WC powder:1.5kg；Cr3C2:0.5kg；VC:0.5kg；
TaC powder:1kg；NbC:0.5kg；Co powder:1.8kg；Ni powder:1.8kg；Fe powder:0.4kg adds in paraffin 200g, will Each raw material is uniformly mixed by ball mill mixing method, and taking-up obtains mixed slurry；
2. mist projection granulating
Mist projection granulating processing is carried out to 1. slurry that step obtains using high speed centrifugation Spray Grain-make Drier, so as to obtain Spherical powder；The mist was granulated technique:Inlet temperature is set as 100 DEG C, and outlet temperature is set as 80 DEG C, and atomizer rotating speed is set For 10kr/min, slurry input speed is 5ml/min；
3. it is heat-treated
By step 2. in obtained spherical powder be placed in vacuum sintering furnace and be heat-treated, heating rate is 3 DEG C/min, at heat It is 800 DEG C to manage temperature, heat treatment time 5h；Then room temperature is cooled to the furnace to get to the spherical shape of cermet composite alloy Powder.
Embodiment 9
1. dispensing batch mixing is dried
Weigh (Ti, 10W, 5Mo, 1Zr) C0.7N0.3 powder:9.4kg；ZrC:0.1kg；Co powder:0.5kg adds in SD glue Each raw material is uniformly mixed by 90g by ball mill mixing method, and taking-up obtains mixed slurry；
2. mist projection granulating
Mist projection granulating processing is carried out to 1. slurry that step obtains using high speed centrifugation Spray Grain-make Drier, so as to obtain Spherical powder；The mist was granulated technique:Inlet temperature is set as 350 DEG C, and outlet temperature is set as 250 DEG C, atomizer rotating speed 25kr/min is set as, slurry input speed is 22ml/min；
3. it is heat-treated
By step 2. in obtained spherical powder be placed in vacuum sintering furnace and be heat-treated, heating rate is 10 DEG C/min, heat Treatment temperature is 1300 DEG C, heat treatment time 0.5h；Then room temperature is cooled to the furnace to get to cermet composite alloy Spherical powder.
Embodiment 10
1. dispensing batch mixing is dried
Weigh TiC0.7N0.3 powder:0.095kg；(Ti,10W,5Ta)C0.3N0.7:0.005kg；WC:3kg；Mo2C powder: 1.5kg；TaC powder:1kg；Cr3C2 powder:1kg；VC powder:0.5kg；Fe powder:2kg；Ni powder:0.9kg；SD glue 400g are added in, it will be each Raw material is uniformly mixed by ball mill mixing method, and ball milling agent is acetone, then vacuum drying obtains mixture；
2. spheroidization
By step, 1. mixture obtained crushes sieving powdered, and the sieving sieve mesh number is 300 mesh；Then using rolling The method of cylinder spheroidization is sieved by powder spheroidization, and with the sieve of 60 mesh, takes the powder by sieve；Again with the sieve of 80 mesh Net sieving is taken not by the powder of sieve to get to the spherical powder of even particle size distribution；
3. slough forming agent and heat treatment
By step 2. in spherical powder obtained be put into vacuum sintering furnace, be evacuated to 1 × 10-1Pa hereinafter, being warming up to 450 DEG C of heat preservations, 5 hours forming agents with removal addition；Then 1 × 10-1Pa is down in air pressure hereinafter, be warming up to again 1000 DEG C into Row is fired 3 hours；Then furnace cooling is to get to the spherical powder of cermet composite alloy；
The spheroidization process is using roller spheroidization, and cylinder wall is double-layer structure, hollow, and hollow space can Circulation water is passed through, at 50 DEG C, drum rotation speed 15r/min, the spheroidization time is 10min for water temperature control.
Embodiment 11
1. dispensing batch mixing is dried
Weigh TiC0.7N0.3 powder:3kg；(Ti,10W,8Mo)C0.5N0.5:1kg；WC：3kg；Mo2C：2kg；Fe powder: 1kg；Buna 450g is added in, each raw material is uniformly mixed by ball mill mixing method, ball milling agent is acetone, then vacuum drying obtains Mixture；
2. it is molded
And be sieved and be granulated with the sieve of 60 mesh, then the pellet green compact after granulation is molded；
3. pre-burned and broken
By step 2. in green compact obtained be put into vacuum sintering furnace, be then continually fed into keep vacuum drying oven in air pressure be, The flowing Ar gas of 1200Pa is warming up to 400 DEG C of heat preservations, 6 hours forming agents with removal addition；Then 1 × 10- is down in air pressure 1Pa is fired 3 hours hereinafter, being warming up to 1200 DEG C again；Then furnace cooling will be broken into 60 microns with sintered green compact Particle.
4. plasma discharging nodularization
By step 3. in composite cermet particle obtained be placed in ball in the radio frequency plasma spheroidization device of stable operation Change and obtain composite cermet spherical powder.Operation power is 60KW, and argon gas working flow is 30slpm, and argon gas protection flow is 120slpm, system negative pressure are 0.3atm, and powder feeding throughput is 6slpm, powder feed rate 30g/min.Wherein it is described electric discharge etc. from The temperature of bulbec plasma is 3200 DEG C.
Embodiment 12
1. dispensing batch mixing is dried
Weigh (Ti, 5W) C0.7N0.3 powder:8kg；Fe powder:2kg adds in paraffin 500g, each raw material is passed through ball mill mixing Method is uniformly mixed, and ball milling agent is alcohol, then vacuum drying obtains mixture；
2. spheroidization
By step, 1. mixture obtained crushes sieving powdered, and the sieving sieve mesh number is 600 mesh；Then using rolling The method of cylinder spheroidization is sieved by powder spheroidization, and with the sieve of 90 mesh, takes the powder by sieve；Again with 100 purposes Sieve is sieved, and takes not by the powder of sieve to get to the spherical powder of even particle size distribution；
3. slough forming agent and heat treatment
By step 2. in spherical powder obtained be put into vacuum sintering furnace, be then continually fed into keep vacuum drying oven in air pressure be The flowing Ar gas of 500Pa is warming up to 600 DEG C of heat preservations, 2 hours forming agents with removal addition；Then 1 × 10- is down in air pressure 1Pa is fired 0.5 hour hereinafter, being warming up to 1300 DEG C again；Then furnace cooling is to get to the ball of cermet composite alloy Shape powder；
The spheroidization process is using roller spheroidization, and cylinder wall is double-layer structure, hollow, and hollow space can Circulation water is passed through, at 80 DEG C, drum rotation speed 35r/min, the spheroidization time is 20min for water temperature control.

Claims (8)

1. a kind of coating spraying and 3D printing cermet material based on TiCN-MxC-Co, it is characterised in that cermet material Expect for spherical powder, component composition includes by percentage to the quality：TiCN-MxC-Co and at least one in Ni, Mo and Fe Kind, the content that the content of TiCN is 20~94%, MxC is 1~40%, Co and containing selected from least one of Ni, Mo and Fe Measure is 5~40%；Carbide MxC is at least one of WC, MoC, Mo2C, TaC, Cr3C2, NbC, VC and ZrC.
2. the preparation method of cermet material described in claim 1, it is characterised in that comprise the following steps that：
(1) batch mixing is dried, and each raw material powder and ball milling agent of formula ratio are added to abundant ball milling mixing in ball milling mixing equipment Mixture is obtained, obtained mixture is placed in drying equipment fully dries, and obtains drying mixture；
(2) the drying mixture that step (1) obtains was crushed 300~600 mesh sieve, sieving powder materials was sent by spheroidization powder Enter roller spheroidization equipment by powder spheroidization, the removing grain size that is then sieved is more than 30 mesh and the spherical powder less than 120 mesh, i.e., Obtain the spherical powder of even particle size distribution；
And forming agent is added in before pelletizing；
(3) spherical powder made from step (2) is put into vacuum sintering furnace, is evacuated to 1 × below 10-1Pa by sintering processes Or it is 500~1200Pa to be continually fed into Ar gas to keep air pressure in vacuum sintering furnace, and it is small to be warming up to 350~600 DEG C of heat preservations 2~8 When to remove the forming agent of addition, then in 1 × 10-1Pa of vacuum hereinafter, be warming up to 800~1300 DEG C fire 0.5~4 hour, Then furnace cooling is to get to the spherical powder of cermet composite alloy；
Or it comprises the following steps that：
(1) batch mixing is dried, and each raw material powder and ball milling agent of formula ratio are added to abundant ball milling mixing in ball milling mixing equipment Mixture is obtained, obtained mixture is placed in drying equipment fully dries, and obtains drying mixture；
(2) green compact is molded, and is sieved and is granulated in the sieve of 30~80 mesh of mixture made from step (1), then will be sieved pellet Green compact is molded；
And forming agent is added in before pelletizing；
(3) fire broken, step (2) obtained in shaping blank merging vacuum sintering furnace, be evacuated to 1 × below 10-1Pa or It is 500~1200Pa that person, which is continually fed into Ar gas and keeps air pressure in vacuum sintering furnace, is warming up to 350~600 DEG C and keeps the temperature 2~8 hours To remove forming agent, then fired 0.5~4 hour in 1 × 10-1Pa of vacuum hereinafter, being warming up to 800~1300 DEG C, then with stove Sintered shaping blank is broken into 30-100 microns of particulate material by cooling；
(4) radio frequency plasma nodularization, the grain size that step (3) is obtained are that 30-100 microns of particulate material is placed in radio frequency plasma ball Makeup carries out nodularization in putting under argon gas is protected, and obtains the spherical powder of cermet composite alloy；
Or it comprises the following steps that：
(1) batch mixing is dried, and each raw material powder, ball milling agent and the forming agent of formula ratio are added to abundant ball in ball milling mixing equipment Mill is mixed to get mixed slurry；
(2) mist projection granulating, the slurry that step (1) is obtained are sent into centrifugal spray granulation drying machine and carry out mist projection granulating, obtain ball Shape powder；
(3) sintering heat treatment, the spherical powder that step (2) obtains is placed in vacuum sintering furnace, with the heating of 3~10 DEG C/min Rate is warming up to 800~1300 DEG C of 0.5~5h of sintering, then cools to room temperature with the furnace to get to cermet composite alloy Spherical powder.
3. the preparation method of cermet material according to claim 2, it is characterised in that ball milling mixing produces mixed slurry The ball milling agent that process adds in is alcohol or acetone.
4. the preparation method of cermet material according to claim 2, it is characterised in that the forming agent for polyethylene glycol, One kind in paraffin, buna and SD glue, the addition of forming agent are the 0.5~5% of raw material powder gross mass.
5. according to Claims 2 or 3 or the preparation method of 4 cermet materials, it is characterised in that powder spheroidization uses Spheroidization roller, cylinder wall is passed through temperature as 50~80 DEG C of circulating water flows to be jacket structured in chuck, drum rotation speed for 15~ 45r/min, spheroidization time are 10~20min.
6. according to Claims 2 or 3 or the preparation method of 4 cermet materials, it is characterised in that radio frequency plasma nodularization Device operation power is 30~100KW, and argon gas working flow is 15~40slpm, and argon gas protection flow is 100~200slpm, System negative pressure is 0.1~0.5atm, and powder feeding throughput is 2~8slpm, and powder feed rate is 20~60g/min.
7. the preparation method of cermet material according to claim 6, it is characterised in that the radio frequency plasma nodularization dress The temperature for the discharge plasma put is not less than 3200 DEG C.
8. according to Claims 2 or 3 or the preparation method of 4 cermet materials, it is characterised in that the centrifugal spray is made Grain drying machine operation inlet temperature is 100~350 DEG C, and outlet temperature is set as 80~250 DEG C, and rotating speed is 10~25kr/min, is starched It is 5~22ml/min that material, which is sent into speed,.
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