CN109439991A - A kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method - Google Patents

A kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method Download PDF

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CN109439991A
CN109439991A CN201811452127.1A CN201811452127A CN109439991A CN 109439991 A CN109439991 A CN 109439991A CN 201811452127 A CN201811452127 A CN 201811452127A CN 109439991 A CN109439991 A CN 109439991A
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tib
whisker
high temperature
toughening
base metal
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赵先锐
刘桂香
朱征宇
陈勇
张强勇
谢荣
方航
方一航
李勤涛
张梦贤
李战江
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Jiangsu Maritime Institute
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Jiangsu Maritime Institute
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/04Alloys 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

Present invention relates particularly to a kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, including following procedure: reaction raw materials proportion is carried out;The percentage of component and each component that reaction raw materials include are as follows: Ti (C, N): 50 ~ 65%;TiB2Whisker: 15 ~ 30%;WC:2 ~ 10%;Mo2C:2 ~ 8%;TaC:2 ~ 8%;NbC:2 ~ 8%;Co:3 ~ 5%;Ni:3 ~ 5%;Material after proportion is sintered through techniques such as compound mixing, granulation drying, cold isostatic compaction, the hot pressing of segmented atmosphere, rapid cooling coolings.Ti (C, N) based composite metal ceramics comprehensive performance that the present invention prepares is good, especially high-speed cutting when with high high temperature hardness and toughness, thus TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material has longer cutter life, can be used as the cutter material of high-speed cutting (partly) finishing.

Description

A kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method
Technical field
The present invention relates to a kind of ceramic tool materials and preparation method thereof, have height more specifically to one kind A kind of TiB that fast cutting is used with hot environment2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method.
Background technique
Machining is processing method most widely used and most basic in machinery manufacturing industry, and High-speed Machining Technology is used as and cuts The developing direction for cutting processing has many advantages, such as to improve production efficiency, reduces production cost, and cutter is the pass of high-efficient cutting technology Key.Currently, being applied to high speed cutting tool field to be most widely used to be Ti (C, N) base ceramet tool bit.
Compared with traditional WC hard alloy, Ti (C, N) based ceramic metal have excellent comprehensive performance, its hardness with In the identical situation of hard alloy, density only has the half of hard alloy, can reduce cost;In the identical situation of service life Under, Ti (C, N) based ceramic metal has higher cutting speed and lower machined surface roughness.In high-speed cutting field, It may replace WC base cemented carbide cutter.
Ti (C, N) based ceramic metal has many performance advantages.With high rigidity, general reachable HRA91-93.5, some Up to HRA94-95, that is, reach nonmetallic ceramics cutter firmness level;Wearability with higher and ideal anti-crescent moon low-lying area mill Damage ability, in shear-steel material, wear rate is extremely low, and wearability ratio WC base cemented carbide is 3-4 times high, closes than coating hard Gold is 0.5-3 times high;Oxidation resistance with higher, heat resistance, and there is preferable chemical stability, Ti (C, N) fund Belong to ceramics and be not likely to produce bonding with steel, does not find bonding situation at 700 ~ 900 DEG C, that is, be not likely to produce built-up edge, finished surface Roughness value is lower.
But the main problem of Ti (C, N) base ceramet tool bit is still that high temperature hardness and toughness are insufficient, is limited Its extensive use in high-speed cutting field.To solve the problems, such as high temperature Strengthening and Toughening, researcher in Ti (C, N) by being added high temperature Adamant, such as TiB2, to pass through TiB2Height is hard, high antioxidant and chemical stability carry out hardening Ti (C, N) Base Metal pottery Porcelain.In China Patent No. ZL201710556296.9, Ti (C, N)-TiB is prepared using reactive hot press sintering technique2Base Metal High hard and high antioxidant cermet is made in ceramics.But the material morphology and tissue of reactive hot pressing preparation are difficult to control System, this generates cutter to mass and forms huge obstruction.China Patent No. 201710604367.8 adopts and is molded with a mold preparation Ti(C,N)- TiB2Based ceramic metal is prepared at high temperature also with the cutter of high rigidity and bending strength.The above patent, Although passing through addition TiB2Hard phase can greatly improve the hardness of cutter at high temperature, but high temperature toughness is still insufficient, can shadow Ring durability of the cutter in high-speed cutting.Therefore, researcher considers that whisker and fibre is wherein added in Ti (C, N) based ceramic metal Dimension, to pass through the toughened and reinforced high temperature Strengthening and Toughening purpose for reaching composite cermet material of whisker and fiber.Such as in China Patent No. ZL200710034792.4, authorized announcement date are on September 30th, 2009, invention and created name are as follows: the crystal whisker toughened carbon of SiC In the application case of titanium nitride based ceramic metal cutting tip and preparation method thereof, using SiC whisker as toughener, nitrogenize carbon Titanium-based metal ceramic cutting insert has high-intensitive, high tenacity and better wearability.In China Patent No. ZL200810048655.0, authorized announcement date are on June 2nd, 2010, a kind of invention and created name are as follows: Whisker-toughened cermet In the application case of cutter and preparation method thereof, using nickel plating SiC whisker as toughening phase, the high temperature of ceramic tool is improved Red hardness, wearability and toughness.In China Patent No. ZL201410289095.3, authorized announcement date is in August, 2016 24 days, invention and created name are as follows: in a kind of application case of TiC whisker reinforcedmetal ceramics and preparation method thereof, using TiC whisker Enhance cermet, improves the bending strength and fracture toughness of existing Ti (C, N) based ceramic metal.In above-mentioned patent application case In, whisker has been all made of as the toughening phase of Ti (C, N) based ceramic metal, improves the toughness of cermet material.But It is, during high-temperature machining, SiC whisker and the easy high-temperature oxydation of TiC whisker, so as to cause the elevated temperature strength of cutter and hardness etc. Reduced performance.Therefore, present invention combination TiB2Whisker high temperature hardness and the very excellent feature of toughness, modified Ti (C, N) base Ceramic tool material, to obtain the high-strength tenacity cutter material under high-speed cutting use.
Summary of the invention
1. technical problem to be solved:
It is an object of the invention to overcome existing whiskers high-toughenedization Ti (C, N) based ceramic metal above shortcomings, one is provided Kind TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method is produced using technical solution of the present invention Cutter material comprehensive performance it is good, high temperature hardness and toughness are excellent, can be used as high-speed cutting (partly) finishing cutting tool Material
2. technical solution:
A kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, which is characterized in that including following step It is rapid:
Step 1: reaction raw materials proportion is carried out;The percentage of component and each component that the reaction raw materials include are as follows: Ti (C, N): 50 ~ 65%;TiB2Whisker: 15 ~ 30%;WC:2 ~ 10%;Mo2C:2 ~ 8%;TaC:2 ~ 8%;NbC:2 ~ 8%;Co:3 ~ 5%;Ni:3 ~ 5%。
Step 2: being added paraffin in the isostatic cool pressing prepared in step 1 and sulfuric acid forms material, is put into pelletizer In carry out mixing granulation;Product after granulation is dried to the material to form drying.
Step 3: Vacuum Package is carried out after the material of the drying generated in step 2 is put into cutter die;It then will be true Material after sky encapsulation carries out cold isostatic compaction into cutter green compact used.
Step 4: being placed in hot pressing in atmosphere hot pressing sintering furnace for the green compact of hydro-forming last in step 3, and furnace temperature is from three Step-up temperature keeps the temperature cooling taking-up sample after 1 ~ 2h to 1600 ~ 1700 DEG C.
In above-mentioned step, by the way that reaction raw materials ingredient is carried out rational proportion and hot-pressing sintering technique, so as to The comprehensive performance for controlling Ti (C, N) based composite metal ceramic material is good, and high temperature hardness and toughness are excellent;Pass through TiB2Whisker The effects of effect, interface debonding and whisker fracture, crack deflection and Ti (C, N) and TiB are extracted in load transmitting2It is formed " core-shell structure copolymer " structure, the comprehensive obdurability and high temperature oxidation resistance for improving composite ceramet material for cutting tools.
Further, the TiB being added in step 12The diameter of whiskers of whisker is between 300 ~ 1000nm, and draw ratio is 1: Between 10 ~ 1:30.The TiB of this diameter and draw ratio range2Whisker, not only TiB2Material has high rigidity, high-melting-point, excellent Chemical stability, good wear resistance and corrosion resistance, good inoxidizability and the special performances such as thermal conductivity is good, and multiple Crystal whisker toughened mechanism can be provided in condensation material, improve the obdurability of material.
Further, reaction raw materials described in step 2 and paraffin and the ratio of sulfuric acid summation are 10:1 ~ 20:1.Pass through stone The prilling of wax and sulfuric acid can make material mixing uniform, and molding and sintering are finer and close, facilitate Ti (C, N) Base Metal The high-speed cutting of ceramic material uses.
Further, the isostatic cool pressing pressure in step 3 is 150 ~ 200MPa;The material of the knife sharpener is resin. The excessive contraction that can avoid ceramic green using isostatic cool pressing, relaxes the requirement to powder particles, manufactured cutter material without Dimensional defects.
Further, the atmosphere pressure in atmosphere hot-pressed sintering furnace described in step 4 is >=5MPa;The atmosphere hot pressed sintering Selected atmosphere is inert gas in furnace.
Further, three step-up temperatures described in step 4 are specifically includes the following steps: step 41, binder removal: 0 ~ 350 DEG C when, heating rate be 2 ~ 5 DEG C/min;Step 42 is rapidly heated: at 350 ~ 1200 DEG C, heating rate is 10 ~ 20 DEG C/min; Step 43, slowly heating: heating rate is 5 ~ 10 DEG C/min at 1200 ~ 1700 DEG C.
Further, cooling in step 4 to use rapid cooling technique;The rapid cooling technique specifically includes: when temperature be 1700 ~ Furnace cooling method is used when between 1400 DEG C;When temperature is 1400 DEG C or less, using heat emission fan in burner hearth is opened, reach fast Cold purpose.
Atmosphere hot pressing sintering technique is used in above process, can be made by atmosphere pressures and three step-up temperatures and rapid cooling Composite cermet material is in lower temperature and reaches densification in the short period, obtains the good Ti of comprehensive performance (C, N) Based composite metal ceramic material.
3. the utility model has the advantages that
(1) a kind of TiB of the invention2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, can prepare Comprehensive performance is good, elevated temperature strength and excellent Ti (C, N) the based composite metal ceramic material of toughness;Electronics is scanned to material Microscope (SEM) analysis, it can be found that resulting materials of the present invention have Ti (C, N) and TiB2Bis- " core-shell structure copolymer " structures, fine and close and knot Structure is evenly distributed.
(2) a kind of TiB of the invention2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, preparation Material hardness reaches 1950 ~ 2200HV, and fracture toughness reaches 8 ~ 10 MPam1/2, bending strength reaches 1100 ~ 1400 MPa, Therefore there is high obdurability;Simultaneously in 1000 DEG C of tests, high temperature hardness reaches 800 ~ 1100HV, can be used for high-speed and high-temperature Cutting tool materials'use.
(3) a kind of TiB of the invention2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, has work Industryization batch prepares the possibility of cutter, realizes the industrial application of cutter.
Detailed description of the invention
Fig. 1 is 1 TiB of the embodiment of the present invention2The scanning electron of whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material Microscope (SEM) photo;
Fig. 2 is 2 TiB of the embodiment of the present invention2The scanning electron microscopy of whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material Mirror (SEM) photo;
Fig. 3 is 1 TiB of reference examples of the present invention2The scanning electron microscopy of whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material Mirror (SEM) photo;
Fig. 4 is 2 TiB of reference examples of the present invention2The scanning electron microscopy of whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material Mirror (SEM) photo.
Specific embodiment
The present invention is specifically described with reference to the accompanying drawing.
A kind of embodiment 1: TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, including it is following Step:
Step 1: reaction raw materials proportion is carried out;Ti (C, N): 50g, TiB is taken respectively2Whisker: 25g, WC:5 g, Mo2C:3g, TaC:4g, NbC:4g, Co:4g, Ni:5g.
Step 2: paraffin 15g and sulfuric acid 5g is added in the powder chosen in step 1, then mixes on batch mixer equal It is even, and carry out pelletizer granulation.Powder through being granulated is dried into final powder on dryer.Above-mentioned TiB2Whisker is chosen High-intensitive TiB2Whisker, diameter of whiskers is between 300 ~ 1000nm, and draw ratio is between 1:10 ~ 1:30.
Step 3: appropriate resin grinding tool is chosen according to the shape of selected cutter, then batch turning and carries out Vacuum Package.Finally It puts into and carries out cold isostatic compaction in hydraulic oil, typed pressure 200MPa.Green compact after molding are placed in drying box standby burning.
Step 4: the green compact of last hydro-forming in step 3 are taken to calcine in atmosphere sintering furnace, atmosphere is argon gas, pressure For 5MPa.Sintering process are as follows: it is 3 DEG C/min that heating process, which is 0 ~ 350 DEG C,;350 ~ 1200 DEG C are 15 DEG C/min;1200~1600℃ For 10 DEG C/min;1600 DEG C of heat preservation 1h;It is that furnace is cold that temperature reduction technology, which is 1400 ~ 1600 DEG C, and 1400 DEG C are opened with heat emission fan in lower hearth It opens, reaches rapid cooling.
By the sample prepared after atmosphere hot pressing sintering in above process progress Mechanics Performance Testing: Vickers hardness is 2080HV;Bending strength is 1247 MPa;Fracture toughness is 8.2MPam1/2, 1000 DEG C of high temperature hardness is 987HV.By gas The sample of atmosphere hot pressed sintering preparation is observed at scanning electron microscope (SEM), as shown in Figure 1, discovery resulting materials have Ti (C, N) and TiB2Bis- " core-shell structure copolymer " structures, and whisker morphology can be clearly seen, fine and close and structure distribution is uniform.Wherein in Fig. 1 A figure from b figure be different amplification factor scanning electron microscope (SEM) photo.
A kind of embodiment 2: TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, including it is following Step:
Step 1: reaction raw materials proportion is carried out;Ti (C, N): 60g, TiB is taken respectively2Whisker: 20g, WC:3 g, Mo2C:3g, TaC:3g, NbC:3g, Co:4g, Ni:4g.
Step 2: paraffin: 17g is added in the powder chosen in step 1, sulfuric acid then: 3g is mixed equal on batch mixer It is even, and carry out pelletizer granulation.Powder through being granulated is dried into final powder on dryer.Above-mentioned TiB2Whisker is chosen High-intensitive TiB2Whisker, diameter of whiskers is between 300 ~ 1000nm, and draw ratio is between 1:10 ~ 1:30.
Step 3: appropriate resin grinding tool is chosen according to the shape of selected cutter, then batch turning and carries out Vacuum Package.Finally It puts into and carries out cold isostatic compaction in hydraulic oil, typed pressure 250MPa.Green compact after molding are placed in drying box standby burning.
Step 4: the green compact of last hydro-forming in step 3 are taken to calcine in atmosphere sintering furnace, atmosphere is argon gas, pressure For 10MPa.Sintering process are as follows: it is 2 DEG C/min that heating process, which is 0 ~ 350 DEG C,;350 ~ 1200 DEG C are 12 DEG C/min;1200~1650 DEG C be 7 DEG C/min;1650 DEG C of heat preservation 1h;It is that furnace is cold that temperature reduction technology, which is 1400 ~ 1650 DEG C, and 1400 DEG C are opened with heat emission fan in lower hearth It opens, reaches rapid cooling.
Sample will be prepared after atmosphere hot pressing sintering in the above process and carry out Mechanics Performance Testing: Vickers hardness is 2120HV;Bending strength is 1159 MPa;Fracture toughness is 7.6MPam1/2, and 1000 DEG C of high temperature hardness is 1023HV.It will The sample of atmosphere hot pressing sintering preparation is observed at scanning electron microscope (SEM), as shown in Fig. 2, discovery resulting materials have Ti (C, N) and TiB2Bis- " core-shell structure copolymer " structures, fine and close and structure distribution are uniform.
A kind of embodiment 3: TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, including it is following Step:
Step 1: reaction raw materials proportion is carried out;Ti (C, N): 55g, TiB is taken respectively2Whisker: 15g, WC:5 g, Mo2C:5g, TaC:5g, NbC:5g, Co:5g, Ni:5g.
Step 2: paraffin: 10g is added in the powder chosen in step 1, sulfuric acid then: 10g is mixed equal on batch mixer It is even, and carry out pelletizer granulation.Powder through being granulated is dried into final powder on dryer.Above-mentioned TiB2Whisker is chosen High-intensitive TiB2Whisker, diameter of whiskers is between 300 ~ 1000nm, and draw ratio is between 1:10 ~ 1:30.
Step 3: appropriate resin grinding tool is chosen according to the shape of selected cutter, then batch turning and carries out Vacuum Package.Finally It puts into and carries out cold isostatic compaction in hydraulic oil, typed pressure 150MPa.Green compact after molding are placed in drying box standby burning.
Step 4: the green compact of last hydro-forming in step 3 are taken to calcine in atmosphere sintering furnace, atmosphere is argon gas, pressure For 8MPa.Sintering process are as follows: it is 5 DEG C/min that heating process, which is 0 ~ 350 DEG C,;350 ~ 1200 DEG C are 20 DEG C/min;1200~1650℃ For 10 DEG C/min;1650 DEG C of heat preservation 1h;It is that furnace is cold that temperature reduction technology, which is 1400 ~ 1650 DEG C, and 1400 DEG C are opened with heat emission fan in lower hearth It opens, reaches rapid cooling.
Sample will be prepared after atmosphere hot pressing sintering in above-mentioned steps and carry out Mechanics Performance Testing: Vickers hardness is 2069HV;Bending strength is 1315 MPa;Fracture toughness is 8.7MPam1/2, 1000 DEG C of high temperature hardness is 969HV.
Reference examples 1:
(1) Ti (C, N): 55g, TiB is taken respectively2Whisker: 15g, WC:5 g, Mo2C:5g, TaC:5g, NbC:5g, Co:5g, Ni: 5g.Above-mentioned TiB2Whisker chooses high intensity TiB2Whisker, diameter of whiskers is between 300 ~ 1000nm, and draw ratio is in 1:10 ~ 1:30 Between.
(2) appropriate resin grinding tool is chosen according to the shape of selected cutter, then batch turning and carries out Vacuum Package.Finally put into Cold isostatic compaction, typed pressure 150MPa are carried out in hydraulic oil.Green compact after molding are placed in drying box standby burning.
(3) above-mentioned green compact are taken to calcine in atmosphere sintering furnace, atmosphere is argon gas, pressure 8MPa.Sintering process are as follows: heating It is 5 DEG C/min that technique, which is 0 ~ 350 DEG C,;350 ~ 1200 DEG C are 20 DEG C/min;1200 ~ 1650 DEG C are 10 DEG C/min;1650 DEG C of heat preservations 1h;It is that furnace is cold that temperature reduction technology, which is 1400 ~ 1650 DEG C, and 1400 DEG C are opened with heat emission fan in lower hearth, reaches rapid cooling.
(4) sample by atmosphere hot pressing sintering preparation carries out Mechanics Performance Testing: Vickers hardness 1793HV;Bending strength For 799 MPa;Fracture toughness is 6.5MPam1/2, 1000 DEG C of high temperature hardness is 678HV.By atmosphere hot pressing sintering preparation Sample is observed at scanning electron microscope (SEM), although as shown in figure 3, can also be observed that Ti (C, N) and TiB2Bis- " cores- Shell " structure, but resulting materials hole increases, and Tissue distribution is uneven, and compactness is not good enough.
It is the specific implementation reference examples of the invention patent below, but the invention patent is not limited to these reference examples.
Reference examples 2:
(1) Ti (C, N): 60g, TiB is taken respectively2Whisker: 20g, WC:3 g, Mo2C:3g, TaC:3g, NbC:3g, Co:4g, Ni: 4g.Paraffin: 10g is added in above-mentioned powder, sulfuric acid: then 10g is uniformly mixed on batch mixer, and carries out pelletizer granulation.Through The powder being granulated is dried into final powder on dryer.Above-mentioned TiB2Whisker chooses high intensity TiB2Whisker, diameter of whiskers Between 300 ~ 1000nm, draw ratio is between 1:10 ~ 1:30.
(2) the 100MPa dry-pressing on H-type hydraulic press of above-mentioned powder is taken, rear demoulding obtains sintering green compact.Take green compact in atmosphere It is calcined in sintering furnace, atmosphere is argon gas, pressure 10MPa.Sintering process are as follows: it is 2 DEG C/min that heating process, which is 0 ~ 350 DEG C,;350 ~ 1200 DEG C are 12 DEG C/min;1200 ~ 1650 DEG C are 7 DEG C/min;1650 DEG C of heat preservation 1h;It is furnace that temperature reduction technology, which is 1400 ~ 1650 DEG C, Cold, 1400 DEG C are opened with heat emission fan in lower hearth, reach rapid cooling.
(3) sample by atmosphere hot pressing sintering preparation carries out Mechanics Performance Testing: Vickers hardness 1870HV;Bending strength For 879 MPa;Fracture toughness is 6.8MPam1/2, 1000 DEG C of high temperature hardness is 745HV.By atmosphere hot pressing sintering preparation Sample is observed at scanning electron microscope (SEM), although as shown in figure 4, can also be observed that Ti (C, N) and TiB2Bis- " cores- Shell " structure, but resulting materials hole increases, and compactness is not good enough.
Above-mentioned reference examples 1 show: prilling in the present invention being removed, since powder forms poor, metal adhesive aggregation Seriously, thus Ti (CN) cermet material of excellent combination property can not be made.Above-mentioned reference examples 2 show: will be in the present invention Isostatic cool pressing is changed to simple compression moulding, since H-type hydraulic press has briquetting pressure direction, can not obtain and uniformly be pressed into Type, therefore Ti (CN) the cermet material mechanical performance deviation obtained.
Although the present invention has been described by way of example and in terms of the preferred embodiments, they be not it is for the purpose of limiting the invention, it is any ripe This those skilled in the art is practised, without departing from the spirit and scope of the invention, can make various changes or retouch from working as, therefore guarantor of the invention Shield range should be subject to what claims hereof protection scope was defined.

Claims (7)

1. a kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, which is characterized in that including following Step:
Step 1: reaction raw materials proportion is carried out;The percentage of component and each component that the reaction raw materials include are as follows: Ti (C, N): 50 ~ 65%;TiB2Whisker: 15 ~ 30%;WC:2 ~ 10%;Mo2C:2 ~ 8%;TaC:2 ~ 8%;NbC:2 ~ 8%;Co:3 ~ 5%;Ni:3 ~ 5%;
Step 2: being added paraffin and sulfuric acid and form material in the isostatic cool pressing prepared in step 1, be put into pelletizer into Row, which mixes, to be granulated;Product after granulation is dried to the material to form drying;
Step 3: Vacuum Package is carried out after the material of the drying generated in step 2 is put into cutter die;Then by vacuum seal Material after dress carries out cold isostatic compaction into cutter green compact used;
Step 4: being placed in hot pressing in atmosphere hot pressing sintering furnace for the green compact of hydro-forming last in step 3, and furnace temperature is from three stages 1600 ~ 1700 DEG C are warming up to, and keeps the temperature cooling taking-up sample after 1 ~ 2h.
2. a kind of TiB according to claim 12Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, It is characterized by: the TiB being added in step 12The diameter of whiskers of whisker is between 300 ~ 1000nm, and draw ratio is in 1:10 ~ 1:30 Between.
3. a kind of TiB according to claim 12Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, It is characterized by: reaction raw materials described in step 2 and paraffin and the ratio of sulfuric acid summation are 10:1 ~ 20:1.
4. a kind of TiB according to claim 12Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, It is characterized by: the isostatic cool pressing pressure in step 3 is 150 ~ 200MPa;The material of the knife sharpener is resin.
5. a kind of TiB according to claim 12Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, It is characterized by: the atmosphere pressure in atmosphere hot-pressed sintering furnace described in step 4 is >=5MPa;Institute in the atmosphere hot-pressed sintering furnace Selecting atmosphere is inert gas.
6. a kind of TiB according to claim 12Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, It is characterized by: three step-up temperatures described in step 4 specifically includes the following steps:
Step 41, binder removal: at 0 ~ 350 DEG C, heating rate is 2 ~ 5 DEG C/min;Step 42 is rapidly heated: 350 ~ 1200 DEG C When, heating rate is 10 ~ 20 DEG C/min;Step 43, slowly heating: heating rate is 5 ~ 10 DEG C/min at 1200 ~ 1700 DEG C.
7. a kind of TiB according to claim 12Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method, It is characterized by: cooling in step 4 use rapid cooling technique;The rapid cooling technique specifically includes: when temperature is 1700 ~ 1400 DEG C Between when use furnace cooling method;When temperature is 1400 DEG C or less, using heat emission fan in burner hearth is opened, reach the mesh of rapid cooling 's.
CN201811452127.1A 2018-11-30 2018-11-30 A kind of TiB2Whisker high temperature Strengthening and Toughening Ti (C, N) base metal-ceramic material preparation method Pending CN109439991A (en)

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Application publication date: 20190308