CN106498208A - Ni in Binder Phase3The generated in-situ cermet material preparation methoies of Al - Google Patents

Abstract

The invention discloses Ni in a kind of Binder Phase₃The preparation method of the generated in-situ cermet materials of Al, is characterized in that first preparing Ni (OH)₂The compoiste adhering phase of cladding AlN, and Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5‑x) (C, N) granule (wherein x=0～0.5) composite ganoine phase, compressing after the operations such as ball milling, filtration, drying after the two mixing, finally carry out two sections of atmosphere sinterings, i.e. Ar/H at low temperature₂Ni (OH) in atmosphere₂Ni is changed into, vacuum-sintering Ni and AlN reacts to form Ni at high temperature₃Al, is finally made Ni in Binder Phase₃The generated in-situ cermet materials of Al.Instant invention overcomes Al is oxidizable in existing technology, crush and dispersed difficult, volatile loss and the problem of sintering migration easily formation hole, Ni is formed in sintering process situ₃Al phases, and realization being uniformly distributed around hard phase, the cermet material for preparing can be used for cutting tool and manufactured with antioxidative parts.

Description

Ni in Binder Phase3The generated in-situ cermet material preparation methoies of Al

Technical field

The present invention relates to a kind of preparation method of cermet material, more particularly to Ni in Binder Phase₃Al is generated in-situ The preparation method of cermet material, belongs to field of compound material.

Background technology

Ti (C, N) based ceramic metal is due to high red hardness and stability at elevated temperature, excellent fatigue resistance And non-oxidizability, relatively low thermal coefficient of expansion and be widely used in cutting tool manufacture.With manufacturing development, cutting speed Degree more and more higher, cutting temperature also more and more higher, this high-temperature behavior to cutting tool are put forward higher requirement.Ceramic metal With metals such as Co, Ni as Binder Phase, under cutting temperature, metallic binding phase is susceptible to softening causes hardness and intensity to decline, Cutter life reduces.The high-temperature behavior for improving Binder Phase is to improve the key of ceramic metal cutting ability.Ni₃Al intermetallics The advantages of thing has stability height, elevated temperature strength and strong high-temperature oxidation resistance, the application prospect ten in high-temperature structural material Point wide, there are many use Ni at present₃Al makees the report of ceramic metal Binder Phase.ZL201410082829.0 has invented one kind and has contained Ni₃Ti (C, the N) based ceramic metal of Al, the percentage by weight of its composition is：TiC34.2～43%, TiN8～15%, Mo10～ 15%th, WC5～10%, graphite 0.8～1.0%, Ni20～24%, the Ni containing B₃Al6～10%.The invention first with purity >= 99.0% Ni, Al and B powder is raw material, Ni87.23～88.48% by weight percentage, Al11.47～12.68%, B0.5～ 1.0% makes compound, carries out wet ball-milling to compound, obtains the uniform compound slip of composition, and compound slip is dried Afterwards, the Ni containing B that vacuum heat obtains porosity and looseness is carried out₃Al sinters block；By the Ni containing B₃Al sintering blocks are crushed, and are obtained The Ni of B must be contained₃Al powder.Then TiC, TiN, Mo, WC, graphite, Ni powder and the Ni containing B are adopted₃Al powder is preparation of raw material gold The ceramic compound of category, then be prepared into through die forming, vacuum degreasing and vacuum-sintering step with Ni₃Al and Ni is binding agent Ti (C, N) based ceramic metal.In CN201510459684.6 be then by mass percentage Ni 87.23%～87.93%, Al12.07%～12.67%, B 0.5%～1.0%, Ni, Al and B powder are mixed, compound are carried out after ball milling, add wine Shedding is ground in soaking wet, obtains the uniform compound slip of composition；Compound slip is vacuum dried, sieve, and obtains the Ni containing B₃Al Powder；Again through ball mill mixing step, die forming step and vacuum-sintering step, make and adopt Ni₃TiC bases of the Al for binding agent Ceramic metal.

It can be seen that, introduce Ni at present₃The method of Al is the mixing and ball milling based on Ni, Al metal dust and (or) sintering crushing shape Into Ni₃Al powder is added.This kind of method has problems with：Oxidizable in Al powder mechanical milling processes, there is plasticity and become in Al powder The broken in the form of sheets difficulties in dispersion of shape, prefabricated Ni₃Also need after Al through shattering process complex process, broken Ni₃Change between Al metals Compound Task-size Controlling and the dispersed control of subsequent ball milling are difficult.

Content of the invention

The present invention is directed to and prepares Ni in Binder Phase at present₃The generated in-situ cermet materials of Al are high using Ni, Al powder With Ni after energy ball milling and (or) sintering crushing₃Oxidizable, Al powder in the Al mechanical milling processes that the method that Al powder types are added is present The broken in the form of sheets difficulties in dispersion of generation plastic deformation, the Ni of generation₃Al dispersed difficulties etc. in follow-up mechanical milling process Problem, proposes using first preparing Ni (OH)₂The compoiste adhering phase of cladding AlN, and Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x)(C, N) the composite ganoine phase of granule (wherein x=0～0.5), is pressed into after the two mixing after the operations such as ball milling, filtration, drying Type, finally carries out two sections of atmosphere sinterings, i.e. Ar/H at low temperature₂Ni (OH) in atmosphere₂Ni is changed into, at high temperature vacuum-sintering Ni and AlN reacts to form Ni₃Al, is finally made Ni in Binder Phase₃The generated in-situ cermet materials of Al.

Ni in the Binder Phase of the present invention₃The preparation method of the generated in-situ cermet materials of Al, it is characterised in that successively Comprise the steps of：

(1)Ni(OH)₂The compoiste adhering of cladding AlN is mutually prepared：First by C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane. are added to deionization In water, percentage composition C by weight₁₈H₂₉NaO₃S accounts for 14%～29%, and n-octyl alcohol accounts for 5%～13%, and isobutyltrimethylmethane. accounts for 6%～14%, Remaining is deionized water, stirs 3～10h with magnetic stirring apparatuss at 60～90 DEG C, then places 10～24h, and preparation forms micro- Emulsion；With the microemulsion prepared as solvent, the AlN powder that granularity is 30～80nm is added, the molar concentration of AlN is 0.1～ 1.5mol/L, 0.5～2h of supersound process forms AlN powder suspensions；NiSO is added as solvent with the microemulsion for preparing again₄, NiSO₄ Molar concentration be 0.1～1mol/L, add ammonia adjust solution ph to 8～9, stirred at 60～90 DEG C with magnetic stirring apparatuss 3～12h is mixed, 10～24h is then placed and is formed Ni (OH)₂Colloidal sol, for coating AlN and (Ti_0.5,Mo_x,W_0.5-x) (C, N) (its Middle x=0～0.5)；Finally by Ni (OH)₂Colloidal sol is added drop-wise in middle AlN powder suspension, AlN and Ni (OH)₂The mol ratio of colloidal sol is 1:5～1:3,3～12h is stirred with magnetic stirring apparatuss at 60～90 DEG C, obtain Ni (OH)₂The compoiste adhering phase of cladding AlN；

(2)Ni(OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) composite ganoine of (C, N) mutually prepared：It it is 0.9～1.5 μm by granularity (Ti_0.5,Mo_x,W_0.5-x) (C, N) add ethanol in, (Ti_0.5,Mo_x,W_0.5-x) mass ratio of (C, N) and ethanol is 1:4～1:3, Add the Tween 80 0.5～2h of supersound process of 0.5～1wt% after 48～72h of ball milling again, make (Ti_0.5,Mo_x,W_0.5-x)(C, N) slip；Then by Ni (OH)₂Colloidal sol is added drop-wise to (Ti_0.5,Mo_x,W_0.5-x) in (C, N) slip, (Ti_0.5,Mo_x,W_0.5-x)(C,N) With Ni (OH)₂The mol ratio of colloidal sol is 5:1～10:1,3～12h is stirred with magnetic stirring apparatuss at 60～90 DEG C, obtain Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) (C, N) composite ganoine phase；

(3) ceramic metal mixed-powder is prepared and is prepared with ceramic metal green compact：By Ni (OH)₂Cladding AlN compoiste adhering phase with Ni(OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) composite ganoine of (C, N) mixes, and by the Ni (OH) in compoiste adhering phase₂With multiple Close (the Ti in hard phase_0.5,Mo_x,W_0.5-x) (C, N) mol ratio be 1:2～1:4 are mixed, then 12～36h of ball milling, warp In 100～150 DEG C of 1～3h of drying after 400 mesh sieve net filtrations, ceramic metal mixed-powder sieves through 100 mesh, by ceramic metal 5～10wt% of mixed-powder weight mixes buna forming agent, pushes in 200～400MPa pressure after 80 mesh sieve The type of making obtains ceramic metal green compact；

(4) two benches atmosphere sintering forms Ni in Binder Phase₃The generated in-situ ceramic metals of Al：Ceramic metal green compact are first with Ar/ H₂2～4h is sintered for sintering atmosphere at 550～650 DEG C, make the Ni (OH) in clad₂It is converted into Ni；Then 1400～1600 DEG C 1～3h of vacuum-sintering makes Ni and AlN react and obtain Ni in Binder Phase₃The generated in-situ ceramic metals of Al.

Ni in the Binder Phase of the present invention₃The preparation method of the generated in-situ cermet materials of Al, its further feature It is：

(1)C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane., NiSO₄, Tween 80, that ethanol and ammonia are analysis is pure；

(2) Ni (OH) is prepared₂The compoiste adhering phase of cladding AlN and Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) (C, N) compound During hard phase, the speed of magnetic agitation is 20～60r/min；

(3) it is hard using the WC-6wt%Co of Φ 6mm during ball milling during ceramic metal mixed-powder is prepared and prepared with ceramic metal green compact Matter alloying pellet, the weight of sintered carbide ball is (Ti_0.5,Mo_x,W_0.5-x) 3～5 times of (C, N) powder；

(4) two benches atmosphere sintering forms Ni in Binder Phase₃Programming rate during the generated in-situ ceramic metals of Al is 5～15 DEG C/min, the cooling rate after reaction terminates is 5～15 DEG C/min, Ar/H used₂Middle H₂Content is 5vol%, and pressure is 0.5MPa, during vacuum-sintering, vacuum is 0.5～5Pa.

It is an advantage of the current invention that：(1) Ni (OH) is formed to coat mode₂The Binder Phase precursor of cladding AlN, and burning Ni is formed in situ during knot₃Al phases, and realization being uniformly distributed around hard phase, therefore avoid mixing high-energy ball milling method Exist as in mechanical milling process Al oxidizable, it is difficult to there is plastic deformation Task-size Controlling and ball milling decentralised control in Al powder Problem.(2) Ni sources are respectively coated by Al sources and (Ti_0.5,Mo_x,W_0.5-x) (C, N), therefore, prevent Al sources from (Ti_0.5,Mo_x, W_0.5-x) (C, N) sintering exposed earlier and react, Al sources primarily form Ni₃Al, so that avoid hard phase (Ti_0.5, Mo_x,W_0.5-x) (C, N) decompose and the generation of intermetallic compound such as TiAl and destroy hard phase and deteriorate ceramic metal performance. (3) Al sources are coated on inside with AlN forms, and do not adopt simple metal Al；The volatilization loss of Al and migration form the phenomenons such as hole Can be controlled.

Description of the drawings

Fig. 1 the inventive method prepares Ni in Binder Phase₃The generated in-situ ceramic-metallic process schematic representations of Al

Specific embodiment

Example 1：Using analytically pure C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane., NiSO₄, Tween 80, ethanol and ammonia chemistry Reagent；(1) Ni (OH) is first carried out₂The compoiste adhering of cladding AlN granules is mutually prepared：First by C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane. It is added in deionized water, by weight percentage composition C₁₈H₂₉NaO₃S accounts for 21%, and n-octyl alcohol accounts for 10%, and isobutyltrimethylmethane. accounts for 9%, remaining For deionized water, 7h is stirred at 60 DEG C with magnetic stirring apparatuss, the speed of magnetic agitation is 40r/min, then places 16h, matches somebody with somebody System forms microemulsion；Microemulsion with preparation adds granularity for the AlN powder of 70nm as solvent, and the molar concentration of AlN is 1.4mol/L, supersound process 1.5h form AlN powder suspensions；NiSO is added as solvent with the microemulsion for preparing again₄, NiSO₄Rub Your concentration is 0.2mol/L, adds ammonia to adjust solution ph to 9, stirs 8h, magnetic agitation with magnetic stirring apparatuss at 60 DEG C Speed be 50r/min, then place 18h formed Ni (OH)₂Colloidal sol, for coating AlN and (Ti_0.5,Mo_x,W_0.5-x)(C,N) (wherein x=0)；Finally by Ni (OH)₂Colloidal sol is added drop-wise in middle AlN powder suspension, AlN and Ni (OH)₂The mol ratio of colloidal sol is 1: 5,8h is stirred at 68 DEG C with magnetic stirring apparatuss, the speed of magnetic agitation is 60r/min, obtains Ni (OH)₂Cladding AlN's is compound Binder Phase；(2) and then Ni (OH) is carried out₂Cladding (Ti_0.5,W_0.5) composite ganoine of (C, N) mutually prepared：It it is 1.0 μm by granularity (Ti_0.5,W_0.5) (C, N) add ethanol in, (Ti_0.5,W_0.5) mass ratio of (C, N) and ethanol is 1:4, add after ball milling 56h again The Tween 80 of 0.6wt% supersound process 0.5h, make (Ti_0.5,W_0.5) (C, N) slip；Then by Ni (OH)₂Colloidal sol is added drop-wise to (Ti_0.5,W_0.5) in (C, N) slip, (Ti_0.5,W_0.5) (C, N) and Ni (OH)₂The mol ratio of colloidal sol is 6:1, use magnetic stirring apparatuss 4h is stirred at 60 DEG C, and the speed of magnetic agitation is 60r/min, obtains Ni (OH)₂Cladding (Ti_0.5,W_0.5) (C, N) compound hard Matter phase；(3) carry out ceramic metal mixed-powder again to prepare and the preparation of ceramic metal green compact：By Ni (OH)₂Cladding AlN's is compound viscous Knot and Ni (OH)₂Cladding (Ti_0.5,W_0.5) composite ganoine of (C, N) mixes, and by the Ni (OH) in compoiste adhering phase₂With multiple Close (the Ti in hard phase_0.5,W_0.5) (C, N) mol ratio be 1:2 are mixed, then ball milling 26h, adopt Φ 6mm during ball milling WC-6wt%Co sintered carbide balls, the weight of sintered carbide ball is (Ti_0.5,W_0.5) 3 times of (C, N) powder, through 400 eye mesh screens 1h is dried at 100 DEG C after filtration, ceramic metal mixed-powder sieves through 100 mesh, by ceramic metal mixed-powder weight 9wt% mixes buna forming agent, compressing under 300MPa pressure after 80 mesh sieve obtains ceramic metal green compact； (4) finally carry out two benches atmosphere sintering and form Ni in Binder Phase₃The generated in-situ ceramic metals of Al：Ceramic metal green compact first with Ar/H₂2h is sintered for sintering atmosphere at 570 DEG C, make the Ni (OH) in clad₂It is converted into Ni；Then in 1490 DEG C of vacuum-sinterings 2h makes Ni and AlN react and generate Ni₃Al；In sintering process, programming rate is 6 DEG C/min, reacts the cooling speed after terminating Spend for 10 DEG C/min, Ar/H used₂Middle H₂Content is 5vol%, and pressure is 0.5MPa, and during vacuum-sintering, vacuum is 0.5Pa, Ni in final acquisition Binder Phase₃The generated in-situ ceramic metals of Al.

Example 2：Using analytically pure C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane., NiSO₄, Tween 80, ethanol and ammonia chemistry Reagent；(1) Ni (OH) is first carried out₂The compoiste adhering of cladding AlN granules is mutually prepared：First by C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane. It is added in deionized water, by weight percentage composition C₁₈H₂₉NaO₃S accounts for 28%, and n-octyl alcohol accounts for 13%, and isobutyltrimethylmethane. accounts for 7%, remaining For deionized water, 9h is stirred at 60 DEG C with magnetic stirring apparatuss, the speed of magnetic agitation is 30r/min, then places 10h, matches somebody with somebody System forms microemulsion；Microemulsion with preparation adds granularity for the AlN powder of 35nm as solvent, and the molar concentration of AlN is 0.25mol/L, supersound process 1h form AlN powder suspensions；NiSO is added as solvent with the microemulsion for preparing again₄, NiSO₄Rub Your concentration is 0.7mol/L, adds ammonia to adjust solution ph to 9, stirs 4h, magnetic agitation with magnetic stirring apparatuss at 90 DEG C Speed be 45r/min, then place 20h formed Ni (OH)₂Colloidal sol, for coating AlN and (Ti_0.5,Mo_x,W_0.5-x)(C,N) (wherein x=0.3)；Finally by Ni (OH)₂Colloidal sol is added drop-wise in middle AlN powder suspension, AlN and Ni (OH)₂The mol ratio of colloidal sol is 1:4,3h is stirred at 60 DEG C with magnetic stirring apparatuss, the speed of magnetic agitation is 20r/min, obtains Ni (OH)₂Cladding AlN is answered Close Binder Phase；(2) and then Ni (OH) is carried out₂Cladding (Ti_0.5,Mo_0.3,W_0.2) composite ganoine of (C, N) mutually prepared：By granularity it is 1.5 μm of (Ti_0.5,Mo_0.3,W_0.2) (C, N) add ethanol in, (Ti_0.5,Mo_0.3,W_0.2) mass ratio of (C, N) and ethanol is 1: 3, add Tween 80 supersound process 2h of 0.9wt% after ball milling 48h again, make (Ti_0.5,Mo_0.3,W_0.2) (C, N) slip；So Afterwards by Ni (OH)₂Colloidal sol is added drop-wise to (Ti_0.5,Mo_0.3,W_0.2) in (C, N) slip, (Ti_0.5,Mo_0.3,W_0.2) (C, N) and Ni (OH)₂ The mol ratio of colloidal sol is 5:1,12h is stirred at 80 DEG C with magnetic stirring apparatuss, the speed of magnetic agitation is 20r/min, obtains Ni (OH)₂Cladding (Ti_0.5,Mo_0.3,W_0.2) (C, N) composite ganoine phase；(3) preparation of ceramic metal mixed-powder and metal are carried out again Prepared by ceramic green：By Ni (OH)₂The compoiste adhering phase of cladding AlN and Ni (OH)₂Cladding (Ti_0.5,Mo_0.3,W_0.2) (C, N) answer Close hard to mix, and by the Ni (OH) in compoiste adhering phase₂With (the Ti in composite ganoine phase_0.5,Mo_0.3,W_0.2) (C, N) Mol ratio is 1:4 are mixed, then ball milling 26h, adopt the WC-6wt%Co sintered carbide balls of Φ 6mm, hard to close during ball milling The weight of gold goal is (Ti_0.5,Mo_0.3,W_0.2) 5 times of (C, N) powder, 3h, metal is dried at 100 DEG C after 400 mesh sieve net filtrations Ceramic mixed-powder sieves through 100 mesh, mixes buna forming agent, warp by the 5wt% of ceramic metal mixed-powder weight Cross and compressing under 400MPa pressure after 80 mesh sieve obtain ceramic metal green compact；(4) two benches atmosphere sintering is finally carried out Form Ni in Binder Phase₃The generated in-situ ceramic metals of Al：Ceramic metal green compact are first with Ar/H₂Sinter at 640 DEG C for sintering atmosphere 4h, makes the Ni (OH) in clad₂It is converted into Ni；Then make Ni react with AlN in 1580 DEG C of vacuum-sintering 1h and generate Ni₃Al；In sintering process, programming rate is 12 DEG C/min, and the cooling rate after reaction terminates is 9 DEG C/min, Ar/H used₂In H₂Content is 5vol%, and pressure is 0.5MPa, and during vacuum-sintering, vacuum is 2.5Pa, Ni in final acquisition Binder Phase₃Al is in situ The ceramic metal of generation.

Claims (2)

1. Ni in a kind of Binder Phase₃The preparation method of the generated in-situ cermet materials of Al, it is characterised in that successively comprising following Step：

(1)Ni(OH)₂The compoiste adhering of cladding AlN is mutually prepared：First by C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane. are added to deionization In water, percentage composition C by weight₁₈H₂₉NaO₃S accounts for 14%～29%, and n-octyl alcohol accounts for 5%～13%, and isobutyltrimethylmethane. accounts for 6%～14%, Remaining is deionized water, stirs 3～10h with magnetic stirring apparatuss at 60～90 DEG C, then places 10～24h, and preparation forms micro- Emulsion；With the microemulsion prepared as solvent, the AlN powder that granularity is 30～80nm is added, the molar concentration of AlN is 0.1～ 1.5mol/L, 0.5～2h of supersound process form AlN powder suspensions；NiSO is added as solvent with the microemulsion for preparing again₄, NiSO₄ Molar concentration be 0.1～1mol/L, add ammonia adjust solution ph to 8～9, stirred at 60～90 DEG C with magnetic stirring apparatuss 3～12h is mixed, 10～24h is then placed and is formed Ni (OH)₂Colloidal sol, for coating AlN and (Ti_0.5,Mo_x,W_0.5-x) (C, N) (its Middle x=0～0.5)；Finally by Ni (OH)₂Colloidal sol is added drop-wise in middle AlN powder suspension, AlN and Ni (OH)₂The mol ratio of colloidal sol is 1:5～1:3,3～12h is stirred with magnetic stirring apparatuss at 60～90 DEG C, obtain Ni (OH)₂The compoiste adhering phase of cladding AlN；

(2)Ni(OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) composite ganoine of (C, N) mutually prepared：It it is 0.9～1.5 μm by granularity (Ti_0.5,Mo_x,W_0.5-x) (C, N) add ethanol in, (Ti_0.5,Mo_x,W_0.5-x) mass ratio of (C, N) and ethanol is 1:4～1:3, Add the Tween 80 0.5～2h of supersound process of 0.5～1wt% after 48～72h of ball milling again, make (Ti_0.5,Mo_x,W_0.5-x)(C, N) slip；Then by Ni (OH)₂Colloidal sol is added drop-wise to (Ti_0.5,Mo_x,W_0.5-x) in (C, N) slip, (Ti_0.5,Mo_x,W_0.5-x)(C,N) With Ni (OH)₂The mol ratio of colloidal sol is 5:1～10:1,3～12h is stirred with magnetic stirring apparatuss at 60～90 DEG C, obtain Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) (C, N) composite ganoine phase；

(3) ceramic metal mixed-powder is prepared and is prepared with ceramic metal green compact：By Ni (OH)₂The compoiste adhering phase of cladding AlN and Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) composite ganoine of (C, N) mixes, and by the Ni (OH) in compoiste adhering phase₂With compound (Ti in hard phase_0.5,Mo_x,W_0.5-x) (C, N) mol ratio be 1:2～1:4 are mixed, then 12～36h of ball milling, warp In 100～150 DEG C of 1～3h of drying after 400 mesh sieve net filtrations, ceramic metal mixed-powder sieves through 100 mesh, by ceramic metal 5～10wt% of mixed-powder weight mixes buna forming agent, pushes in 200～400MPa pressure after 80 mesh sieve The type of making obtains ceramic metal green compact；

(4) two benches atmosphere sintering forms Ni in Binder Phase₃The generated in-situ ceramic metals of Al：Ceramic metal green compact are first with Ar/H₂ 2～4h is sintered for sintering atmosphere at 550～650 DEG C, make the Ni (OH) in clad₂It is converted into Ni；Then 1400～1600 DEG C 1～3h of vacuum-sintering makes Ni and AlN react and obtain Ni in Binder Phase₃The generated in-situ ceramic metals of Al.

2. Ni in Binder Phase according to claim 1₃The preparation method of the generated in-situ cermet materials of Al, which enters one Step is characterised by：

(1)C₁₈H₂₉NaO₃S, n-octyl alcohol, isobutyltrimethylmethane., NiSO₄, Tween 80, that ethanol and ammonia are analysis is pure；

(2) Ni (OH) is prepared₂The compoiste adhering phase of cladding AlN and Ni (OH)₂Cladding (Ti_0.5,Mo_x,W_0.5-x) (C, N) compound hard During matter phase, the speed of magnetic agitation is 20～60r/min；

(3) it is hard using the WC-6wt%Co of Φ 6mm during ball milling during ceramic metal mixed-powder is prepared and prepared with ceramic metal green compact Matter alloying pellet, the weight of sintered carbide ball is (Ti_0.5,Mo_x,W_0.5-x) 3～5 times of (C, N) powder；

(4) two benches atmosphere sintering forms Ni in Binder Phase₃Programming rate during the generated in-situ ceramic metals of Al is 5～15 DEG C/ Min, the cooling rate after reaction terminates is 5～15 DEG C/min, Ar/H used₂Middle H₂Content is 5vol%, and pressure is 0.5MPa, during vacuum-sintering, vacuum is 0.5～5Pa.