CN105296835B - A kind of nickel-base alloy makees the Mo of Binder Phase2NiB2Based ceramic metal and preparation method thereof - Google Patents
A kind of nickel-base alloy makees the Mo of Binder Phase2NiB2Based ceramic metal and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the Mo that a kind of nickel-base alloy makees Binder Phase2NiB2Based ceramic metal, is prepared by the following raw material：The dispensing that a variety of Ni elements according to the B element of 3.5 7 parts by weight, the Mo elements of 31.5 65 parts by weight and 28 65 parts by weight in MoB powder, NiB powder, Mo powder, B powder and Ni powder are carried out, and add in dispensing appropriate glucose, binding agent and decentralized medium.Also disclose the Mo2NiB2The preparation method of based ceramic metal, including a variety of be well mixed with glucose, binding agent and decentralized medium in MoB powder, NiB powder, Mo powder, B powder and Ni powder is obtained into slurry, spray drying granulation, then powder is handled in hydrogen atmosphere in 900 1100 DEG C, powder is loaded to the jacket processed again and carries out high temperature insostatic pressing (HIP), temperature is 1,100 1300 DEG C, and pressure is 100 200MPa.Prepared Mo2NiB2The oxide inclusion content of base metal-ceramic material is low, and the strength of materials, toughness are high, and blank is shunk in hot isostatic pressing uniformly, it is regular, be difficult torsional deformation.
Description
Technical field
The present invention relates to a kind of Mo using nickel-base alloy as Binder Phase2NiB2Base metal-ceramic material, and this kind of material
Preparation method, belong to cermet material technical field.
Background technology
Cutter, mould and other abrasion and corrosion resistance process equipments that industrial circle is used are frequently with traditional hard alloy
Hard phase in manufacture, hard alloy is generally tungsten carbide or tungsten carbide and titanium carbide, titanium nitride, titanium carbonitride, vanadium carbide and carbon
Change the composite of one or more of compositions in tantalum.But, the manufacture of hard alloy depends on tungsten, and tungsten is made
For strategic reserves resource in short supply, its development and application can be all in by restriction state at this stage with future, cause hard to close
The yield of gold is restricted, it is impossible to adapt to the growing device requirement of industrial circle.
In addition to hard alloy, researcher has found to make the Mo of Binder Phase with nickel-base alloy2NiB2Base metal-ceramic material equally has
There is wear-resisting, corrosion resistance feature, therefore this material is developed more and more, for substituting hard alloy.Such as China
Patent document CN102191393A discloses a kind of preparation method of molybdenum nickel boron ternary boride base hard alloy, including with Mo
Powder, Ni powder and B powder are raw material, are made successively through ball milling mixing, drying, shaping and sintering step with Mo2NiB2Ternary boride is
Hard phase, using nickel-base alloy as the hard alloy of Binder Phase.Its process costs is low, step is simple.
Above-mentioned technology can obtain Mo2NiB2Based ceramic metal, still, due to material powder, granularity becomes after ball milling
It is very tiny, it is very easy to oxidation, even if anti-oxidation measure is taken in exactissima diligentia in operation, above-mentioned technology
Mo2NiB2A large amount of oxides are still had in based ceramic metal to be mingled with, and cause cermet low intensity, poor toughness, material internal defect
It is many so that the performance reduction of cermet material.
The content of the invention
The technical problems to be solved by the invention are the Mo of prior art2NiB2It is mingled with a large amount of in base metal-ceramic material
Oxide so that material internal defect is more, the strength of materials is low, poor toughness；And then a kind of oxide of proposition is mingled with less, the strength of materials
High nickel-base alloy makees the Mo of Binder Phase2NiB2Based ceramic metal.
Another technical problem to be solved by this invention is to prepare Mo by high temperature insostatic pressing (HIP) in the prior art2NiB2Base Metal
When ceramic, cermet blank amount of contraction is big, shrinks uneven, the problem of easy torsional deformation；And then propose that a kind of blank is received
Contracting is uniform, rule, and be difficult torsional deformation prepares the Mo that nickel-base alloy makees Binder Phase by heat and other static pressuring processes2NiB2Base Metal
The method of ceramics.
In order to solve the above technical problems, the invention provides the Mo that a kind of nickel-base alloy makees Binder Phase2NiB2Base Metal is made pottery
Porcelain, is prepared by the following raw material：
A variety of B element, 31.5-65 weight according to 3.5-7 parts by weight in MoB powder, NiB powder, Mo powder, B powder and Ni powder
The dispensing that the Mo elements of part and the Ni elements of 28-65 parts by weight are carried out；
Glucose；
Binding agent；
Decentralized medium.
The glucose is 1-2 parts by weight.
The binding agent is the polymethyl methacrylate of 0.3-1 parts by weight and the polyvinyl alcohol contracting fourth of 0.2-1 parts by weight
Aldehyde；The decentralized medium is the absolute ethyl alcohol of 15-25 parts by weight.
The Mo2NiB2The preparation method of based ceramic metal, comprises the following steps,
(1) B element by a variety of in MoB powder, NiB powder, Mo powder, B powder and Ni powder according to 3.5-7 parts by weight, 31.5-65
After the Mo elements of parts by weight and the Ni element dispensings of 28-65 parts by weight, then mix with glucose, binding agent and decentralized medium
It is even, obtain slurry；
(2) by slurry spray drying granulation；
(3) obtained powder will be spray-dried in hydrogen atmosphere in 900-1100 DEG C of processing；
(4) powder that hydrogen treat is crossed is fitted into jacket and carries out hip treatment, treatment temperature is 1100-1300
DEG C, processing pressure is 100-200MPa；
(5) the blank processing in jacket is taken out.
The synthetic method of the MoB is：By Mo powder and B powder according to mol ratio (1-1.1)：Abrasive material after 1 mixing, then from climing
Prolong in synthesizer and SHS process is carried out in argon gas atmosphere, synthesis pressure is 0.1-5MPa.
The synthetic method of the NiB is：By Ni powder and B powder according to mol ratio (1-1.2)：Abrasive material after 1 mixing, then from climing
Prolong in synthesizer and SHS process is carried out in argon gas atmosphere, synthesis pressure is 0.1-5MPa.
Spray drying condition is atomisation pressure 0.6-1.5MPa, 180-220 DEG C of drying tower EAT.
In step (4), the powder size being fitted into the jacket is not more than 100 mesh.
The solid content of the slurry is 45-60vol%.
In step (4), the powder that hydrogen treat is crossed loads after the jacket, and the jacket is entered at 400-600 DEG C
Row degassing, until the vacuum in the jacket reaches 1 × 10-2After Pa, the jacket soldering and sealing is subjected to hip treatment.
The self-propagating synthesis device in the prior art carry out SHS process common equipment, it include furnace shell,
Ignitor in furnace shell cooling system and stove；In use, electrode is powered, the resistance heating on electrode is connected to, is ignited in furnace shell
Reactant carries out SHS process.
The SHS process is to carry out self-heating using the high heat produced by reactant reaction and make from conduction
With so as to proceed synthesis until reacting complete technology.
SHS process MoB and NiB powder, synthesize 10 kilograms of MoB or NiB, stove are entered to powder from powder in the present invention
Come out of the stove and take around time of 1 hour, power consumption is within 2KWh.
Slurry spray drying make the equipment that powder craft uses mainly include spray drying tower, it is supporting with spray drying tower
Air feed system, feeding system, material-receiving system and solvent recovering system, slurry enter spray drying tower in, entered by air feed system
Wind, hot blast injection slurry, makes the solvent of slurry volatilize to form powder.The atomisation pressure is the inside that spray drying tower is run
Pressure, the drying tower EAT is the EAT by air feed system.
The present invention has the advantages that compared with prior art：
(1) nickel-base alloy of the present invention makees the Mo of Binder Phase2NiB2Based ceramic metal, is prepared by the following raw material：MoB powder,
It is a variety of according to the B element of 3.5-7 parts by weight, the Mo elements of 31.5-65 parts by weight and 28- in NiB powder, Mo powder, B powder and Ni powder
The dispensing that the Ni elements of 65 parts by weight are carried out；Glucose；Binding agent；Decentralized medium.In preparation process, glucose thermal decomposition is produced
High-activity carbon effectively the metal oxide in powder can be reduced, so as to reduce gained Mo2NiB2Base Metal is made pottery
The inclusion content of metal oxide in porcelain so that the internal flaw of cermet is few, intensity is high, good toughness.
(2) nickel-base alloy of the present invention makees the Mo of Binder Phase2NiB2Based ceramic metal, the glucose is 1-2 parts by weight.Institute
It is the polymethyl methacrylate of 0.3-1 parts by weight and the polyvinyl butyral resin of 0.2-1 parts by weight to state binding agent；It is described scattered
Medium is the absolute ethyl alcohol of 15-25 parts by weight.Above-mentioned composition can further reduce the oxide content of cermet material, enter
One step improves the intensity and toughness of cermet.
(3) nickel-base alloy of the present invention makees the Mo of Binder Phase2NiB2The preparation method of based ceramic metal, including by MoB
In powder, NiB powder, Mo powder, B powder and Ni powder it is a variety of according to the B element of 3.5-7 parts by weight, the Mo elements of 31.5-65 parts by weight and
The Ni element dispensings of 28-65 parts by weight, then slurry is mixed into glucose, binding agent and decentralized medium, slurry spraying is dry
It is dry to make powder, obtained powder will be spray-dried in hydrogen atmosphere in 900-1100 DEG C of processing, then the powder that hydrogen treat is crossed
It is fitted into jacket and carries out hip treatment, treatment temperature is 1100-1300 DEG C, and processing pressure is 100-200MPa, in hydrogen
During processing and hip treatment, the high-activity carbon that glucose thermal decomposition is produced can be aoxidized effectively to the metal in powder
Thing is reduced；Moreover, by drying process with atomizing to material powder granulate, be greatly improved material powder mobility and
Tap density, its tap density can reach 45-52%, so that the contraction of blank is regular after high temperature insostatic pressing (HIP), be difficult to turn round
Song deformation.
(4) nickel-base alloy of the present invention makees the Mo of Binder Phase2NiB2The preparation method of based ceramic metal, MoB and NiB are equal
Using SHS process so that the purity of MoB powder and NiB powder is high, so as to improve Mo2NiB2Based ceramic metal
Mechanical property and corrosion resistance, the efficiency high of self-propagating synthesis, cost are low in addition, contribute to Mo2NiB2Based ceramic metal it is low into
This production.
Brief description of the drawings
Fig. 1 is the Mo that embodiment 8 is obtained2NiB2The SEM photograph of based ceramic metal；
Fig. 2 is the Mo that comparative example 1 is obtained2NiB2The SEM photograph of based ceramic metal；
Fig. 3 is the Mo for the jacket cladding that embodiment 8 is obtained2NiB2Based ceramic metal picture；
Fig. 4 is the Mo for the jacket cladding that comparative example 3 is obtained2NiB2Based ceramic metal picture.
Embodiment
Embodiment 1
(1) by 1945gMoB powder, 955gNiB powder, 1404gMo powder and 1995gNi powder dispensings, then glucose with 100g,
The absolute ethyl alcohol mixing of 30g polymethyl methacrylate, 20g polyvinyl butyral resin and 1500g, ball milling 10h is consolidated
Content 45vol% slurry；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1：Ball milling 2h after 1 mixing, then in self- propagating
Synthesized in synthesizer in argon gas atmosphere, synthesis pressure is 0.1MPa；The synthetic method of the NiB is：By Ni powder and B powder according to
Mol ratio 1：Ball milling 2h after 1 mixing, then synthesized in self-propagating synthesis device in argon gas atmosphere, synthesis pressure is
0.1MPa；
(2) slurry makes powder using pressure spray drying granulation machine, and condition is atomisation pressure 0.6MPa, and drying tower enters wind-warm syndrome
180 DEG C of degree；
(3) obtained powder will be spray-dried and handles 3h in 900 DEG C in hydrogen atmosphere；
(4) powder that hydrogen treat is crossed is fitted into stainless steel capsule and carries out hip treatment, treatment temperature is 1100
DEG C, processing pressure is 200MPa, and processing time is 3h；
(5) blank taken out in jacket carries out wire cutting, obtains Mo2NiB2Based ceramic metal 1.
Embodiment 2
(1) by 2918gMoB powder, 1909gNiB powder, 100gB powder, 3882gMo powder and 4891gNi powder dispensings, then with 200g
Glucose, 100g polymethyl methacrylate, 100g polyvinyl butyral resin and 2500g absolute ethyl alcohol mixing, shake
It is dynamic to grind the slurry that 30h obtains solid content 60vol%；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 5MPa；The synthetic method of the NiB is：By Ni powder and B powder according to
Mol ratio 1.2：Ball milling 2h after 1 mixing, then synthesized in self-propagating synthesis device in argon gas atmosphere, synthesis pressure is
5MPa；
(2) slurry makes powder using pressure spray drying granulation machine, and condition is atomisation pressure 1.5MPa, and drying tower enters wind-warm syndrome
220 DEG C of degree；
(3) obtained powder will be spray-dried and handles 1h in 1100 DEG C in hydrogen atmosphere；
(4) powder that hydrogen treat is crossed is fitted into carbon steel jacket and carries out hip treatment, treatment temperature is 1300 DEG C,
Processing pressure is 100MPa, and processing time is 1h；
(5) ground after taking out the blank wire cutting in jacket, obtain Mo2NiB2Based ceramic metal 2.
Embodiment 3
(1) by 1945gMoB powder, 1909gNiB powder, 100gB powder, 2255gMo powder and 1391gNi powder dispensings, then with 150g
Glucose, 50g polymethyl methacrylate, 50g polyvinyl butyral resin and 2000g absolute ethyl alcohol mixing, vibration
Grind the slurry that 20h obtains solid content 50vol%；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；The synthetic method of the NiB is：By Ni powder and B powder according to
Mol ratio 1.1：Ball milling 2h after 1 mixing, then synthesized in self-propagating synthesis device in argon gas atmosphere, synthesis pressure is
4MPa；
(2) slurry makes powder using pressure spray drying granulation machine, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that hydrogen treat is crossed is fitted into carbon steel jacket and carries out hip treatment, treatment temperature is 1200 DEG C,
Processing pressure is 150MPa, and processing time is 2h；
(5) ground after taking out the blank wire cutting in jacket, obtain Mo2NiB2Based ceramic metal 3.
Embodiment 4
(1) by 1945gMoB powder, 1272gNiB powder, 3255gMo powder and 2927gNi powder dispensings, then glucose with 150g,
The absolute ethyl alcohol mixing of 50g polymethyl methacrylate, 50g polyvinyl butyral resin and 2000g, vibromill grinds 20h
Obtain solid content 47vol% slurry；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；The synthetic method of the NiB is：By Ni powder and B powder according to
Mol ratio 1.1：Ball milling 2h after 1 mixing, then synthesized in self-propagating synthesis device in argon gas atmosphere, synthesis pressure is
4MPa；
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1200 DEG C, processing pressure is 150MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal 4.
Embodiment 5
(1) by 1500g Mo powder, 1335g Ni powder, 165g B powder dispensings, then glucose, 6g poly- methyl with 30g
Methyl acrylate, 9g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind 20h and obtain solid content 45vol%'s
Slurry；
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1250 DEG C, processing pressure is 200MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal 5.
Embodiment 6
(1) by the Ni powder dispensings of 1665g MoB powder and 1335g, then glucose, 15g polymethylacrylic acid with 45g
Methyl esters, 18g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind the slurry that 20h obtains solid content 50vol%；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1250 DEG C, processing pressure is 180MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal 6.
Embodiment 7
(1) by the Ni powder dispensings of 1053g MoB powder, 450g NiB powder and 1485g, then glucose with 51g, 24g
Polymethyl methacrylate, 9g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind 20h and obtain solid content
53vol% slurry；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；The synthetic method of the NiB is：By Ni powder and B powder according to
Mol ratio 1.1：Ball milling 2h after 1 mixing, then synthesized in self-propagating synthesis device in argon gas atmosphere, synthesis pressure is
4MPa；
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1200 DEG C, processing pressure is 180MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal 7.
Embodiment 8
(1) by the Ni powder dispensings of 1665g MoB powder, 75g Mo powder and 1260g, then glucose with 57g, 9g poly- first
Base methyl acrylate, 15g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind 20h and obtain solid content 48vol%
Slurry；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1260 DEG C, processing pressure is 200MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal 8.
Comparative example 1
(1) by the Ni powder dispensings of 1665g MoB powder, 75g Mo powder and 1260g, then the poly-methyl methacrylate with 9g
Ester, 15g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind the slurry that 20h obtains solid content 48vol%；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1260 DEG C, processing pressure is 200MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal A.
Comparative example 2
(1) by the Ni powder dispensings of 1665g MoB powder, 75g Mo powder and 1260g, then the poly-methyl methacrylate with 9g
Ester, 15g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind the slurry that 20h obtains solid content 48vol%；
MoB and NiB powder therein using graphite heater vacuum resistance furnace synthesize, synthesis temperature be respectively 1200 DEG C and
1050 DEG C, 5 kilograms of MoB or NiB are synthesized, entering stove from powder and synthesizing thermal cycle to coming out of the stove one about needs 20 hours, power consumption difference
About 1000KWh and 800KWh.
(2) slurry makes powder using closed type centrifugal spray dryer, and condition is atomisation pressure 1MPa, drying tower EAT
200℃；
(3) obtained powder will be spray-dried and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1260 DEG C, processing pressure is 200MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal B.
Comparative example 3
(1) by the Ni powder dispensings of 1665g MoB powder, 75g Mo powder and 1260g, then glucose with 57g, 9g poly- first
Base methyl acrylate, 15g polyvinyl butyral resin and absolute ethyl alcohol mixing, vibromill grind 20h and obtain well mixed slurry
Material；
Wherein, MoB synthetic method is：By Mo powder and B powder according to mol ratio 1.1：Ball milling 2h after 1 mixing, then from climing
Prolong in synthesizer and synthesized in argon gas atmosphere, synthesis pressure is 3MPa；
(2) slurry is dried in vacuo with vacuum drying oven, 80 DEG C of drying temperature；
(3) obtained powder will be dried in vacuo and handles 2h in 1000 DEG C in hydrogen atmosphere；
(4) powder that the hydrogen treats of no more than 100 mesh crosses is isolated to be fitted into carbon steel jacket, it is right at 400-600 DEG C
The jacket is de-gassed, until the vacuum in the jacket reaches 1 × 10-2Hip treatment, processing temperature are carried out after Pa
Spend for 1260 DEG C, processing pressure is 200MPa, processing time is 3h；
(5) ground after taking out the blank line Milling Machining in jacket, obtain Mo2NiB2Based ceramic metal C.
Test case
1. the testing example 1-8 and gained Mo of comparative example 12NiB2The oxygen content of base metal-ceramic material, and it is corresponding hard
Degree, bending strength and fracture toughness, the results are shown in Table 1.
Oxygen content is tested using ICP-AES methods；Hardness is carried out using Rockwell apparatus by GB/T230.1-2004
Test；Bending strength is tested by GB/T6569-200；Fracture toughness is tested according to GB/T23806-2009.
Table 1
As shown in Table 1, embodiment 1-8 cermet material has lower oxygen content compared to comparative example 1, so that
Embodiment 1-8 Mo2NiB2The subscale inclusion content of base metal-ceramic material is few, with the hardness higher than comparative example 1,
Bending strength and fracture toughness.
In addition, Fig. 1-2 is embodiment 8 and the gained Mo of comparative example 12NiB2The SEM photograph of base metal-ceramic material, wherein more
The stain for dissipating distribution is the oxide being mingled with, and is understood by contrast, and embodiment 8 compares the cermet of comparative example 1, its oxygen being mingled with
Compound content is substantially reduced.
2. major impurity oxygen in MoB and NiB, aluminium and iron are used using ICP-MS methods testing example 8 and comparative example 2
Content, the results are shown in Table 2.
Table 2
As shown in Table 2, embodiment 8 is using the MoB and NiB of SHS process, and its impurity content is far below comparative example 2
Impurity content in MoB and NiB prepared by heating furnace, it is known that MoB the and NiB purity of self-propagating synthesis is higher in the present invention.
3. the Mo of the jacket cladding manufactured by embodiment 8 and comparative example 32NiB2Base metal-ceramic material as shown in Figure 3-4,
Because comparative example 3 does not make powder using spray drying, powder tap density is low, and serious distortion deformation occurs after jacket high temperature insostatic pressing (HIP),
And the material powder of embodiment 8 is spray-dried makes powder, tap density is largely increased, after high temperature insostatic pressing (HIP) jacket shrink compared with
It is small, remain in that regular shape.
Although the present invention has carried out detailed elaboration by above-mentioned specific embodiment to it, this specialty is common
Technical staff should be understood that any form without departing from claims made on this basis and the change of details
Change, belong to invention which is intended to be protected.
Claims (10)
1. a kind of nickel-base alloy makees the Mo of Binder Phase2NiB2Based ceramic metal, is prepared by the following raw material：
A variety of in MoB powder, NiB powder, Mo powder, B powder and Ni powder B element according to 3.5-7 parts by weight, 31.5-65 parts by weight
The dispensing that Mo elements and the Ni elements of 28-65 parts by weight are carried out；
Glucose；
Binding agent；
Decentralized medium；
Wherein, the synthetic method of the MoB is：By Mo powder and B powder according to mol ratio (1-1.1)：Batch mixing after 1 mixing, then certainly
Spread in synthesizer and SHS process is carried out in argon gas atmosphere, synthesis pressure is 0.1-5MPa；
The synthetic method of the NiB is：By Ni powder and B powder according to mol ratio (1-1.2)：Batch mixing after 1 mixing, then closed in self- propagating
SHS process is carried out in argon gas atmosphere in growing up to be a useful person, synthesis pressure is 0.1-5MPa.
2. Mo according to claim 12NiB2Based ceramic metal, it is characterised in that the glucose is 1-2 parts by weight.
3. Mo according to claim 1 or 22NiB2Based ceramic metal, it is characterised in that the binding agent is 0.3-1 weight
The polymethyl methacrylate of part and the polyvinyl butyral resin of 0.2-1 parts by weight；The decentralized medium is 15-25 parts by weight
Absolute ethyl alcohol.
4. any Mo of claim 1-32NiB2The preparation method of based ceramic metal, comprises the following steps,
(1) by a variety of B element, 31.5-65 weight according to 3.5-7 parts by weight in MoB powder, NiB powder, Mo powder, B powder and Ni powder
Part Mo elements and 28-65 parts by weight Ni element dispensings after, then be well mixed with glucose, binding agent and decentralized medium, obtain
To slurry；
(2) by slurry spray drying granulation；
(3) obtained powder will be spray-dried in hydrogen atmosphere in 900-1100 DEG C of processing；
(4) powder that hydrogen treat is crossed is fitted into jacket and carries out hip treatment, treatment temperature is 1100-1300 DEG C, place
Reason pressure is 100-200MPa；
(5) the blank processing in jacket is taken out.
5. preparation method according to claim 4, it is characterised in that the synthetic method of the MoB is：By Mo powder and B powder
According to mol ratio (1-1.1)：Batch mixing after 1 mixing, then the progress self propagating high temperature conjunction in argon gas atmosphere in self-propagating synthesis device
Into synthesis pressure is 0.1-5MPa.
6. preparation method according to claim 4, it is characterised in that the synthetic method of the NiB is：By Ni powder and B powder
According to mol ratio (1-1.2)：Batch mixing after 1 mixing, then the progress self propagating high temperature conjunction in argon gas atmosphere in self-propagating synthesis device
Into synthesis pressure is 0.1-5MPa.
7. according to any described preparation methods of claim 4-6, it is characterised in that spray drying condition is atomisation pressure 0.6-
1.5MPa, 180-220 DEG C of drying tower EAT.
8. preparation method according to claim 4, it is characterised in that in step (4), the powder grain being fitted into the jacket
Degree is not more than 100 mesh.
9. preparation method according to claim 4, it is characterised in that the solid content of the slurry is 45-60vol%.
10. the preparation method according to claim 4,5,6,8 or 9, it is characterised in that in step (4), by hydrogen treat mistake
Powder load after the jacket, the jacket is de-gassed at 400-600 DEG C, until the vacuum in the jacket reaches
To 1 × 10-2After Pa, the jacket soldering and sealing is subjected to hip treatment.
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