CN104593626B - Ni-Fe base high temperature coheres the preparation method of phase cemented carbide - Google Patents
Ni-Fe base high temperature coheres the preparation method of phase cemented carbide Download PDFInfo
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- CN104593626B CN104593626B CN201510007162.2A CN201510007162A CN104593626B CN 104593626 B CN104593626 B CN 104593626B CN 201510007162 A CN201510007162 A CN 201510007162A CN 104593626 B CN104593626 B CN 104593626B
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Abstract
The invention discloses a kind of Ni Fe base high temperature and cohere the preparation method of phase cemented carbide, first nikel powder, iron powder, chromium powder, molybdenum powder and aluminium powder are pressed predetermined mass ratio mixing high-energy ball milling；Again high-energy ball milling gained powder and tungsten carbide powder, carbonized titanium powder, carbonization vanadium powder are carried out general milling, it is thus achieved that mixed-powder；Prepared mixed-powder is loaded mould, is pressed into green compact with cold press；To green material sinter molding under protective atmosphere, the final Ni Fe base high temperature that obtains coheres phase cemented carbide material.Present invention Ni Fe base mechanical alloying powder substitutes Co powder as adhesive, the hard alloy Vickers hardness >=1530/kg mm of preparation‑2, bending strength >=4880MPa, 1000 DEG C of hot strength >=4562MPa.
Description
Technical field
The present invention relates to the preparation method of a kind of Hardmetal materials.
Background technology
Hard alloy is as base with refractory metal hard compounds (WC, TiC etc.), with metal as adhesive,
The high temperature wear resistant material prepared by the PM technique of chip energy-conservation, green, few or chipless near-net-shape
Material.Excellent comprehensive performance and the high machining efficiency of hard alloy make it be widely used in high-strength steel, high-quality
The high speed cutting tools such as casting alloy, powder forming and Metal Forming mould, percussion tool etc..Should
Current social industrial energy saving, green, efficient development trend, to the combination property of hard alloy tool and mould and
Life-span proposes requirements at the higher level, particularly the high-end industrial application such as Aero-Space, microelectronics, micro Process,
Urgent demand produces disc cutter, high-speed cutting blade, miniature tool and mould etc. and has excellent High-temperature-resandant andant wear-resistant
Hardmetal materials
Co unit procatarxis has excellent comprehensive performance, good with hard carbide wettability and be used as hard alloy
The crucial adhesive of material.But there is the shortcomings such as hot mastication, high-temperature oxydation, decarburization due to it, shorten
In the service life of hard alloy, limit its application under higher temperature (＞ 800 DEG C).Therefore, anxious
A kind of novel binder materials with excellent high performance is needed to substitute Co metal.
Summary of the invention
The present invention be directed to Co cohere phase cemented carbide and apply the research and development field of restriction existing at relatively high temperatures
Shape, it is provided that a kind of Ni-Fe original washing powder using high-energy ball milling as high temperature adhesive to prepare Hardmetal materials
Method.So-called high-energy ball milling is to utilize specific material ball ratio and the rotating speed of ball mill or frequency of vibration,
Make abrading-ball that powder to carry out strong shock, grinding and stirring, powder is pulverized as nano_scale particle
Method.
For reaching object above, the present invention adopts the following technical scheme that and is achieved,
A kind of Ni Fe base high temperature coheres the preparation method of phase cemented carbide, it is characterised in that include following step
Rapid:
(1) by mass percentage, weigh 34～the chromium powder of the iron powder of the nikel powder of 38%, 29～36%, 16～20%,
5～the molybdenum powder of 8% and 3～8% aluminium powder premixing less than 2 hours, then by premixing powder in argon gas atmosphere
The lower high-energy ball milling of protection at least 15 hours, in 150 DEG C of vacuum drying after taking-up, becomes Ni-Fe base high energy ball
Pulverizing；
(2) 70～the VC of the TiC of the WC of 74%, 17～23%, 0.1～0.3% by mass percentage, are weighed
With 7～the Ni-Fe base high-energy ball milling powder of 10%, general milling at least 24 hours under argon gas atmosphere is protected；
(3) step (2) gained ball-milled powder is loaded mould cold-press moulding；
(4) under argon gas atmosphere is protected, the green compact of step (3) gained cold-press moulding are loaded pipe type sintering furnace
In, in the sintering of 1350～1380 DEG C under argon shield, at least insulation 1 hour；
(5), in cooling procedure, control sintering furnace rate of temperature fall, finally obtain hard alloy block.
In said method, step (1) described high-energy ball milling, drum's speed of rotation is 230～280 revs/min, ball milling
Medium is dehydrated alcohol, and abrading-ball and ball grinder material are rustless steel, material: ball: dehydrated alcohol=1:18～21:
0.3。
Step (2) described general milling, uses planetary ball mill, and rotating speed 150～190 revs/min, abrading-ball is
Sintered carbide ball, ball grinder material is the rustless steel containing nylon inner lining, and ratio of grinding media to material is 15:1.
Step (4) described sintering, heating rate is 3～6 DEG C/min.Step (5) described rate of temperature fall is 9～18 DEG C
/min。
Compared with prior art, the invention have the characteristics that and advantage:
(1) during preparation Ni-Fe base high temperature coheres phase cemented carbide block, the present invention has changed completely
Simple employing Co metal and alloy thereof in method is had to prepare the thinking of hard alloy as binder materials, but
According to lot of research, use a kind of Ni-Fe based powders as the adhesive of hard alloy, and study Ni-Fe
Based powders proportioning, hard alloy material component, relation between thing phase composition and interfacial characteristics, it may be assumed that for
Ni-Fe base high temperature coheres phase cemented carbide, keeps higher force performance under the conditions of operating ambient temperature ＞ 900 DEG C
Optimum N i-Fe based powders proportioning and hard alloy material proportioning.It is high that the method has Composition Control precision, work
Skill stability and repeatability are relatively strong, overcome because Co metallic high temperature decarburization and solute segregation are to hard alloy high temperature
The harmful effect of mechanical property.
(2) essential characteristic in terms of the high-energy-milling of Ni-Fe base mixed-powder is: pass through high-energy ball milling
Ni-Fe base mixed-powder is carried out mechanical alloying, suppression hard alloy preparation process occurs hard carbide
Decarburization, generation metallic compound and harmful third phase.Its principles of science is: by adjusting high-energy-milling
Parameter and material, ball, medium spread than control element, control further to generate phase.Mechanical alloying makes Ni-Fe
Form multivariate solid solution between base mixed-powder, on the one hand promote hard alloy compacting sintering alloying, beneficially material
Material molding；On the other hand Ni, Fe and the alternate reaction of hard carbide during suppression sintering, it is to avoid generate de-
Carbon phase and harmful third phase；And can ensure that high-temperature-phase content.
Present invention Ni-Fe base mechanical alloying powder substitutes Co powder as adhesive, the hard of preparation
Alloy Vickers hardness >=1530/kg mm-2, bending strength >=4880MPa, 1000 DEG C of hot strengths
≥4562MPa。
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Hard alloy block material bending strength test condition prepared by following example meets " GB3851-83 "
Standard, Testing Tensile Strength at Elevated Temperature test condition meets " GB4338-84 " standard.
Embodiment 1
First by pre-for nikel powder, iron powder, chromium powder, molybdenum powder and aluminium powder 36:34:18:6:6 by mass percentage
Mix 1.5 hours (premixing flour equipment is three-dimensional eddy current batch mixer, rotating speed 51 revs/min), then by premixed powder
End is high-energy ball milling 18 hours under argon gas atmosphere is protected, and the ball mill speed of mainshaft 250 revs/min, ball-milling medium is
Dehydrated alcohol, abrading-ball and ball grinder material are rustless steel, and powder, ball, the mass ratio of dehydrated alcohol are 1:18:
0.3, ball milling powder takes out and is placed in 150 DEG C of vacuum drying ovens drying 2.5 hours.74:18 by mass percentage:
0.2:7.8 weighs WC, TiC, VC and Ni-Fe base high-energy ball milling powder, loads ball under argon gas atmosphere is protected
Grinding jar carries out general milling 25 hours, uses planetary ball mill, and drum's speed of rotation 170 revs/min, abrading-ball is
Sintered carbide ball, ball grinder material is the rustless steel containing nylon inner lining, ratio of grinding media to material 15:1.
Ball-milled powder is loaded in the cold stamping die of yg-type carbide, cold press is pressed into green compact, pressure
Power processed is 230MPa；Under argon gas atmosphere is protected, green compact are loaded sinter molding in high-temperature tubular sintering furnace,
Sintering temperature 1350 DEG C, temperature retention time 1.5 hours, 6 DEG C/min of heating rate, furnace cooling after burning, fall
Temperature 15 DEG C/min of speed.
Embodiment 2
First by pre-for nikel powder, iron powder, chromium powder, molybdenum powder and aluminium powder 38:33:19:7:3 by mass percentage
Mix 1.5 hours, then by premixing powder high-energy ball milling 18 hours, ball milling owner under argon gas atmosphere is protected
Axle rotating speed 280 revs/min, powder, ball, the mass ratio of dehydrated alcohol are 1:21:0.3, and ball milling powder takes out and is placed in
150 DEG C of vacuum drying ovens are dried 2.5 hours；By mass percentage 72:17.7:0.3:10 weigh WC, TiC,
VC and Ni-Fe base high-energy ball milling powder, loading ball grinder under argon gas atmosphere is protected, to carry out general milling 25 little
Time, drum's speed of rotation 190 revs/min, ratio of grinding media to material 15:1.
Ball-milled powder loading cold stamping die and is pressed into green compact in cold press, press power is 230MPa；At argon
Under gas atmosphere protection, green compact are loaded sinter molding in high-temperature tubular sintering furnace, sintering temperature 1380 DEG C, protects
Temperature time 2 h, 3 DEG C/min of heating rate, furnace cooling after burning, 10 DEG C/min of rate of temperature fall.
Embodiment 3
First by pre-for nikel powder, iron powder, chromium powder, molybdenum powder and aluminium powder 34:36:16:8:6 by mass percentage
Mix 1.5 hours, then by premixing powder high-energy ball milling 18 hours, ball milling owner under argon gas atmosphere is protected
Axle rotating speed 260 revs/min, powder, ball, the mass ratio of dehydrated alcohol are 1:16:0.3, and ball milling powder takes out and is placed in
150 DEG C of vacuum drying ovens are dried 2.5 hours；By mass percentage 73:18:0.2:8.8 weigh WC, TiC,
VC and Ni-Fe base high-energy ball milling powder, loading ball grinder under argon gas atmosphere is protected, to carry out general milling 25 little
Time, drum's speed of rotation 180 revs/min, ratio of grinding media to material 15:1.
Ball-milled powder loading cold stamping die and is pressed into green compact in cold press, press power is 230MPa；At argon
Under gas atmosphere protection, green compact are loaded sinter molding in high-temperature tubular sintering furnace, sintering temperature 1360 DEG C, protects
The 1.3 hours time of temperature, 5 DEG C/min of heating rate, furnace cooling after burning, 16 DEG C/min of rate of temperature fall.
Embodiment 4
First by pre-for nikel powder, iron powder, chromium powder, molybdenum powder and aluminium powder 37:29:18:8:8 by mass percentage
Mix 1.5 hours, then by premixing powder high-energy ball milling 18 hours, ball milling owner under argon gas atmosphere is protected
Axle rotating speed 240 revs/min, powder, ball, the mass ratio of dehydrated alcohol are 1:16:0.3, and ball milling powder takes out and is placed in
150 DEG C of vacuum drying ovens are dried 2.5 hours；By mass percentage 69.7:23:0.3:7 weigh WC, TiC,
VC and Ni-Fe base high-energy ball milling powder, loading ball grinder under argon gas atmosphere is protected, to carry out general milling 25 little
Time, drum's speed of rotation 150 revs/min, ratio of grinding media to material 15:1.
Ball-milled powder loading cold stamping die and is pressed into green compact in cold press, press power is 230MPa；At argon
Under gas atmosphere protection, green compact are loaded sinter molding in high-temperature tubular sintering furnace, sintering temperature 1350 DEG C, protects
The 1 hour time of temperature, 3 DEG C/min of heating rate, furnace cooling after burning, 18 DEG C/min of rate of temperature fall.
The different embodiment of table 1 is prepared Ni-Fe base high temperature and is cohered the performance parameter of phase cemented carbide
As can be seen from Table 1, the Ni-Fe base high temperature prepared by embodiment 1-4 method coheres phase cemented carbide tool
There are densification, crystal grain tiny and the feature such as mechanical behavior under high temperature is good.
The present invention coheres the interfacial combined function of phase cemented carbide block materials according to standby Ni-Fe base high temperature of drawing up
With thing phase composition accuracy controlling Ni-Fe based powders proportioning, coordinate the raw material group optimizing design synthesis hard alloy
Point, ball-milling technology and compacting sintering technique, it is provided that a complete preparation Ni-Fe base high temperature coheres the conjunction of phase hard
The technology path of gold copper-base alloy.
Claims (4)
1. a Ni-Fe base high temperature coheres the preparation method of phase cemented carbide, it is characterised in that comprise the steps:
(1) 34～the chromium powder of the iron powder of the nikel powder of 38%, 29～36%, 16～20%, 5～8% by mass percentage, are weighed
Molybdenum powder and 3～8% aluminium powder premixing less than 2 hours, then by premixing powder high energy ball under argon gas atmosphere is protected
It is milled to few 15 hours, in 150 DEG C of vacuum drying after taking-up, becomes Ni-Fe base high-energy ball milling powder；Described high-energy ball milling,
Drum's speed of rotation is 230～280 revs/min, and ball-milling medium is dehydrated alcohol, and abrading-ball and ball grinder material are rustless steel,
Material: ball: dehydrated alcohol=1:18～21:0.3；
(2) 70～the VC of the TiC of the WC of 74%, 17～23%, 0.1～0.3% and 7～10% by mass percentage, are weighed
Ni-Fe base high-energy ball milling powder, general milling at least 24 hours under argon gas atmosphere is protected；
(3) step (2) gained ball-milled powder is loaded mould cold-press moulding；
(4) under argon gas atmosphere is protected, the green compact of step (3) gained cold-press moulding are loaded in pipe type sintering furnace, argon
In the sintering of 1350～1380 DEG C under protection, at least insulation 1 hour；
(5), in cooling procedure, control sintering furnace rate of temperature fall, finally obtain hard alloy block.
2. Ni-Fe base high temperature as claimed in claim 1 coheres the preparation method of phase cemented carbide, it is characterised in that
Step (2) described general milling, uses planetary ball mill, and rotating speed 150～190 revs/min, abrading-ball is hard alloy
Ball, ball grinder material is the rustless steel containing nylon inner lining, and ratio of grinding media to material is 15:1.
3. Ni-Fe base high temperature as claimed in claim 1 coheres the preparation method of phase cemented carbide, it is characterised in that
Step (4) described sintering, heating rate is 3～6 DEG C/min.
4. Ni-Fe base high temperature as claimed in claim 1 coheres the preparation method of phase cemented carbide, it is characterised in that
Step (5) described rate of temperature fall is 9～18 DEG C/min.
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| CN115233068A (en) * | 2022-07-07 | 2022-10-25 | 广东正信硬质材料技术研发有限公司 | Light high-strength hard alloy material and preparation method thereof |
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| CN1464073A (en) * | 2002-06-24 | 2003-12-31 | 核工业第八研究所 | Nano crystal Ce-doping cemented carbide powder and process for preparing the same |
| CN1566387A (en) * | 2003-06-13 | 2005-01-19 | 中南大学 | Preparation method of fine-grain tungsten-copper composite material |
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| CN102796933A (en) * | 2012-09-04 | 2012-11-28 | 四川大学 | High-entropy alloy binder phase-based nitrogen-containing hard alloy and preparation method thereof |
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Patent Citations (4)
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| CN1464073A (en) * | 2002-06-24 | 2003-12-31 | 核工业第八研究所 | Nano crystal Ce-doping cemented carbide powder and process for preparing the same |
| CN1566387A (en) * | 2003-06-13 | 2005-01-19 | 中南大学 | Preparation method of fine-grain tungsten-copper composite material |
| CN1827817A (en) * | 2006-04-14 | 2006-09-06 | 韶关学院 | Hard alloy sintered by high-entropy alloy binder and compound carbide and preparation method thereof |
| CN102796933A (en) * | 2012-09-04 | 2012-11-28 | 四川大学 | High-entropy alloy binder phase-based nitrogen-containing hard alloy and preparation method thereof |
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