CN102787249B - Sintering process for preparing high-density tungsten ferro-nickel alloy - Google Patents
Sintering process for preparing high-density tungsten ferro-nickel alloy Download PDFInfo
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Abstract
The invention discloses a sintering process for preparing high-density tungsten ferro-nickel alloy. The sintering process comprises the following steps: (1) preparing materials: enabling content of W in tungsten powder to be larger than 99.95%, enabling content of Ni in nickel powder to be larger than 99.8%, and enabling content of Fe in iron powder to be larger than 99.5%; (2) selecting powder: using a sieve of 200 mesh to screen the raw material powder; (3) blending the powder; (4) performing die-filling: filling the mixed alloy powder in a rubber die bag; (5) performing cold isostatic pressing forming; and (6) sintering: adopting a two-step sintering method to sinter in a medium frequency induction furnace with hydrogen protection, and enabling the sintering process to be divided into three stages which are presintering, solid phase sintering and liquid phase sintering. The high-specific-gravity tungsten ferro-nickel alloy processed by the sintering process has the advantages that the tungsten ferro-nickel alloy is not deformed, interior chemical constituents and microstructures are uniform, the relative density is no smaller than 99%, the inside of the tungsten ferro-nickel alloy has no cracks or bubbles and is free of crystallization, and the machining property is excellent.
Description
Technical field
The present invention relates to a kind of sintering process of tungsten nickel iron alloy, particularly relate to a kind of sintering process of preparing high density tungsten Rhometal.
Background technology
Tungsten nickel iron alloy is a kind of take tungsten as matrix (W content is 85%-98%), adds a small amount of Ni, two kinds of elementary composition alloys of Fe, and its density is up to 16.5-19.0g/cm
3, heavy alloy or heavy metal are otherwise known as.Tungsten nickel iron alloy has that density is high, intensity and hardness is high, physical and mechanical property and the use properties of electroconductibility and a series of excellences such as thermal conductivity is good, thermal expansivity is little, anticorrosive and good in oxidation resistance, machinability and weldability are good, therefore tungsten nickel iron alloy is all widely used in national defense industry and civilian industry, particularly W-Ni-Fe alloy is as injuring by force warhead material in national defense industry, and it is considered to replace the military novel material of the potential feature of environmental protection of tool of depleted uranium bomb.
Tungsten nickel iron alloy is by dystectic tungsten phase and have γ phase (Ni-Fe) two phase composites compared with low melting point, and two-phase fusing point differs greatly (tungsten phase fusing point is 3410 ℃, and the fusing point of γ phase is extremely low), and therefore tungsten nickel iron alloy is a kind of typical liquid phase sintering alloy.In liquid phase sintering, the interfacial energy of solubleness, solid phase and the liquid phase of solid phase in liquid phase and liquid phase affect the variation of sintering velocity and microstructure to a great extent along the solid-perviousness of die bond circle.Sintering process parameter also has considerable influence to the performance of material as particle size, sintering temperature, sintering time, sintering atmosphere and pressed density.
Summary of the invention
The object of the present invention is to provide a kind of sintering process of preparing high density tungsten Rhometal; adopt the medium-frequency induction furnace indirect heating sintering process of logical hydrogen shield to replace traditional high temperature molybdenum wire sintering furnace heat-agglomerating method; and propose the distortion in the liquid phase sintering stage with control tungsten nickel iron alloy of " two-step sintering method " sintering process, thereby the various performance requriementss such as the density of assurance tungsten nickel iron alloy bar, purity, internal microstructure.
The present invention adopts following technical scheme:
A sintering process of preparing high density tungsten Rhometal, comprises the steps:
1) get the raw materials ready: W content > 99.95 % of tungsten powder; The Ni content > 99.8% of nickel powder; The Fe content > 99.5% of iron powder;
2) select powder: use 200 object sieves, raw material powder is screened; 3) join powder;
4) dress mould: by above-mentioned mixed alloy powder, be filled in rubber model bag;
5) isostatic cool pressing compression moulding;
6) sintering: adopt two-step sintering method sintering in the medium-frequency induction furnace of logical hydrogen shield, be divided into presintering, solid state sintering, liquid phase sintering three phases, specific embodiment is as follows:
A) presintering: room temperature is warming up to 700 ~ 900 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃ ~ 1420 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃ ~ 1550 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
As preferably, described in join powder step and be:
A) by weight W:95, Ni:3.5, Fe:1.5 takes the garbled tungsten powder of corresponding weight, iron powder, nickel powder;
B) tungsten powder, nickel powder, iron powder are tentatively mixed in Stainless Steel Disc;
C) preliminary mixed alloy powder is packed in mixer and mix, mixing time is 24h～48h.
As preferably, described preliminary mixing step is: in stainless container, advanced pedestrian's work is mixed.
As preferably, described isostatic cool pressing compression moulding step is:
A), by the rubber model bag clamping, put into the high-pressure work container of isostatic pressing machine;
B) start pressure pump liquid medium is pressed into high-pressure work container until be full of and emerge from venting hole;
C) start immediately topping-up pump and make pressure rise to 200Mpa with the speed of 5MPa/min, then pressurize 1-2 minute, last stress-relief process speed is 8MPa/min;
D) after pressure is removed, rubber coating is taken out from high-pressure work container, open rubber coating, the tungsten nickel iron alloy slab of compression moulding can be taken out, so that the sintering of intermediate frequency equipment.
As preferably, the concrete operation step of described two-step sintering method is:
1) the tungsten nickel iron alloy base that waits static pressure compression moulding is called in intermediate frequency furnace, and arrange, can not have mutual extruding, between each material more than spacing 10mm;
2) build bell, and ON cycle water coolant, pass into hydrogen as protective atmosphere, then start intermediate frequency furnace power supply and start heating;
3) operate according to temperature, heat-up rate and the soaking time set;
4) whole heating process is closed heating power supply after completing, but continues to pass into hydrogen and recirculated cooling water until room temperature.
As preferably, in described sintering step 6, specific embodiment is as follows:
A) presintering: room temperature is warming up to 700 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
As preferably, in described sintering step 6, specific embodiment is as follows:
A) presintering: room temperature is warming up to 900 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1400 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1520 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
As preferably, in described sintering step 6, specific embodiment is as follows:
A) presintering: room temperature is warming up to 800 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1200 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1550 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
In whole sintering process, when producing in stove after warm area, operator carried out one time temperature detection at every 15 minutes, used optical pyrometer, self-service instrument three factories in Shanghai produce: WGG2-201 measures, and is controlled at rational interval to control sintering stock heating curve.
Beneficial effect of the present invention is:
High purity tungsten, nickel powder, the iron powder that the present invention is applicable to be greater than 99.5 % by purity prepared the sintering process of high-gravity tungsten Rhometal; adopt the medium-frequency induction furnace indirect heating sintering process of logical hydrogen shield to replace traditional high temperature molybdenum wire sintering furnace heat-agglomerating method, and propose " two-step sintering method " sintering process to control the distortion of tungsten nickel iron alloy in the liquid phase sintering stage.Tungsten nickel iron alloy can reach 90～93% in solid state sintering stage density, liquid phase sintering can reach full densification, and owing to having formed firm tetrakaidecahedron three-dimensional networks skeleton in the solid state sintering stage, hindered the tungsten particle segregation in liquid phase sintering stage, the performance of alloy and the homogeneity of microstructure improve greatly.
The advantage of process synthesis solid state sintering of the present invention and liquid phase sintering, before liquid phase sintering, first under solid solubility line 1400 ℃ carry out solid state sintering, and then adopt " two-step sintering method " sintering process of liquid phase sintering; And the Medium frequency induction furnace apparatus of the logical hydrogen shield of uses advanced replacement conventional high-temperature molybdenum wire furnace, thereby the sintering parameters such as the atmosphere to sintering process, temperature rise rate, soaking time are carried out complete controllable operating.The high-gravity tungsten Rhometal that adopts producing and manufacturing technique of the present invention to process has following performance: tungsten nickel iron alloy is not out of shape, inner chemical composition and microstructure evenly, relative density >=99%; Inner flawless, bubble and large crystallization, machining property are good.
Other advantages of the present invention, target and feature will be set forth to a certain extent in the following description, and to a certain extent, based on will be apparent to those skilled in the art to investigating below, or can be instructed from the practice of the present invention.Target of the present invention and other advantages can be realized and be obtained by specification sheets specifically noted structure below.
embodiment:
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
Processing step of the present invention is as follows:
1) starting material chemical composition analysis: adopt the purity of ICP atomic absorption spectrometry tungsten powder, nickel powder, iron powder, meet following requirement:
W content > 99.95 % of tungsten powder; The Ni content > 99.8% of nickel powder; The Fe content > 99.5% of iron powder.
2) select powder: use 200 object sieves, raw material powder is screened;
3) join powder:
A) first in clean Working environment, weight ratio on request takes the garbled tungsten powder of corresponding weight, iron powder, nickel powder, and tungsten ferronickel weight ratio is W:95, Ni:3.5, Fe:1.5;
B) tungsten powder, nickel powder, iron powder are tentatively mixed in Stainless Steel Disc, preliminary object of mixing is for next step mechanically mixing is more even, first in clean Working environment, in stainless container, manually mixes: one deck tungsten powder one deck nickel powder one deck iron powder;
C) pack preliminary mixed alloy powder into mixer and carry out mechanically mixing, mixing time is 24h～48h.
4) dress mould: by above-mentioned mixed alloy powder, be filled in rubber model bag;
5) isostatic cool pressing compression moulding:
A), by the rubber model bag clamping, put into the high-pressure work container of isostatic pressing machine;
B) start pressure pump liquid medium is pressed into high-pressure work container until be full of and emerge from venting hole;
C) start immediately topping-up pump and make pressure rise to 200MPa with the speed of 5MPa/min, then pressurize 1-2 minute, last stress-relief process speed is 8MPa/min;
D) after pressure is removed, rubber coating is taken out from high-pressure work container, open rubber coating, the tungsten nickel iron alloy slab of compression moulding can be taken out, so that the sintering of intermediate frequency equipment.
6) sintering: adopt two-step sintering method sintering in the medium-frequency induction furnace of logical hydrogen shield, replace conventional high-temperature molybdenum wire furnace, thereby the sintering parameters such as the atmosphere to sintering process, temperature rise rate, soaking time are carried out complete controllable operating.Be divided into presintering, solid state sintering, liquid phase sintering three phases, specific embodiment is as follows:
A) presintering: room temperature is warming up to 900 ℃, used times 4 h, at 900 ℃ of insulation 1 ~ 2h;
B) solid state sintering: be heated to 1400 ℃ from 900 ℃, used time 6h, at 1400 ℃ of insulation 1 ~ 2h;
C) liquid phase sintering: be heated to 1520 ℃ ~ 1530 ℃, used time 1h, insulation 1 ~ 1.5h from 1400 ℃;
D) blowing out was come out of the stove after cooling for some time, and be 9h cooling time.
The concrete operation step of two-step sintering method is:
1) the tungsten nickel iron alloy base that waits static pressure compression moulding is called in intermediate frequency furnace, and arrange, can not have mutual extruding, between each material more than spacing 10mm;
2) build bell, and ON cycle water coolant, pass into hydrogen as protective atmosphere, then start intermediate frequency furnace power supply and start heating;
3) in operating process, rationally set heating current, strictly operate by the heat-up rate of technique initialization and soaking time, within every 15 minutes, carry out operating record;
4) whole heating process is closed heating power supply after completing, but continues to pass into hydrogen and recirculated cooling water until room temperature.
In whole sintering process, when producing in stove after warm area, operator carried out one time temperature detection at every 15 minutes, used optical pyrometer, self-service instrument three factories in Shanghai produce: WGG2-201 measures, and is controlled at rational interval to control sintering stock heating curve.
7) alloy preform check after sintering.Its assay is:
A) there is metalluster on the surface of slab, there is no the defect such as crackle, pore;
B) adopt draining check weighing method, detect tungsten nickel iron alloy plate Bear-grudge global density situation, density meets GB/T26038-2010 standard-required after testing;
C) use alloy analysis instrument to analyze the chemical composition of sintered alloy base different sites, analyze and show that each position composition is identical;
C) check the crystalline structure of slab by microscopic examination microsection, assay crystalline structure evenly, there is no excessive or too small crystal grain, the tungsten metal metallographic inspecting standard GB/T4197-84 of reference standard country, intergranule does not have cavity.
Concrete step is as follows:
1. sampling: from tungsten nickel iron alloy front end reserved part, get the length of side and be approximately the cube specimen of 10mm;
2. corase grind: uneven due to test specimen surface, tentatively polishes the surface of test specimen with emery wheel;
3. fine grinding: undertaken by order from coarse to fine on the different sand paper of granularity;
4. polishing: the test specimen after fine grinding is placed on and carries out polishing on polishing machine;
5. corrode: the polished surface of test specimen is immersed in etchant, because flour milling atom is dissolved in etchant, in dissolving, crystal grain and intergranule, the dissolution rate difference between grain and grain boundary, microstructure just displays;
6. the microsection test specimen preparing is put observe under the microscope its crystalline structure evenly, do not have excessive or too small crystal grain, intergranule there is no cavity;
D) by ultrasonic nondestructive test equipment Inspection, do not find that there is obvious crackle (crack length is less than 0.4mm) inside.
Tungsten nickel iron alloy belongs to typical liquid phase sintering, but serious problems that exist in high-density alloy production process when caving in and being out of shape in liquid sintering process, this is to differ greatly due to tungsten phase and density of liquid phase, and heavy tungsten particle is made the result of shearing motion downwards in liquid phase; Although caving in and being out of shape in liquid sintering process can be reached full densification and be overcome by solid state sintering.But solid state sintering can not meet density and the performance requriements of high-density alloy under normal circumstances.Therefore the advantage of comprehensive solid state sintering and liquid phase sintering, before liquid phase sintering, first under solid solubility line 1400 ℃ carry out solid state sintering, and then adopt " two-step sintering method " sintering process of liquid phase sintering.
Adopt the detected result of tungsten nickel iron alloy sample prepared by technique of the present invention to be: sample is not out of shape, and the composition of sample all directions is even; And proportion is high, density reaches 18.4, and density reaches more than 97%.
Embodiment 2:
Concrete sintering process process is as follows:
A) presintering: room temperature is warming up to 700 ℃, used time 3h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃, used time 4h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃, used time 1h, insulation 1 ~ 2h;
D) blowing out was come out of the stove after cooling for some time.
Other process is with embodiment 1.
Embodiment 3:
Concrete sintering process process is as follows:
A) presintering: room temperature is warming up to 800 ℃, used times 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1200 ℃, used time 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1550 ℃, used time 2h, insulation 1 ~ 2h;
D) blowing out was come out of the stove after cooling for some time.
Other process is with embodiment 1.
Embodiment 4:
Concrete sintering process process is as follows:
A) presintering: room temperature is warming up to 850 ℃, used times 3.5 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1350 ℃, used time 5h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1500 ℃, used time 2h, insulation 1 ~ 2h;
D) blowing out was come out of the stove after cooling for some time.
Other process is with embodiment 1.
Embodiment 5: directly liquid phase sintering
Other parameter is with embodiment 1, and directly liquid phase sintering, does not have solid state sintering soaking time, and direct heating is to liquid phase.There are two temperature sections: 700 ℃ ~ 900 ℃ of presintering, insulation 1h ~ 2h, then direct heating to 1470 ℃ ~ 1530 ℃, insulation 1h ~ 2h.
The tungsten nickel iron alloy test result of preparation is: sample deformation is serious and composition is inhomogeneous, and nickel, iron sink to sample bottom.
Embodiment 6: there is no liquid phase sintering, be only sintered to solid-state temperature
Other parameter, with embodiment 1, does not have liquid phase sintering, is only sintered to solid-state temperature: have two temperature sections: 700 ℃ ~ 900 ℃ of presintering, insulation 1h ~ 2h, is then heated to 1350 ℃ ~ 1400 ℃, insulation 1h ~ 2h.
The tungsten nickel iron alloy test result of preparation is: although sample is indeformable, composition is also more even, and density is very low, is only 17.0, and density can only reach 85%, does not meet the demands.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, other modifications that those of ordinary skills make technical scheme of the present invention or be equal to replacement, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of claim scope of the present invention.
Claims (7)
1. a sintering process of preparing high density tungsten Rhometal, is characterized in that: comprise the steps:
1) get the raw materials ready: W content > 99.95 % of tungsten powder; The Ni content > 99.8% of nickel powder; The Fe content > 99.5% of iron powder;
2) select powder: use 200 object sieves, raw material powder is screened;
3) join powder; The described powder step of joining is:
A) by weight W:95, Ni:3.5, Fe:1.5 takes the garbled tungsten powder of corresponding weight, iron powder, nickel powder;
B) tungsten powder, nickel powder, iron powder are tentatively mixed in Stainless Steel Disc;
C) preliminary mixed alloy powder is packed in mixer and mix, mixing time is 24h～48h;
4) dress mould: by above-mentioned mixed alloy powder, be filled in rubber model bag;
5) isostatic cool pressing compression moulding;
6) sintering: adopt two-step sintering method sintering in the medium-frequency induction furnace of logical hydrogen shield, be divided into presintering, solid state sintering, liquid phase sintering three phases, specific embodiment is as follows:
A) presintering: room temperature is warming up to 700 ~ 900 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃ ~ 1420 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃ ~ 1550 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
2. a kind of sintering process of preparing high density tungsten Rhometal according to claim 1, is characterized in that: described preliminary mixing step is: in stainless container, advanced pedestrian's work is mixed.
3. a kind of sintering process of preparing high density tungsten Rhometal according to claim 1, is characterized in that: described isostatic cool pressing compression moulding step is:
A), by the rubber model bag clamping, put into the high-pressure work container of isostatic pressing machine;
B) start pressure pump liquid medium is pressed into high-pressure work container until be full of and emerge from venting hole;
C) start immediately topping-up pump and make pressure rise to 200MPa with the speed of 5MPa/min, then pressurize 1-2 minute, last stress-relief process speed is 8MPa/min;
D) after pressure is removed, rubber coating is taken out from high-pressure work container, open rubber coating, the tungsten nickel iron alloy slab of compression moulding can be taken out, so that the sintering of intermediate frequency equipment.
4. a kind of sintering process of preparing high density tungsten Rhometal according to claim 1, is characterized in that: the concrete operation step of described two-step sintering method is:
1) the tungsten nickel iron alloy base that waits static pressure compression moulding is called in intermediate frequency furnace, and arrange, can not have mutual extruding, between each material more than spacing 10mm;
2) build bell, and ON cycle water coolant, pass into hydrogen as protective atmosphere, then start intermediate frequency furnace power supply and start heating;
3) operate according to temperature, heat-up rate and the soaking time set;
4) whole heating process is closed heating power supply after completing, but continues to pass into hydrogen and recirculated cooling water until room temperature.
5. a kind of sintering process of preparing high density tungsten Rhometal according to claim 1, is characterized in that: in described sintering step 6, specific embodiment is as follows:
A) presintering: room temperature is warming up to 700 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
6. a kind of sintering process of preparing high density tungsten Rhometal according to claim 1, is characterized in that: in described sintering step 6, specific embodiment is as follows:
A) presintering: room temperature is warming up to 900 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1400 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1520 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
7. a kind of sintering process of preparing high density tungsten Rhometal according to claim 1, is characterized in that: in described sintering step 6, specific embodiment is as follows:
A) presintering: room temperature is warming up to 800 ℃, used times 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1200 ℃, used time 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1550 ℃, used time 1 ~ 2h, insulation 1 ~ 2h;
D) blowing out is come out of the stove after cooling.
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| CN101230427A (en) * | 2008-02-22 | 2008-07-30 | 中南大学 | Method for preparing grain-refining W-Ni-Fe alloy containing rare earth |
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