CN102787249A - 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 for preparing the high density tungsten Rhometal.
Background technology
Tungsten nickel iron alloy be a kind of be matrix (W content is 85%-98%) with tungsten, add little amount of N i, two kinds of elementary composition alloys of Fe, 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 density height, intensity and hardness is high, the 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 weldableness are good; Therefore tungsten nickel iron alloy has all obtained using widely in national defense industry and civilian industry; Particularly as injuring the warhead material by force, it is considered to replace the military novel material of the feature of environmental protection of the potentialization of depleted uranium bomb to the W-Ni-Fe alloy in national defense industry.
Tungsten nickel iron alloy by dystectic tungsten mutually with have more low-melting γ (Ni-Fe) two phase composites mutually, two phase fusing points differ greatly (tungsten phase fusing point is 3410 ℃, and the fusing point of γ phase is extremely low), so tungsten nickel iron alloy is a kind of typical liquid phase sintering alloy.In liquid phase sintering, Gu the interfacial energy of solubleness, solid phase and the liquid phase of solid phase in liquid phase and liquid phase influence the variation of sintering velocity and microstructure to a great extent along the solid-perviousness of crystal boundary.Sintering process parameter such as particle size, sintering temperature, sintering time, sintering atmosphere and pressed density also have considerable influence to the performance of material.
Summary of the invention
The object of the present invention is to provide a kind of sintering process for preparing the 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 " two-step sintering method " sintering process, thereby various performance requriementss such as the density of assurance tungsten nickel iron alloy bar, purity, internal microstructure with of the distortion of control tungsten nickel iron alloy in the liquid phase sintering stage.
The present invention adopts following technical scheme:
A kind of sintering process for preparing the high density tungsten Rhometal comprises the steps:
1) gets the raw materials ready: the W content of tungsten powder＞99.95 %; Ni content＞99.8% of nickel powder; Fe content＞99.5% of iron powder;
2) select powder: use 200 purpose sieves, raw material powder is screened; 3) join powder;
4) dress mould:, be filled in the rubber model bag with above-mentioned mixed alloy powder;
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, concrete technological process is following:
A) presintering: room temperature is warming up to 700 ~ 900 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃ ~ 1420 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃ ~ 1550 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
As preferably, the said powder step of joining is:
A) by weight W:95, Ni:3.5, Fe:1.5 take by weighing 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 into mix in the mixer, mixing time is 24h～48h.
As preferably, described preliminary mixing step is: advanced pedestrian worker mixes in stainless container.
As preferably, described isostatic cool pressing compression moulding step is:
A), put into the high-pressure work container of isostatic pressing machine with the rubber model bag that clamps;
B) start pressure pump and be pressed into the high-pressure work container to liquid medium till being full of and from venting hole, emerging;
C) start topping-up pump immediately and make pressure rise to 200Mpa with the speed of 5MPa/min, pressurize 1-2 minute then, last stress-relief process speed was 8MPa/min;
D) after pressure is removed, rubber coating is taken out from the high-pressure work container, open rubber coating, can the tungsten nickel iron alloy slab of compression moulding be taken out, so that the sintering of intermediate frequency equipment.
As preferably, the concrete operations step of described two-step sintering method is:
1) will wait the tungsten nickel iron alloy base of static pressure compression moulding to call in the intermediate frequency furnace, and arrange, mutual extruding can not be arranged, each the material between more than the spacing 10mm;
2) build bell, and the ON cycle water coolant, feed hydrogen as protective atmosphere, start the intermediate frequency furnace power supply then and begin heating;
3) operate according to temperature, heat-up rate and the soaking time set;
4) whole heating process is closed heating power supply after accomplishing, but continuation feeding hydrogen and recirculated cooling water are until room temperature.
As preferably, in the said sintering step 6, concrete technological process is following:
A) presintering: room temperature is warming up to 700 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
As preferably, in the said sintering step 6, concrete technological process is following:
A) presintering: room temperature is warming up to 900 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1400 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1520 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
As preferably, in the said sintering step 6, concrete technological process is following:
A) presintering: room temperature is warming up to 800 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1200 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1550 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
In whole sintering process; After producing warm area in the stove, operator carried out one time temperature detection at per 15 minutes, used optical pyrometer; Self-service instrument three factories in Shanghai produce: WGG2-201 measures, and is controlled at rational interval with control sintering stock heating curve.
Beneficial effect of the present invention is:
The present invention is applicable to the sintering process that is prepared the high-gravity tungsten Rhometal by purity greater than high purity tungsten, nickel powder, the iron powder of 99.5 %; 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 with of the distortion of control 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 formed firm tetrakaidecahedron property three-dimensional networks skeleton in the solid state sintering stage; Hindered the tungsten particle segregation in liquid phase sintering stage, the performance and the microstructure uniformity of alloy improve greatly.
The advantage of process synthesis solid state sintering of the present invention and liquid phase sintering, before liquid phase sintering, at first under the 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 replaces the conventional high-temperature molybdenum wire furnace, thereby sintering parameters such as the atmosphere of 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 even, specific density >=99% of distortion, inner chemical ingredients and microstructure not; Inner flawless, bubble and big crystallization, machining property are good.
Other advantages of the present invention, target and characteristic will be set forth in specification sheets subsequently to a certain extent; And to a certain extent; Based on being conspicuous to those skilled in the art, perhaps can from practice of the present invention, obtain instruction to investigating of hereinafter.Target of the present invention can realize through the following structure that specification sheets particularly pointed out and obtain with other advantages.
Embodiment:
Below in conjunction with embodiment the present invention is further described:
Embodiment 1:
Process step of the present invention is following:
1) starting material chemical composition analysis: adopt the purity of ICP atomic absorption spectrometry tungsten powder, nickel powder, iron powder, satisfy following the requirement:
The W content of tungsten powder＞99.95 %; Ni content＞99.8% of nickel powder; Fe content＞99.5% of iron powder.
2) select powder: use 200 purpose sieves, raw material powder is screened;
3) join powder:
A) at first in the Working environment of cleaning on request weight ratio take by weighing the garbled tungsten powder of corresponding weight, iron powder, nickel powder, 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 blended purpose is for next step mechanically mixing is more even, in the Working environment of cleaning, in stainless container, carries out artificial mixed earlier: one deck tungsten powder one deck nickel powder one deck iron powder;
C) the preliminary mixed alloy powder mixer of packing into is carried out mechanically mixing, mixing time is 24h～48h.
4) dress mould:, be filled in the rubber model bag with above-mentioned mixed alloy powder;
5) isostatic cool pressing compression moulding:
A), put into the high-pressure work container of isostatic pressing machine with the rubber model bag that clamps;
B) start pressure pump and be pressed into the high-pressure work container to liquid medium till being full of and from venting hole, emerging;
C) start topping-up pump immediately and make pressure rise to 200MPa with the speed of 5MPa/min, pressurize 1-2 minute then, last stress-relief process speed was 8MPa/min;
D) after pressure is removed, rubber coating is taken out from the high-pressure work container, open rubber coating, can the tungsten nickel iron alloy slab of compression moulding 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 the conventional high-temperature molybdenum wire furnace, thereby sintering parameters such as the atmosphere of 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, concrete technological process is following:
A) presintering: room temperature is warming up to 900 ℃, and times spent 4 h is at 900 ℃ of insulation 1 ~ 2h;
B) solid state sintering: be heated to 1400 ℃ from 900 ℃, time spent 6h is at 1400 ℃ of insulation 1 ~ 2h;
C) liquid phase sintering: be heated to 1520 ℃ ~ 1530 ℃, time spent 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 operations step of two-step sintering method is:
1) will wait the tungsten nickel iron alloy base of static pressure compression moulding to call in the intermediate frequency furnace, and arrange, mutual extruding can not be arranged, each the material between more than the spacing 10mm;
2) build bell, and the ON cycle water coolant, feed hydrogen as protective atmosphere, start the intermediate frequency furnace power supply then and begin heating;
3) in operating process, rationally set heating current, strict heat-up rate by technique initialization, and soaking time operate, carried out operating record in per 15 minutes;
4) whole heating process is closed heating power supply after accomplishing, but continuation feeding hydrogen and recirculated cooling water are until room temperature.
In whole sintering process; After producing warm area in the stove, operator carried out one time temperature detection at per 15 minutes, used optical pyrometer; Self-service instrument three factories in Shanghai produce: WGG2-201 measures, and is controlled at rational interval with control sintering stock heating curve.
7) alloy preform check behind the sintering.Its assay is:
A) there is metalluster on the surface of slab, does not have defectives such as crackle, pore;
b)? using drainage gravimetric method to detect tungsten nickel alloy plates bear grudge overall density conditions, the detection density meet GB/T26038-2010 standard requirements;
C) utilization alloy analysis appearance is analyzed the chemical ingredients of sintered alloy base different sites, analyzes to show that each position composition is identical;
C) check the crystalline structure of slab through the microscopic examination microsection, the assay crystalline structure evenly, do not have excessive or too small crystal grain, the tungsten metal metallographic inspecting standard GB/T4197-84 of reference standard country, intergranule does not have the cavity.
Concrete step is following:
1. sampling:, get the cube specimen that the length of side is approximately 10mm from tungsten nickel iron alloy front end reserved part;
2. roughly grind:, tentatively polish with the surface of emery wheel with test specimen because the test specimen surface is uneven;
3. fine grinding: on the different sand paper of granularity, undertaken by order from coarse to fine;
4. polish: the test specimen after the fine grinding is placed on the polishing machine polishes;
5. corrode: the polished surface of test specimen is immersed in the etchant, owing to the flour milling atom is dissolved in the etchant, in dissolving, crystal grain and intergranule, the dissolution rate between crystal grain and the crystal boundary is different, and microstructure just displays;
6. with the microsection test specimen for preparing be placed on microscopically observe its crystalline structure evenly, do not have excessive or too small crystal grain, intergranule not to have the cavity;
D) through the ultrasonic nondestructive test Equipment Inspection, do not find that there is tangible crackle (crack length is less than 0.4mm) inside.
Tungsten nickel iron alloy belongs to typical liquid phase sintering; But the serious problems of caving in and existing in the high-density alloy production process when being out of shape in the liquid phase sintering process; This is because tungsten differs greatly with density of liquid phase, and heavy tungsten particle is made the result of shearing motion downwards in liquid phase; Though caving in and being out of shape in the liquid phase sintering process can reach full densification and overcome through solid state sintering.But generally solid state sintering can not satisfy the density and the performance requriements of high-density alloy.So the advantage of comprehensive solid state sintering and liquid phase sintering, before liquid phase sintering, at first under the solid solubility line 1400 ℃ carry out solid state sintering, and then " two-step sintering method " sintering process of employing liquid phase sintering.
Adopt the detected result of the tungsten nickel iron alloy sample of prepared of the present invention to be: sample is distortion not, and the composition of sample all directions is even; And proportion is high, and density reaches 18.4, and density reaches more than 97%.
Embodiment 2:
Concrete sintering process process is following:
A) presintering: room temperature is warming up to 700 ℃, time spent 3h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃, time spent 4h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃, time spent 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 following:
A) presintering: room temperature is warming up to 800 ℃, times spent 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1200 ℃, time spent 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1550 ℃, time spent 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 following:
A) presintering: room temperature is warming up to 850 ℃, times spent 3.5 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1350 ℃, time spent 5h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1500 ℃, time spent 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 the solid state sintering soaking time, and direct heating is to liquid phase.Two temperature sections are arranged: 700 ℃ ~ 900 ℃ of presintering, insulation 1h ~ 2h, direct heating to 1470 ℃ ~ 1530 ℃ then, 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 the sample bottom.
Embodiment 6: do not have liquid phase sintering, only be sintered to solid-state temperature
Other parameter does not have liquid phase sintering with embodiment 1, only is sintered to solid-state temperature: two temperature sections are arranged: 700 ℃ ~ 900 ℃ of presintering, insulation 1h ~ 2h is heated to 1350 ℃ ~ 1400 ℃ then, insulation 1h ~ 2h.
The tungsten nickel iron alloy test result of preparation is: though sample is indeformable, composition also relatively evenly, density is very low, is merely 17.0, and density can only reach 85%, does not meet the demands.
Explanation is at last; 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 perhaps are equal to replacement; Only otherwise break away from the spirit and the scope of technical scheme of the present invention, all should be encompassed in the middle of the claim scope of the present invention.
Claims (8)
1. a sintering process for preparing the high density tungsten Rhometal is characterized in that: comprise the steps:
1) gets the raw materials ready: the W content of tungsten powder＞99.95 %; Ni content＞99.8% of nickel powder; Fe content＞99.5% of iron powder;
2) select powder: use 200 purpose sieves, raw material powder is screened; 3) join powder;
4) dress mould:, be filled in the rubber model bag with above-mentioned mixed alloy powder;
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, concrete technological process is following:
A) presintering: room temperature is warming up to 700 ~ 900 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃ ~ 1420 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃ ~ 1550 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
2. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 1 is characterized in that: the said powder step of joining is:
A) by weight W:95, Ni:3.5, Fe:1.5 take by weighing 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 into mix in the mixer, mixing time is 24h～48h.
3. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 2 is characterized in that: described preliminary mixing step is: advanced pedestrian worker mixes in stainless container.
4. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 1 and 2 is characterized in that: described isostatic cool pressing compression moulding step is:
A), put into the high-pressure work container of isostatic pressing machine with the rubber model bag that clamps;
B) start pressure pump and be pressed into the high-pressure work container to liquid medium till being full of and from venting hole, emerging;
C) start topping-up pump immediately and make pressure rise to 200Mpa with the speed of 5MPa/min, pressurize 1-2 minute then, last stress-relief process speed was 8MPa/min;
D) after pressure is removed, rubber coating is taken out from the high-pressure work container, open rubber coating, can the tungsten nickel iron alloy slab of compression moulding be taken out, so that the sintering of intermediate frequency equipment.
5. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 1 and 2 is characterized in that: the concrete operations step of described two-step sintering method is:
1) will wait the tungsten nickel iron alloy base of static pressure compression moulding to call in the intermediate frequency furnace, and arrange, mutual extruding can not be arranged, each the material between more than the spacing 10mm;
2) build bell, and the ON cycle water coolant, feed hydrogen as protective atmosphere, start the intermediate frequency furnace power supply then and begin heating;
3) operate according to temperature, heat-up rate and the soaking time set;
4) whole heating process is closed heating power supply after accomplishing, but continuation feeding hydrogen and recirculated cooling water are until room temperature.
6. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 1 is characterized in that: in the said sintering step 6, concrete technological process is following:
A) presintering: room temperature is warming up to 700 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1070 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1470 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
7. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 1 is characterized in that: in the said sintering step 6, concrete technological process is following:
A) presintering: room temperature is warming up to 900 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1400 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1520 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
8. a kind of sintering process for preparing the high density tungsten Rhometal according to claim 1 is characterized in that: in the said sintering step 6, concrete technological process is following:
A) presintering: room temperature is warming up to 800 ℃, times spent 3 ~ 4 h, insulation 1 ~ 2h;
B) solid state sintering: continue to be heated to 1200 ℃, time spent 4 ~ 6h, insulation 1 ~ 2h;
C) liquid phase sintering: continue to be heated to 1550 ℃, time spent 1 ~ 2h, insulation 1 ~ 2h;
D) come out of the stove after the blowing out cooling.
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