CN102166653A - Preparation method of tungsten-steel/iron functionally graded material - Google Patents
Preparation method of tungsten-steel/iron functionally graded material Download PDFInfo
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- CN102166653A CN102166653A CN 201110093161 CN201110093161A CN102166653A CN 102166653 A CN102166653 A CN 102166653A CN 201110093161 CN201110093161 CN 201110093161 CN 201110093161 A CN201110093161 A CN 201110093161A CN 102166653 A CN102166653 A CN 102166653A
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Abstract
The invention provides a method for preparing a tungsten-steel/iron functionally graded material, comprising the following concrete steps of: selecting tungsten powder with the particle size of 1-10 micrometers and steel powder or iron powder with the particle size of 45-150 micrometers; mixing the tungsten powder and the steel powder/iron powder in a designed volume fraction; performing laminated pressure forming on the mixed powder under the forming pressure of 50-300MPa; putting the formed green body into a pyrophyllite mold, putting into a press, applying pressure of 1-10GPa, and applying alternating current of 2-6kW at two ends, wherein the electrifying current is 1000-3000A and the sintering time is 15-100 seconds; and after electrifying and sintering, keeping the pressure for 30-180 seconds. The invention has the advantages of preparing two materials such as tungsten and steel/iron powder with greatly different physical properties into a functionally graded material (FGM) once by consuming a short time at low cost. By cold-press forming, the residual gas in the body is removed as much as possible, and simultaneously, the thickness of each layer can be well controlled to be consistent with that of the design components.
Description
Technical field
The invention belongs to being connected and, particularly providing a kind of method for preparing tungsten-steel/iron FGM of refractory metal and structural material towards the technical field of plasma high heat load parts preparation.
Background technology
Refractory metals tungsten that the present invention relates to and steel (iron) FGM (Function Graded Materials, a kind of preparation method FGM).Adopt composition and structure continually varying FGM, make the tungsten with high-melting-point, high strength, high thermal conductivity and high rigidity and the structural material steel (iron) of high strength, high-ductility combine, bring into play the advantage of two kinds of materials.Therefore has potential extensive use in fields such as nuclear energy.As the heat deposition material, the divertor material in the nuclear fusion device and towards plasma parts etc.
At the divertor position of following fusion facility, refractory metals tungsten and structural material steel need be linked together.Because the thermal coefficient of expansion of tungsten and steel (iron) differs huge, the tungsten that conventional welding method obtains and the joint of steel (iron) have bigger residual stress and operating pressure, can cause distortion, cracking equivalent damage.Preparation tungsten and steel (iron) FGM are the important channels that addresses this problem.But tungsten and steel (iron) fusing point differs huge, and tungsten and steel (iron) at high temperature can react, usual way be difficult to a step obtained performance well, tungsten/steel (iron) FGM cheaply.Have not yet to see report about tungsten/steel (iron) FGM preparation.The hyperpressure that the present invention proposes energising sintering method down can prepare relative density and reaches that 98 ﹪ are above, tungsten/steel (iron) FGM of good mechanical performance, and sintering time is short, and one step of sintering process finishes, and has improved efficient when reducing cost greatly.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of preparation technology simple, the time is short, density height, good mechanical performance, and the preparation method of gained gradient composition and corresponding to tungsten/steel of design component or iron FGM.
Technical scheme of the present invention is: a kind of method for preparing tungsten-steel/iron FGM specifically may further comprise the steps:
The preparation of a, raw material: select the tungsten powder of 1～10 micron of granularity, the granularity of comminuted steel shot/iron powder is 45～150 microns.Above-mentioned tungsten powder and comminuted steel shot iron powder is evenly mixed according to the volume fraction of design;
The moulding of b, green compact: it is molded that the above-mentioned powder that mixes is carried out palletizing die, and briquetting pressure is 50 300 MPa;
C, sintering: the green compact after the above-mentioned moulding are placed a pyrophillite mould, put into press, apply the pressure of 1-10GPa, pressure is two-way pressurization or six pressurizations; Two ends apply the alternating current of 2-6 kW then, and electrical current is 1000A-3000A, and sintering time is 15 seconds-100 seconds, continue pressurize 30-180 seconds; Sintered body is through grinding and polishing, and relative density is 98-99.9%, can consistent tungsten-steel with design component/iron FGM.
Further, described comminuted steel shot is the 9-12%Cr ferrite---martensite comminuted steel shot.
The invention has the advantages that: can once physical property be differed bigger two kinds of materials such as tungsten/steel (iron) and make FGM, consuming time few, cost is low.By cold moudling, in the residual gas of as far as possible getting rid of in the base substrate, can well control each layer thickness, make it consistent with design component.Adopt hyperpressure down the method for energising sintering prepare tungsten and steel (iron) FGM, apply hyperpressure with the sintering of strengthening functionally gradient material (FGM) and shorten sintering time, avoid contingent combination reaction in sintering process.Applying high alternating current makes the FGM base substrate obtain the sintering temperature that needs by the self-resistance heating.The FGM for preparing has mechanical property and thermal-shock resistance preferably, is suitable for the heat deposition material and high temperature resistant plasma washes away parts, as divertor material in the nuclear fusion device etc.
The invention has the beneficial effects as follows: compare with similarity methods such as hot pressing, method provided by the present invention has basic difference on the sintering effect of sintering parameter, sintering mechanism and acquisition, show as: on the sample institute applied pressure, methods such as hot pressing are the highest can only to reach hundreds of MPa in sintering process.And the present invention at pressure that sintering process applies sample more than the GPa level, promptly usually said hyperpressure; On heating means, methods such as hot pressing, discharge plasma sintering all need to be delivered to sample by the heater heating by modes such as radiation, conduction, make sample obtain uniform temperature, so required heating and sintering time are longer, required sintering temperature is higher.And among the present invention by the sample that has applied hyperpressure directly being passed to big alternating current, make sample obtain sintering, its time only needs the weak point of a few minutes, with method such as hot pressing fundamental difference is arranged on sintering mechanism and effect.By cold moudling, under the prerequisite that densified (being grain growth) do not take place, get rid of the residual gas in the base substrate simultaneously as far as possible, avoid in the base substrate residual gas when carrying out ultra-high pressure sintering owing to applying of hyperpressure has a negative impact.This base substrate of colding pressing is carried out the energising sintering just of the present invention core of hyperpressure under applying.Make and adopt sample density height, the good mechanical performance that the technology of the present invention obtained, and gained gradient composition is consistent with design component.
The specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described further.
The preparation of 1: five layer of ferrotungsten FGM of embodiment.
Being 2 microns tungsten powder and the granularity iron powder that is 50 microns with granularity, (W25%Fe75%, W50%Fe50% W75%Fe25%) mix, and mixed-powder grinds in agate mortar, mixes by the volume ratio of design.Mixed powder is pressed design mix (pure tungsten layer, the W25%Fe75% layer, the W50%Fe50% layer, the W75%Fe25% layer, and pure iron layer) the lamination lamination is packed in the steel grinding tool, compression molding under the 100MPa oil pressure, the base substrate of forming is put into the pyrophillite mould, under the 8GPa high pressure, input power is to carry out sintering under the 3 kW alternating current effects, sintering time is 15 seconds, continue pressurize 30 seconds, the gained sample is behind grinding and polishing, the relative density that records alloy sample all reaches more than 99.34 %, is respectively 292.8 HV from pure iron to each layer of pure tungsten micro-vickers hardness, 457.7 HV, 509.7 HV, 642.9 HV, 729.7 HV.
The preparation of 2: five layers of ferrotungsten FGM of embodiment.
Being 5 microns tungsten powder and the granularity iron powder that is 75 microns with granularity, (W25%Fe75%, W50%Fe50% W75%Fe25%) mix, and mixed-powder grinds in agate mortar, mixes by the volume ratio of design.Mixed powder and pure tungsten powder and straight iron powder are put into the lamination steel grinding tool of packing into by the design mix lamination, compression molding under the 150MPa oil pressure, the base substrate of forming is put into the pyrophillite mould, under 3 GPa high pressure, input power is to carry out sintering under the 4 kW alternating current effects, and sintering time is 50 seconds, continues pressurize 60 seconds, the gained sample is behind grinding and polishing, and the relative density that records alloy sample all reaches more than 98.13 %.
The preparation of 3: six layers of wolfram steel FGM of embodiment.
Being 2 microns tungsten powder and the granularity Cr 9 % ferrite/martensite comminuted steel shots that are 105 microns with granularity mixes by the volume ratio (volume ratio of W is followed successively by 20%, 40%, 60% and 80%) of design, and mixed-powder grinds in agate mortar, mixes.Mixed powder and pure tungsten powder and comminuted steel shot are packed in the steel grinding tool by the design mix lamination, compression molding under the 200MPa oil pressure, the base substrate of forming is put into the pyrophillite mould, under the 9GPa high pressure, input power is to carry out sintering under the 5 kW alternating current effects, and sintering time is 80 seconds, continues pressurize 150 seconds, the gained sample is behind grinding and polishing, and the relative density that records alloy sample all reaches more than 98.81 %.
The preparation of 4: three layers of wolfram steel FGM of embodiment.
Being 8 microns tungsten powder and the granularity 12 %Cr ferrite/martensite comminuted steel shots that are 125 microns with granularity mixes in planetary ball mill by the volume ratio W50%Eurofer50% of design.Pure tungsten powder, tungsten 50% steel 50% powder, clean steel powder lamination are packed in the steel grinding tool, compression molding under the 2500MPa oil pressure, the base substrate of forming is put into the pyrophillite mould, under 6 GPa high pressure, input power is to carry out sintering under the 5 kW alternating current effects, and sintering time is 100 seconds, continues pressurize 180 seconds, the gained sample is behind grinding and polishing, and the relative density that records alloy sample all reaches more than 98.22 %.
Claims (2)
1. the preparation method of tungsten-steel/iron FGM is characterized in that, specifically may further comprise the steps:
The preparation of a, raw material: select the tungsten powder of 1～10 micron of granularity, the granularity of comminuted steel shot/iron powder is 45～150 microns, and above-mentioned tungsten powder and comminuted steel shot/iron powder is evenly mixed according to the volume fraction of design;
The moulding of b, green compact: it is molded that the above-mentioned powder that mixes is carried out palletizing die, and briquetting pressure is 50 300 MPa;
C, sintering: the green compact after the above-mentioned moulding are placed a pyrophillite mould, put into press, apply the pressure of 1-10GPa, pressure is two-way pressurization or six pressurizations; Two ends apply the alternating current of 2-6 kW then, and electrical current is 1000A-3000A, and be 15 seconds-100 seconds conduction time, carries out sintering, behind the sintering of wherein switching on, continue pressurize 30-180 seconds; Sintered body is through grinding and polishing, and relative density is 98-99.9%, can with the corresponding to tungsten-steel of design component/iron FGM.
2. the preparation method of tungsten-steel according to claim 1/iron FGM is characterized in that, described comminuted steel shot is 9-12%Cr ferrite-martensite comminuted steel shot.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102615416A (en) * | 2012-04-17 | 2012-08-01 | 北京科技大学 | Method for preparing fusion reactor plasma facing tungsten module through ultra-high-pressure sintering |
| CN106216674A (en) * | 2016-06-08 | 2016-12-14 | 四川大学 | W V alloy FGM and discharge plasma sintering method thereof |
| CN106825583A (en) * | 2016-12-30 | 2017-06-13 | 中南大学 | A kind of tungsten and low activation stainless steel nanometer gradient composite connecting method |
| CN108039209A (en) * | 2017-11-28 | 2018-05-15 | 中国科学院合肥物质科学研究院 | The divertor monolith type component with gradient adaptation layer for fusion reactor |
| CN109811169A (en) * | 2019-01-18 | 2019-05-28 | 衢州学院 | A kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite |
| CN115194146A (en) * | 2022-07-22 | 2022-10-18 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Functional gradient layer material suitable for fusion reactor tungsten and steel connection |
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| CN1290653C (en) * | 2004-07-01 | 2006-12-20 | 北京科技大学 | Method for preparing tungsten/copper functional gradient material by infiltration - weld method |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1290653C (en) * | 2004-07-01 | 2006-12-20 | 北京科技大学 | Method for preparing tungsten/copper functional gradient material by infiltration - weld method |
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| 《Journal of Materials Processing Technology》 20051231 Z.J.Zhou et al Fabrication of W-Cu composite by resistance sintering under ultra-high pressure 107-111 1-2 , 第168期 * |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102615416A (en) * | 2012-04-17 | 2012-08-01 | 北京科技大学 | Method for preparing fusion reactor plasma facing tungsten module through ultra-high-pressure sintering |
| CN102615416B (en) * | 2012-04-17 | 2014-04-16 | 北京科技大学 | Method for preparing fusion reactor plasma facing tungsten module through ultra-high-pressure sintering |
| CN106216674A (en) * | 2016-06-08 | 2016-12-14 | 四川大学 | W V alloy FGM and discharge plasma sintering method thereof |
| CN106216674B (en) * | 2016-06-08 | 2018-04-24 | 四川大学 | W-V alloys functionally graded material and its discharge plasma sintering method |
| CN106825583A (en) * | 2016-12-30 | 2017-06-13 | 中南大学 | A kind of tungsten and low activation stainless steel nanometer gradient composite connecting method |
| CN108039209A (en) * | 2017-11-28 | 2018-05-15 | 中国科学院合肥物质科学研究院 | The divertor monolith type component with gradient adaptation layer for fusion reactor |
| CN108039209B (en) * | 2017-11-28 | 2020-08-25 | 中国科学院合肥物质科学研究院 | Divertor monolith type component with gradient adaptation layer for fusion reactor |
| CN109811169A (en) * | 2019-01-18 | 2019-05-28 | 衢州学院 | A kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite |
| CN115194146A (en) * | 2022-07-22 | 2022-10-18 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Functional gradient layer material suitable for fusion reactor tungsten and steel connection |
| CN115194146B (en) * | 2022-07-22 | 2023-11-17 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Functionally graded layer material suitable for fusion reactor tungsten and steel connection |
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