CN104726728A - Method for preparing beryllium-vanadium alloy by adopting spark plasma sintering technique - Google Patents
Method for preparing beryllium-vanadium alloy by adopting spark plasma sintering technique Download PDFInfo
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- CN104726728A CN104726728A CN201310717834.XA CN201310717834A CN104726728A CN 104726728 A CN104726728 A CN 104726728A CN 201310717834 A CN201310717834 A CN 201310717834A CN 104726728 A CN104726728 A CN 104726728A
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- sintering
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- vanadium alloy
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Abstract
The invention belongs to a preparation method of beryllium-vanadium alloy and in particular relates to a method for preparing beryllium-vanadium alloy by adopting a spark plasma sintering technique. The method comprises the following steps: firstly, material proportioning; secondly, sintering; and thirdly, polishing. The method for preparing the beryllium-vanadium alloy by adopting the spark plasma sintering technique has the advantages that firstly, sintering time is greatly shortened so that energy source is greatly saved; secondly, due to activation of plasma, low-temperature sintering can be realized, and since sintering temperature is lower than melting points of beryllium and vanadium, growth of crystalline grains is inhibited and the alloy performance is essentially improved; and thirdly, sintering is carried out in a closed environment and therefore beryllium protection pressure is reduced; the prepared beryllium-vanadium alloy can be proved by adopting test means such as X ray diffraction and an electron probe; meanwhile, a scanning electron microscope finds that development of the crystalline grains of surface sintering bodies is comparatively complete, shape is regular, size is consistent, arrangement is tight, overall structure is compact, and distribution is uniform.
Description
Technical field
The invention belongs to a kind of preparation method of beryllium vanadium alloy, be specifically related to a kind of method that discharge plasma sintering technique prepares beryllium vanadium alloy.
Background technology
The raw material of deuterium triton fusion reaction is deuterium (extracting from seawater) and tritium, and need to consume a large amount of tritium in deuterium-tritium reaction, tritium is a kind of radioactive substance, does not have natural tritium on earth, needs to produce tritium by neutron bombardment lithium material.In order to maintain the continual and steady operation of fusion reactor, need to produce in tritium covering at fusion reactor to carry out tritium propagation, with the tritium of supplementary burnup.
Produce tritium covering and be divided into solid-state product tritium covering and liquid product tritium covering with the form of tritium multiplication agent material.In solid-state product tritium covering, in order to increase the probability of neutron bombardment lithium core, need to place neutron-multiplier material multiplication neutrons in solid-state product tritium covering.Due to spherical neutron multiplication agent handling easily, have and to have between larger surface-area, bead that more duct, permeability are good, the diffusion that is conducive to tritium and release, be conducive to alleviating the swelling that neutron irradiation causes.Therefore, neutron multiplication agent material generally adopts spheroidal particle.
Because beryllium has larger reaction cross-section, higher fusing point and reaction threshold is lower, be placed on for multiplication neutrons in covering, namely a neutron and beryllium react and can produce two neutrons.But in the design of the DEMO fusion reactor blanket in future, neutron-multiplier material needs temperature and the neutron high capacity amount of bearing the highest 900 DEG C, produce helium and 50 knocking out damages of about 20000appm.Metallic beryllium bead can not bear such extreme environment, and beryllium alloy has higher fusing point and at high temperature has higher chemical stability, and beryllium alloy bead may become most promising neutron-multiplier material.From the angle of low activation and high beryllium content, beryllium vanadium alloy is a kind of neutron-multiplier material of prioritizing selection.Thus, before employing rotating electrode method prepares beryllium vanadium alloy bead, need preparation to be used as the beryllium vanadium alloy of rotating electrode.
The general sintering time of making method of the prior art is long, and energy dissipation is large, and grain growth degree is high, thus causes alloy property bad.Based on above deficiency, we have employed discharge plasma sintering technique and prepare beryllium vanadium alloy.
Discharge plasma sintering (Spark Plasma Sintering is called for short SPS) technology, because of advantages such as its heat-up rate are fast, sintering time is short, weave construction is controlled, shows wide application prospect in field of material preparation.This technology has been successfully applied to the preparation of the multiple novel materials such as function-graded material, nano material, porous material, metal-base composites, fibre reinforced composites at present.Wherein, preparing in intermetallic compound, due to intermetallic compound brittleness at room temperature and dystectic feature, high-energy and high vacuum system is often needed in preparation process, and utilize SPS technology to prepare intermetallic compound, because effectively make use of intergranular spontaneous heating effect and surface activation, low temperature, Fast Sintering can be realized, so SPS technology prepares a kind of effective ways of inter-metallic compound material.
Summary of the invention
The object of this invention is to provide a kind of method that discharge plasma sintering technique prepares beryllium vanadium alloy, it can overcome the defect of prior art.
The present invention is achieved in that a kind of discharge plasma sintering technique prepares the method for beryllium vanadium alloy, and it comprises the following steps,
Step one: batching;
Step 2: sintering;
Step 3: polishing.
Described step one comprises
Step 1.1: batch mixing
Prepare mutually beryllium vanadium binary alloy according to design requirements, number by weight percentage during configuration, the particle diameter of beryllium powder and vanadium powder is less than 70 μm;
Step 1.2: grinding and charging
Beryllium powder and vanadium powder are put into beveller mixed grinding 30 ~ 60min, then mixed beryllium vanadium alloy powder is inserted in high purity graphite mould, wrap up one deck graphite carbon felt muff at the outside surface of mould, be placed in discharge plasma sintering stove.
Described step 2 comprises
Step 2.1: vacuumize
Vacuumize sintering oven, vacuum tightness at least should reach 10
-2pa, applies the pressure of the axis of 30 ~ 60Mpa to sintering mould;
Step 2.2: add pulse
Keep the constant pressure in step 2.1, and add pulsed voltage, pulsed current is 350 ~ 550A, pulse discharge time 30-50ms, and interval electric discharge in 1 second 1 time, continues 30s;
Step 2.3: pressure sintering
Improve pressure to 50 ~ 60Mpa, start sintering, sintering temperature is 900 ~ 1300 DEG C; During sintering from normal temperature with the ramp of 100 ~ 200 DEG C/min, until reach sintering temperature; 20 ~ 40min is kept in sintering temperature;
Step 2.4: cooling
Stop heating, cancel pressure, be cooled to room temperature with the speed of 100 ~ 200 DEG C/min.
Advantage of the present invention is, (1) reduces sintering time greatly, thus has greatly saved the energy; (2) due to the activation of plasma body, can realize low-temperature sintering, sintering temperature, lower than the fusing point of beryllium, vanadium, so just inhibits growing up of crystal grain, inherently improves the performance of alloy; (3) the present invention sinters in closed environment, reduces the pressure of beryllium protection; The beryllium vanadium alloy prepared with the present invention, with the preparation of the means of testing such as X-ray diffraction, electronic probe proof is beryllium vanadium alloy; The grain development of scanning electron microscope surface sintered compact is fairly perfect, shape matching rule, and in the same size, and closely, structure comparison is fine and close on the whole, distributes more even in arrangement.Show discharge plasma sintering method be can be used for preparing beryllium vanadium alloy one effectively, means efficiently.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail:
Discharge plasma sintering technique prepares a method for beryllium vanadium alloy, and it comprises the following steps:
Step one: batching
Step 1.1: batch mixing
Prepare mutually beryllium vanadium binary alloy according to design requirements, number by weight percentage during configuration, the particle diameter of beryllium powder and vanadium powder is less than 70 μm.
Step 1.2: grinding and charging
Beryllium powder and vanadium powder are put into beveller mixed grinding 30 ~ 60min, then mixed beryllium vanadium alloy powder is inserted in high purity graphite mould, wrap up one deck graphite carbon felt muff at the outside surface of mould, be placed in discharge plasma sintering stove;
Step 2: sintering
Step 2.1: vacuumize
Vacuumize sintering oven, vacuum tightness at least should reach 10
-2pa, to be better than 10
-3pa is best, sintering mould is applied to the pressure of the axis of 30 ~ 60Mpa;
Step 2.2: add pulse
Keep the constant pressure in step 2.1, and add pulsed voltage, pulsed current is 350 ~ 550A, pulse discharge time 30-50ms, and interval electric discharge in 1 second 1 time, continues 30s.
This step produces plasma body, activates, supervene a small amount of heat to particle surface, removes the impurity being overlying on surface;
Step 2.3: pressure sintering
Improve pressure to 50 ~ 60Mpa, start sintering, sintering temperature is 900 ~ 1300 DEG C; During sintering from normal temperature with the ramp of 100 ~ 200 DEG C/min, until reach sintering temperature; 20 ~ 40min is kept in sintering temperature.
Step 2.4: cooling
Stop heating, cancel pressure, be cooled to room temperature with the speed of 100 ~ 200 DEG C/min.
Step 3: polishing
Sample after having sintered is polished, removes the cementation zone on surface.
Provide two examples specifically sintered below:
Example one
Sintering 67.92%Be-32.08%V(weight percent) optimum process condition of powdered material of proportioning is: pulsed current 500A, pulse turn-on time 50ms plasma activation time 30s, pressure is 55Mpa, at 1150 DEG C of sintering 20min, temperature rise rate is 180 DEG C/min, and rate of cooling is 200 DEG C/min.Be after sintering
12the content of V phase is 98.5%, other beryllium vanadium alloys (Be
2v, Be
17v
2) be the content of 0.9%, Be be mutually 0.6%.
Example two
Sintering 60.0%Be-40%V(weight percent) optimum process condition of powdered material of proportioning is: pulsed current 550A, pulse turn-on time 50ms plasma activation time 30s, pressure is 60Mpa, at 1280 DEG C of sintering 30min, temperature rise rate is 180 DEG C/min, and rate of cooling is 200 DEG C/min.Be after sintering
17v
2the content of phase is 98.2%, other beryllium vanadium alloys (Be
2v, Be
12v) be the content of 1.3%, α phase Be be mutually 0.5%.
The present invention is explained in detail above, but the present invention is not limited to above-described embodiment in conjunction with the embodiments, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.The content be not described in detail in the present invention all can adopt prior art.
The discharge plasma sintering method that the application provides has following characteristics: heating, cooling speed is fast, can sinter at a lower temperature; Sintering time is short, and grain-size is little; Plasma discharging, except the feature with hot pressed sintering, can also be heated sample by pulsed current, and sample is sintered very soon.It is generally acknowledged that discharge plasma sintering may exist following several densification approach: (1) intercrystalline electric discharge produces localized hyperthermia, evaporation and fusing is caused at grain surface, and form " neck " at grain contact point, thus directly facilitate the process of densification; (2) under the effect of pulsed current, grain surface easily activates, and various diffusion is all strengthened, thus facilitates the process of densification.In discharge plasma sintering body, each uniform particles ground self-heating makes particle surface activate, thus has very high thermo-efficiency, and sintered compact can be made within the quite short time fine and close.
Claims (3)
1. discharge plasma sintering technique prepares a method for beryllium vanadium alloy, it is characterized in that: it comprises the following steps,
Step one: batching;
Step 2: sintering;
Step 3: polishing.
2. a kind of discharge plasma sintering technique as claimed in claim 1 prepares the method for beryllium vanadium alloy, it is characterized in that: described step one comprises
Step 1.1: batch mixing
Prepare mutually beryllium vanadium binary alloy as requested, number by weight percentage during configuration, the particle diameter of beryllium powder and vanadium powder is less than 70 μm;
Step 1.2: grinding and charging
Beryllium powder and vanadium powder are put into beveller mixed grinding 30 ~ 60min, then mixed beryllium vanadium alloy powder is inserted in high purity graphite mould, wrap up one deck graphite carbon felt muff at the outside surface of mould, be placed in discharge plasma sintering stove.
3. a kind of discharge plasma sintering technique as claimed in claim 1 prepares the method for beryllium vanadium alloy, it is characterized in that: described step 2 comprises
Step 2.1: vacuumize
Vacuumize sintering oven, vacuum tightness at least should reach 10
-2pa, applies the pressure of the axis of 30 ~ 60Mpa to sintering mould;
Step 2.2: add pulse
Keep the constant pressure in step 2.1, and add pulsed voltage, pulsed current is 350 ~ 550A, pulse discharge time 30-50ms, and interval electric discharge in 1 second 1 time, continues 30s;
Step 2.3: pressure sintering
Improve pressure to 50 ~ 60Mpa, start sintering, sintering temperature is 900 ~ 1300 DEG C; During sintering from normal temperature with the ramp of 100 ~ 200 DEG C/min, until reach sintering temperature; 20 ~ 40min is kept in sintering temperature;
Step 2.4: cooling
Stop heating, cancel pressure, be cooled to room temperature with the speed of 100 ~ 200 DEG C/min.
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Cited By (2)
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| CN108486397A (en) * | 2018-04-17 | 2018-09-04 | 中国工程物理研究院材料研究所 | A kind of discharge plasma sintering preparation method of beryllium alumin(i)um alloy |
| CN111570813A (en) * | 2020-05-29 | 2020-08-25 | 西藏智材新材料有限公司 | Beryllium-aluminum alloy powder and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108486397A (en) * | 2018-04-17 | 2018-09-04 | 中国工程物理研究院材料研究所 | A kind of discharge plasma sintering preparation method of beryllium alumin(i)um alloy |
| CN111570813A (en) * | 2020-05-29 | 2020-08-25 | 西藏智材新材料有限公司 | Beryllium-aluminum alloy powder and preparation method and application thereof |
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Application publication date: 20150624 |