CN105154694A - Method for preparing magnetic heat material Mn-Ni-Ge:Fe-based series alloy bar through electric arc melting and copper mold spray casting - Google Patents
Method for preparing magnetic heat material Mn-Ni-Ge:Fe-based series alloy bar through electric arc melting and copper mold spray casting Download PDFInfo
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- CN105154694A CN105154694A CN201510628568.2A CN201510628568A CN105154694A CN 105154694 A CN105154694 A CN 105154694A CN 201510628568 A CN201510628568 A CN 201510628568A CN 105154694 A CN105154694 A CN 105154694A
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Abstract
The invention discloses a method for preparing a magnetic heat material Mn-Ni-Ge:Fe-based series alloy bar through electric arc melting and copper mold spray casting. The method comprises the specific steps that burdening is conducted, wherein the masses of needed metal simple substances of Mn, Ni, Fe, Ge and the like are calculated according to the stoichiometric ratio, and MnNi1 xFexGe and Mn1 xFexNiGe are adopted as the composition proportion; electric arc melting is conducted, wherein the burdened raw materials are put into a water cooling type copper crucible, argon is back charged into the vacuum environment to conduct electric arc melting, and an Mn-Ni-Ge:Fe-based alloy ingot is obtained; copper mold spray casting is conducted, wherein the Mn-Ni-Ge:Fe-based alloy ingot is sheared and loaded into a quarts tube with the inner diameter being 10 mm, the ingot in the quarts tube is melted through a high-frequency induction heating device, a melted sample is sprayed to a copper mold with water cooling through a small hole in the bottom of the quarts tube through nitrogen pressurizing, and the alloy bar is obtained; and heat treatment is conducted, wherein a part of the bar sample is taken and sealed in the quarts tube, annealing heat treatment is conducted in a high-temperature furnace, and a part of the bar sample is put into cold water to be quenched or cooled to the room temperature along with the furnace. The preparing method is simple and convenient to implement and is used for easily preparing bars in regular shapes to serve as magnetic refrigerating materials, and the preparing cost and the energy consumption are reduced.
Description
Technical field
The present invention relates to preparation and the character research thereof of Mn-Ni-Ge:Fe base system row alloy bar material, particularly relate to a kind of method being prepared Novel Room Temperature magneto-caloric material Mn-Ni-Ge:Fe base system row alloy bar material by arc melting and copper mold spray to cast.
Background technology
Magnetic Refrigeration Technique based on magnetothermal effect is efficient with it, environmental protection, energy-conservation, volume is little and the advantage such as reliable is described as the most possible Refrigeration Technique substituting current vapor compression refrigeration, at present, magnetic refrigerating material is just along the future development of room temperature, low field, large Entropy Changes, little magnetic hysteresis, for secondary magnetic phase transition material, although do not have the puzzlement of heat stagnation and magnetic hysteresis, little magnetothermal effect limits it and moves towards practical application; And for primary magnetic phase change material, although there is large magnetothermal effect, inevitably heat stagnation and magnetic hysteresis loss are again the bottlenecks that it further develops.Therefore develop there is large magnetothermal effect and little heat stagnation simultaneously, the magnetic refrigerating material of magnetic hysteresis is the research direction of current magnetothermal effect.Wherein room-temperature zone magnetic Refrigeration Technique especially in national economy and the major areas such as scientific research, national defence in occupation of very important status, therefore become focus that countries in the world scientist falls over each other to study and the emphasis that national governments competitively pay close attention to.And the gordian technique of room-temperature zone magnetic refrigeration finds the magnetic refrigeration techniques of excellent performance, this working medium requires to have large magnetothermal effect and little heat stagnation, magnetic hysteresis, to reduce magnetic hysteresis loss.Mn-Ni-Ge:Fe base series alloy is the room-temperature zone magnetic refrigerating material with certain development potentiality of recent researches, but find to there is following problem at the Mn-Ni-Ge:Fe base system row alloy sample ground at present according to existing result of study: (1) current research concentrates on block and strip mostly, and also rarely has report about the research of bar; (2) for the single-phase sample that will obtain homogeneous block, required annealing time length very, usually need the annealing time of 4-5 days to become phase, cost adds greatly.Bar has lived through a quenching process relative to block, and therefore do not need annealing process for a long time just can become phase, the time of required annealing substantially reduces, and has saved the energy, and cost is easy to control, and is conducive to practical application.
Summary of the invention
The object of the present invention is to provide a kind of method being prepared magneto-caloric material Mn-Ni-Ge:Fe base system row alloy bar material by arc melting and copper mold spray to cast, it has high-efficiency environment friendly, less energy-consumption and the advantage such as simple and convenient.
The present invention is achieved like this, and is prepared the method for magneto-caloric material Mn-Ni-Ge:Fe base system row alloy bar material by arc melting and copper mold spray to cast, it is characterized in that method steps is:
(1) prepare burden: stoichiometrically calculate required Mn, Ni, Fe, Ge and etc. the quality of metal simple-substance, the proportioning 3at.% more than the amount of calculating of its Mn; Composition proportion adopts MnNi
1-
x fe
x ge and Mn
1-
x fe
x niGe, wherein
xlimited range is to MnNi
1-
x fe
x ge is 0.12<
x<0.21; To Mn
1-
x fe
x niGe is 0.04<
x<0.10;
(2) arc melting: the copper crucible raw material prepared being put into water-cooled electric arc furnace, is then evacuated to 10 by vacuum tightness
-4below Pa, recharging purity is carry out arc melting after 99.999% argon gas reaches 0.9 normal atmosphere, repeats 3-4 time, obtains more uniform Mn-Ni-Ge:Fe base alloy cast ingot;
(3) copper mold spray to cast: the zone of oxidation polishing off melted Mn-Ni-Ge:Fe base alloy cast ingot surface, shreds, then put into the silica tube of internal diameter 10mm, vacuum tightness in furnace chamber is evacuated to 10
-4pa, recharge again into purity be 99.999% argon gas to 1 normal atmosphere, by HF induction heating apparatus by ingot melting, the aperture then making fusing sample be about 0.1-0.2mm by diameter by nitrogen pressurization is sprayed onto on the copper mold with water-cooled, thus obtain bar, sample diameter 2-6mm;
(4) homogenizing thermal treatment: Bar samples is got its part and put into the internal diameter 10mm silica tube closed one end, vacuum tightness is evacuated to below 4Pa, be filled with 0.5 atmospheric argon gas and be used for gas washing, repetitive operation 3-5 time, then rapidly elongated silica tube is blown with acetylene flame, Bar samples is enclosed in the silica tube after vacuumizing; Then the sample sealed is put into High Temperature Furnaces Heating Apparatus and carry out annealing thermal treatment, annealing temperature is set in 600 DEG C-900 DEG C according to concrete composition, time setting 24h-100h, then take out and put into rapidly cold quenching-in water or be cooled to room temperature with stove, namely obtain desirable Mn-Ni-Ge:Fe base system row alloy bar material.
In step (one) described batching each metal simple-substance calculate according to stechiometry needed for quality be generally accurate to 0.1mg, the purity of each metal simple-substance is all more than 99.99%.For volatile metal, such as Mn, generally can increase its quality to reduce the loss in its fusion process, generally will consider to add 3at.% for Mn-Ni-Ge:Fe base system row alloy sample more.Composition proportion adopts MnNi
1-
x fe
x ge and Mn
1-
x fe
x niGe, wherein
xlimited range is to MnNi
1-
x fe
x ge is 0.12<
x<0.21; To Mn
1-
x fe
x niGe is 0.04<
x<0.10; Also to consider to add different substitute element, such as Cr, Si etc. for different compositions.
Step (two) described arc melting is that the metal just prepared puts into the clean copper crucible of polishing, and vacuum tightness is evacuated to 10
-4below Pa, recharge into 0.9 atmospheric high-purity Ar gas (99.999%), the step of arc melting is: starting working chamber is first from Zr, its objective is and absorbs remnant oxygen in furnace chamber.For Mn-Ni-Ge:Fe base system row alloy sample, during first time melting, with 20A electric current by melting of metal, see that crucible inner metal liquid flows, cooling is taken out, by the bulk sample turn-over of first time melting, high current to 25 ~ 30A melting the 2nd time, then turn-over melts and can obtain Mn-Ni-Ge:Fe base system row alloy cast ingot for 2-3 time.
Step (three) described copper mold spray to cast is the zone of oxidation melted ingot casting sample being polished off surface, shreds the silica tube then putting into 10mm internal diameter, furnace chamber vacuum tightness is evacuated to 10
-4pa, be filled with 1 atmospheric high-purity argon gas, open high-frequency induction heating power, the method of high-frequency induction heating is, first use 10A current preheating 15-20s, if then 30-35A again preheating 15-20s see that in silica tube, ingot casting reddens slightly, then electric current is adjusted to 40-45A heat rapidly make ingot melting, until see that fusing solution is in bright white light.
The described homogenizing thermal treatment of step (four) Bar samples obtained is got its part to put into the internal diameter 10mm silica tube closed one end, vacuum tightness is evacuated to below 4Pa, be filled with about 0.5 normal atmosphere argon gas and be used for gas washing, repeat 3-5 time, then rapidly elongated silica tube is blown with acetylene flame, Bar samples is enclosed in the silica tube after vacuumizing.Then the sample sealed is put into High Temperature Furnaces Heating Apparatus and carry out annealing thermal treatment, annealing temperature is set in 600 DEG C-900 DEG C, and then time 24-100h takes out and put into rapidly cold quenching-in water.
Technique effect of the present invention is: preparation method of the present invention is simple to operation, annealing heat treatment time can be reduced, reduce energy consumption, the pollution to air is decreased relative to conventional refrigeration mode, reduce preparation cost, be applicable to suitability for industrialized production, the present invention can obtain the magnetic property of Mn-Ni-Ge:Fe base system row alloy bar material sample excellence, Bar samples prepared by the present invention has violent magnetization change, first-order phase transition is obvious, reduce relative to block sample heat stagnation and magnetic hysteresis, can be used as magneto-caloric material, also can as other magnetic functional materialss through exploring.
Accompanying drawing explanation
Fig. 1 MnNi
0.85fe
0.15the M-T curve of Ge diameter 2mm annealing 24h bar;
Fig. 2 MnNi
0.85fe
0.15the dM/dT-T curve of Ge diameter 2mm annealing 24h bar;
Fig. 3 MnNi
0.85fe
0.15the M-H curve of Ge diameter 2mm annealing 24h bar;
Fig. 4 MnNi
0.85fe
0.15the isothermal magnetic entropy varied curve of Ge diameter 2mm annealing 24h bar.
Embodiment
Embodiment one:
(1) prepare burden: the quality stoichiometrically calculating the metal simple-substances such as required Mn, Ni, Ge, Fe is prepared burden, and is generally accurate to 0.1mg, and the purity of metal simple-substance is all more than 99.99%.For volatile metal, such as Mn, general its quality that increases, to make up the loss in fusion process, generally will be considered to add 3at.% for Mn-Ni-Ge:Fe base system row alloy sample more.Composition proportion adopts MnNi
1-
x fe
x ge and Mn
1-
x fe
x niGe, wherein
xlimited range is to MnNi
1-
x fe
x ge is 0.12<
x<0.21; To Mn
1-
x fe
x niGe is 0.04<
x<0.10;
(2) arc melting: the raw material prepared is put into water-cooled copper crucible electric arc furnace, vacuum tightness is evacuated to 10
-4below Pa, the argon gas that to recharge into purity be 99.999% reaches 0.9 normal atmosphere, then arc melting is carried out, during first time melting, with 20A electric current by melting of metal, see that crucible inner metal liquid flows, cooling is taken out, by the bulk sample turn-over of first time melting, high current to 25 a little ~ 30A melting 2-3 time again, can obtain Mn-Ni-Ge:Fe base system row alloy cast ingot;
(3) copper mold spray to cast: the zone of oxidation of melted ingot casting sample surfaces polished off, puts into the silica tube that internal diameter is 10mm after being shredded by the Mn-Ni-Ge:Fe base system row alloy cast ingot good through arc melting, vacuum tightness in furnace chamber is evacuated to 10
-4pa, the argon gas that to recharge into purity be again 99.999% reaches 1 normal atmosphere, by HF induction heating apparatus by ingot melting, then makes fusing sample be sprayed onto on the copper mold with water-cooled by the aperture that diameter is 0.1-0.2mm by nitrogen pressurization, thus obtain bar, Bar samples diameter 2-6mm; When opening high-frequency induction heating power, first use 15A current preheating 15-20s, if then 30-35A again preheating 15-20s see that in silica tube, ingot casting reddens slightly, then electric current is adjusted to 40-45A heat rapidly make ingot melting, until see that fusing solution is in bright white light;
(4) homogenizing thermal treatment: the Bar samples obtained is got its part and put into the internal diameter 10mm silica tube closed one end, vacuum tightness is evacuated to below 4Pa, be filled with 0.5 normal atmosphere argon gas and be used for gas washing, repeat 3-5 time, then rapidly elongated silica tube is blown with acetylene flame, Bar samples is enclosed in the silica tube after vacuumizing; Then the sample sealed is put into High Temperature Furnaces Heating Apparatus and carry out annealing thermal treatment, annealing temperature is set in 800 DEG C, and the time is 24h and 100h, then takes out and puts into rapidly cold quenching-in water, namely obtains desirable Mn-Ni-Ge:Fe base system row alloy bar material.MnNi can be seen by Fig. 1
0.82fe
0.18ge Bar samples has the change of the larger specific magnetising moment, and along with heat stagnation; Its transformation temperature is at 269K, close to room temperature to have Fig. 2 to see; Can be seen by Fig. 3, MnNi
0.82fe
0.18there is magnetic hysteresis in Ge Bar samples, phase transformation simultaneously more violent hardly; There is Fig. 4 to find out and can obtain 6.88Jkg under the variation magnetic field of 0-2.2T
-1k
-1magnetic entropy become, have lower preparation cost simultaneously.
Present embodiment preparation method is simple to operation, because this kind of method have passed through the process of a chilling, greatly reduces the time needed for anneal, reduce cost of manufacture, decrease energy consumption, be applicable to suitability for industrialized production, can be used as magnetic functional materials, especially magnetic refrigerating material.
Embodiment two: the difference of present embodiment and embodiment one is that step () is prepared burden according to fame composition Mn
1-xcr
xniGe(x=0.07,0.08,0.09,0.10) to carry out, the purity of each metallic element is all higher than 99.99%; Step (three) nitrogen pressurization is 0.2MPa, and being ejected into diameter is respectively in the cylindrical hole of 2-6mm, and in step (four), annealing temperature is 800 DEG C, and the time is respectively 24h and 100h.Other step and selected parameter identical with embodiment one.Result obtains the Bar samples that magnetic property well has primary magnetic phase change, has the magnetothermal effect than bigger numerical.
Embodiment three: the difference of present embodiment and embodiment one is that step () is prepared burden according to fame composition Mn
1-xco
xniGe(x=0.06,0.07,0.08,0.09,0.10) to carry out, the purity of each metallic element is all higher than 99.99%; Step (three) nitrogen pressurization is 0.2MPa, and being ejected into diameter is respectively in the cylindrical hole of 2-6mm, and in step (four), annealing temperature is 800 DEG C, and the time is respectively 24h and 100h.Other step and selected parameter identical with embodiment one.Result obtains the Bar samples that magnetic property well has primary magnetic phase change, has the magnetothermal effect than bigger numerical.
Although introduce and describe the specific embodiment of the present invention, but the present invention is not limited thereto, but specific implementation can also be carried out in other modes be in the scope of the technical scheme defined in claims, make corresponding Bar samples by modifying ingredients, obtain desirable primary magnetic phase change and corresponding magnetic thermal properties thereof.
Claims (4)
1. prepared a method for magneto-caloric material Mn-Ni-Ge:Fe base system row alloy bar material by arc melting and copper mold spray to cast, said method comprising the steps of:
(1) prepare burden: the quality stoichiometrically calculating the metal simple-substances such as required Mn, Ni, Fe, Ge, the proportioning 3at.% more than the amount calculated of its Mn; Composition proportion adopts MnNi
1-
x fe
x ge and Mn
1-
x fe
x niGe, wherein
xlimited range is to MnNi
1-
x fe
x ge is 0.12<
x<0.21; To Mn
1-
x fe
x niGe is 0.04<
x<0.10;
(2) arc melting: the copper crucible raw material prepared being put into water-cooled electric arc furnace, is then evacuated to 10 by vacuum tightness
-4below Pa, recharging purity is carry out arc melting after 99.999% argon gas reaches 0.9 normal atmosphere, repeats 3-4 time, obtains more uniform Mn-Ni-Ge:Fe base alloy cast ingot;
(3) copper mold spray to cast: the zone of oxidation polishing off melted Mn-Ni-Ge:Fe base alloy cast ingot surface, shreds, then put into the silica tube of internal diameter 10mm, vacuum tightness in furnace chamber is evacuated to 10
-4pa, recharge again into purity be 99.999% argon gas to 1 normal atmosphere, by HF induction heating apparatus by ingot melting, the aperture then making fusing sample be about 0.1-0.2mm by diameter by nitrogen pressurization is sprayed onto on the copper mold with water-cooled, thus obtain bar, sample diameter 2-6mm;
(4) homogenizing thermal treatment: Bar samples is got its part and put into the internal diameter 10mm silica tube closed one end, vacuum tightness is evacuated to below 4Pa, be filled with 0.5 atmospheric argon gas and be used for gas washing, repetitive operation 3-5 time, then rapidly elongated silica tube is blown with acetylene flame, Bar samples is enclosed in the silica tube after vacuumizing; Then the sample sealed is put into High Temperature Furnaces Heating Apparatus and carry out annealing thermal treatment, annealing temperature is set in 600 DEG C-900 DEG C according to concrete composition, time setting 24h-100h, then take out and put into rapidly cold quenching-in water or be cooled to room temperature with stove, namely obtain desirable Mn-Ni-Ge:Fe base system row alloy bar material.
2. a kind of arc melting as claimed in claim 1 and copper mold spray to cast prepare the method for Mn-Ni-Ge:Fe base system row alloy bar material, it is characterized in that, the purity of described Mn, Ni, Ge and Fe is all more than 99.99%.
3. a kind of method being prepared magneto-caloric material Mn-Ni-Ge:Fe base system row alloy bar material by arc melting and copper mold spray to cast as claimed in claim 1, it is characterized in that, the step of described arc melting is: first from Zr, during first time melting, with 20A electric current by melting of metal, see that crucible inner metal liquid flows, cooling is taken out, by the bulk sample turn-over of first time melting, high current to 25 ~ 30A melting the 2nd time, then turn-over melts and can obtain Mn-Ni-Ge:Fe base system row alloy cast ingot for 2-3 time.
4. a kind of arc melting as claimed in claim 1 and copper mold spray to cast prepare the method for Mn-Ni-Fe-Ge base alloy bar material, it is characterized in that, the method of described high-frequency induction heating first uses 15A current preheating 15-20s, if then 30-35A again preheating 15-20s see that in silica tube, ingot casting reddens slightly, then electric current is adjusted to 40-45A heat rapidly make ingot melting, until see that fusing solution is in bright white light.
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|---|---|---|---|
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|---|---|---|---|---|
| CN106546458A (en) * | 2016-10-14 | 2017-03-29 | 江西理工大学 | A kind of method of observation MnNiGe based alloy martensite variants |
| CN107164681A (en) * | 2017-06-01 | 2017-09-15 | 江西理工大学 | A kind of method that induced by magnetic field metamagnetism martensitic traoformation is realized in MnCoGe based alloys |
| CN108300882A (en) * | 2018-02-11 | 2018-07-20 | 江西理工大学 | The method that magnetic structure coupling phase transformation is realized in MnCoGe based alloys |
| CN108300881A (en) * | 2018-02-08 | 2018-07-20 | 江西理工大学 | A method of realizing the huge negative expansion of wide warm area in MnCoGe based alloys |
| CN108486449A (en) * | 2018-03-23 | 2018-09-04 | 南京理工大学 | A kind of MnNiGe base magnetic phase transition alloys that low-heat is stagnant |
| CN111655871A (en) * | 2017-12-22 | 2020-09-11 | 山特维克知识产权股份有限公司 | Process for refining nitrogen-containing metal alloy |
| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
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| CN106546458A (en) * | 2016-10-14 | 2017-03-29 | 江西理工大学 | A kind of method of observation MnNiGe based alloy martensite variants |
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| CN108300881A (en) * | 2018-02-08 | 2018-07-20 | 江西理工大学 | A method of realizing the huge negative expansion of wide warm area in MnCoGe based alloys |
| CN108300882A (en) * | 2018-02-11 | 2018-07-20 | 江西理工大学 | The method that magnetic structure coupling phase transformation is realized in MnCoGe based alloys |
| CN108486449A (en) * | 2018-03-23 | 2018-09-04 | 南京理工大学 | A kind of MnNiGe base magnetic phase transition alloys that low-heat is stagnant |
| CN108486449B (en) * | 2018-03-23 | 2020-06-26 | 南京理工大学 | Low-thermal-hysteresis MnNiGe-based magnetic phase change alloy |
| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN112885549B (en) * | 2021-01-08 | 2022-09-20 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN114905183A (en) * | 2022-05-11 | 2022-08-16 | 湘潭大学 | Bi-Ag-Zn lead-free solder and preparation method and application thereof |
| CN114905183B (en) * | 2022-05-11 | 2024-04-09 | 湘潭大学 | Bi-Ag-Zn lead-free solder and preparation method and application thereof |
| CN115652118A (en) * | 2022-11-10 | 2023-01-31 | 湘潭大学 | High-strength degradable Fe-Se alloy material and preparation method and application thereof |
| CN115652118B (en) * | 2022-11-10 | 2023-09-15 | 湘潭大学 | High-strength degradable Fe-Se alloy material and preparation method and application thereof |
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