CN105448443A - Preparation method of bonding martensitic phase change material - Google Patents

Preparation method of bonding martensitic phase change material Download PDF

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Publication number
CN105448443A
CN105448443A CN201510844896.6A CN201510844896A CN105448443A CN 105448443 A CN105448443 A CN 105448443A CN 201510844896 A CN201510844896 A CN 201510844896A CN 105448443 A CN105448443 A CN 105448443A
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preparation
martensitic transformation
powder
transformation materials
binding agent
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张虎
李亚伟
吴美玲
陶坤
王一旭
周厚博
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/012—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials adapted for magnetic entropy change by magnetocaloric effect, e.g. used as magnetic refrigerating material
    • H01F1/015—Metals or alloys
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention provides a preparation method of a bonding martensitic phase change material, and belongs to the field of metal materials. A martensitic phase change material is crushed into powder with a certain size and is mixed with a binder and a curing agent evenly; the mixture is pressed into required size and shape and then is cured at a certain curing temperature for a certain period of time; and the bonding martensitic phase change material is finally obtained. Compared with a traditional martensitic phase change material, the bonding martensitic phase change material prepared by the method has relatively high mechanical property; the bonding material with arbitrary shape and size can be fabricated according to the actual requirements; meanwhile, the bonding martensitic phase change material prepared by the preparation method provided by the invention has a good magnetothermal effect and can be well applied to manufacturing of refrigerating materials; furthermore, the preparation method provided by the invention is simple in technology and easy to operate; industrial production is easy to achieve; the required binder is wide and low in price; and practical application of the preparation technology is facilitated.

Description

A kind of preparation method of the Martensitic Transformation Materials that bonds
Technical field
The invention belongs to metal material field, relate to a kind of preparation method of the Martensitic Transformation Materials that bonds, for the manufacture of refrigerating material.
Background technology
Martensitic traoformation is defined as: replace atom through without diffusion displacement (all even differential deformation), the phase transformation producing alteration of form and surface relief, one-level in lnvariant-plane Strain feature, forming core-type of growing up thus.Usually, there is martensite positive and be deformed into martensitic phase in Martensitic Transformation Materials, and reverse transformation formation parent phase occurs when heating when cooling.Martensitic Transformation Materials in the strengthening of steel, material malleableize, reduce there are many application in quenching distortion, shape memory effect, super-elasticity and pseudoelasticity etc., be good functional material.
Because the structure of martensitic phase and parent phase exists very big-difference, often along with violent changes in crystal structure in Martensitic Transformation, this effect is used in marmem, namely the material with certain shape from higher than martensitic transformation temperature (T m) High-temperature cooling, make it to form low-temperature martensite phase, load deflection in this case, then, by material warms to martensite Reverse Martensitic Transformation Temperatures (T a) more than, material returns to again original shape.
Traditional marmem controls its deformation primarily of temperature and STRESS VARIATION, and this causes its response frequency low, and sensitivity enhancement is difficult.By comparison, novel ferromagnetic shape memory alloys (FerromagneticShapeMemoryAlloys, FSMAs) is the class shape memory alloy material having ferromagnetism and thermoelastic martensitic transformation concurrently.Except temperature field and stress field, the martensitic traoformation of this material can also be regulated and controled by magnetic field, make us that best external influence field coupling condition can be selected to go to impel a certain performance of material more outstanding, thus make the application function of material stronger, range of application is wider.
At present, a class maximum in ferromagnetic shape memory alloys is Heusler alloy, comprises Ni-Mn-Ga, Ni-Mn-Al, Ni-Mn-In, Ni-Mn-Sn etc.Recently, researcher finds to have hexagonal Ni 2the ternary alloy three-partalloy of In type structure, as MnCoGe, MnNiGe etc., also the magnetic structure coupling martensitic traoformation of induced by magnetic field is shown, along with huge changes in crystal structure and magneto-caloric effect in phase transition process, and its phase transition temperature can regulate in very wide warm area, is considered to ferromagnetic shape memory alloys of new generation and magnetic refrigerating material.
But, no matter be Ni-Mn-Ga series Hesuler alloy or Ni of new generation 2the Martensitic Transformation Materials of In type structure, due to the huge Crystal Structure Distortion in Martensitic Transformation, all can cause fragmentation after such material phase transformation, cannot carry out shaping and machining, significantly limit the application of this kind of Martensitic Transformation Materials.And at present also report is rarely had to the research improving this kind of material mechanical performance.
In view of above research background and Martensitic Transformation Materials key issue urgently to be resolved hurrily, how processing machinery Martensitic Transformation Materials of good performance has become the emphasis instantly studied, the present invention proposes a kind of preparation method of the Martensitic Transformation Materials that bonds, the martensitic material having good mechanical properties and martensitic phase change nature concurrently can be prepared, and show good magnetic refrigeration performance, magnetic refrigerating field can be applied it to.
Summary of the invention
Therefore, the object of the invention is the preparation method providing a kind of Martensitic Transformation Materials that bonds, and the bonding Martensitic Transformation Materials obtained according to preparation method provided by the invention, for the manufacture of refrigerating material.
The object of the invention is to be achieved through the following technical solutions:
On the one hand, the invention provides a kind of preparation method of the Martensitic Transformation Materials that bonds, its concrete preparation method comprises the following steps:
1) Martensitic Transformation Materials is broken into the powder of certain size;
2) by step 1) in the Martensitic Transformation Materials powder prepared mix with binding agent, curing agent;
3) by step 2) in the mixed powder compaction size and dimension that becomes to need.
4) by step 3) in the moulding material prepared under certain curing temperature, solidify certain hour, finally obtain bonding Martensitic Transformation Materials.
According to preparation method provided by the invention, preferably, step 1) can comprise particularly: Martensitic Transformation Materials is broken by one or more in the modes such as grinding, vibration milling, rolling mill, ball milling or airflow milling, and by being greater than 10 object standard screens, be preferably 100 ~ 150 orders; Filter out the powder being less than 2mm, be preferably 0 ~ 0.5mm.
Further, according to preparation method provided by the invention, described step 2) can comprise particularly: by step 1) in the Martensitic Transformation Materials powder prepared mix with binding agent, curing agent; Described binding agent can be various binding agents conventional in prior art, such as, one or more in epoxy resin, phenolic resins, Merlon, polyethylene naphthoic acid fat, polyethylene terephthalate, polyimides, polyamide, Kynoar, polystyrene, polybutene, polyvinyl chloride, polyethylene etc. can be selected from, preferably, one or both in epoxide-resin glue and polyimides glue are selected from for the binding agent in the present invention; Described curing agent is the macromolecular material matched with selected binding agent, preferably, is phenolic aldehyde amine for the curing agent in the present invention; Described curing agent presses volume ratio and the binding agent mixing of 5-50%, is preferably 10 ~ 30%; Then be that 0.5 ~ 20wt.% adds in Martensitic Transformation Materials powder by mixed curing agent and binding agent by interpolation mass ratio, be preferably 1 ~ 10wt.%.
Further, according to preparation method provided by the invention, described step 3) can comprise particularly: by step 2) in mixed powder be pressed into the size and dimension of needs by rolling process, die pressing, extrusion, powder injection forming or discharge plasma sintering process, pressure is 300 ~ 1500MPa, is preferably 600 ~ 1000MPa; Press temperature is 0 ~ 900 DEG C, is preferably 0 ~ 300 DEG C; Press time is 5 ~ 240 minutes, is preferably 10 ~ 120 minutes.
Further, according to preparation method provided by the invention, in step 4) in, described curing temperature can be 0 ~ 500 DEG C, is preferably 0 ~ 150 DEG C; Described curing time can be 1 ~ 10 day, is preferably 3 ~ 7 days.
The bonding Martensitic Transformation Materials obtained according to preparation method provided by the invention is for the manufacture of refrigerating material.
Compared with prior art, advantage of the present invention is: the bonding Martensitic Transformation Materials 1) utilizing preparation method provided by the invention to prepare has the mechanical performance higher than conventional martensitic phase-change material; 2) preparation method provided by the invention is utilized can to make the binding material of arbitrary shape and size according to actual needs; 3) the bonding Martensitic Transformation Materials utilizing preparation method provided by the invention to prepare has good magneto-caloric effect, can be good at being applied to manufacturing refrigerating material aspect; 4) preparation method's technique provided by the invention is simple, and be easy to operation and realize suitability for industrialized production, required binding agent is extensive and cheap, and to practical application, this preparation method has great importance.
Accompanying drawing explanation
Below, describe embodiments of the invention in detail by reference to the accompanying drawings, wherein:
Fig. 1 is the bonding Mn that embodiment 1 obtains 0.6fe 0.4niSi 0.5ge 0.5the load-deformation curve of Martensitic Transformation Materials;
Fig. 2 is the Mn that embodiment 1 obtains 0.6fe 0.4niSi 0.5ge 0.5martensitic Transformation Materials under different magnetic field Δ S to the dependence of temperature;
Fig. 3 is the Ni that embodiment 2 obtains 50mn 34co 2sn 14martensitic Transformation Materials under different magnetic field Δ S to the dependence of temperature.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, the embodiment provided only in order to illustrate the present invention, instead of in order to limit the scope of the invention.
Embodiment 1: preparation bonding Mn 0.6fe 0.4niSi 0.5ge 0.5martensitic Transformation Materials and uses thereof
1, preparation method
1) by Mn 0.6fe 0.4niSi 0.5ge 0.5the chemical formula preparation raw material of Martensitic Transformation Materials, raw material is purity higher than the commercial metals Mn of 99.9wt.%, Fe, Ni, Si, Ge.By arc process, above raw material is smelted into ingot casting, then ingot casting being sealed in vacuum degree is 5 × 10 -3in the quartz ampoule of Pa, at 850 DEG C of annealing in process 5-7 days.Utilize agate mortar by the material fragmentation after annealing, and filtered out the irregular particle powder being less than 0.1mm by 150 object standard screens.
2) in step 1) Mn for preparing 0.6fe 0.4niSi 0.5ge 0.5the binding agent (this binding agent is curing agent phenolic aldehyde amine T-31 by the volume ratio of 20%:80% and epoxy resin E-51 mixing gained) of 3wt.% is added in Martensitic Transformation Materials powder;
3) by step 2) powder and binding agent mix after within 60 minutes, to obtain the cylindrical bonding Mn of Φ 10mm × 10mm in the press temperature of 170 DEG C and 900MPa pressure system 0.6fe 0.4niSi 0.5ge 0.5martensitic traoformation moulding material;
4) by step 3) in the bonding Mn for preparing 0.6fe 0.4niSi 0.5ge 0.5martensitic traoformation moulding material solidifies 3 days at 20 DEG C, the final bonding Mn obtaining satisfactory mechanical property 0.6fe 0.4niSi 0.5ge 0.5martensitic traoformation moulding material.
2, product characterizes and performance measurement
WDW200D type microcomputer control universal testing machine measures bonding Mn 0.6fe 0.4niSi 0.5ge 0.5the load-deformation curve of Martensitic Transformation Materials, as shown in Figure 1, this bonding Mn 0.6fe 0.4niSi 0.5ge 0.5the compression strength of Martensitic Transformation Materials is 91MPa, and corresponding strain is 8.7%.
VersalabFree measures Mn 0.6fe 0.4niSi 0.5ge 0.5the isothermal magnetization curve (M-H curve) of Martensitic Transformation Materials, then according to Maxwell relation: Δ S can be become from isothermal magnetization curve calculation magnetic entropy.Fig. 2 shows Mn 0.6fe 0.4niSi 0.5ge 0.5Δ S is to the dependence of temperature under different magnetic field for Martensitic Transformation Materials, and can find out, sample is at phase transition temperature T coccur the maximum that magnetic entropy becomes near=297K, under changes of magnetic field is respectively 0-1T, 0-2T, 0-3T, the maximum magnetic entropy variable of sample is respectively 5.2J/kgK, 11.4J/kgK, 17.5J/kgK.At present, utilize permanent magnet NdFeB can obtain the magnetic field of 2T, therefore the magnetic entropy zoom of material under 0-2T changes of magnetic field is concerned.Can find out, under 0-2T changes of magnetic field, Mn 0.6fe 0.4niSi 0.5ge 0.5the maximum magnetic entropy variable (11.4J/kgK) of Martensitic Transformation Materials is significantly higher than magnetic entropy change (under 2T magnetic field, magnetic entropy becomes 5.0J/kgK) of conventional chamber temperature magnetic refrigerating material Gd, and the bonding Mn that embodiment 1 is obtained is described 0.6fe 0.4niSi 0.5ge 0.5martensitic Transformation Materials is more excellent room temperature magnetic refrigerating material.
Embodiment 2: preparation bonding Ni 50mn 34co 2sn 14martensitic Transformation Materials and uses thereof
1, preparation method
1) by Ni 50mn 34co 2sn 14the chemical formula preparation raw material of Martensitic Transformation Materials, raw material is purity higher than the commercial metals Ni of 99.9wt.%, Mn, Co, Sn.By arc process, above raw material is smelted into ingot casting, then ingot casting being sealed in vacuum degree is 5 × 10 -3in the quartz ampoule of Pa, at 900 DEG C of annealing in process 4-7 days.Utilize ball mill by the material fragmentation after annealing, and filtered out the irregular particle powder being less than 0.1mm by 150 object standard screens.
2) in step 1) Ni for preparing 50mn 34co 2sn 14add in Martensitic Transformation Materials powder 5wt.% binding agent (this binding agent be curing agent phenolic aldehyde amine T-31, epoxy resin E-44, polyimides glue P-32 by 30%:60%:10% volume ratio mixing gained);
3) by step 2) powder and binding agent mix after within 50 minutes, to obtain the disc bonding Ni of Φ 10mm × 0.7mm in the press temperature of 30 DEG C and 1100MPa pressure system 50mn 34co 2sn 14martensitic traoformation moulding material;
4) by step 3) in the bonding Ni for preparing 50mn 34co 2sn 14martensitic traoformation moulding material solidifies 7 days at 100 DEG C, the final Ni obtaining satisfactory mechanical property 50mn 34co 2sn 14martensitic traoformation moulding material.
2, product characterizes and performance measurement
VersalabFree measures Ni 50mn 34co 2sn 14the isothermal magnetization curve (M-H curve) of Martensitic Transformation Materials, then according to Maxwell relation: Δ S can be become from isothermal magnetization curve calculation magnetic entropy.Fig. 3 shows Ni 50mn 34co 2sn 14Δ S is to the dependence of temperature under different magnetic field for Martensitic Transformation Materials, and can find out, sample is at phase transition temperature T cthere is the maximum that magnetic entropy becomes near=278K, changes of magnetic field be respectively 0-1T, 0-2T, 0-3T, 0-4T, 0-5T, under, the maximum magnetic entropy variable of sample is respectively 11.5J/kgK, 22.9J/kgK, 33.9J/kgK, 44.3J/kgK, 48.8J/kgK.At present, utilize permanent magnet NdFeB can obtain the magnetic field of 2T, therefore the magnetic entropy zoom of material under 0-2T changes of magnetic field is concerned.Can find out, under 0-2T changes of magnetic field, the Ni that embodiment 2 is obtained 50mn 34co 2sn 14the maximum magnetic entropy variable (22.9J/kgK) of Martensitic Transformation Materials is significantly higher than magnetic entropy change (under 2T magnetic field, magnetic entropy becomes 5.0J/kgK) of conventional chamber temperature magnetic refrigerating material Gd, and the bonding Ni that embodiment 2 is obtained is described 50mn 34co 2sn 14martensitic Transformation Materials is more excellent room temperature magnetic refrigerating material.
Comparative example 1: the magneto-caloric effect of rare metal Gd
The rare metal Gd of the room temperature magnetic refrigerating material 99.9wt% of we selected typical as a comparison case.It is 293K that VersalabFree records its Curie temperature, under 0-2T changes of magnetic field, becomes 5.0J/kgK at the magnetic entropy at Curie temperature place.Easy discovery, the Mn in above embodiment 0.6fe 0.4niSi 0.5ge 0.5and Ni 50mn 34co 2sn 14the magnetic entropy of Martensitic Transformation Materials becomes significantly more than Gd, and the bonding Mn that preparation method provided by the invention prepares is described 0.6fe 0.4niSi 0.5ge 0.5and Ni 50mn 34co 2sn 14martensitic Transformation Materials has larger magneto-caloric effect.
Below describe in detail the present invention with reference to embodiment, to those skilled in the art, should be understood that, above-mentioned embodiment should not be understood to limit scope of the present invention.Therefore, various changes and improvements can made to embodiment of the present invention without departing from the spirit and scope of the present invention.

Claims (9)

1. a preparation method for the Martensitic Transformation Materials that bonds, is characterized in that concrete preparation process is as follows:
1) Martensitic Transformation Materials is broken into the powder of certain size;
2) by step 1) in the Martensitic Transformation Materials powder prepared mix with binding agent, curing agent;
3) by step 2) in the mixed powder compaction size and dimension that becomes to need;
4) by step 3) in the moulding material prepared under certain curing temperature, solidify certain hour, finally obtain bonding Martensitic Transformation Materials.
2. preparation method according to claim 1, it is characterized in that described step 1) comprising: Martensitic Transformation Materials is broken by one or more in the modes such as grinding, vibration milling, rolling mill, ball milling or airflow milling, and by being greater than 10 object standard screens; Filter out the powder being less than 2mm.
3. preparation method according to claim 2, is characterized in that standard screen is 100 ~ 150 orders, and the particle size filtered out is 0 ~ 0.5mm.
4. preparation method according to claim 1, is characterized in that described step 2) comprising: by step 1) in the Martensitic Transformation Materials powder prepared mix with binding agent, curing agent; Described binding agent is one or more in epoxy resin, phenolic resins, Merlon, polyethylene naphthoic acid fat, polyethylene terephthalate, polyimides, polyamide, Kynoar, polystyrene, polybutene, polyvinyl chloride, polyethylene; Described curing agent is the macromolecular material matched with selected binding agent, described curing agent presses volume ratio and the binding agent mixing of 5-50%, then mixed curing agent and binding agent is added in Martensitic Transformation Materials powder by 0.5 ~ 20wt.% of Martensitic Transformation Materials powder.
5. preparation method according to claim 4, it is characterized in that binding agent is selected from epoxide-resin glue and polyimides glue one or both, curing agent is phenolic aldehyde amine, curing agent by 10 ~ 30% volume ratio and binding agent mixing; Mixed curing agent and binding agent add in Martensitic Transformation Materials powder by 1 ~ 10wt.% of Martensitic Transformation Materials powder.
6. preparation method according to claim 1, it is characterized in that described step 3) comprising: by step 2) in mixed powder be pressed into the size and dimension of needs by rolling process, die pressing, extrusion, powder injection forming or discharge plasma sintering process, pressing pressure is 300 ~ 1500MPa, press temperature is 0 ~ 900 DEG C, and the press time is 5 ~ 240 minutes.
7. preparation method according to claim 6, it is characterized in that pressing pressure is 600 ~ 1000MPa, press temperature is 0 ~ 300 DEG C, and the press time is 10 ~ 120 minutes.
8. preparation method according to claim 1, is characterized in that described step 4) described curing temperature is 0 ~ 500 DEG C, curing time is 1 ~ 10 day.
9. preparation method according to claim 8, is characterized in that described curing temperature is 0 ~ 150 DEG C; Curing time is 3 ~ 7 days.
CN201510844896.6A 2015-11-26 2015-11-26 Preparation method of bonding martensitic phase change material Pending CN105448443A (en)

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CN106917029A (en) * 2017-04-13 2017-07-04 佛山市程显科技有限公司 A kind of MM ' X Y metal composite functional materials and preparation method thereof
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CN107058848A (en) * 2017-05-04 2017-08-18 大连大学 A kind of high intensity Ni50Mn34In16The preparation method of Magnetic Memory alloy
CN107142389A (en) * 2017-05-04 2017-09-08 大连大学 High-strength, the high-ductility Ni of one kind50Mn34In16‑xCoxThe preparation method of Magnetic Memory alloy
CN108531139A (en) * 2018-05-08 2018-09-14 武汉博茗低碳产业股份有限公司 A kind of forming and sintering carbon is the shaping phase-change material and preparation method thereof of carrier
CN108620582A (en) * 2018-06-05 2018-10-09 哈尔滨工程大学 A kind of composite material and preparation method of magnetic memorial alloy and copper
CN112442337A (en) * 2019-08-29 2021-03-05 张立强 Resin type phase change energy storage material and preparation method thereof

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CN106917029B (en) * 2017-04-13 2018-08-21 佛山市程显科技有限公司 A kind of ferromagnetic martensitic traoformation MM ' X-Y metal composite functional materials and preparation method thereof
CN106917029A (en) * 2017-04-13 2017-07-04 佛山市程显科技有限公司 A kind of MM ' X Y metal composite functional materials and preparation method thereof
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CN106967923A (en) * 2017-04-14 2017-07-21 北京科技大学 A kind of compound magnetic refrigerating material and its production and use
CN107142389B (en) * 2017-05-04 2018-11-02 大连大学 High-strength, the high-ductility Ni of one kind50Mn34In16-xCoxThe preparation method of Magnetic Memory alloy
CN108085523A (en) * 2017-05-04 2018-05-29 大连大学 High-strength, the high-ductility Ni of one kind50Mn34In11Co5The preparation method of Magnetic Memory alloy
CN107142389A (en) * 2017-05-04 2017-09-08 大连大学 High-strength, the high-ductility Ni of one kind50Mn34In16‑xCoxThe preparation method of Magnetic Memory alloy
CN107058848A (en) * 2017-05-04 2017-08-18 大连大学 A kind of high intensity Ni50Mn34In16The preparation method of Magnetic Memory alloy
CN108085523B (en) * 2017-05-04 2019-09-13 大连大学 High-strength, the high-ductility Ni of one kind50Mn34In11Co5The preparation method of Magnetic Memory alloy
CN108531139A (en) * 2018-05-08 2018-09-14 武汉博茗低碳产业股份有限公司 A kind of forming and sintering carbon is the shaping phase-change material and preparation method thereof of carrier
CN108620582A (en) * 2018-06-05 2018-10-09 哈尔滨工程大学 A kind of composite material and preparation method of magnetic memorial alloy and copper
CN108620582B (en) * 2018-06-05 2020-02-14 哈尔滨工程大学 Composite material of magnetic memory alloy and copper and preparation method thereof
CN112442337A (en) * 2019-08-29 2021-03-05 张立强 Resin type phase change energy storage material and preparation method thereof

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Application publication date: 20160330