CN101003117A - A sort of Fe-Ga magnetostriction alloy wire and preparation method - Google Patents
A sort of Fe-Ga magnetostriction alloy wire and preparation method Download PDFInfo
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- CN101003117A CN101003117A CN 200710062867 CN200710062867A CN101003117A CN 101003117 A CN101003117 A CN 101003117A CN 200710062867 CN200710062867 CN 200710062867 CN 200710062867 A CN200710062867 A CN 200710062867A CN 101003117 A CN101003117 A CN 101003117A
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Abstract
A magnetostrictive Fe-Ga alloy wire with better mangetostrain power [(21-118) *10 to the power -6] is prepared through smelting, casting rod, hot spinning forging, and cold drawing.
Description
Technical field
The present invention relates to a kind of technology for preparing a material, more particularly say, be meant that a kind of employing hot-swage and cold-drawn engage technology, prepare the method for Fe-Ga magnetostriction alloy wire.
Background technology
Magnetic striction wire is widely used in sensor field (as torque sensor, pressure sensor, displacement transducer).The composition of now common magnetic striction wire is generally Ni, Fe-Ni, Fe-Ni-Co, and the plasticity of these alloys is better, is processed into a material easily, but its magnetostriction performance is lower, only is 20 * 10
-6About, limited the precision and the measurement category of sensor.In the magnetostriction materials of research, giant magnetostriction material TbDyFe has great magnetostriction, reaches 2000 * 10 at present
-6, but its fragility is very big, is unfavorable for machine-shaping, and cost an arm and a leg (the rare earth material price is expensive).Therefore, a kind of good magnetostriction performance and good novel magnetic striction wire of plasticity of having concurrently becomes the emphasis that people pay close attention to.
Fe-Ga is that alloy has magnetostriction performance preferably and mechanical property, be fit to very much become the material of magnetic striction wire, it is alloy monocrystalline or orientation polycrystalline that the method for common now employing directional solidification prepares Fe-Ga, the alloy of this method preparation has preferred orientation preferably, but the finished product that makes is generally bar.
In order better the Fe-Ga alloy to be applied to sensor field, the inventor will provide a kind of preparation method of Fe-Ga alloy silk.
Summary of the invention
The objective of the invention is to propose a kind of method of the Fe-Ga of preparation magnetostriction alloy wire, this method can make under downfield 100Oe environment by melting, casting rod, hot-swage and cold-drawn operation, has the novel Fe-Ga magnetostriction alloy wire of better magnetostriction performance.
Of the present inventionly a kind ofly adopt hot-swage and cold-drawn to engage the method that technology prepares the Fe-Ga magnetostriction alloy wire, it has the following step:
A, molten alloy casting rod
Take by weighing 15～20at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa～4 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga;
After melting treated that alloying element melted fully in 2～5 minutes, current interruption formed alloy pig;
Ingot casting overturn makes the composition in the alloy even after the melt back 1～4 time, inhales casting then and makes the Fe-Ga rod that diameter is 7～10mm; The cooling back is taken out stand-by;
B, polishing
To make ganoid Fe-Ga rod through the outer rim of on centerless grinder, polishing of the Fe-Ga rod after the A step process;
C, hot-swage
To be in 700 ℃～800 ℃ in temperature through the smooth Fe-Ga rod after the B step process, and make Fe-Ga rod after the pulling through the hot-swage of 2～4 passages, its passage amount of feeding be 0.5mm～1mm;
After the hot-swage diameter be 7～10mm Fe-Ga rod reduced about 2～3mm;
D, cold-drawn
To through the Fe-Ga rod after the pulling after the C step process at room temperature adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 3～5 times, between each drawing passes the Fe-Ga rod after the pulling is being carried out annealing in process, and annealing temperature is 800 ℃～900 ℃, and annealing time is 15～40 minutes; Making diameter is the Fe-Ga alloy silk of 0.5mm～1.5mm;
E, heat treatment
To through being incubated half an hour under 900 ℃ in the tubular type vacuum heat treatment furnace after, the Fe-Ga alloy silk after the D step process adopt the cold room temperature that is cooled to of shrend or stove respectively.
The advantage of preparation Fe-Ga magnetostriction alloy wire method of the present invention is: (1) develops a kind of novel Fe-Ga magnetic striction wire, and its magneto-strain is 21 * 10 under downfield 100Oe environment
-6～118 * 10
-6, be better than other traditional magnetic striction wires; (2) reasonably select the technological parameter of hot-swage and drawing for use, successfully adopt the method for plastic working to prepare Fe-Ga alloy silk, reduced manufacturing cost significantly, make its batch process become possibility; (3) the Fe-Ga alloy can produce preferred orientation in the plastic forming process, helps obtaining good magnetostriction performance; (4) can adopt the method for directional solidification to make the Fe-Ga alloy have preferred orientation earlier, it is prepared into a material again, the magnetostriction performance of the Fe-Ga alloy silk that makes like this can be further enhanced.
Description of drawings
Fig. 1 is Fe
85Ga
15The magnetostriction performance chart of magnetostriction alloy wire.
Fig. 2 is Fe
85Ga
15The X ray diffracting spectrum of magnetostriction alloy wire.
The specific embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention a kind ofly adopts hot-swage and cold-drawn to engage the method that technology prepares the Fe-Ga magnetostriction alloy wire, and it has the following step:
A, molten alloy casting rod
Take by weighing 15～20at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa～4 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga;
After melting treated that alloying element melted fully in 2～5 minutes, current interruption formed alloy pig;
Ingot casting overturn makes the composition in the alloy even after the melt back 1～4 time, inhales casting then and makes the Fe-Ga rod that diameter is 7～10mm; The cooling back is taken out stand-by;
B, polishing
To polish on centerless grinder through the Fe-Ga rod after the A step process, (polishing is for defectives such as the wrinkle of removing Fe-Ga rod surface, holes, hole to outer rim, reduction causes bar distortion fracture because of blemish), make ganoid Fe-Ga rod (diameter be the Fe-Ga rod of 7～10mm might reduced about 0.15～0.5mm);
C, hot-swage
To be in 700 ℃～800 ℃ in temperature through the smooth Fe-Ga rod after the B step process, and make Fe-Ga rod after the pulling through the hot-swage of 2～4 passages, its passage amount of feeding be 0.5mm～1mm;
After the hot-swage diameter be 7～10mm Fe-Ga rod reduced about 2～3mm;
Smooth Fe-Ga rod is carried out hot-swage under hot conditions, be in order to smash as-cast structure, to make grain refinement, so that cold-drawing technology, and make bar produce deformation to satisfy drawing process to billet size and performance demands.
D, cold-drawn
To through the Fe-Ga rod after the pulling after the C step process at room temperature adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 3～5 times, between each drawing passes the Fe-Ga rod after the pulling is being carried out annealing in process, and annealing temperature is 800 ℃～900 ℃, and annealing time is 15～40 minutes; Making diameter is the Fe-Ga alloy silk of 0.5mm～1.5mm.
Adopting annealing heat treatment in the drawing process, is in order to make a structure refinement, to reduce work hardening, improve material plasticity, being convenient to further processing.
E, heat treatment
For Different Heat Treatment Conditions is relatively got two groups of samples to the influence of properties of product from the above-mentioned Fe-Ga magnetic striction wire that makes, in the tubular type vacuum heat treatment furnace 900 ℃ down after insulation half an hour, adopt the cold room temperature that is cooled to of shrend or stove respectively.
Adopt the eddy displacement sensor method that the Fe-Ga magnetic striction wire under the different conditions is tested, its magnetostriction performance is as shown in the table.
The sample of above-mentioned three kinds of different conditions is ground to form powdery, adopt X-ray diffraction analysis to study its microcosmic phase structure, analyze phase structure product magnetostriction Effect on Performance.As shown in Figure 2, the main phase structure of the Fe-Ga alloy of drawing attitude and quenching attitude be A2 mutually, and in the Fe-Ga of stove cold conditions alloy L1 has appearred
2Phase is because L1
2Meeting produces negative magnetostriction, and attitude is low so the magneto-strain of the Fe-Ga magnetic striction wire of stove cold conditions quenches.And drawing attitude magneto-strain low be because the internal stress and the dislocation that produce in the processing are pricked the great magneto-strain that limited surely.
In preparation process of the present invention, can be in (A) step and (B) adopt directional freeze method to prepare between the step to have＜100 or＜110〉preferred orientation Fe-Ga alloy bar, adopt this Fe-Ga alloy bar through plastic working Cheng Sicai, can improve the magnetostriction performance of Fe-Ga alloy silk better.
Embodiment 1:System Fe
85Ga
15The alloy silk
Take by weighing 15at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga; After melting treated that alloying element melted fully in 3 minutes, current interruption formed alloy pig; Ingot casting overturn makes the composition in the alloy even after the melt back 4 times, inhales casting then and makes the Fe-Ga rod that diameter is 7mm; The cooling back is taken out stand-by;
The outer rim of then the Fe-Ga rod of 7mm being polished on centerless grinder makes the Fe-Ga rod about smooth surface 6.5mm;
Then with the Fe-Ga rod of 6.5mm in 800 ℃ of temperature, make the Fe-Ga rod of 5mm through the hot-swage of 3 passages, its passage amount of feeding is 0.5mm;
Then with the Fe-Ga rod of 5mm under 20 ℃ of room temperatures, adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 3 times, between each drawing passes the Fe-Ga rod after the pulling is being carried out annealing in process, and annealing temperature is 850 ℃, and annealing time is 20 minutes; Making diameter is the Fe-Ga alloy silk of 1.5mm;
With the Fe-Ga alloy silk of 1.5mm in the tubular type vacuum heat treatment furnace 900 ℃ down after insulation half an hour, shrend is cooled to room temperature then.
Adopt the eddy displacement sensor method to measure the 1.5mm Fe-Ga alloy silk that makes, it is under downfield 100Oe environment, and magneto-strain is 66 * 10
-6
Adopt the eddy displacement sensor method to Fe
85Ga
15Magnetostriction alloy wire is tested, and its magnetostriction performance as shown in Figure 1.Among the figure, drawing attitude Fe
85Ga
15The saturated magneto-strain of magnetostriction alloy wire is 21 * 10
-6, stove cold conditions Fe
85Ga
15The saturated magneto-strain of magnetostriction alloy wire is 52 * 10
-6, quenching attitude Fe
85Ga
15The saturated magneto-strain of magnetostriction alloy wire is 66 * 10
-6Therefore, quenching attitude Fe
85Ga
15The magnetostriction performance of magnetostriction alloy wire is better than other two states.
Embodiment 2:System Fe
82Ga
18The alloy silk
Take by weighing 18at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga; After melting treated that alloying element melted fully in 4 minutes, current interruption formed alloy pig; Ingot casting overturn makes the composition in the alloy even after the melt back 4 times, inhales casting then and makes the Fe-Ga rod that diameter is 10mm; The cooling back is taken out stand-by;
The outer rim of then the Fe-Ga rod of 10mm being polished on centerless grinder makes the Fe-Ga rod about smooth surface 9.5mm;
Then with the Fe-Ga rod of 9.5mm in 800 ℃ of temperature, make the Fe-Ga rod of 7.5mm through the hot-swage of 2 passages, its passage amount of feeding is 1mm;
Then with the Fe-Ga rod of 7.5mm under 20 ℃ of room temperatures, adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 5 times, between each drawing passes the Fe-Ga rod after the pulling is being carried out annealing in process, and annealing temperature is 850 ℃, and annealing time is 20 minutes; Making diameter is the Fe-Ga alloy silk of 0.5mm;
With the Fe-Ga alloy silk of 0.5mm in the tubular type vacuum heat treatment furnace 900 ℃ down after insulation half an hour, shrend is cooled to room temperature then.
Adopt the eddy displacement sensor method to measure the 0.5mm Fe-Ga alloy silk that makes, it is under downfield 100Oe environment, and magneto-strain is 74 * 10
-6
Embodiment 3:Fixture has＜100〉orientation Fe
85Ga
15The alloy silk
Take by weighing 15at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga; After melting treated that alloying element melted fully in 3 minutes, current interruption formed alloy pig; Ingot casting overturn makes the composition in the alloy even after the melt back 4 times, inhales casting then and makes the Fe-Ga rod that diameter is 7mm; The cooling back is taken out stand-by;
With the diameter that makes is that the Fe-Ga rod of 7mm is put into directional solidification high-temperature gradient vaccum sensitive stove, and excellent overcoat one interior diameter is the alundum tube of 7.2mm, fixes with anchor clamps.With the gallium indium alloy as cooling fluid, suction to 3 * 10
-3Pa feeds argon gas, and keeping vacuum is 2 * 10
4Pa.Make thermograde be about 500 ℃/cm by regulating gallium indium alloy liquid level, carry out directional solidification with the setting rate of 720mm/h, obtain to have＜100〉preferred orientation diameter is the Fe-Ga magnetostriction bar of 7.2mm.
The outer rim of then the Fe-Ga rod of 7.2mm being polished on centerless grinder makes the Fe-Ga rod about smooth surface 7mm;
Then with the Fe-Ga rod of 7mm in 800 ℃ of temperature, make the Fe-Ga rod of 6mm through the hot-swage of 2 passages, its passage amount of feeding is 0.5mm; Then with the Fe-Ga rod of 6mm under 20 ℃ of room temperatures, adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 3 times, between each drawing passes the Fe-Ga rod after the pulling is being carried out annealing in process, and annealing temperature is 850 ℃, and annealing time is 20 minutes; Making diameter is the Fe-Ga alloy silk of 1.5mm;
With the Fe-Ga alloy silk of 1.5mm in the tubular type vacuum heat treatment furnace 900 ℃ down after insulation half an hour, shrend is cooled to room temperature then.
Adopt the eddy displacement sensor method to measure the 1.5mm Fe-Ga alloy silk that makes, it is under downfield 100Oe environment, and magneto-strain is 118 * 10
-6
Have good＜100 by the Fe-Ga alloy after the directional solidification through the XRD test〉preferred orientation, in the process that is drawn into silk subsequently, this orientation still can keep getting off, and can well improve the magnetostriction performance of Fe-Ga alloy silk.
Embodiment 4:System (Fe
81Ga
19)
99.5B
0.5The alloy silk
Take by weighing 0.5at% purity and be 99.99% B, 18.9at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga, B; After melting treated that alloying element melted fully in 4 minutes, current interruption formed alloy pig; Ingot casting overturn makes the composition in the alloy even after the melt back 4 times, inhales casting then and makes the Fe-Ga-B rod that diameter is 10mm; The cooling back is taken out stand-by;
The outer rim of then the Fe-Ga-B rod of 10mm being polished on centerless grinder makes the Fe-Ga-B rod about smooth surface 9.5mm;
Then with the Fe-Ga-B rod of 9.5mm in 800 ℃ of temperature, make the Fe-Ga-B rod of 7.5mm through the hot-swage of 2 passages, its passage amount of feeding is 1mm;
Then with the Fe-Ga-B rod of 7.5mm under 20 ℃ of room temperatures, adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 5 times, between each drawing passes the Fe-Ga-B rod after the pulling is being carried out annealing in process, and annealing temperature is 850 ℃, and annealing time is 20 minutes; Making diameter is the Fe-Ga-B alloy silk of 1mm;
With the Fe-Ga-B alloy silk of 1mm in the tubular type vacuum heat treatment furnace 900 ℃ down after insulation half an hour, shrend is cooled to room temperature then.
Adopt the eddy displacement sensor method to measure the 1mm Fe-Ga-B alloy silk that makes, it is under downfield 100Oe environment, and magneto-strain is 45 * 10
-6
By adding the grain refinement that three elements B makes the Fe-Ga alloy, plasticity increases, and is more conducive to plastic working and is shaped.In Fe-Ga-B alloy silk of the present invention, can also add as Mo, In, Ge, Si, Al, Ni.
Prepare the Fe-Ga alloy silk of the general 0.5～1.5mm of diameter through method of the present invention, this Fe-Ga alloy silk can be used as magnetic striction wire and is applied to can improve the certainty of measurement of sensor in torque sensor, pressure sensor, the displacement transducer.
Claims (3)
1, a kind of employing hot-swage and cold-drawn engage technology, prepare the method for Fe-Ga magnetostriction alloy wire, it is characterized in that the following step is arranged:
A, molten alloy casting rod
Take by weighing 15～20at% purity and be 99.99% Ga, surplus purity and be 99.99% Fe raw material; Put into the water jacketed copper crucible of vacuum arc furnace ignition, suction to 2 * 10
-3Pa～4 * 10
-3Pa; Feed argon gas, keep vacuum to 2 * 10
4Pa, beginning electric arc melting Fe, Ga;
After melting treated that alloying element melted fully in 2～5 minutes, current interruption formed alloy pig;
Ingot casting overturn makes the composition in the alloy even after the melt back 1～4 time, inhales casting then and makes the Fe-Ga rod that diameter is 7～10mm; The cooling back is taken out stand-by;
B, polishing
To polish on centerless grinder through the Fe-Ga rod after the A step process, (polishing is for defectives such as the wrinkle of removing Fe-Ga rod surface, holes, hole to outer rim, reduction causes bar distortion fracture because of blemish), make ganoid Fe-Ga rod (diameter be the Fe-Ga rod of 7～10mm might reduced about 0.15～0.5mm);
C, hot-swage
To be in 700 ℃～800 ℃ in temperature through the smooth Fe-Ga rod after the B step process, and make Fe-Ga rod after the pulling through the hot-swage of 2～4 passages, its passage amount of feeding be 0.5mm～1mm;
After the hot-swage diameter be 7～10mm Fe-Ga rod reduced about 2～3mm;
D, cold-drawn
To through the Fe-Ga rod after the pulling after the C step process at room temperature adopt horizontal drawbench to carry out drawing; Wherein, total drawing passes is 3～5 times, between each drawing passes the Fe-Ga rod after the pulling is being carried out annealing in process, and annealing temperature is 800 ℃～900 ℃, and annealing time is 15～40 minutes; Making diameter is the Fe-Ga alloy silk of 0.5mm～1.5mm;
E, heat treatment
To through being incubated half an hour under 900 ℃ in the tubular type vacuum heat treatment furnace after, the Fe-Ga alloy silk after the D step process adopt the cold room temperature that is cooled to of shrend or stove respectively.
2, the method for preparing the Fe-Ga magnetostriction alloy wire according to claim 1 is characterized in that: in (A) step and (B) adopt the directional solidification method fixture to have＜100〉preferred orientation Fe-Ga alloy bar between the step.
3, the method for preparing the Fe-Ga magnetostriction alloy wire according to claim 1 is characterized in that: Fe-Ga alloy silk its magneto-strain under downfield 1000e environment is 21 * 10
-6～118 * 10
-6
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