CN103924153B - A kind of low bulk magnetic shielding Alloy And Preparation Method - Google Patents
A kind of low bulk magnetic shielding Alloy And Preparation Method Download PDFInfo
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Abstract
The invention belongs to Precise Alloy field, particularly a kind of low bulk magnetic shielding Alloy And Preparation Method for optical fiber loop framework.The chemical composition of this alloy by weight % is: Ni32.0 ~ 35.2, Co3.0 ~ 3.5, Mn0.10 ~ 0.25, Si≤0.15, Cu≤0.02, C≤0.01, P≤0.01, S≤0.01, and surplus is Fe; This low bulk magnetic shielding alloy is prepared as follows: high-purity raw preparation → composition proportion → vacuum induction furnace smelting and vacuum consumable remelting → forging processing → sampling → thermal treatment → performance test.Heat treating regime is: high-purity hydrogen is protected, and is warming up to 970 ± 10 DEG C with stove, and insulation 2.5 ~ 3h, is cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, is chilled to less than 300 DEG C soon and comes out of the stove.The present invention, compared with existing low expansion alloy 4J32, under the prerequisite keeping low expansion character, has higher initial permeability, makes alloy have low bulk performance and the large advantage of magnetic shield performance two concurrently.That is: in-45 ~+75 DEG C of temperature ranges, the coefficient of expansion of alloy is 1.0 × 10
-6/ DEG C below; Initial permeability is higher than 1.5mH/m.
Description
Technical field
The invention belongs to Precise Alloy field, particularly a kind of low bulk magnetic shielding Alloy And Preparation Method for making optical fiber loop framework.
Background technology
Compared with traditional mechanism, fiber device has the advantages such as structure is simple, lightweight, response is fast, the life-span is long.On the one hand, for overcoming the disadvantageous effect of temperature variation to fiber device precision, require that the material making optical fiber loop framework has the low linear expansivity consistent with optical fiber; On the other hand, for reducing magnetic field to the Faraday effect of light, require that optical fiber is in downfield environment.So, for improving the precision of fiber device further, optical fiber loop framework material need have low-expansion coefficient and higher magnetic property concurrently.
The linear expansivity of metal is generally 4.45 ~ 39 × 10
-6/ DEG C within the scope of, linear expansivity and its fusing point of most of pure metal are inversely proportional to.The alloy that Fe, Ni, Co form, due to invarable effect, has unusual thermal expansion character, has lower linear expansivity in the temperature range below Curie temperature.Ni content is that the linear expansivity of the pure 4J36 alloy of 36% can be low to moderate 0.6 × 10
-6/ DEG C.If but Ni content departs from this content, linear expansivity just can be caused sharply to increase.4J32 alloy containing Fe62.2%, Ni33%, Co4.5% has lower linear expansivity, by adjusting the per-cent of micro-Cu further, the coefficient of expansion of this alloy can be made to be low to moderate 0.12 × 10
-6/ DEG C, but this alloy initial magnetic permeability is generally only 0.4mH/m, and magnetic shield performance is poor.
In Fe-Ni system alloy, the initial permeability of the high magnetic conduction permalloy of Ni content near 74% ~ 80% is maximum is greater than 100mH/m, has good magnetic shield performance.And this alloy does not possess invarable effect, linear expansivity is very high, about 11 × 10
-6/ DEG C, low expansion is poor.Although high magnetic permeability permalloy is better for the effect of magnetic shielding device, because its coefficient of expansion is far longer than fiber optic materials, and can not directly as optical fiber loop framework materials'use.Not yet find the method that effectively can reduce high magnetic conduction permalloy linear expansivity at present.
U.S. CarpenterTechnology company is for Litton company of U.S. Study and Development has the matrix material of low-expansion coefficient and magnetic shield performance concurrently.Carry out technology and products export restriction to China in this regard due to external, domestic research and development unit still uses hard aluminium alloy processing optical fiber skeleton usually.Although aluminium alloy optical fiber skeleton has the advantages such as heat conduction is fast, lightweight, can not mate with optical fiber well, also not there is magnetic screen function.Thus only have and be equipped with high permeability alloy (as permalloy) outer cover again, reach magnetic shielding object.
Current, although existing domestic research and development unit tries out low-expansion 4J32 alloy as optical fiber loop framework, then be equipped with permalloy outer cover, realize mating and Magnetic Shielding Effectiveness with the optical fiber coefficient of expansion, improve over-all properties.But due to the restriction in fiber device weight and space, adopting the low-expansion material having magnetic shield performance concurrently to make optical fiber skeleton is an optimal selection.
Summary of the invention
One object of the present invention is, provides a kind of low bulk magnetic shielding alloy with good low linear expansion coefficient and high magnetic characteristics combination, to meet the integration requirement of optical fiber loop framework material.
Another object of the present invention is, provides the preparation method of above-mentioned low bulk magnetic shielding alloy.
For achieving the above object, technical scheme of the present invention is as follows:
For a low bulk magnetic shielding alloy for optical fiber loop framework, the chemical composition of this alloy by weight % is: Ni32.0 ~ 35.2, Co3.0 ~ 3.5, Mn0.10 ~ 0.25, Si≤0.15, Cu≤0.02, C≤0.01, P≤0.01, S≤0.01, and surplus is Fe;
This low bulk magnetic shielding alloy is prepared as follows: high-purity raw preparation → composition proportion → vacuum induction furnace smelting and vacuum consumable remelting → forging processing → sampling → thermal treatment → performance test.
Described heat treating regime is: high-purity hydrogen is protected, and is warming up to 970 ± 10 DEG C with stove, and insulation 2.5 ~ 3h, is cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, is chilled to less than 300 DEG C soon and comes out of the stove.
The chemical composition of this alloy by weight % is: Ni32.09 ~ 35.19, Co3.01 ~ 3.43, Mn0.13 ~ 0.21, Si0.015 ~ 0.150, Cu0.0052 ~ 0.0140, C0.0022 ~ 0.0044, P0.0030 ~ 0.0055, S0.0030 ~ 0.0040, surplus is Fe.
This alloy, in-45 ~+75 DEG C of temperature ranges, has the combination of following low bulk performance and magnetic shield performance: the coefficient of expansion≤1.0 × 10
-6/ DEG C, initial permeability>=1.5mH/m.
Described high-purity raw is the starting material that purity is greater than 99.0%.
For a preparation method for the low bulk magnetic shielding alloy of described optical fiber loop framework, the chemical composition of this alloy by weight % is: Ni32.0 ~ 35.2, Co3.0 ~ 3.5, Mn0.10 ~ 0.25, Si≤0.15, Cu≤0.02, C≤0.01, P≤0.01, S≤0.01, surplus is Fe;
This low bulk magnetic shielding alloy is prepared as follows: high-purity raw preparation → composition proportion → vacuum induction furnace smelting and vacuum consumable remelting → forging processing → sampling → thermal treatment → performance test.
In vacuum induction smelting and the heavy stove molten alloy of vacuum consumable, vacuum tightness is greater than 0.2Pa.
Heat treating regime is: high-purity hydrogen is protected, and is warming up to 970 ± 10 DEG C with stove, and insulation 2.5 ~ 3h, is cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, is chilled to less than 300 DEG C soon and comes out of the stove.
Because linear expansivity depends primarily on alloying constituent, in Fe-Ni system alloy, usual Ni content, 32% ~ 36% time, just presents invarable effect, has low linear expansivity.If Ni content departs from this scope, linear expansivity just can be caused sharply to increase.Research finds, except Co, micro Cu element, the elements such as C, P, S, N, Cr, Mn, Ti all make the linear expansivity of alloy increase.Wherein the impact of C alloy linear expansivity is the most remarkable, and a small amount of Si alloy linear expansivity impact is little.Therefore, the content of the elements such as Si, Mn, C in alloy should be reduced under the prerequisite ensureing alloy processing characteristics as far as possible.
The present invention is based on low bulk Fe-Ni-Co system alloy 4J32, by adjustment chemical composition, controls foreign matter content, particularly optimizes thermal treatment process, develops novel to have low-expansion coefficient and the low bulk magnetic shielding alloy compared with high magnetic characteristics concurrently.
Compared with the chemical composition of low expansion alloy 4J32, for improving magnetic property, adding Ni content, suitably having turned down the content of Co, Mn, strict limitation having been carried out to Si, Cu and C, P, S etc. simultaneously.
Compared with the 4J32 heat treating regime of standard, invention increases thermal treatment temp, add soaking time, eliminate the low-temperaturetempering after shrend and reprocessing.
This low bulk magnetic shielding alloy is prepared as follows: high-purity raw preparation → composition proportion → vacuum induction furnace smelting and vacuum consumable remelting → forging processing → sampling → thermal treatment → performance test.
1, reasonable offer
For ensureing the low-expansion coefficient of alloy, must the strict content controlling impurity element in alloy.The starting material that material adopts purity to be greater than 99.0%, and main raw material pure iron is purified further by vacuum induction.Alloy smelting process adopts vacuum induction to add the two vacuum melting technique of vacuum consumable, and vacuum tightness is better than 0.2Pa.The scaling loss amount of alloying element strictly will be controlled in fusion process, control refining temperature and time, accomplish accurate control composition, fully degassed, abundant scum silica frost, reduce the content of C, P, S impurity as far as possible, in actual alloying constituent, above-mentioned element all controls below 0.01%.Under ensureing hot worked prerequisite, conservative control Mn, Si content, in experiment, Mn content controls to control below 0.15% at 0.25%, Si content, better performances.
2, optimization of Heat Treatment Process
The thermal treatment process presenting the minimum line coefficient of expansion (830 DEG C of shrend+low-temperaturetemperings) and optimum magnetic energy (high temperature 1180 DEG C of tempering also control cooling rate) due to alloy is completely different.Under must ensureing in alloying constituent, foreign matter content etc. that alloy has the prerequisite of minimum linear expansivity, adopt high-temperature tempering process, finally make the low bulk magnetic shielding alloy of high performance index requirement.
For this reason, We conducted from 820 DEG C ~ 1180 DEG C multiple thermal treatment process researchs, filtered out optimal heat resolving system.Through the heat treatment experiment of many wheels, finally determine that heat treating regime is: high-purity hydrogen is protected, and is warming up to 970 ± 10 DEG C with stove; insulation 2.5 ~ 3h; be cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, be chilled to less than 300 DEG C soon and come out of the stove, the material over-all properties obtained with this heat treating regime is optimum.
Beneficial effect of the present invention is:
The present invention, compared with existing low expansion alloy 4J32, under the prerequisite keeping low expansion character, has higher initial permeability, makes alloy have low bulk performance and the large advantage of magnetic shield performance two concurrently.
Accompanying drawing explanation
Fig. 1 is the linear expansivity of the alloy of the embodiment of the present invention 1 after heat treatments at different in-45 ~+75 DEG C of temperature ranges and initial permeability.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.
The concrete technology step of the low bulk magnetic shielding alloy for making optical fiber loop framework of the present invention is as follows:
A) to purify pure Fe with 200kg vacuum induction furnace, remove the impurity such as gas wherein and C, S, P, remove the surface oxide layer of W metal, Co and Fe through polishing;
B) adopt 25kg vacuum induction furnace and consumable electroarc furnace molten alloy, vacuum tightness is better than 0.2Pa, the strict composition controlling main alloying element in fusion process, and after melting, the actual constituent of alloy lists in table 1;
The chemical composition (wt%) of table 1 molten alloy
| Numbering | Ni | Co | Mn | Si | Cu | C | P | S | Fe |
| Embodiment 1 | 33.05 | 3.43 | 0.17 | 0.063 | 0.0052 | 0.0026 | 0.0049 | 0.0031 | More than |
| Embodiment 2 | 32.69 | 3.43 | 0.20 | 0.110 | 0.0130 | 0.0043 | 0.0055 | 0.0040 | More than |
| Embodiment 3 | 35.19 | 3.36 | 0.21 | 0.015 | 0.0140 | 0.0022 | 0.0030 | 0.0030 | More than |
| Embodiment 4 | 33.48 | 3.37 | 0.16 | 0.150 | 0.0070 | 0.0044 | 0.0050 | 0.0040 | More than |
| Embodiment 5 | 32.09 | 3.01 | 0.13 | 0.140 | 0.0070 | 0.0038 | 0.0050 | 0.0040 | More than |
C) alloy pig forges after Homogenization Treatments in air-heating furnace, and first pier is thick, rear pulling;
D) rod iron after forge hot is sampled;
E) sample is heat-treated, the expansion character of alloy and magnetic property after test thermal treatment.
First, in order to the best low bulk performance that alloy after understanding composition adjustment can reach, we heat-treat embodiment 1, embodiment 2 according to the heat treating regime of low expansion alloy.Technique is as follows: be warming up to 830 DEG C with stove, insulation 1h, 320 DEG C of tempering insulation 1h after shrend.The linear expansivity of the alloy recorded in-45 ~+75 DEG C of temperature ranges and initial permeability as shown in table 2.Learnt by data, alloy maintains good low expansion, but initial permeability is less than 0.7mH/m, can not meet magnetic shielding requirement.
The alloy property of low expansion alloy heat treating regime process pressed by table 2
| Numbering | Linear expansivity (× 10 -6/℃) | Initial permeability (mH/m) |
| Embodiment 1 | 0.12 | 0.65 |
| Embodiment 2 | 0.13 | 0.69 |
Secondly, in order to obtain the optimum magnetic energy index of this composition alloy, we have carried out thermal treatment according to high magnetic conduction permalloy thermal treatment process to embodiment 1, embodiment 2 again.Technique is as follows: in high-purity hydrogen atmosphere, is warming up to 1180 DEG C with stove, and insulation 2.5h, is cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, is chilled to less than 300 DEG C soon and comes out of the stove.The linear expansivity of the alloy recorded in-45 ~+75 DEG C of temperature ranges and initial permeability list in table 3.The magnetic permeability of alloy obviously increases, but also sacrifices too many low bulk performance simultaneously, fails to meet composite request.
Table 3 is by the alloy property of high magnetic conduction permalloy heat treating regime process
| Numbering | Linear expansivity (× 10 -6/℃) | Initial permeability (mH/m) |
| Embodiment 1 | 1.04 | 2.05 |
| Embodiment 2 | 1.13 | 2.68 |
In order to meet the requirement of linear expansivity and magnetic permeability simultaneously, we explore by the heat treating regime of the alloy sample alloy of embodiment 1, embodiment 2 further.Table 4 be embodiment 1, embodiment 2 after heat treatments at different, be cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, be chilled to less than 300 DEG C soon and come out of the stove, the linear expansivity in-45 ~+75 DEG C of temperature ranges and initial permeability.Data show, along with the increase of thermal treatment temp, magnetic permeability and linear expansivity increase all thereupon.Fig. 1 is embodiment 1 linear expansivity and initial permeability and thermal treatment temp graph of a relation.Through contrast, when heat treating regime is 970 DEG C × 2.5h, alloy over-all properties is optimum.Therefore, thermal treatment temp of the present invention is defined as by 970 ± 10 DEG C.
The alloy property of table 4 after heat treatments at different
Table 5 is embodiment 3, embodiment 4, the alloy property of embodiment 5 after thermal treatment process process of the present invention, all meets the composite request of low-expansion coefficient and high magnetic permeability.
The alloy property of table 5 after thermal treatment process process of the present invention
| Numbering | Linear expansivity (× 10 -6/℃) | Initial permeability (mH/m) |
| Embodiment 3 | 0.83 | 2.28 |
| Embodiment 4 | 0.67 | 2.18 |
| Embodiment 5 | 0.63 | 1.96 |
Can prepare according to present component design, preparation technology and heat treating regime the low bulk magnetic shielding alloy having low-expansion coefficient and higher magnetic property concurrently, this alloy has the coefficient of expansion and is less than 1.0 × 10
-6/ DEG C, initial permeability is greater than the over-all properties of 1.5mH/m.This alloy is used for optical fiber loop framework, can make the raising of fiber device precision, structure simplifies, weight saving, have broad application prospects.
Claims (5)
1., for a low bulk magnetic shielding alloy for optical fiber loop framework, it is characterized in that:
The chemical composition of this alloy by weight % is: Ni32.0 ~ 35.2, Co3.0 ~ 3.5, Mn0.10 ~ 0.25, Si≤0.15, Cu≤0.02, C≤0.01, P≤0.01, S≤0.01, and surplus is Fe;
This low bulk magnetic shielding alloy is prepared as follows: high-purity raw preparation → composition proportion → vacuum induction furnace smelting and vacuum consumable remelting → forging processing → sampling → thermal treatment → performance test;
Heat treating regime is: high-purity hydrogen is protected, and is warming up to 970 ± 10 DEG C with stove, and insulation 2.5 ~ 3h, is cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, is chilled to less than 300 DEG C soon and comes out of the stove; Described high-purity raw is the starting material that purity is greater than 99.0%.
2. low bulk magnetic shielding alloy as claimed in claim 1, is characterized in that:
The chemical composition of this alloy by weight % is: Ni32.09 ~ 35.19, Co3.01 ~ 3.43, Mn0.13 ~ 0.21, Si0.015 ~ 0.150, Cu0.0052 ~ 0.0140, C0.0022 ~ 0.0044, P0.0030 ~ 0.0055, S0.0030 ~ 0.0040, surplus is Fe.
3. low bulk magnetic shielding alloy as claimed in claim 1, is characterized in that:
This alloy, in-45 ~+75 DEG C of temperature ranges, has the combination of following low bulk performance and magnetic shield performance: the coefficient of expansion≤1.0 × 10
-6/ DEG C, initial permeability>=1.5mH/m.
4. a preparation method for the low bulk magnetic shielding alloy of optical fiber loop framework as claimed in claim 1, is characterized in that:
The chemical composition of this alloy by weight % is: Ni32.0 ~ 35.2, Co3.0 ~ 3.5, Mn0.10 ~ 0.25, Si≤0.15, Cu≤0.02, C≤0.01, P≤0.01, S≤0.01, and surplus is Fe;
This low bulk magnetic shielding alloy is prepared as follows: high-purity raw preparation → composition proportion → vacuum induction furnace smelting and vacuum consumable remelting → forging processing → sampling → thermal treatment → performance test; Wherein,
Heat treating regime is: high-purity hydrogen is protected, and is warming up to 970 ± 10 DEG C with stove, and insulation 2.5 ~ 3h, is cooled to 550 ± 10 DEG C with 200 ~ 250 DEG C/h, is chilled to less than 300 DEG C soon and comes out of the stove.
5. the preparation method of low bulk magnetic shielding alloy as claimed in claim 4, is characterized in that:
In vacuum induction smelting and the heavy stove molten alloy of vacuum consumable, vacuum tightness is greater than 0.2Pa.
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| CN106756582B (en) * | 2016-12-30 | 2018-08-10 | 钢铁研究总院 | A kind of enhanced low-expansion alloy of intermetallic compound and preparation method |
| CN109746455B (en) * | 2019-03-19 | 2022-08-12 | 湖南恒基粉末科技有限责任公司 | Copper-containing kovar alloy and preparation method thereof |
| CN110760764B (en) * | 2019-11-05 | 2021-09-28 | 重庆材料研究院有限公司 | Iron-nickel-based Al-containing high-strength constant-expansion alloy |
| CN112195369B (en) * | 2020-11-06 | 2021-07-23 | 西安稀有金属材料研究院有限公司 | Corrosion-resistant high-strength neutron shielding alloy material and preparation method thereof |
| CN112496219A (en) * | 2020-11-23 | 2021-03-16 | 苏州市吴中不锈钢有限公司 | Manufacturing and processing method of 4J32 alloy ring piece |
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| CN1138634A (en) * | 1995-05-05 | 1996-12-25 | 安费公司 | Fe-Ni-Co alloy and use for manufacture of shadow mask |
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| CN102127652A (en) * | 2011-03-03 | 2011-07-20 | 重庆仪表材料研究所 | Super-pure electro-slag remelting method for super-invar alloy |
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| JPS5830940B2 (en) * | 1978-12-21 | 1983-07-02 | 日立電線株式会社 | Thermal expansion adjustment material and its manufacturing method |
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| CN1138634A (en) * | 1995-05-05 | 1996-12-25 | 安费公司 | Fe-Ni-Co alloy and use for manufacture of shadow mask |
| CN101379210A (en) * | 2006-02-02 | 2009-03-04 | 蒂森克鲁普德国联合金属制造有限公司 | Iron-nickel-cobalt alloy |
| CN102127652A (en) * | 2011-03-03 | 2011-07-20 | 重庆仪表材料研究所 | Super-pure electro-slag remelting method for super-invar alloy |
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