CN106011710A - Processing method for obtaining high-proportion special grain boundary from tin bronze - Google Patents
Processing method for obtaining high-proportion special grain boundary from tin bronze Download PDFInfo
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- CN106011710A CN106011710A CN201610392219.XA CN201610392219A CN106011710A CN 106011710 A CN106011710 A CN 106011710A CN 201610392219 A CN201610392219 A CN 201610392219A CN 106011710 A CN106011710 A CN 106011710A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
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Abstract
The invention discloses a processing method for obtaining a high-proportion special grain boundary from tin bronze. The processing method for obtaining the high-proportion special grain boundary from tin bronze comprises the steps that firstly, a plurality of workpieces with the dimension being 20 mm, a plurality of workpieces with the dimension being 9 mm and a plurality of workpieces with the dimension being 3 mm are obtained by cutting the tin bronze in the rolling direction, the transverse direction and the normal direction correspondingly through a linear cutting tool, then the workpieces are placed in the environment at the temperature of 400-800 DEG C for heat preservation for 0.5-5 hours, and then the workpieces are subjected to water quenching to the room temperature; secondly, polishing is conducted stage by stage with 200-2500# metallographic abrasive paper, and then mechanical polishing is conducted; and thirdly, electrochemical polishing is conducted in a polishing solution, the polishing temperature is 20-30 DEG C, the polishing voltage is 9 V, and the polishing time is 90 s. According to the processing method, it is proved through test analysis that the proportion of the special grain boundary is remarkably increased before the recrystallization annealing temperature is reached completely along with the rise of the annealing temperature; the structure obtained through the heat treatment process is stable, the change rule is obvious, and the experiment repeatability is good; and operation of the heat treatment process is simple, the technique is reliable, and the efficiency is high.
Description
Technical field
The present invention relates to a kind of processing method obtaining special grain boundary at high proportion in tin bronze, the method is to obtain special grain boundary at high proportion in tin bronze alloys material by Technology for Heating Processing, belongs to bounding engineering field.
Background technology:
For polycrystalline material, crystal boundary is a kind of most important microstructure, and each physics, chemical property are closely related with engineering material.1984 Watanabe propose the concept of " crystal boundary controls and design ", the overall performance that material is relevant with crystal boundary is improved by the way improving the Grain Boundary Character distribution of the ratio of low Σ-CSL crystal boundary, control material in the material, develop " bounding engineering " (Grain Boundary Engineering, GBE) this concept subsequently.Special grain boundary (Special Boundaries, SBs) is often referred to coincidence lattice grain boundary.Wherein coincidence site lattice (Coincidence Site Lattice, CSL) refer to two unlimited extensions, there is in identical dot matrix structure crystal relative to another crystal when the crystallographic axis of a certain low index rotates certain special angle, can get up in some lattice point position in the two crystal lattice in well-regulated coincidence, the lattice point of these overlapping positions will constitute three-dimensional superstructure in space.Misorientation relation between coincidence site lattice model two crystal but do not define the crystal geometry relation residing for crystal boundary face.Owing to up to the present measuring the common equipment of crystal orientation, such as EBSD, misorientation can only be measured, and the crystal geometry relation residing for crystal boundary face cannot be made.On the other hand, in material in addition to coherence twin boundary most crystal boundary be bending, even if can determine the crystallographic parameter in crystal boundary face, as the bending in crystal boundary face and constantly change, this gives the geometric parameter of fully defining crystal boundary, i.e. defines all degree of freedom and brings difficulty.Although there being result of study to show the most effectively to define the crystal geometry relation in crystal boundary face by single cross section trace analysis method and five parameter crystal boundary face algoscopys at present, they are that method based on probability statistics defines crystal boundary facial index, extensively should have the most immature.So, current most research work the most only uses misorientation to describe crystal boundary, i.e. the Σ value with coincidence site lattice model represents the feature of crystal boundary.Based on coincidence site lattice model, crystal boundary is divided into low Σ-CSL crystal boundary and random grain boundary.Low Σ-CSL crystal boundary refers to the crystal boundary of Σ≤29.And random grain boundary refers to general high-angle boundary and Σ > the CSL crystal boundary of 29.Having many experimental works to prove, low Σ-CSL crystal boundary has the characteristic being better than random grain boundary, ratio if any lower crystal boundary free energy, more preferable anti-Grain Boundary Segregation, more preferable decay resistance, more preferable anti-Grain Boundary Sliding performance etc..
Bounding engineering research at present focuses primarily upon the Face-centred Cubic Metals material of low stacking fault energy, and formation based on annealing twin improves the ratio of this kind of material low Σ-CSL crystal boundary.So having at a relatively high ratio annealing twin (Σ 3 crystal boundary) in Grain Boundary Character is distributed.So also known as bounding engineering based on annealing twin.The content of this area research specifically includes that research control and improves technological method for processing and the mechanism of low Σ-CSL crystal boundary ratio；Study some relevant performances of crystal boundary and low Σ-CSL crystal boundary ratio and spatial relationship thereof.The present invention will provide a kind of processing method obtaining special grain boundary at high proportion in tin bronze, have that equipment is simple and convenient to operate, technically reliable, efficiency is high and the advantage such as favorable repeatability.
Summary of the invention:
The invention provides a kind of processing method obtaining special grain boundary at high proportion in tin bronze, to realize being obtained the purpose of special grain boundary at high proportion by heat treatment method.
For achieving the above object, the present invention provides following technical scheme: a kind of processing method obtaining special grain boundary at high proportion in tin bronze, utilize thread-cutting tool will gather in the crops state material, described results state material specifically by tin bronze sheet material that cold deformation is 5% ~ 40% along roll to, laterally, normal direction cut 20,9 and 3 millimeters of workpiece several pieces respectively, then described workpiece is annealed in 400 ~ 800 ° of C environment；Annealing process is incubated 0.5 ~ 5h for being first placed in by workpiece in 400 ~ 800 DEG C of environment, then by its shrend to room temperature；Polish step by step with 200 ~ 2500# abrasive paper for metallograph again, then through mechanical polishing (2.5 μm SiC spraying polishing agent)；Then carrying out electrobrightening in polishing fluid, polish temperature is-20 ~-30 ° of C, and polishing voltage is 9 V, and polishing time is 90s.Polishing fluid can be suitable liquid of the prior art；The present invention provides a kind of phosphoric acid and the polishing fluid of deionized water mixed liquor, and its volume ratio is: the phosphoric acid of 70 %, the deionized water of 30 %.
Beneficial effects of the present invention: a kind of processing method obtaining special grain boundary at high proportion in tin bronze provided by the present invention, analyzes after tested, and with the rising of annealing temperature before perfect recrystallization annealing temperature, the ratio of special grain boundary significantly increases.The processing method obtaining special grain boundary at high proportion in tin bronze provided by the present invention, it is formation on the basis of the texture development rule in research QSn6 heat treatment process, test result shows, the texture that the Technology for Heating Processing that the present invention provides obtains is stable, Changing Pattern is obvious, the favorable repeatability of experiment.Technology for Heating Processing is easy to operate, and equipment is simple, technically reliable, and efficiency is high.
Accompanying drawing illustrates:
Fig. 1 provides results state tin bronze alloys material rear special grain boundary ratio variation diagram before heat treatment for embodiment；
Fig. 2 provides (a) results state tin bronze alloys material and through (b) 400 ° of C for embodiment, (c) 500 ° of C, (d) 600 ° of C, e the crystal boundary restructuring figure after () 700 ° of C and (f) 800 ° of C heat treatment 1h, in (f), arrow is linked up twin and the typical segments of random high angle crystal boundary segmentation.
Detailed description of the invention:
Below with reference to the drawings and specific embodiments, the present invention is described in detail.
The invention provides a kind of processing method obtaining special grain boundary at high proportion in tin bronze, it is characterised in that comprise the steps:
Utilize thread-cutting tool by tin bronze material, described tin bronze material is specifically by tin bronze sheet material that cold deformation is 5% ~ 40%, along roll to, laterally, normal direction cut the length of technological requirement respectively, obtain stereo structure workpiece several piece, as along roll to, laterally, normal direction cut 20,9 and 3 millimeters respectively, obtain cuboid bulk workpiece, then described workpiece is annealed in 400 ~ 800 ° of C environment；Annealing process is incubated 0.5 ~ 5h for being first placed in by workpiece in 400 ~ 800 DEG C of environment, then by its shrend to room temperature；Polish step by step with 200 ~ 2500# abrasive paper for metallograph again, successively with 200#, 400#, 800#, 1000#, 1500#, 2000# and 3000# sand papering；Again through mechanical polishing, as used 2.5 μm SiC spraying polishing agents；Then carrying out electrobrightening in polishing fluid, polish temperature is-20 ~-30 ° of C, and polishing voltage is 9 V, and polishing time sets according to technological requirement, is 60 200s.Polishing fluid can be suitable liquid of the prior art；The present invention provides a kind of phosphoric acid and the polishing fluid of deionized water mixed liquor, and its volume ratio is: the phosphoric acid of 60 78%, the deionized water of 22 40 %；More excellent proportioning is the phosphoric acid of 70 %, the deionized water of 30 %.Concrete holding temperature, 400 DEG C, 420 DEG C, 450 DEG C, 480 DEG C, 500 DEG C, 510 DEG C, 530 DEG C, 550 DEG C, 560 DEG C, 580 DEG C, 600 DEG C, 620 DEG C, 650 DEG C, 680 DEG C, 700 DEG C, 710 DEG C, 730 DEG C, 750 DEG C, 760 DEG C, 780 DEG C, 800 DEG C etc. can be chosen, concrete temperature retention time, 0.5h, 0.8h, 1.0h, 1.5h, 1.8h, 2.0h, 2.3h, 2.5h, 2.7h, 3.0h, 3.2h, 3.5h, 3.8h, 4.0h, 4.5h, 5h etc. can be chosen, the needs of the present invention can be met.
Listing the percentage ratio that various special grain boundary length is shared in total crystal boundary length in Fig. 1, the SBs (Special boundaries) in figure i.e. represents special proportion situation.For not carrying out the material of crystal boundary optimization, the ratio of its special grain boundary is typically smaller than 30%(such as should As-received state sample in figure).And it will be seen from figure 1 that after annealing temperature is more than 500 ° of C, the ratio of special grain boundary can be even up to 75% more than 60%, be therefore a high proportion of (or be interpreted as in unit volume grain boundary density the highest).
In Fig. 2, black lines represents that common crystal boundary, Lycoperdon polymorphum Vitt and blue lines all represent special grain boundary (Σ 3 special grain boundary).Fig. 2 (a) is the crystal boundary scattergram of the sample after deformation without annealing, the distribution situation of various crystal boundaries after can representing conventional process；And (b-f) correspondence respectively carries out 400-800 ° of C (with 100 ° of C for interval) respectively and optimizes the situation of sample after annealing.It can be seen that after annealing temperature is more than 500 ° of C, quantity and the density of special grain boundary representated by Lycoperdon polymorphum Vitt and blue lines all dramatically increase.
The thermomechanical annealing of the present invention processes can obtain low Σ-CSL crystal boundary, obtain special grain boundary at high proportion, its mechanism is as follows: for the face-centred cubic structure metal that stacking fault energy is relatively low, accidental atomic plane staggered arrangement can occur during thermomechanical annealing, { 111} twin (has Σ 3 special grain boundary) in generation, and the common Grain-Boundary Phase interaction that in follow-up insulating process, this Σ 3 special grain boundary can move with other and produce increment, and then to make low Σ-CSL crystal boundary (be particularly Σ 3n, n=1,2,3) dramatically increase.
Finally it should be noted that, above example is only in order to illustrate technical scheme rather than restriction technologies scheme, although the present invention has been described in detail by applicant with reference to preferred embodiment, it will be understood by those within the art that, technical scheme is modified or equivalent by those, without deviating from objective and the scope of the technical program, all should contain in the middle of scope of the presently claimed invention.
Claims (3)
1. the processing method obtaining special grain boundary at high proportion in tin bronze, it is characterised in that comprise the following steps:
(1)
The preparation of workpiece:
Utilize thread-cutting tool by tin bronze sheet material that cold deformation is 5% ~ 40% along roll to, laterally, normal direction cut certain length respectively, it is thus achieved that stereochemical structure workpiece several piece；
(2)
The heat treatment of workpiece:
Being annealed in 400 ~ 800 ° of C environment by workpiece, its annealing process is incubated 0.5 ~ 5h for being first placed in by workpiece in 400 ~ 800 DEG C of environment, then by its shrend to room temperature；
(3)
The polishing of workpiece:
Workpiece after heat treatment is sequentially passed through 200 ~ 2500# abrasive paper for metallograph polish step by step, be then passed through mechanical polishing；In-20 ~-30 ° of C electrolytic polishing liquids, under the conditions of voltage 9V, electrochemical polish sets the time the most again.
A kind of processing method obtaining special grain boundary at high proportion in tin bronze the most according to claim 1, it is characterised in that: in step (1), tin bronze sheet material along roll to, laterally, normal direction cut 20,9 and 3 millimeters respectively, it is thus achieved that cuboid workpiece.
A kind of processing method obtaining special grain boundary at high proportion in tin bronze the most according to claim 1, it is characterised in that: in step (3), described polishing fluid, the volume ratio of component is: the phosphoric acid of 70 %, the deionized water of 30 %.
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Cited By (5)
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| CN108754386A (en) * | 2018-07-27 | 2018-11-06 | 北方工业大学 | Thermal shock resistant MCrAlY coating and preparation method thereof |
| CN109668839A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院化学研究所 | A method of identifying copper sheet crystal boundary and crystal face |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN112326656A (en) * | 2020-10-28 | 2021-02-05 | 福建工程学院 | Quantitative characterization method for grain boundary interface matching |
| CN114686789A (en) * | 2022-04-12 | 2022-07-01 | 福建工程学院 | Method for improving pure copper grain boundary corrosion resistance by increasing proportion of coherent twin grain boundary |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109668839A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院化学研究所 | A method of identifying copper sheet crystal boundary and crystal face |
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| CN112326656B (en) * | 2020-10-28 | 2023-06-02 | 福建工程学院 | Quantitative characterization method for matching grain boundary interface |
| CN114686789A (en) * | 2022-04-12 | 2022-07-01 | 福建工程学院 | Method for improving pure copper grain boundary corrosion resistance by increasing proportion of coherent twin grain boundary |
| CN114686789B (en) * | 2022-04-12 | 2023-09-01 | 福建工程学院 | Method for improving pure copper grain boundary corrosion resistance by increasing coherent twin boundary proportion |
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