CN110523776A - A kind of even high-throughput preparation of ternary diffusion and heat treatment method - Google Patents
A kind of even high-throughput preparation of ternary diffusion and heat treatment method Download PDFInfo
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- CN110523776A CN110523776A CN201910794666.1A CN201910794666A CN110523776A CN 110523776 A CN110523776 A CN 110523776A CN 201910794666 A CN201910794666 A CN 201910794666A CN 110523776 A CN110523776 A CN 110523776A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
- C21D1/42—Induction heating
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of even high-throughput preparation of ternary diffusion and heat treatment methods, this method comprises: sheet metal strip prepares, band fluting, polishing, pickling, the composite strip of three kinds of materials is obtained by cold compound or hot composite rolling, then it is sealed against in quartz ampoule, heat treatment is diffused to sample using high-frequency induction heating, can once prepare the diffusion couple of temperature consecutive variations.The present invention is easily achieved, success rate height, efficient quick, and can save a large amount of experimental period, is of great significance for the exploitation of alloy phase diagram.
Description
Technical field
The present invention relates to diffusion couple preparation and diffusion couple Field of Heat-treatment, specially a kind of even high-throughput preparation of ternary diffusion
With diffusion heat treatments method.
Technical background
For material science, phasor is to indicate the balance existence condition of various phases in metal or alloy and respectively balance each other
A kind of concise diagram of Coexistence, is material development, production and the important references of processing data, carries out green wood for scientific research personnel
The offer reliable basis of research and development is provided.
Usual scientific research personnel generally uses the method for diffusion couple to provide related data for the drafting of phasor.Conventional diffusion is occasionally made
The basic principle of standby technology is: different pure metal or alloy being tied up, carried out at long-time diffusion under assigned temperature
Reason, forms diffusion layer in the boundary of each metal, the composition in diffusion layer is mutually exactly that the system exists at such a temperature
Phase.
Traditional diffusion couple preparation method has the disadvantage that
(1) it is often difficult to find suitable method offer interface binding power to ensure combining closely for diffusion couple, and guarantees to expand
Scattered constituent element can be smoothly through interface and be diffused, and success rate is low.
(2) when diffusion couple is diffused processing, the diffusion couple DIFFUSION TREATMENT time is long, and generally -60 days 5 days, and one
A sample or a kind of alloy can only be handled at a temperature, if to carry out multi-temperature section diffusion couple research, it is necessary to successively into
Row, it is low efficiency, at high cost.
Summary of the invention
In view of the problems of the existing technology, the high pass for providing a kind of diffusion couple prepares and diffusion heat treatments side by the present invention
Method.The method that the present invention uses composite rolling obtains multi-element metal composite strip, then using high-frequency induction heating to composite band
Material is heat-treated, and the diffusion couple of temperature consecutive variations is obtained.
The present invention be solve its technical problem and the technical solution adopted is that:
(1) raw material prepare: being required according to sample, prepare 3 kinds of pure metal bands, most cheap metal band by size requirement
Fluting, whole bands carry out surface polishing, pickling.
(2) Rolling compund: first three kinds of bands are positioned, it is ensured that metal 2 is embedded in 1 slot of metal, and metal 3 covers completely
Lid metal 2.When cold laminating rolling, the deflection of single pass is in 70%-75%.When heat is laminating, the deflection of single pass is in 50%-
60%, the laminating temperature of heat is determined by metallic character.
(3) vacuum sealing tube: intercepting the composite strip being well combined, length 20-30cm, the edge of composite strip every
Certain distance makes marks, and is convenient for subsequent thermometric and record.Composite strip is placed in quartz ampoule, it will using quartz ampoule tube sealing machine
It is sealed, and sealing area is vacuum or inert gas shielding atmosphere.
(4) diffusion heat treatments: HF induction heating apparatus is used, radio-frequency induction coil is individual pen, the composite band being sealed
The center of material is placed in induction coil position, and induction heating power is advisable so that composite strip is non-fusible, as high as possible.Stablize to temperature
Afterwards, the temperature and record of each mark are measured using infrared radiation thermometer.The continuous heat time is 1h-12h.
(5) prepared by sample: after the heat treatment time for reaching design, closing Efco-Northrup furnace, the quartz ampoule of sample will be housed
Chilling into the water takes out sample, and the corresponding temperature of each label is truncated in mark, obtains the diffusion couple of different temperatures,
Carry out subsequent detection analysis.
Beneficial effects of the present invention:
(1) composite strip is prepared using composite rolling, is used for diffusion couple sample, the sample block combination interface of solution loosely etc. is asked
Topic, substantially increases successfully efficiency.
(2) composite strip is prepared using composite rolling, is used for diffusion couple sample, length is controllable, and composite strip can be with
Make multiple samples.
(3) interface of composite strip is mechanical snap (cold composite rolling) or metallurgical bonding (hot composite rolling), in conjunction with jail
Gu substantially reducing the time of diffusion heat treatments, the diffusion couple heat treatment time of conventional method preparation is generally 5-60 days, and is adopted
1-12h is only needed with the method, working efficiency greatly improves.
(4) heat treatment is diffused using high-frequency induction heating, local heating is carried out to composite strip, utilizes metal itself
Heat conductivity, can once make the diffusion couple of temperature consecutive variations, and conventional method can only once do a temperature spot
Diffusion couple, working efficiency greatly improve.
Detailed description of the invention
Fig. 1: composite strip schematic diagram,
Fig. 2: composite strip equidistantly punches label,
Fig. 3: diffusion couple is heat-treated schematic diagram
Specific embodiment
A kind of even high-throughput preparation of ternary diffusion of the invention and heat treatment method, comprising the following steps:
Step 1: preparing 3 kinds of pure metal bands, i.e. metal 1, metal 2 and metal 3 by size requirement；
Step 2: one of is band slotted metal；
Step 3: whole bands carry out surface polishing, pickling；
Step 4: three kinds of bands are cold compound or hot composite rolling；
Step 5: the composite strip of interception suitable length, is evacuated and hermetically sealed in quartz glass tube；
Step 6: being heated using high-frequency induction to sample；
Step 7: preparing the diffusion couple of temperature consecutive variations, subsequent detection analysis is carried out.
Three kinds of metals in the step 1 are both needed to certain cold or thermal processing distortion ability, 1 strip width of metal
For 10-20mm, thickness 2-3mm, 2 strip width of metal is 0.2-0.5 times of 1 width of metal, with a thickness of the 0.6- of 1 thickness of metal
0.7 times, the width of metal 3 is greater than the width of metal 2, less than or equal to the width of metal 1, metal 3 with a thickness of 1-2mm.
Band slotted metal in the step 2 is metal 1, and groove depth is 2 thickness -0.05mm of metal, the width of fluting
Degree is 2 width+0.05mm of metal.
The step 3 is: in order to guarantee strip surface cleaning, improving composite strip binding force, all strips surface is both needed to
Polishing, and carry out pickling, it is ensured that faying face free from admixture, no greasy dirt.
The step 4 is: first positioning to three kinds of bands, it is ensured that metal 2 is embedded in 1 slot of metal, and metal 3 is complete
Metal 2 is covered, when cold laminating rolling, the deflection of single pass is in 70%-75%, and when heat is laminating, the deflection of single pass exists
50%-60%, the laminating temperature of heat are determined by metallic character.
The step 5 is: intercepting the composite strip being well combined, length 20-30cm is every at the edge of composite strip
It makes marks at a certain distance, is convenient for subsequent thermometric and record, composite strip is placed in quartz ampoule, using quartz ampoule tube sealing machine
It is sealed against, sealing area is vacuum or inert gas shielding atmosphere.
The step 6 is: radio-frequency induction coil is individual pen, and the center for the composite strip being sealed is placed in induction coil position,
Induction heating power is advisable so that composite strip is non-fusible, as high as possible, after temperature is stablized, is measured using infrared radiation thermometer each
The temperature and record of mark, continuous heat time are 1-12h.
The step 7 is: the corresponding temperature of each label is truncated in mark, carries out sample preparation in case subsequent inspection
Survey analysis.
The preparation of embodiment 1:Cu-Au-Ag diffusion couple high throughput
(1) prepare pure metal band, specific size is shown in Table 1
(2) the standby band of institute is subjected to surface polishing, pickling, rinsing and drying.
(3) band positions: by Au band insertion Cu slot, Ag band is overlying on Cu belt surface, and Au band is completely covered.
(4) composite rolling, single pass deformation cold composite rolling: are carried out using cold compound special rolling mill to the band having good positioning
Amount is 75%, so that three kinds of bands is realized mechanical snap and is firmly combined.
(5) sample interception and label: the composite strip that selection is well combined, length is 30cm, at the edge of composite strip
A line is carved every 10mm to make marks.
(6) vacuum sealing tube: the composite strip of interception being placed in 40cm long quartz ampoule, is first vacuumized, then using quartz
Dedicated tube sealing machine is managed to seal it.
(7) High frequency induction hardening: using sub-thread coil, the middle position of composite strip be put in induction coil position, by
Induction heating power is gradually slowly increased, using the temperature of the composite strip of infrared radiation thermometer measurement induction coil corresponding position, to temperature
When degree reaches 750 DEG C or so, stop power per liter.After temperature is stablized, keep induction heating power constant, using infrared radiation thermometer
Measure the temperature of each mark position, so the corresponding temperature in each position, and the right and left be it is symmetrical, once can be with
Two mutually synthermal positions are made, convenient for examining the accuracy of subsequent experimental.The induction heating time is 5h.Heat treatment is completed
Afterwards, entire quartz is thrown away in water, it is made to keep high temperature microstructure as far as possible.
(8) it the preparation of different temperatures diffusion couple: is truncated in each mark position, obtains the Cu-Au- under different temperatures
Ag ternary diffusion is even, and there are two samples for each temperature, then by its sample preparation, then carry out subsequent analysis detection and analysis.
The preparation of embodiment 2:Cu-Ag-Ni diffusion couple high throughput
(1) prepare pure metal band, specific size is shown in Table 2.
Table 2
(2) the standby band of institute is subjected to surface polishing, pickling, rinsing and drying.
(3) hot composite rolling: composite rolling is carried out using the compound special rolling mill of heat, hot combined temp is 600 DEG C, compound speed
Degree is 1.5m/min, and protective atmosphere is ammonia dissolving atmosphere, and single pass heavy deformation 55%, under temperature action, three kinds of metals have
Certain metallurgical bonding.
(4) sample interception and label: the composite strip that selection is well combined, length is 32cm, at the edge of composite strip
A line is carved every 8mm to make marks.
(6) vacuum sealing tube: the composite strip of interception being placed in 40cm long quartz ampoule, is first vacuumized, then using quartz
Dedicated tube sealing machine is managed to seal it.
(7) High frequency induction hardening: using sub-thread coil, the middle position of composite strip be put in induction coil position, by
Induction heating power is gradually slowly increased, using the temperature of the composite strip of infrared radiation thermometer measurement induction coil corresponding position, to temperature
When degree reaches 760 DEG C or so, stop power per liter.After temperature is stablized, keep induction heating power constant, using infrared radiation thermometer
The temperature of each mark position is measured, the corresponding temperature in position each in this way, the induction heating time is 8h.Heat treatment is completed
Afterwards, entire quartz is thrown away in water, it is made to keep high temperature microstructure as far as possible.
(8) it the preparation of different temperatures diffusion couple: is truncated in each mark position, obtains the Cu-Ag- under different temperatures
Ni ternary diffusion is even, and there are two samples for each temperature tool, then by its sample preparation, then carry out subsequent analysis detection and analysis.
Claims (8)
1. a kind of even high-throughput preparation of ternary diffusion and heat treatment method, it is characterised in that the following steps are included:
Step 1: preparing 3 kinds of pure metal bands, i.e. metal 1, metal 2 and metal 3 by size requirement；
Step 2: one of is band slotted metal；
Step 3: whole bands carry out surface polishing, pickling；
Step 4: three kinds of bands are cold compound or hot composite rolling；
Step 5: the composite strip of interception suitable length, is evacuated and hermetically sealed in quartz glass tube；
Step 6: being heated using high-frequency induction to sample；
Step 7: preparing the diffusion couple of temperature consecutive variations, subsequent detection analysis is carried out.
2. the even high-throughput preparation of ternary diffusion and heat treatment method according to claim 1, it is characterised in that: the step 1
In three kinds of metals be both needed to certain cold or thermal processing distortion ability, 1 strip width of metal is 10-20mm, thickness 2-
3mm, 2 strip width of metal are 0.2-0.5 times of 1 width of metal, with a thickness of 0.6-0.7 times of 1 thickness of metal, the width of metal 3
Degree is greater than the width of metal 2, less than or equal to the width of metal 1, metal 3 with a thickness of 1-2mm.
3. the even high-throughput preparation of ternary diffusion and heat treatment method according to claim 1, it is characterised in that: the step 2
In band slotted metal be metal 1, groove depth is 2 thickness -0.05mm of metal, the width of fluting be 2 width of metal+
0.05mm。
4. requiring the even high-throughput preparation of 1 ternary diffusion and heat treatment method according to sharp, it is characterised in that: the step
Three, in order to guarantee strip surface cleaning, composite strip binding force is improved, all strips surface is both needed to polish, and carries out pickling, really
Protect faying face free from admixture, no greasy dirt.
5. the even high-throughput preparation of ternary diffusion and heat treatment method according to claim 1, it is characterised in that: the step
Four, first three kinds of bands are positioned, it is ensured that metal 2 is embedded in 1 slot of metal, and metal 3 is completely covered metal 2, cold laminating to roll
When processed, the deflection of single pass is in 70%-75%, and when heat is laminating, the deflection of single pass is in 50%-60%, the laminating temperature of heat
It is determined by metallic character.
6. the even high-throughput preparation of ternary diffusion and heat treatment method according to claim 1, it is characterised in that: the step
Five, the composite strip being well combined is intercepted, length 20-30cm makes marks, just at a certain distance at the edge of composite strip
In subsequent thermometric and record, composite strip is placed in quartz ampoule, is sealed against using quartz ampoule tube sealing machine, sealing area is
Vacuum or inert gas shielding atmosphere.
7. the even high-throughput preparation of ternary diffusion and heat treatment method according to claim 1, it is characterised in that: the step
Six, radio-frequency induction coil is individual pen, and the center for the composite strip being sealed is placed in induction coil position, and induction heating power is with compound
Band is non-fusible to be advisable, as high as possible, and after temperature is stablized, the temperature and note of each mark are measured using infrared radiation thermometer
Record, continuous heat time are 1-12h.
8. the even high-throughput preparation of ternary diffusion and heat treatment method according to claim 1, which is characterized in that the step
Seven, the corresponding temperature of each label is truncated in mark, carries out sample preparation in case subsequent detection is analyzed.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113189127A (en) * | 2021-04-13 | 2021-07-30 | 昆明贵金属研究所 | Method for preparing high-melting-point metal ternary diffusion couple |
| CN113238020A (en) * | 2021-04-13 | 2021-08-10 | 贵研铂业股份有限公司 | Method for rapidly researching and developing novel electric contact material |
| CN113899603A (en) * | 2021-09-16 | 2022-01-07 | 贵研铂业股份有限公司 | Method for preparing diffusion couple by hole type rolling mill |
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| CN113189127A (en) * | 2021-04-13 | 2021-07-30 | 昆明贵金属研究所 | Method for preparing high-melting-point metal ternary diffusion couple |
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