CN107675011A - A kind of preparation method of TiB2/Cu materials - Google Patents
A kind of preparation method of TiB2/Cu materials Download PDFInfo
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- CN107675011A CN107675011A CN201710797172.XA CN201710797172A CN107675011A CN 107675011 A CN107675011 A CN 107675011A CN 201710797172 A CN201710797172 A CN 201710797172A CN 107675011 A CN107675011 A CN 107675011A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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Abstract
The invention discloses a kind of TiB2The preparation method of/Cu materials, TiB is prepared for using the method for jet deposition2/ Cu composites, in vacuum induction melting copper-titanium alloy；Copper-titanium alloy Boron Coated powder jet deposition；High temperature sintering reaction in-situ；Then TiB is obtained2/ Cu alloys.Composition of the present invention is reasonable, and alloying level is high, and simple production process is easy to operate.The TiB of the present invention2/ Cu composites are compared with traditional casting method with crystal grain is tiny, alloying element gross segregation is small, the uniform advantage of composition, hardly introduce impurity, improve the electric conductivity and mechanical property of alloy, it can be used in Aero-Space high-performance conductive elastic element, such as the application of lead frame and electrical contact etc..
Description
Technical field
The invention belongs to ceramic particle phase TiB2Strengthen metal-base composites preparing technical field, and in particular to a kind of
TiB2The preparation method of/Cu materials.
Background technology
Copper and its copper alloy are widely used in highly conductive and high heat conduction working environment, when operating ambient temperature exceedes
The intensity of alloy and creep-resistant property are decreased obviously during the softening temperature of alloy, thus improve alloy high-temp stability have it is important
Meaning.Due to ceramic particle phase TiB2With fusing point is high, hardness is high, modulus of elasticity is high, thermal coefficient of expansion is low and high-temperature stability
The characteristics of good, therefore can be used for strengthening Cu-base composites.The method for preparing TiB2/Cu composites has mechanical alloying
The activity of method, contact reaction method, self-propagating high-temperature reaction and spray deposition, titanium and boron is all higher, in ma process
Easily oxidation, enhancing phase is easily reunited when high-temp in-situ reacts, and direct quick shaping process has compared with classical production process
Strong adaptability, cost is low, also has competitiveness in performance, particle enhancing Reinforced Cu-Base Composites is turned into most possible and realizes
One of new material of industrialization.
The content of the invention
It is an object of the invention to provide a kind of TiB2The preparation method of/Cu composites, solves ceramic particle reinforced phase
The problem of reuniting and be thick, alloy is reduced because ball milling causes the phenomenon more than impurity content, improves TiB2Enhancing mutually and matrix it
Between contact wetting, ensure alloy structure it is more uniform, there is higher intensity and electric conductivity.
To achieve the above object, the present invention uses following technical scheme：
A kind of TiB2The preparation method of/Cu materials, comprises the following steps：
Step 1, prepared by copper-titanium alloy；
Weigh a certain amount of fine copper and pure titanium block is surface-treated, under the conditions of protective atmosphere, in vacuum induction melting
Melting in stove；
Step 2, material mixture ratio；
A certain amount of melted copper-titanium alloy and boron powder are weighed, determines that actual boron powder is used according to the proportion of goods damageds during powder feeding
Amount；
Step 3, alloy melting；
Copper-titanium alloy is put into intermediate frequency furnace in crucible, the boron powder of certain mass is put into powder feeding room, uses vacuum
Induction furnace carries out melting；
Step 4, jet deposition；
Determine that spray deposition technology parameter, including atomizing pressure, nozzle diameter, deposited distance, deposition rotating speed, aluminium alloy reach
Jet deposition and coated composite powder operation are carried out after to certain degree of superheat；
Step 5, in-situ sintering；
The deposit preform that step 4 obtains will be sintered in atmosphere protection tube furnace, obtained after the completion of sintering
TiB2/ Cu ceramic particles strengthen Cu-base composites.
As the further scheme of the present invention, protective atmosphere is argon gas in the step 1, and titanium accounts for the 2- of alloy gross mass
3wt%, copper account for the 97-98wt% of alloy gross mass, remelting 2-3 times repeatedly during melting copper titanium, ensure the uniformity of alloy cast ingot.
As the further scheme of the present invention, Cu, Ti, B ratio are 96.5-98% in the step 2：1.5-2.5%：
0.5-1%, the proportion of goods damageds 20-40%, powder feeding air-flow 10-25L/min, powder feeding motor speed 50-120r/ of boron powder in blending process
min。
As the further scheme of the present invention, the step 3 fusion process vacuum reaches 5-9 × 10-2Argon is filled with after Pa
For gas to+0.02-0.1MPa, the rate of heat addition is about 1-2 DEG C/s, and the degree of superheat is 200-250 DEG C, is incubated 5-8min at such a temperature.
As the further scheme of the present invention, spray deposition technology in the step 4:Atomization gas is nitrogen, atomization gas
Pressure 2.5-4MPa, nozzle diameter 3-5mm, deposited distance 140-190mm, sediment pan rotating speed 30-100r/min, powder feeding powder feeding speed
Rate is 25-45g/min.
As the further scheme of the present invention, the reaction of step 5 high-temp in-situ is carried out in argon gas atmosphere protection tube furnace, is burnt
Junction temperature is 900-950 DEG C, sintering time 50-70min.
The beneficial effects of the invention are as follows：The TiB of the present invention2/ Cu composites have introducing miscellaneous compared to mechanical attrition method
The characteristics of quality is few, technique simplifies；Spray deposition has the characteristics of small gross segregation, even tissue compared with casting method,
Nano boron powder is sent in lithosomic body by Models of Spray Deposition, can obtain TiB more, that size is more tiny2Nanometer enhancing
Phase, hence it is evident that the electric conductivity and mechanical property of alloy are improved, available for the high property electrically conductive elastic of high-temperature copper alloy operation and Aero-Space
Device.
Brief description of the drawings
Fig. 1 is flow chart of steps of the present invention；
Fig. 2 is alloy interior tissue pattern in the embodiment of the present invention；
Fig. 3 is the micro-organization chart of the embodiment of the present invention；
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of as shown in figure 1, TiB2The preparation method of/Cu materials, comprises the following steps：
Step 1, prepared by copper-titanium alloy；
Weigh a certain amount of fine copper and pure titanium block is surface-treated, under the conditions of protective atmosphere, in vacuum induction melting
Melting in stove；
Step 2, material mixture ratio；
A certain amount of melted copper-titanium alloy and boron powder are weighed, determines that actual boron powder is used according to the proportion of goods damageds during powder feeding
Amount；
Step 3, alloy melting；
Copper-titanium alloy is put into intermediate frequency furnace in crucible, the boron powder of certain mass is put into powder feeding room, uses vacuum
Induction furnace carries out melting；
Step 4, jet deposition；
Determine that spray deposition technology parameter, including atomizing pressure, nozzle diameter, deposited distance, deposition rotating speed, aluminium alloy reach
Jet deposition and coated composite powder operation are carried out after to certain degree of superheat；
Step 5, in-situ sintering；
The deposit preform that step 4 obtains will be sintered in atmosphere protection tube furnace, obtained after the completion of sintering
TiB2/ Cu ceramic particles strengthen Cu-base composites.
Embodiment 1
A certain proportion of copper-titanium alloy ingot casting is prepared first, and the mass fraction of titanium is 2.0wt%, weighs the copper of certain mass
Titan alloy casting ingot is as deposition raw material, according to Cu:Ti:B=97:2.1:The quality of 0.9 ratio-dependent boron powder.Determine powder feeding work
Skill parameter：Powder feeding motor speed 120r/min, air-flow size are 25L/min.Vacuumized using three pole vacuum pump systems, this
Secondary melting vacuum is 0.1Pa, and argon gas is+0.01MPa as protective atmosphere, argon gas amount, is added using vacuum induction melting
Heat, the rate of heat addition are 2 DEG C/s, and the degree of superheat is 250 DEG C, and 8min, the spray deposition technology of use are incubated after being heated to predetermined temperature：
Atomization pressure is 3.5MPa, and nozzle diameter 4mm, sediment pan is away from nozzle 175mm, sediment pan rotating speed 50r/min.This deposition
Process is 15s, deposited samples quality 750g.High-temperature atmosphere sintering processes, sintering temperature 950 are carried out to sample after the completion of deposition
DEG C, sintering time 60min, TiB is obtained after the completion of sintering2/ Cu ceramic particles strengthen Cu-base composites.Obtained alloy examination
Sample consistency is 95.9%, conductance 22%IACS, hardness 93HBS.
Fig. 2 is deposited samples interior tissue pattern made from the present embodiment, and alloy grain size is in 10m or so, enhancing phase
Quantity is more, size is small, and Dispersed precipitate is in matrix.
Fig. 3 is TiB manufactured in the present embodiment2/ Cu composite microscopic appearances, it can be seen that have in copper crystal grain strip and
Graininess Ti and B strengthen phase.
Embodiment 2
A certain proportion of copper-titanium alloy ingot casting is prepared, the mass fraction of titanium is 2.0wt%, and the copper titanium for choosing certain mass closes
Gold is used as jet deposition raw material, according to Cu:Ti:B=97:2:1 ratio carries out proportioning alloy, true according to the scaling loss of powder feeding process
Determine the quality of boron powder；Determine powder feeding technological parameter：Separated motor rotating speed 115r/min is sent, air-flow size is 25L/min.；Using three
Pole vacuum pump system is vacuumized, and this melting vacuum is 1Pa, and for argon gas as protective atmosphere, argon gas amount is+0.1MPa,
Heated using vaccum sensitive stove, the rate of heat addition is 2 DEG C/s, and the degree of superheat is 250 DEG C, is incubated after being heated to predetermined temperature
10min；The spray deposition technology of use：Atomization pressure is 3.6MPa, and nozzle diameter 3.5mm, sediment pan is away from nozzle
175mm, sediment pan rotating speed 50r/min；Jet deposition, deposition process 20s, deposited samples quality are carried out after normally going out powder
765g.Sample is subjected to high-temperature atmosphere sintering processes after the completion of deposition, sintering temperature is 940 DEG C, sintering time 65min, is burnt
TiB is obtained after the completion of knot2/ Cu ceramic particles strengthen Cu-base composites.Obtained alloy sample consistency is 94.6%, conductive
Rate is 26.4%IACS, hardness 96HBS.
Embodiment 3
A certain proportion of copper-titanium alloy ingot casting is prepared, the mass fraction of titanium is 2.0wt%, and the copper titanium for choosing certain mass closes
Gold is used as jet deposition raw material, according to Cu:Ti:B=97:1.9:1.1 ratio carries out proportioning alloy, according to the burning of powder feeding process
Damage determines the quality of boron powder；Determine powder feeding technological parameter：Separated motor rotating speed 125r/min is sent, air-flow size is 20L/min；Using
Three pole vacuum pump systems are vacuumized, and this melting vacuum is 0.5Pa, argon gas as protective atmosphere, argon gas amount for+
0.03MPa, heated using vaccum sensitive stove, the rate of heat addition is 2 DEG C/s, and the degree of superheat is 300 DEG C, after being heated to predetermined temperature
It is incubated 5min；The spray deposition technology of use：Atomization pressure is 4MPa, nozzle diameter 3mm, sediment pan away from nozzle 170mm,
Sediment pan rotating speed 60r/min；Jet deposition, deposition process 25s, deposited samples quality 804g are carried out after normally going out powder.Deposition
After the completion of sample is subjected to high-temperature atmosphere sintering processes, sintering temperature is 960 DEG C, sintering time 55min, after the completion of sintering
To TiB2/ Cu ceramic particles strengthen Cu-base composites.Obtained alloy sample consistency is 95.5%, conductance 22%
IACS, hardness 97HBS.
Described above is present pre-ferred embodiments, for the ordinary skill in the art, according to the present invention's
Teaching, in the case where not departing from the principle of the present invention and spirit, the changes, modifications, replacement and the change that are carried out to embodiment
Type is still fallen within protection scope of the present invention.
Claims (6)
- A kind of 1. TiB2The preparation method of/Cu materials, it is characterised in that comprise the following steps：Step 1, prepared by copper-titanium alloy；Weigh a certain amount of fine copper and pure titanium block is surface-treated, under the conditions of protective atmosphere, in vacuum induction melting furnace Melting；Step 2, material mixture ratio；A certain amount of melted copper-titanium alloy and boron powder are weighed, actual boron powder dosage is determined according to the proportion of goods damageds during powder feeding；Step 3, alloy melting；Copper-titanium alloy is put into intermediate frequency furnace in crucible, the boron powder of certain mass is put into powder feeding room, uses vacuum induction Stove carries out melting；Step 4, jet deposition；Determine that spray deposition technology parameter, including atomizing pressure, nozzle diameter, deposited distance, deposition rotating speed, aluminium alloy reach one Jet deposition and coated composite powder operation are carried out after determining the degree of superheat；Step 5, in-situ sintering；The deposit preform that step 4 obtains will be sintered in atmosphere protection tube furnace, TiB is obtained after the completion of sintering2/Cu Ceramic particle strengthens Cu-base composites.
- 2. TiB according to claim 12The preparation method of/Cu materials, it is characterised in that protective atmosphere in the step 1 For argon gas, titanium accounts for the 2-3wt% of alloy gross mass, and copper accounts for the 97-98wt% of alloy gross mass, remelting 2- repeatedly during melting copper titanium 3 times, ensure the uniformity of alloy cast ingot.
- 3. TiB according to claim 12The preparation method of/Cu materials, it is characterised in that Cu, Ti, B in the step 2 Ratio is 96.5-98%：1.5-2.5%：0.5-1%, the proportion of goods damageds 20-40%, powder feeding air-flow 10- of boron powder in blending process 25L/min, powder feeding motor speed 50-120r/min.
- 4. TiB according to claim 12The preparation method of/Cu materials, it is characterised in that step 3 fusion process is true Reciprocal of duty cycle reaches 5-9 × 10-2Argon gas is filled with after Pa to+0.02-0.1MPa, the rate of heat addition is about 1-2 DEG C/s, degree of superheat 200- 250 DEG C, 5-8min is incubated at such a temperature.
- 5. TiB according to claim 12The preparation method of/Cu materials, it is characterised in that jet deposition in the step 4 Technique:Atomization gas is nitrogen, atomization gas pressure 2.5-4MPa, nozzle diameter 3-5mm, deposited distance 140-190mm, sediment pan Rotating speed 30-100r/min, powder feeding powder feeding rate are 25-45g/min.
- 6. TiB according to claim 12The preparation method of/Cu materials, it is characterised in that the reaction of step 5 high-temp in-situ exists Carried out in argon gas atmosphere protection tube furnace, sintering temperature is 900-950 DEG C, sintering time 50-70min.
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| CN201710797172.XA CN107675011B (en) | 2017-09-06 | 2017-09-06 | A kind of preparation method of TiB2/Cu material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559866A (en) * | 2018-05-15 | 2018-09-21 | 西安理工大学 | A kind of high-strength high-conductivity Cu-Ti alloys and preparation method thereof |
| CN108570572A (en) * | 2018-05-15 | 2018-09-25 | 西安理工大学 | A kind of nano oxide dispersion strengthens Cu-Ti alloys and preparation method thereof |
| CN109207764B (en) * | 2018-09-26 | 2020-10-27 | 西安理工大学 | Method for strengthening CuW alloy by in-situ autogenous titanium diboride |
| CN112760521A (en) * | 2021-01-28 | 2021-05-07 | 株洲艾美新材料有限公司 | Beryllium-copper alloy and preparation method thereof |
| CN115433848A (en) * | 2022-09-30 | 2022-12-06 | 西安理工大学 | Preparation method of boride particle reinforced copper-based composite material |
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|---|---|---|---|---|
| CN1940103A (en) * | 2005-09-30 | 2007-04-04 | 中南大学 | Cu.TiB nano-diffusion alloy and its production |
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2017
- 2017-09-06 CN CN201710797172.XA patent/CN107675011B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940103A (en) * | 2005-09-30 | 2007-04-04 | 中南大学 | Cu.TiB nano-diffusion alloy and its production |
Non-Patent Citations (2)
| Title |
|---|
| JONGSANG LEE，等: "Microstructure and properties of titanium boride dispersed Cu alloys fabricated by spray forming", 《MATERIALS SCIENCE AND ENGINEERING A》 * |
| 刘建华: "《材料成型工艺基础（第3版）》", 29 February 2016 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559866A (en) * | 2018-05-15 | 2018-09-21 | 西安理工大学 | A kind of high-strength high-conductivity Cu-Ti alloys and preparation method thereof |
| CN108570572A (en) * | 2018-05-15 | 2018-09-25 | 西安理工大学 | A kind of nano oxide dispersion strengthens Cu-Ti alloys and preparation method thereof |
| CN109207764B (en) * | 2018-09-26 | 2020-10-27 | 西安理工大学 | Method for strengthening CuW alloy by in-situ autogenous titanium diboride |
| CN112760521A (en) * | 2021-01-28 | 2021-05-07 | 株洲艾美新材料有限公司 | Beryllium-copper alloy and preparation method thereof |
| CN112760521B (en) * | 2021-01-28 | 2022-01-14 | 株洲艾美新材料有限公司 | Beryllium-copper alloy and preparation method thereof |
| CN115433848A (en) * | 2022-09-30 | 2022-12-06 | 西安理工大学 | Preparation method of boride particle reinforced copper-based composite material |
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