CN1710124A - Method for preparing reactive hot-press in-situ autogenesis copper-base composite material - Google Patents
Method for preparing reactive hot-press in-situ autogenesis copper-base composite material Download PDFInfo
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Abstract
The invention discloses a preparation technique of reaction heat pressing original position autogeny copper base material, relates to preparation technique of a copper base material applied to micro electric industry. Focusing on the problem that existing original position autogeny preparation technique is of expensive devices, complex operation while the product is hard to specify. The technique is achieved through following steps: a, put powder of Ti, B, Cu into ball milling cylinder and vacuum the cylinder, aerate with argon gas, blend the mixed powder for 6 to 12 hours for while the ratio of grinding media to material is 1 to 20 : 1 and rotating speed at 200 to 400 round per minutes; b: shape the blended powder in black lead moulds making the density to 20 to 40 percent; c, sinter the powder together with the mould into vacuum heat press furnace and make the density to 90 to 99 percent, furnace cool to room temperature, unmould to acquire the TiB2/Cu complex material. The device in the invention is of simple and easy operation, the volume fraction is easy to control while the reaction temperature needs not to be very high and without side reaction product.
Description
The technical field is as follows:
the invention relates to a preparation process of a copper-based composite material for the microelectronic industry, in particular to a preparation process of a powder metallurgy reaction hot-pressing in-situ authigenic copper-based composite material.
Background art:
with the continuous development of information technology, the microelectronic industry has higher and higher requirements for conductive metal materials, and the trend of the requirements is to expect that the conductive metal materials have high conductivity, high strength and high temperature resistance. The indexes of the current microelectronic development are as follows: the tensile strength of the material is more than or equal to 600MPa, the electric conductivity is more than or equal to 80 percent IACS (International Annealed Copper Standard), and the high-temperature softening temperature is more than or equal to 800K. Copper and copper alloys have long been used as conductive metal materials in industry, and over 75% of copper and copper alloys are used in the electrical and electronic industries. Pure copper, although having good electrical and thermal conductivity, has the obvious disadvantage of low hardness, tensile strength and creep strength, such as 230 to 290 MPa. The traditional main method for improving the strength of the copper alloy is solution treatment and subsequent aging treatment, because the alloy content and precipitation strengthening effect are limited, and the addition of alloy elements can also influence the conductivity to a great extent, for example, the conductivity of the copper alloy containing 0.3% of Zn is 85% IACS, the conductivity of the copper alloy containing 1.25% of Al is 70%, the conductivity of the copper alloy containing 0.1% of P is 50% IACS, and the conductivity of the copper alloy of a fixed grade can be ensured to be 90% IACS only when the copper content of the copper alloy is more than 99%, so that the high conductivity and the high strength of pure copper and the copper alloy of the existing grade are difficult to be considered simultaneously. The composite strengthening mode of introducing the strengthening phase(s) can simultaneously play the synergistic effect of the matrix and the strengthening material, and has great design freedom, and meanwhile, the conduction theory indicates that the scattering effect of copper atom lattice distortion caused by atoms dissolved in the copper matrix on electrons is much stronger than that caused by the second phase, so that the conductivity of the copper matrix cannot be obviously reduced by the composite strengthening.
The copper-based composite material is a novel material which is developed in recent years and has wide application prospect, has high strength, high conductivity and good thermal property, high hardness and good wear resistance, and the preparation method can be divided into two types of ex-situ synthesis and in-situ synthesis according to the introduction mode of the reinforcement. The ex-situ synthesis technology is also called as an additional forcing technology, and means that reinforcing phases, namely fibers or particles, are artificially added into a copper matrix and are uniformly distributed in the copper matrix, and the existence of the reinforcing phases increases the motion resistance of dislocation, so that the composite material is reinforced. The in-situ reaction technology is one of the effective methods for preparing the particle-reinforced metal matrix composite (PRMMC). The basic principle is that alloy elements or compounds capable of generating certain second phase are added or introduced into a metal matrix and react in situ in the metal matrix at a certain temperature to form the in-situ composite material. The reinforcing phase generated by the in-situ reaction has the advantages of submicron size, clean interface, good combination with the matrix, dispersion distribution and the like. Compared with the traditional composite material with the externally added reinforcement, the strength of the composite material is greatly improved, and simultaneously, better toughness and good high-temperature performance are kept.
Compared with the copper-based composite material synthesized in situ, the copper-based composite material synthesized in situ is not limited by the volume fraction of the reinforcement, so that the obtained reinforcement has small size, is dispersed in distribution, has clear and pollution-free interface with a matrix, has strong interface bonding strength, and is a composite material with a great development prospect. The most economical and practical preparation method is selected from the existing multiple in-situ synthesis methods, the volume fraction of the side reaction inclusion and the reinforcement body is accurately controlled, the interface condition and the strengthening mechanism are deeply researched, the side reaction inclusion is controlled, and the direction of future work is to improve the mechanical property and reduce the descending amplitude of the electrical conductivity. Although the in-situ synthesis of the copper-based composite material has the advantages, the existing in-situ synthesis method of the copper-based composite material has the disadvantages of expensive equipment, complex operation and difficult control of reaction products.
The invention content is as follows:
in order to solve the defects of expensive equipment, complex operation and difficult control of reaction products in the conventional method for synthesizing the copper-based composite material in situ, the invention provides a preparation method of a reaction hot-pressing in-situ authigenic copper-based composite material, which is realized by the following steps: a. mixing powder by a ball milling method: placing the prepared Ti powder, B powder and Cu powder into a ball milling tank, vacuumizing and then filling argon, and mixing the powder for 6-12 hours under the conditions that the ball material ratio is 1-20: 1 and the rotating speed is 200-400 r/min; b. cold press molding: putting the mixed powder into a graphite die for cold press molding, so that the density of the material reaches 20-40Percent; c. vacuum hot-pressing sintering: putting the powder and the graphite mold into a vacuum hot-pressing furnace for hot-pressing sintering, pressing the material until the density is 95-99%, cooling the material to room temperature along with the furnace, and demolding to obtain TiB2a/Cu composite material.
TiB2The crystal belongs to a C32-AlB2 type structure, the melting point is 3225 ℃, and the hardness is second to that of diamond, BN and B4C, bending strength up to 750MPa, and resistivity of 10-5Omega cm, excellent electric and heat conducting performance, and double purposes of structural ceramics and functional ceramics, and is a material with unique and excellent performance, so the material attracts great attention as a reinforcing phase of a metal matrix composite material. Because of TiB2The particles have excellent thermal stability, TiB2the/Cu composite material has higher high-temperature strength than dispersion-strengthened copper alloys (such as Cu-Zr and Cu-Cr). TiB2the/Cu composite material is desired to achieve a large improvement in mechanical properties while reducing the decrease in electrical conductivity. The invention prepares Ti powder, B powder and Cu powder which are uniformly mixed by a ball milling powder mixing method, and then prepares TiB by cold press molding and vacuum hot pressing sintering2a/Cu composite material. To is coming toFurther improving the structure and the performance of the composite material, and carrying out hot extrusion deformation on the composite material prepared by reaction, thereby finally obtaining TiB with uniform structure and excellent performance2a/Cu composite material. The reaction hot-pressing equipment is simple, easy to operate, easy to control the volume fraction of the reinforcement body, and the reaction temperature does not need to be too high, so that side reaction inclusions cannot be generated. In the hot pressing process of the present invention, the following reaction will occur in the composite: the metal Ti and the nonmetal element B are chemically reacted to generate TiB2Ceramic reinforcement distributed in the Cu matrix to form TiB2TiB with ceramic particles as reinforcement and Cu as matrix2a/Cu composite material. The strength of the composite material prepared by adopting the reaction hot pressing method is improved by 20-30%, the plasticity is improved by 10-20%, and the conductivity is improved by 10% compared with the composite material prepared by adopting other in-situ generation processes under the same conditions.
Description of the drawings:
FIG. 1 is a process flow diagram of the present invention.
The specific implementation mode is as follows:
the first embodiment is as follows: the implementation mode is carried out according to the following steps: a. mixing powder by a ball milling method: placing the prepared Ti powder, B powder and Cu powder into a ball milling tank, firstly vacuumizing, then filling argon to prevent the powder from being oxidized in the ball milling process, and in the process of TiB2In the preparation process of the/Cu composite material, ball milling process parameters are crucial to successfully preparing the composite material, and if the ball milling rotating speed is too low, the ball material is small or the powder mixing time is too short, the powder is easily mixed unevenly; on the contrary, if the ball milling rotation speed is too high, the ball-to-material ratio is too large or the powder mixing time is too long, a mechanical alloying phenomenon (i.e. a chemical reaction has occurred in the ball milling process to generate a composite material) occurs, and the mechanical alloying is easily introduced into components in the ball milling tank or the steel ball to form impurities, so that the powder is mixed for 6-12 hours under the conditions that the ball-to-material ratio is 1-20: 1 and the rotation speed is 200-400 r/min, and the optimal powder mixing effect is achieved; b. cold press molding: putting the mixed powder into a graphite mold for cold press molding, so that the density of the material reaches 20-40%; c. vacuum hot-pressing sintering: putting the powder and the graphite mold into a vacuum hot-pressing furnace for hot-pressing sintering, pressing the material until the density is 95-99%, cooling the material to room temperature along with the furnace, and demolding to obtain TiB2a/Cu composite material. The size range of the copper powder particles is 1-50 mu m, the size range of the titanium powder particles is 1-50 mu m, and the size of the boron powder particles is less than or equal to 10 mu m; the vacuum hot-pressing sintering process comprises the following steps: putting the mixed powder and a graphite mold into a vacuum hot-pressing furnace, firstly vacuumizing, then heating at a heating rate of 5-30 ℃/min to 600-700 ℃, preserving heat for 20-40 minutes, degassing, pressing the material to a density of 70-85%, continuously heating to 900-980 ℃, preserving pressure for 1-3 hours at a pressure of 20-30 MPa, pressing the material to a density of 95-99%, preserving heat for 50-70 minutes, cooling to room temperature along with the furnace, and demolding to obtain TiB2a/Cu composite material having a vacuum degree of 10-2～10-4Torr。The process method of the embodiment is not only suitable for the copper-based composite material prepared from the Ti powder, the B powder and the Cu powder, wherein the proportion of the Ti powder, the B powder and the Cu powder can be properly adjusted according to the performance requirements, but also suitable for other copper-based composite materials capable of realizing high strength, high plasticity and high conductivity.
The second embodiment is as follows: this embodiment is different from the first embodiment in that TiB is further improved2The structure of the Cu composite material improves the performance of the composite material, and the composite material prepared by reaction hot pressing needs to be subjected to hot extrusion: coating the composite material with low-carbon steel, heating the composite material to 900-1000 ℃, simultaneously heating an extrusion die to 480-540 ℃, taking out the composite material from a heating furnace, putting the composite material into the extrusion die, and carrying out hot extrusion on the composite material, thereby obtaining high-quality TiB2a/Cu composite material. The extrusion ratio is 20-30: 1, and the taper angle of the female die is 120 degrees.
The third concrete implementation mode: the embodiment is realized as follows:
a. mixing powder by a ball milling method: and putting the prepared Ti powder, B powder and Cu powder into a ball milling tank, firstly vacuumizing, and then filling argon to prevent the powder from being oxidized in the ball milling process. Mixing powder on a planetary ball mill, wherein the ball material ratio is 5: 1, the rotating speed is 300 r/min, and the powder mixing time is 8 hours.
b. Cold press molding: and putting the mixed powder into a graphite mold for cold press molding, wherein the density of the material reaches 30%.
c. Hot-pressing and sintering: and then putting the powder and the graphite mould into a vacuum hot-pressing furnace for hot-pressing sintering. Firstly, vacuumizing to a vacuum degree of 10-3And (3) Torr (argon oxygen decarburization), starting heating at the heating rate of 10 ℃/min, heating to 650 ℃, keeping the temperature for 30 minutes, degassing, and pressing the material to the density of 80%. And continuously heating to 950 ℃, pressing the material until the density is close to 100%, and keeping the temperature for 60 minutes. Cooling to room temperature along with the furnace, and demoulding to obtain TiB2a/Cu composite material.
d. Hot extrusion: firstly, coating the composite material with low-carbon steel, then heating the composite material to 950 ℃, and simultaneously heating an extrusion die to 650 DEG CTaking the composite material out of the heating furnace, putting the composite material into an extrusion die, and carrying out hot extrusion on the composite material, wherein the extrusion ratio is 25: 1, and the taper angle of the female die is 120 degrees, so that high-quality TiB is obtained2a/Cu composite material. In the hot extrusion process, a method of separately pressurizing the composite material and the extrusion die is adopted, so that the composite material can be smoothly extruded while the extrusion die keeps high strength.
The fourth concrete implementation mode: TiB is 15vol2Preparation of the/Cu compositeas an example, the dimensions of the composite were Φ 60X 60 mm.
a. The mass percentages of the required raw materials such as Ti powder, B powder and Cu powder are calculated according to the volume fraction of the designed reinforcement body and are shown in table 1, and then the raw material powder and the steel ball are placed into a ball milling tank according to the ball material ratio of 5: 1, and the steel ball adopts three specifications of large, medium and small. Vacuumizing and filling argon to protect the powder from being oxidized in the ball milling process. Mixing powder on a planetary ball mill by adopting a powder mixing method combining positive rotation and reverse rotation, wherein the rotating speed is 300 revolutions per minute, and the powder mixing time is 8 hours.
TABLE 1 Mass percents of the respective raw powders
| Cu | Ti | B |
| 91.86 | 5.58 | 2.56 |
b. And (3) carrying out cold forming on the uniformly mixed powder in a graphite die, wherein the cold forming size is phi 60mm, and the density is about 50%.
c. And thenputting the powder and the graphite mould into a vacuum hot-pressing furnace for hot-pressing sintering. Firstly, vacuumizing to a vacuum degree of 10-3And (3) Torr (mount, mill) is used, heating is started, the heating rate is 10 ℃/min, the temperature is heated to 650 ℃, the heat preservation is carried out for 30 minutes, and the material is pressed to the density of 80%. And continuously heating to 950 ℃, pressing the material until the density is close to 100%, and keeping the temperature for 60 minutes. Cooling to room temperature along with the furnace, and demoulding to obtain TiB2a/Cu composite material.
d. For successfully prepared TiB2the/Cu composite material adopts forward extrusion, the extrusion ratio is 25: 1, and the taper angle of a concave die is 120 degrees. Firstly, coating a composite material with low-carbon steel, then heating the composite material to 950 ℃, simultaneously heating an extrusion die to 650 ℃, then taking out the composite material from a heating furnace and putting the composite material into the extrusion die, and carrying out hot extrusion on the composite material, thereby obtaining high-quality TiB2The specific process flow diagram of the/Cu composite material is shown in figure 1.
The fourth concrete implementation mode: in this embodiment, the TiB prepared by the process of the present invention2The properties of the/Cu composite are shown in Table 2,
TABLE 2 reaction Hot pressing in situ autogenous TiB2Properties of the/Cu composite
| Material | Tensile strength at room temperature (MPa) | Electrical conductivity of (IACS) | High temperature softening temperature (K) |
| Pure copper | 250 | 99 | 498 |
| 5vol.TiB2/Cu | 348 | 94 | 607 |
| 10vol.TiB2/Cu | 471 | 89 | 703 |
| 15vol.TiB2/Cu | 562 | 83 | 800 |
| 20vol.TiB2/Cu | 645 | 79 | 839 |
| 25vol.TiB2/Cu | 683 | 75 | 887 |
Claims (6)
1. The preparation method of the reaction hot-pressing in-situ authigenic copper-based composite material is characterized by comprising the following steps: a. mixing powder by a ball milling method: placing the prepared Ti powder, B powder and Cu powder into a ball milling tank, vacuumizing and then filling argon, and mixing the powder for 6-12 hours under the conditions that the ball material ratio is 1-20: 1 and the rotating speed is 200-400 r/min; b. cold press molding: putting the mixed powder into a graphite mold for cold press molding, so that the density of the material reaches 20-40%; c. vacuum hot-pressing sintering: putting the powder and the graphite mold into a vacuum hot-pressing furnace for hot-pressing sintering, pressing the material until the density is 95-99%, cooling the material to room temperature along with the furnace, and demolding to obtain TiB2a/Cu composite material.
2. The method for preparing the reactive hot-pressing in-situ authigenic copper-based composite material according to claim 1, characterized by further comprising d steps of d, hot-pressing: coating the composite material with low-carbon steel, heating the composite material to 900-1000 ℃, simultaneously heating an extrusion die to 480-540 ℃, taking out the composite material from a heating furnace, and putting the composite material into an extrusion diePressing the die to perform hot extrusion on the composite material so as to obtain high-quality TiB2a/Cu composite material.
3. The method for preparing the reactive hot-pressing in-situ authigenic copper-based composite material according to claim 1, wherein the size of the copper powder particles is 1-50 μm, the size of the titanium powder particles is 1-50 μm, and the size of the boron powder particles is less than or equal to 10 μm.
4. The method for preparing the reactive hot-pressing in-situ authigenic copper-based composite material according to claim 1, wherein the vacuum hot-pressing sintering process is as follows: putting the mixed powder and a graphite mold into a vacuum hot-pressing furnace, firstly vacuumizing, then heating at a heating rate of 5-30 ℃/min to 600-700 ℃, preserving heat for 20-40 minutes, degassing, pressing the material to a density of 70-85%, continuously heating to 900-980 ℃, preserving pressure for 1-3 hours at a pressure of 20-30 MPa, pressing the material to a density of 95-99%, preserving heat for 50-70 minutes, cooling to room temperature along with the furnace, and demolding to obtain TiB2a/Cu composite material.
5. The method for preparing the reactive hot-pressing in-situ authigenic copper-based composite material according to claim 4, wherein the vacuum degree in the vacuum hot-pressing furnace is 10-2～10-4Torr。
6. The method for preparing the reactive hot-pressing in-situ authigenic copper-based composite material according to claim 2, wherein an extrusion ratio in a hot extrusion process is 20-30: 1, and a die cone angle is 120 °.
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| CN103667772A (en) * | 2013-12-24 | 2014-03-26 | 刘伟 | Copper-based powder dispersion ceramic as well as preparation method and application thereof |
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| CN101333607B (en) * | 2008-07-31 | 2010-06-23 | 哈尔滨工业大学 | Process for preparing TiBw/Ti alloy-based composite material |
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| CN103667772B (en) * | 2013-12-24 | 2015-07-08 | 刘伟 | Copper-based powder dispersion ceramic as well as preparation method and application thereof |
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| CN107675009A (en) * | 2017-08-03 | 2018-02-09 | 西安理工大学 | Three-dimensional net structure titanium diboride enhancing Cu-base composites and preparation method thereof |
| CN107675009B (en) * | 2017-08-03 | 2019-07-23 | 西安理工大学 | Three-dimensional net structure titanium diboride enhances Cu-base composites and preparation method thereof |
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| 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 |
| CN110257664A (en) * | 2019-07-31 | 2019-09-20 | 河南科技大学 | A kind of Cu-base composites and preparation method thereof |
| CN113278863A (en) * | 2021-04-30 | 2021-08-20 | 西安理工大学 | Method for preparing titanium diboride copper-based composite material by vacuum hot pressing |
| CN113278863B (en) * | 2021-04-30 | 2021-12-17 | 西安理工大学 | Method for preparing titanium diboride copper-based composite material by vacuum hot pressing |
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