CN114107714B - Production process for improving mechanical property of tungsten-nickel-copper alloy - Google Patents

Production process for improving mechanical property of tungsten-nickel-copper alloy Download PDF

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CN114107714B
CN114107714B CN202111419158.9A CN202111419158A CN114107714B CN 114107714 B CN114107714 B CN 114107714B CN 202111419158 A CN202111419158 A CN 202111419158A CN 114107714 B CN114107714 B CN 114107714B
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tungsten
nickel
copper
copper alloy
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CN114107714A (en
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刘方舟
赵永华
张广卫
潘王虎
白磊
彭媛
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Xi'an Huashan Tungsten Products Co ltd
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon

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Abstract

The invention discloses a production process for improving mechanical property of tungsten-nickel-copper alloy, which comprises the following steps: firstly, dry-grinding and mixing raw materials to obtain mixed powder; secondly, carrying out wet grinding, and then carrying out spray drying and granulation to obtain a prepared granule; thirdly, pressing to obtain a tungsten-nickel-copper green compact; fourthly, preheating, heating and insulating to obtain a tungsten-nickel-copper sintering blank; fifthly, rapidly cooling after heating and heat preservation, and then heating and heat preservation; and sixthly, carrying out vacuum annealing to obtain the tungsten-nickel-copper alloy. According to the invention, the mixed powder crystal blocks are refined and the activity is improved by adopting two-time ball milling, the copper solution is fully contacted with tungsten particles and nickel by combining with the control of the sintering temperature, so that impurities in the tungsten nickel copper sintering blank are removed before the air hole is sealed and densified, the tissue form of the tungsten nickel copper alloy at high temperature is kept to the room temperature by combining with modulation treatment, the internal stress is effectively eliminated, the harmful hydrogen element is removed by combining with vacuum annealing treatment, the mechanical property of the tungsten nickel copper alloy is synergistically improved, and the problem of low mechanical property of the tungsten nickel copper alloy is solved.

Description

Production process for improving mechanical property of tungsten-nickel-copper alloy
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a production process for improving mechanical properties of a tungsten-nickel-copper alloy.
Background
The tungsten alloy material mainly comprises two main series: tungsten nickel copper alloys and tungsten nickel iron alloys. The tungsten-nickel-copper alloy is formed by adding nickel and copper into tungsten and adding other metal elements (such as Co, Mn, Cr and the like) on the basis of the alloy. The tungsten-nickel-copper alloy has no ferromagnetism and relatively good electric and heat conducting properties, and is often applied to occasions with special requirements, such as a gyroscope rotor and a counterweight of a nuclear submarine, and parts of other devices and instruments which need to work under the action of a magnetic field are used as balance and counterweight materials in an attitude instrument of a communication satellite and a Scheberg engine. However, poor wettability of copper and tungsten often limits W-Ni-Cu due to low tensile strength and ductilityThe development of alloys. Taking 90WNiCu alloy with 90 percent of tungsten content and 93WNiCu alloy with 93 percent of tungsten content as examples, the tensile strength of the 90WNiCu alloy is less than or equal to 800MPa, the elongation is less than or equal to 5 percent, and the impact toughness is less than or equal to 30J/cm3The tensile strength of 93NiCu alloy is less than or equal to 780MPa, the elongation is less than or equal to 4 percent, and the impact toughness is less than or equal to 26J/cm3
Disclosure of Invention
The technical problem to be solved by the invention is to provide a production process for improving the mechanical property of the tungsten-nickel-copper alloy aiming at the defects of the prior art. The process adopts two ball milling to refine and improve the activity of mixed powder crystal blocks, fully contacts a copper solution with tungsten particles and nickel by combining with the control of sintering temperature so as to remove impurities in a tungsten nickel copper sintering blank before air hole sealing densification, retains the tissue form of the tungsten nickel copper alloy at high temperature to room temperature and effectively eliminates internal stress by combining with modulation treatment, removes harmful hydrogen elements by combining with vacuum annealing treatment, improves the wettability of copper and tungsten under the synergistic action of the process, effectively improves the mechanical property of the tungsten nickel copper alloy, and solves the problem of low mechanical property of the tungsten nickel copper alloy.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a production process for improving mechanical properties of tungsten-nickel-copper alloy is characterized by comprising the following steps:
step one, mixing materials: selecting tungsten powder, cobalt powder, nickel powder and copper powder as raw materials according to the nominal components of the target product tungsten-nickel-copper alloy, weighing the raw materials, and putting the raw materials into an inclined mixer for dry grinding and mixing to obtain mixed powder;
step two, granulation: adding polyethylene glycol into the mixed powder obtained in the step one, then carrying out wet grinding and mixing, and carrying out spray drying and granulation to obtain a prepared granule;
step three, press forming: pressing the granulated material obtained in the step two to obtain a tungsten-nickel-copper green compact;
step four, sintering: placing the tungsten-nickel-copper green compact obtained in the third step into a two-belt heating furnace, preheating to 1100-1200 ℃ under the condition of introducing gas protection, then heating to 1300-1400 ℃, preserving heat for 30-60 min, and cooling along with the furnace to obtain a tungsten-nickel-copper sintered blank;
step five, modulation processing: placing the tungsten-nickel-copper sintered blank obtained in the fourth step into a heating furnace, preserving heat for 40-70 min at 1300-1400 ℃ under the condition of gas introduction protection, then placing the tungsten-nickel-copper sintered blank into water at 25-80 ℃ for rapid cooling, then transferring the tungsten-nickel-copper sintered blank into the heating furnace, heating to 1400-1500 ℃ under the condition of gas introduction protection, preserving heat for 40-70 min, and cooling along with the furnace;
step six, vacuum annealing: the tungsten-nickel-copper sintered blank after the modulation treatment in the step five is processed at the temperature of 900-1300 ℃ and the vacuum degree of 10-1~10-2Keeping the temperature for 6-12 h under the condition of Pa, and then cooling along with the furnace to obtain the tungsten-nickel-copper alloy.
According to the invention, raw materials for preparing the tungsten-nickel-copper alloy are sequentially subjected to dry grinding mixing and wet grinding mixing, the mixed powder crystal mass is refined by utilizing the collision effect of a metal grinding ball on the powder, the uniform mixing of the raw materials is promoted, the activity is improved, and then the raw materials are subjected to spray drying granulation to obtain granules, so that the subsequent compression molding is facilitated to obtain a tungsten-nickel-copper green compact; keeping the tungsten-nickel-copper compact at a temperature slightly higher than the melting point (1083 ℃) of copper, namely 1100-1200 ℃, wherein nickel and tungsten are not melted at the temperature, copper in the tungsten-nickel-copper compact is converted into a molten liquid and fully contacted with tungsten particles and nickel, so that C, S, O impurities which are converted into gas at the temperature are removed before a solid phase framework and crystal grains grow and pores are sealed and densified, and then the temperature is increased to heat and keep the temperature to enhance the effect, so that the structural tissues of the front end, the middle end and the rear end of the tungsten-nickel-copper alloy are uniform, the quality of the tungsten-nickel-copper alloy is improved, and the improvement of the mechanical properties of all parts of the tungsten-nickel-copper alloy is facilitated; then, the tungsten-nickel-copper sintered blank is subjected to modulation treatment, secondary sintering is carried out by heating and insulating the tungsten-nickel-copper sintered blank, the performance that tungsten has better compatibility in a nickel-copper phase at high temperature and the characteristics that a tungsten framework blocks segregation of tungsten particles, tungsten crystal grains are gathered to grow and dissolved out in liquid phase sintering during secondary sintering are combined with rapid cooling, the phenomenon that the tungsten and the copper are separated due to the immiscible state of the tungsten and the copper when the temperature is lower after slow cooling and the mechanical property of the tungsten-nickel-copper alloy is reduced is avoided, the structural form of the tungsten-nickel-copper alloy at high temperature is kept to the room temperature, and the internal stress caused by rapid cooling is effectively eliminated; finally, the tungsten-nickel-copper sintered blank after modulation treatment is subjected to vacuum annealing treatment, so that harmful hydrogen elements introduced by adopting a hydrogen atmosphere in the sintering and modulation treatment processes are effectively removed, and the problem of stress concentration caused by rapid cooling in the modulation treatment is further solved.
In conclusion, the method adopts the dry grinding and two-time ball milling process of graphite, combines the modulation treatment of temperature-controlled sintering, secondary sintering and rapid quenching and the vacuum annealing treatment, improves the wettability of copper and tungsten, effectively avoids the separation phenomenon of tungsten and copper in the tungsten-nickel-copper alloy in the production process, effectively improves the mechanical properties of the tungsten-nickel-copper alloy, including the tensile strength, the elongation and the impact toughness of the tungsten-nickel-copper alloy, and solves the problem of low mechanical properties of the tungsten-nickel-copper alloy.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that the ball-material ratio of dry grinding and mixing in the step one is 4:1, and the time is 7-9 hours. The optimized technological parameters improve the uniformity of the mixed powder, and the analysis deviation of all components of the three-point sampling of the mixed powder does not exceed 0.02% through detection.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that the mass of the added polyethylene glycol in the step two is 2.0% of the mass of the mixed powder. The adding quality of the polyethylene glycol meets the forming requirement of a subsequent pressed compact, ensures that the content of residual C in the product is not more than 0.1 percent, and avoids the adverse effect on the product performance.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that in the second step, the wet grinding and mixing are carried out in a ball mill, the adopted medium is an ethanol solution, and the ball-to-material ratio is 3: 1, the time for wet grinding and mixing is 8-16 h. The technological parameters ensure that the polyethylene glycol is uniformly dispersed in the mixed powder, and the mixed powder is further refined, so that the activity of the mixed powder is enhanced.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that spray drying in the second step is carried out by adopting a spray drying tower. The spray drying tower is adopted for spray drying, which is beneficial to obtaining mixed powder with certain granularity, fluidity and formability.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that the pressing in the third step is pressing by a dry bag press, the pressing pressure is 120-150 MPa, and the pressing time is 0.5-3 min. The dry bag press is adopted to press to conveniently obtain slender tungsten nickel copper pressed compact bars, the pressing efficiency is improved, and the strength of the tungsten nickel copper pressed compact is ensured.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that the pressing time of the dry bag press is 1 min.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that in the fourth step, the two-belt heating furnace is a two-belt temperature-control muffle furnace. The optimized equipment ensures that the sintering process of preheating and heating is completed in the equipment at one time, and the flow is shortened.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that the gas introduced in the fourth step and the gas introduced in the fifth step are ammonia decomposition gases. The protective gas effectively prevents the tungsten-nickel-copper sintered blank from being oxidized in the sintering and modulation treatment processes, and the protective gas has low cost and is harmless to the environment.
The production process for improving the mechanical property of the tungsten-nickel-copper alloy is characterized in that in the sixth step, the modulated tungsten-nickel-copper sintered blank is subjected to temperature of 1200 ℃ and vacuum degree of 10-12Keeping the temperature for 10 hours under the condition of Pa, and then cooling along with the furnace to obtain the tungsten-nickel-copper alloy. The preferred vacuum annealing process parameters not only eliminate hydrogen embrittlement, but also further eliminate stress concentration problems caused by modulation processing.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts dry grinding and two ball milling processes of graphite to refine and improve the activity of mixed powder crystal blocks, fully contacts a copper solution with tungsten particles and nickel by controlling the sintering temperature in combination to remove impurities in a tungsten-nickel-copper sintering blank before the closed densification of air holes, retains the tissue form of the tungsten-nickel-copper alloy at high temperature to room temperature and effectively eliminates internal stress by combining modulation treatment, removes harmful hydrogen elements by combining vacuum annealing treatment, improves the wettability of copper and tungsten under the synergistic action of the processes, effectively improves the mechanical properties of the tungsten-nickel-copper alloy, including tensile strength, elongation and impact toughness, and solves the problem of low mechanical properties of the tungsten-nickel-copper alloy.
2. Compared with the common 90WNiCu alloy of tungsten-nickel-copper alloy, the tensile strength is less than or equal to 800MPa, the elongation is less than or equal to 5 percent, and the impact toughness is less than or equal to 30J/cm3The tensile strength of the 90WNiCu alloy prepared by the invention is not less than 930MPa, the elongation is not less than 15%, and the impact toughness is not less than 50J/cm3
3. The process is simple, the production process of the high-density tungsten-nickel-copper alloy can be completed by adopting conventional equipment in the technical field of the existing powder metallurgy, special equipment is not needed, and the process is easy to realize.
4. The production process of the invention has stable state, and the produced tungsten-nickel-copper alloy has stable performance and is suitable for popularization.
5. The invention further expands the application range and the processing performance of the tungsten-nickel-copper alloy by improving the mechanical property of the tungsten-nickel-copper alloy.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a flow chart of the production process for improving mechanical properties of tungsten-nickel-copper alloy.
Detailed Description
Example 1
As shown in fig. 1, the present embodiment includes the following steps:
step one, mixing materials: selecting tungsten powder, cobalt powder, nickel powder and copper powder as raw materials according to the nominal components of the target product 90WNiCu alloy, weighing the raw materials, and putting the raw materials into an inclined mixer for dry grinding and mixing to obtain mixed powder; the dry-milling mixed ball material ratio is 4:1, the time is 7 h;
step two, granulation: adding polyethylene glycol into the mixed powder obtained in the step one, wet-grinding and mixing, and performing spray drying granulation by using a spray drying tower to obtain 40-120-mesh granules; the adding mass of the polyethylene glycol is 2.0 percent of the mass of the mixed powder; the wet grinding and mixing are carried out in a ball mill, the adopted medium is ethanol solution, and the ball-material ratio is 3: 1, wet grinding and mixing for 12 hours;
step three, press forming: pressing the granulated material obtained in the step two by using a dry bag press to obtain a 90WNiCu alloy pressed blank; the pressing pressure of the dry bag press is 130MPa, and the pressing time is 1 min;
step four, sintering: placing the 90WNiCu alloy pressed blank obtained in the third step into a two-belt heating furnace, preheating to 1100 +/-10 ℃ under the protection of ammonia decomposition gas, then heating to 1300 +/-10 ℃ and preserving heat for 30min, and cooling along with the furnace to obtain a 90WNiCu alloy sintered blank;
step five, modulation processing: placing the 90WNiCu alloy sintered blank obtained in the fourth step into a heating furnace, preserving heat for 40min at 1300 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then placing the blank into water at 35 +/-10 ℃ for rapid cooling, transferring the blank into the heating furnace, heating to 1400 +/-10 ℃ under the condition of introducing ammonia decomposition gas for heat preservation for 45min, and cooling along with the furnace;
step six, vacuum annealing: the 90WNiCu alloy sintered blank after modulation treatment in the step five is processed at the temperature of 920 +/-20 ℃ and the vacuum degree of 10-2Keeping the temperature for 6h under the condition of Pa, and then cooling along with the furnace to obtain the 90WNiCu alloy.
The 90WNiCu alloy produced by the embodiment has the advantages of tensile strength value of 965MPa, elongation of 18 percent and impact toughness of 70J/cm3
Example 2
As shown in fig. 1, the present embodiment includes the following steps:
step one, mixing materials: selecting tungsten powder, cobalt powder, nickel powder and copper powder as raw materials according to the nominal composition of a target product 92WNiCu alloy, weighing the raw materials, and putting the raw materials into an inclined mixer for dry grinding and mixing to obtain mixed powder; the dry-milling mixed ball material ratio is 4:1, the time is 8 h;
step two, granulation: adding polyethylene glycol into the mixed powder obtained in the step one, wet-grinding and mixing, and performing spray drying granulation by using a spray drying tower to obtain 40-120-mesh granules; the adding mass of the polyethylene glycol is 2.0 percent of the mass of the mixed powder; the wet grinding and mixing are carried out in a ball mill, the adopted medium is ethanol solution, and the ball-material ratio is 4:1, wet grinding and mixing for 8 hours;
step three, press forming: pressing the granulated material obtained in the step two by using a dry bag press to obtain a 92WNiCu alloy pressed blank; the pressing pressure of the dry bag press is 120MPa, and the pressing time is 3 min;
step four, sintering: placing the 90WNiCu alloy pressed blank obtained in the third step into a two-belt heating furnace, preheating to 1110 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then heating to 1310 +/-10 ℃ and preserving heat for 60min, and cooling along with the furnace to obtain a 92WNiCu alloy sintered blank;
step five, modulation processing: placing the 92WNiCu alloy sintered blank obtained in the fourth step into a heating furnace, preserving heat for 70min at 1310 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then placing the blank into water at 35 +/-10 ℃ for rapid cooling, transferring the cooled blank into the heating furnace, heating to 1410 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, preserving heat for 40min, and cooling along with the furnace;
step six, vacuum annealing: the 92WNiCu alloy sintering blank after modulation treatment in the step five is processed at the temperature of 1200 +/-20 ℃ and the vacuum degree of 10-1Keeping the temperature for 6h under the condition of Pa, and then cooling along with the furnace to obtain the 92WNiCu alloy.
The 92WNiCu alloy produced by the embodiment is detected to have the tensile strength value of 965MPa, the elongation of 18 percent and the impact toughness of 68J/cm3
Example 3
As shown in fig. 1, the present embodiment includes the following steps:
step one, mixing materials: according to the nominal composition of a target product 93WNiCu alloy, selecting tungsten powder, cobalt powder, nickel powder and copper powder as raw materials, weighing the raw materials, and putting the raw materials into an inclined mixer for dry grinding and mixing to obtain mixed powder; the dry-milling mixed ball material ratio is 4:1, the time is 9 h;
step two, granulation: adding polyethylene glycol into the mixed powder obtained in the step one, wet-grinding and mixing, and performing spray drying granulation by using a spray drying tower to obtain 40-120-mesh granules; the adding mass of the polyethylene glycol is 2.0 percent of the mass of the mixed powder; the wet grinding and mixing are carried out in a ball mill, the adopted medium is ethanol solution, and the ball-material ratio is 4:1, wet-grinding and mixing for 16 h;
step three, press forming: pressing the granulated material obtained in the step two by using a dry bag press to obtain a 93WNiCu alloy pressed blank; the pressing pressure of the dry bag press is 150MPa, and the time is 0.5 min;
step four, sintering: placing the 93WNiCu alloy pressed blank obtained in the third step into a two-belt heating furnace, preheating to 1190 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then heating to 1310 +/-10 ℃ and preserving heat for 60min, and cooling along with the furnace to obtain a 93WNiCu alloy sintered blank;
step five, modulation processing: placing the 93WNiCu alloy sintered blank obtained in the fourth step into a two-belt temperature-controlled muffle furnace, preserving heat for 70min at 1310 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then placing the blank into water at 35 +/-10 ℃ for rapid cooling, transferring the cooled blank into a heating furnace, heating to 1410 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, preserving heat for 70min, and cooling along with the furnace;
step six, vacuum annealing: the 93WNiCu alloy sintered blank after modulation treatment in the step five is processed at the temperature of 1200 +/-20 ℃ and the vacuum degree of 10-2Keeping the temperature for 10 hours under the condition of Pa, and then cooling along with the furnace to obtain the 93WNiCu alloy.
The 93WNiCu alloy produced in this example was found to have a tensile strength of 958MPa, an elongation of 17.5% and an impact toughness of 62J/cm3
Example 4
As shown in fig. 1, the present embodiment includes the following steps:
step one, mixing materials: selecting tungsten powder, cobalt powder, nickel powder and copper powder as raw materials according to the nominal components of the target product 95WNiCu alloy, weighing the raw materials, and putting the raw materials into an inclined mixer for dry grinding and mixing to obtain mixed powder; the dry-milling mixed ball material ratio is 4:1, the time is 9 h;
step two, granulation: adding polyethylene glycol into the mixed powder obtained in the step one, wet-grinding and mixing, and performing spray drying granulation by using a spray drying tower to obtain 40-120-mesh granules; the adding mass of the polyethylene glycol is 2.0 percent of the mass of the mixed powder; the wet grinding and mixing are carried out in a ball mill, the adopted medium is ethanol solution, and the ball-material ratio is 4:1, wet-grinding and mixing for 16 h;
step three, press forming: pressing the granulated material obtained in the step two by using a dry bag press to obtain a 95WNiCu alloy pressed blank; the pressing pressure of the dry bag press is 150MPa, and the pressing time is 1 min;
step four, sintering: placing the 95WNiCu alloy pressed blank obtained in the third step in a two-belt heating furnace, preheating to 1190 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then heating to 1390 +/-10 ℃ and preserving heat for 60min, and cooling along with the furnace to obtain a 95WNiCu alloy sintered blank;
step five, modulation processing: placing the 95WNiCu alloy sintered blank obtained in the fourth step into a two-belt temperature-controlled muffle furnace, preserving heat for 40min at 1390 +/-10 ℃ under the condition of introducing ammonia decomposition gas for protection, then placing the blank into water at 70 +/-10 ℃ for rapid cooling, transferring the blank into a heating furnace, heating to 1490 +/-10 ℃ under the condition of introducing ammonia decomposition gas for heat preservation for 70min, and cooling along with the furnace;
step six, vacuum annealing: the 95WNiCu alloy sintered blank after modulation treatment in the step five is processed at the temperature of 1280 +/-20 ℃ and the vacuum degree of 10-2Keeping the temperature for 12h under the condition of Pa, and then cooling along with the furnace to obtain the 95WNiCu alloy.
The 95WNiCu alloy produced by the embodiment is detected to have the tensile strength value of 938MPa, the elongation of 13.5 percent and the impact toughness of 42J/cm3
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (10)

1. A production process for improving mechanical properties of tungsten-nickel-copper alloy is characterized by comprising the following steps:
step one, mixing materials: selecting tungsten powder, cobalt powder, nickel powder and copper powder as raw materials according to the nominal components of the target product tungsten-nickel-copper alloy, weighing the raw materials, and putting the raw materials into an inclined mixer for dry grinding and mixing to obtain mixed powder;
step two, granulation: adding polyethylene glycol into the mixed powder obtained in the step one, then carrying out wet grinding and mixing, and carrying out spray drying and granulation to obtain a prepared granule;
step three, press forming: pressing the granulated material obtained in the step two to obtain a tungsten-nickel-copper green compact;
step four, sintering: placing the tungsten-nickel-copper green compact obtained in the third step into a two-belt heating furnace, preheating to 1100-1200 ℃ under the condition of introducing gas protection, then heating to 1300-1400 ℃, preserving heat for 30-60 min, and cooling along with the furnace to obtain a tungsten-nickel-copper sintered blank;
step five, modulation processing: placing the tungsten-nickel-copper sintered blank obtained in the fourth step into a heating furnace, preserving heat for 40-70 min at 1300-1400 ℃ under the condition of gas introduction protection, then placing the tungsten-nickel-copper sintered blank into water at 25-80 ℃ for rapid cooling, then transferring the tungsten-nickel-copper sintered blank into the heating furnace, heating to 1400-1500 ℃ under the condition of gas introduction protection, preserving heat for 40-70 min, and cooling along with the furnace;
step six, vacuum annealing: the tungsten-nickel-copper sintered blank after the modulation treatment in the step five is processed at the temperature of 900-1300 ℃ and the vacuum degree of 10-1~10-2Keeping the temperature for 6-12 h under the condition of Pa, and then cooling along with the furnace to obtain the tungsten-nickel-copper alloy.
2. The production process for improving the mechanical property of the tungsten-nickel-copper alloy as claimed in claim 1, wherein the dry-grinding mixing ball-material ratio in the step one is 4:1, and the time is 7-9 h.
3. The production process for improving the mechanical property of the tungsten-nickel-copper alloy as claimed in claim 1, wherein the mass of the added polyethylene glycol in the second step is 2.0% of the mass of the mixed powder.
4. The production process for improving the mechanical property of the tungsten-nickel-copper alloy as claimed in claim 1, wherein the wet grinding and mixing in the step two are carried out in a ball mill, the adopted medium is ethanol solution, and the ball-to-material ratio is 3: 1, the time for wet grinding and mixing is 8-16 h.
5. The production process for improving the mechanical property of the tungsten-nickel-copper alloy as claimed in claim 1, wherein the spray drying in the second step is performed by using a spray drying tower.
6. The production process for improving the mechanical property of the tungsten-nickel-copper alloy as claimed in claim 1, wherein the pressing in the third step is pressing by a dry bag press, the pressing pressure is 120MPa to 150MPa, and the pressing time is 0.5min to 3 min.
7. The production process for improving the mechanical property of the tungsten-nickel-copper alloy as claimed in claim 6, wherein the pressing time of the dry bag press is 1 min.
8. The production process for improving the mechanical property of the tungsten-nickel-copper alloy according to claim 1, wherein the two-band heating furnace in the fourth step is a two-band temperature-controlled muffle furnace.
9. The production process for improving the mechanical property of the tungsten-nickel-copper alloy according to claim 1, wherein the gas introduced in the fourth step and the gas introduced in the fifth step are ammonia decomposition gases.
10. The production process for improving the mechanical property of the tungsten-nickel-copper alloy according to claim 1,characterized in that in the sixth step, the tungsten-nickel-copper sintered blank after modulation treatment is processed at the temperature of 1200 ℃ and the vacuum degree of 10-2Keeping the temperature for 10 hours under the condition of Pa, and then cooling along with the furnace to obtain the tungsten-nickel-copper alloy.
CN202111419158.9A 2021-11-26 2021-11-26 Production process for improving mechanical property of tungsten-nickel-copper alloy Active CN114107714B (en)

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