CN111822700B - Method for eliminating internal quality defects of tungsten alloy - Google Patents
Method for eliminating internal quality defects of tungsten alloy Download PDFInfo
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- B22F1/0003—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1035—Liquid phase sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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Abstract
The invention discloses a method for eliminating internal quality defects of tungsten alloy, which comprises the following steps: firstly, mixing iron powder or copper powder with tungsten powder, nickel powder and cobalt powder to obtain mixed powder; secondly, pressing the mixed powder into a green compact and trimming; thirdly, sintering the trimmed pressed compact to obtain a sticky lump; fourthly, placing the bonding block on the top end of the tungsten alloy base material with quality defects inside, and sintering to obtain a tungsten alloy sintered blank; fifthly, carrying out internal quality ultrasonic flaw detection on the tungsten alloy sintered blank; and sixthly, carrying out vacuum heat treatment or quenching treatment on the tungsten alloy sintered blank qualified by detection to obtain the tungsten alloy with the internal quality defect eliminated. According to the invention, the low-melting-point alloy sticky lumps are melted and then flow to the positions with quality defects such as looseness, cracks and the like in the tungsten alloy matrix material through solid phase diffusion and liquid phase diffusion to eliminate the defects, so that the internal quality problems of looseness, cracks and the like in the core part of the tungsten alloy product in the liquid phase sintering process are solved, and the waste of resources is avoided.
Description
Technical Field
The invention belongs to the technical field of tungsten alloy material manufacturing, and particularly relates to a method for eliminating internal quality defects of a tungsten alloy.
Background
The tungsten alloy is an alloy which takes tungsten as a matrix and is added with a small amount of elements such as Ni, Fe, Cu, Co, Mo, Cr and the like, and the density of the tungsten alloy is as high as 16.5g/cm3～19.0g/cm3Also known as high specific gravity alloys. Because the tungsten alloy has high density, high strength, high hardness and better ductility, and good conductivityThermal conductivity, and is widely used in defense industry, aerospace, medical shielding and industrial shielding. With the rapid development of the national defense industry, the ship industry and the medical shielding industry, the demand of large-scale powder metallurgy tungsten alloy products is increasing day by day. However, for large products, especially cylindrical products, due to the "thin shell dome" effect, the compression amount of each layer from the surface layer to the core part is gradually decreased during pressing, and from density, the surface layer density is the largest, the core density is the smallest, and the density difference becomes larger along with the increase of the diameter of the circular section of the product, so that core part quality problems such as looseness, cracks and the like tend to occur in the core part during the liquid phase sintering process for preparing the large cylindrical products, so that the product rejection rate is high, the manufacturing cost of the products is increased, and the development and application of the large products are limited. Therefore, in order to eliminate the internal defects and reduce waste products caused by the internal defects such as core cracks, a process method for eliminating the internal quality defects such as internal porosity and cracks of the tungsten alloy is urgently needed to be developed, and the internal quality defects are improved and repaired on the premise that the product meets the use requirements.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for eliminating the internal quality defect of tungsten alloy in view of the above-mentioned deficiencies of the prior art. According to the method, after being melted, the low-melting-point alloy, namely the bonding block flows to the defects such as looseness, cracks and the like in the tungsten alloy matrix material through solid phase diffusion and liquid phase diffusion, and the alloying process of tungsten alloy liquid phase generation, particle rearrangement, dissolution and precipitation is carried out, so that the quality defects such as looseness, cracks and the like in the tungsten alloy are eliminated, and the quality problems of cores such as looseness, cracks and the like of the tungsten alloy products, particularly large tungsten alloy products, which are prone to occur in the liquid phase sintering process are solved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for eliminating internal quality defects of tungsten alloy is characterized by comprising the following steps:
pouring the powder A, tungsten powder, nickel powder and cobalt powder into a mixer for mixing to obtain mixed powder; the mass content of tungsten powder in the mixed powder is 0-40%, the mass content of nickel powder is 35.7-70%, the mass content of cobalt powder is 0-0.5%, the mass content of A powder is 23.8-34%, and the A powder is iron powder or copper powder;
step two, sieving the mixed powder obtained in the step one, then putting the sieved mixed powder into a latex sleeve, pressing the mixed powder into a pressed blank by adopting isostatic cool pressing, and then finishing the pressed blank by a wire saw or a lathe;
thirdly, placing the pressed blank trimmed in the second step into a muffle furnace for sintering for pre-alloying treatment to prepare a sticky lump;
placing the bonding block obtained in the third step on the top end of the tungsten alloy base material with quality defects inside, and then sending the tungsten alloy base material into a muffle furnace or an intermediate frequency furnace for sintering to obtain a tungsten alloy sintering blank; the tungsten alloy base material with quality defects inside is obtained by performing internal quality ultrasonic flaw detection on an AA-grade standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method;
fifthly, carrying out internal quality ultrasonic flaw detection on the tungsten alloy sintered compact obtained in the fourth step according to an AA standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method;
and step six, placing the qualified tungsten alloy sintered blank subjected to the internal quality ultrasonic flaw detection in the step five into a vacuum heat treatment furnace for vacuum heat treatment or quenching treatment to obtain the tungsten alloy with the internal quality defects eliminated.
The invention adopts the traditional powder metallurgy method to prepare the sticky lumps, because the content of high-melting-point component tungsten in the sticky lumps is lower, the proportion of low-melting-point component is higher, the sintering liquefaction temperature is reduced, so that the sticky lumps have the performance of low melting point, then the sticky lumps are placed at the top end of a tungsten alloy base material with quality defects of looseness, cracks and the like in the interior for sintering, along with the rise of the sintering temperature and when the sintering temperature of the tungsten alloy base material liquid phase is not reached, the low-melting-point alloy sticky lumps are completely melted, the tungsten alloy base material is still in a solid phase sintering stage, liquid phase sintering does not occur or only generates a small amount of liquid phase, the melting liquid of the low-melting-point alloy sticky lumps flows through solid phase diffusion (namely, the material migration caused by the proliferation and diffusion of the quality defects and the atomic diffusion before the liquid phase is generated) and the melting liquid phase diffusion flows and moves and diffuses to the inside the tungsten alloy base material to be loose and loose under the action of gravity effect and capillary effect, Performing alloying processes of tungsten alloy liquid phase generation, particle rearrangement, dissolution and precipitation at the mass defects of cracks and the like, thereby eliminating the mass defects of tungsten alloy such as internal looseness, cracks and the like and improving the internal quality of the tungsten alloy; in addition, because the solubility between the tungsten framework in the tungsten alloy matrix material and the low-melting-point alloy bonding block molten liquid is low, the collapse deformation degree of the tungsten alloy matrix material is slight, and the quality defects of internal looseness and cracks are eliminated on the premise of ensuring that the tungsten alloy matrix material is not deformed.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that the mixing time in the step one is 6-10 hours, and the ball-material ratio in mixing is 0.225: 1, the adopted grinding ball is a steel ball with the diameter of 12 mm-16 mm. The optimized technological parameters are beneficial to fully and uniformly mixing all raw material powder in the mixed powder, so that a pressed compact with uniform components is obtained, and a cohesive block with uniform components is obtained.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that the mass ratio of the nickel powder to the powder A in the mixed powder in the step one is (1.5-2.33): 1. the liquefaction temperature of the sticky lumps prepared by the mixed powder with the optimized mass ratio is lower, and the solid solubility of tungsten in the sticky lumps is high, so that the diffusion and movement of a liquid phase in a tungsten alloy matrix material are facilitated.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that manganese powder is added into the mixed powder in the step one, and the adding mass of the manganese powder is 0.05-2% of the mass of the mixed powder. The preferred addition of manganese powder improves the immergeability of the bonding block to the tungsten phase in the tungsten alloy matrix material, and is beneficial to the bonding block molten liquid to enter the defects of internal looseness, cracks and the like.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that the mixed powder in the step two is sieved by a 140-mesh sieve, then is put into a latex sleeve, and then is put into a cold isostatic press to be kept for 2-10 min under the condition that the pressing pressure is 120-180 MPa. The preferred mesh size facilitates filtration of agglomerated powder and removal of contaminant particles; the optimized pressing technological parameters ensure the forming of the pressed compact and improve the strength of the pressed compact.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that the temperature for pre-alloying treatment in the sintering in the third step is 1300-1450 ℃, and the heat preservation time is 30-60 min. Under the preferred sintering parameters, the solid phase in the green compact has low solubility in the molten liquid phase, and the amount of the liquid phase is small, so that densification is not completed, and sticky lumps with small grain sizes are obtained.
The method for eliminating the internal quality defect of the tungsten alloy is characterized in that in the fourth step, the top end of the tungsten alloy base material is machined to form a circular groove, the sticky block is placed in the circular groove, and the size of the sticky block is matched with that of the circular groove. The top processing of preferred at tungsten alloy base member material is used for holding the recess of gluing the caking, has avoided gluing the piece meltwater and has flowed away from the side for cohere the piece meltwater and pass through gravity action and capillary action, from the surface of tungsten alloy base member material to the core down flow diffusion get into inside, be favorable to realizing the effect of the inside crackle healing of tungsten alloy fast.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that in the fourth step, the bonding block is placed at the top end of the tungsten alloy base material with the internal quality defects and then is buried and sintered by adopting zirconium sand. Preferably, zirconium sand is used for burying, burning and adhering the blocks, so that the flowing of molten liquid of the adhered blocks is avoided, a groove does not need to be processed at the top end of the tungsten alloy base material, and the loss of the tungsten alloy base material is reduced.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that the sintering process in the fourth step is as follows: under the condition of reducing atmosphere, firstly heating to 950-1200 ℃ within 2-4 h, preserving heat for 4-7 h, then heating to 1390-1460 ℃ within 2-4 h, preserving heat for 3-5 h, and then cooling. In the optimized sintering process, the temperature is firstly raised to 950-1200 ℃ and the temperature is kept, so that the tungsten alloy matrix material with quality defects inside is fully heated, gas and water adsorbed by the tungsten alloy matrix material are completely volatilized, meanwhile, oxides on the surfaces of particles formed by the tungsten alloy matrix material are completely reduced, and sintering necks are formed on particle interfaces; and then heating to 1360-1460 ℃ and preserving heat, ensuring that the bonding block is completely liquefied and the matrix alloy is still in a solid phase or only a small amount of liquid phase is generated, wherein the liquid bonding phase has sufficient time to flow and diffuse to the defect part along the pores among the particles or the pores in the particles under the action of capillary force and gravity, and eliminating the internal quality defect of the matrix alloy.
The method for eliminating the internal quality defects of the tungsten alloy is characterized in that the temperature of the vacuum heat treatment in the sixth step is 1000-1200 ℃, and the vacuum degree is not more than 6.65 multiplied by 10-1Pa, keeping the temperature for 3-10 h, and cooling along with the furnace after vacuum heat treatment; the quenching treatment temperature is 1320 ℃, the heat preservation time is 50min, and nitrogen blowing is adopted for cooling after heat preservation. The optimized vacuum heat treatment process parameters are beneficial to desorbing hydrogen adsorbed in the tungsten alloy sintering blank during sintering in a hydrogen atmosphere and discharging the hydrogen to the outside of the tungsten alloy sintering blank body through vacuumizing, and the optimized quenching treatment process parameters are beneficial to solid solution of impurities in the tungsten alloy sintering blank into crystals, so that the uniformity degree of impurity distribution is improved, the segregation of the impurities on a fragile interface is reduced, and the performance of the tungsten alloy with internal quality defects eliminated is greatly improved.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, after the low melting point alloy, namely the bonding block, is melted, the low melting point alloy flows to the defects such as porosity and cracks in the tungsten alloy matrix material through solid phase diffusion and liquid phase diffusion, and the alloying process of tungsten alloy liquid phase generation, particle rearrangement, dissolution and precipitation is carried out, so that the quality defects such as porosity and cracks in the tungsten alloy are eliminated, and the internal quality of the tungsten alloy is improved.
2. The collapse deformation degree of the tungsten alloy matrix material is slight in the quality defect elimination process, so that the quality defects of internal looseness and cracks are eliminated on the premise of ensuring that the tungsten alloy matrix material is not deformed.
3. The method effectively eliminates the quality defects of internal looseness and cracks of the tungsten alloy, breaks through the fixed thinking that waste products caused by sintering in the traditional powder metallurgy industry cannot be saved through subsequent procedures, and solves the core quality problems that cores of tungsten alloy products, particularly large tungsten alloy products are easy to loosen, crack and the like in the liquid phase sintering process.
4. The method is relatively simple, is suitable for tungsten-nickel-copper and tungsten-nickel-iron alloys with different components, has wide application range, can be carried out on conventional molybdenum wire sintering and intermediate frequency furnaces, and has lower requirements on sintering equipment.
5. The invention adopts vacuum heat treatment or quenching treatment, further improves the density of the tungsten alloy, and can meet the requirement of the tungsten-based high-density alloy B777-15 standard.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic diagram of a 90WNiFe substrate with a defective top circular groove in the bonded block of example 1 of the present invention.
FIG. 2a is a schematic representation of a sintered tungsten alloy billet obtained in example 1 of the present invention.
FIG. 2b is a metallographic structure diagram of a sintered compact of a tungsten alloy obtained in example 1 of the present invention.
FIG. 3a is a schematic representation of a sintered tungsten alloy billet obtained in example 2 of the present invention.
Fig. 3b is a metallographic structure diagram of a tungsten alloy sintered compact obtained in example 2 of the present invention.
FIG. 4a is a schematic representation of a sintered tungsten alloy billet obtained in example 3 of the present invention.
FIG. 4b is a metallographic structure diagram of a sintered compact of a tungsten alloy obtained in example 3 of the present invention.
FIG. 5a is a schematic representation of a sintered tungsten alloy billet obtained in example 4 of the present invention.
FIG. 5b is a metallographic structure diagram of a sintered compact of a tungsten alloy obtained in example 4 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
pouring iron powder and nickel powder into a mixer to be mixed for 6 hours to obtain mixed powder; the mass content of nickel powder in the mixed powder is 70%, the mass content of iron powder is 30%, manganese powder is added into the mixed powder, and the adding amount of the manganese powder is 0.05% of the mass of the mixed powder; the ball-material ratio adopted by mixing is 0.225: 1, adopting a grinding ball with the diameter of 12mm as a steel ball;
step two, sieving the mixed powder obtained in the step one by a sieve of 140 meshes, then putting the powder into a latex sleeve, pressing the powder into a pressed blank by adopting isostatic cool pressing, and then trimming the pressed blank by a wire saw; the pressure of the cold isostatic pressing is 120MPa, and the pressure maintaining time is 2 min;
thirdly, placing the pressed blank trimmed in the second step into a muffle furnace for sintering for pre-alloying treatment to prepare a sticky lump; the temperature for pre-alloying treatment in the sintering process is 1390 ℃, and the heat preservation time is 30 min;
step four, machining the top end of the 90WNiFe base material with the quality defect inside to form a circular groove, wherein the wall thickness of the circular groove is 5mm, the depth of the circular groove is 10mm, machining the contact position of the bonding block obtained in the step three and the top end of the 90WNiFe base material with the quality defect inside until the bonding block reaches the visible light, enabling the size of the bonding block to be matched with the size of the circular groove, then placing the bonding block into the circular groove at the top end of the 90WNiFe base material with the quality defect inside, as shown in figure 1, and then placing the bonding block into a muffle furnace for sintering to obtain a tungsten alloy sintering blank, as shown in figure 2 a; the 90WNiFe base material with quality defects inside is obtained by performing internal quality ultrasonic flaw detection on an AA-level standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method; the sintering process comprises the following specific steps: under the condition of hydrogen atmosphere, firstly heating to 950 ℃ within 2h and preserving heat for 4h, then heating to 1400 ℃ within 2h and preserving heat for 3h, and then cooling;
fifthly, carrying out internal quality ultrasonic flaw detection on the tungsten alloy sintered compact obtained in the fourth step according to the AA standard specified by the GJB1580A-2004 deformed metal ultrasonic inspection method, and enabling the detection result to be qualified;
step six, the internal quality in the step five is detected by ultrasonic flaw detection to be qualifiedPlacing the tungsten alloy sintered blank in a vacuum heat treatment furnace for vacuum heat treatment to obtain the tungsten alloy with the internal porosity, cracks and other quality defects eliminated; the temperature of the vacuum heat treatment is 1000 ℃, and the vacuum degree is not more than 6.65 multiplied by 10-1Pa, the heat preservation time is 3h, and the furnace is cooled after the vacuum heat treatment.
Fig. 2b is a metallographic structure diagram of the tungsten alloy sintered compact obtained in this example, and it can be seen from fig. 2b that the structure of the tungsten alloy sintered compact is a typical tungsten alloy structure, i.e., hard phase tungsten particles are surrounded by a relatively soft solid solution of binder phase, and the binder phase is uniformly distributed, and the average diameter of the tungsten particles is grade 2 (20.91 μm).
Example 2
The embodiment comprises the following steps:
pouring tungsten powder, iron powder, nickel powder and cobalt powder into a mixer to be mixed for 8 hours to obtain mixed powder; the mass content of tungsten powder in the mixed powder is 30%, the mass content of nickel powder is 44%, the mass content of iron powder is 25.7%, the mass content of cobalt powder is 0.3%, manganese powder is added in the mixed powder, and the addition amount of the manganese powder is 0.5% of the mass of the mixed powder; the ball-material ratio adopted by mixing is 0.225: 1, adopting a grinding ball with the diameter of 14 mm;
step two, sieving the mixed powder obtained in the step one by a sieve of 140 meshes, then putting the powder into a latex sleeve, pressing the powder into a pressed blank by adopting isostatic cool pressing, and then trimming the pressed blank by a wire saw; the pressure of the cold isostatic pressing is 150MPa, and the pressure maintaining time is 8 min;
thirdly, placing the pressed blank trimmed in the second step into a muffle furnace for sintering for pre-alloying treatment to prepare a sticky lump; the temperature for pre-alloying treatment in the sintering process is 1400 ℃, and the heat preservation time is 45 min;
step four, machining the top end of the 93WNiFe base material with the quality defect inside to form a circular groove, wherein the wall thickness of the circular groove is 5mm, the depth of the circular groove is 10mm, machining the contact position of the bonding block obtained in the step three and the top end of the 93WNiFe base material with the quality defect inside, and the size of the bonding block is matched with that of the circular groove, then placing the bonding block into the circular groove at the top end of the 93WNiFe base material with the quality defect inside, and then placing the bonding block into an intermediate frequency furnace for sintering to obtain a tungsten alloy sintering blank, wherein the tungsten alloy sintering blank is shown in figure 3 a; the 93WNiFe base material with quality defects inside is obtained by performing internal quality ultrasonic flaw detection on an AA-level standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method; the sintering process comprises the following specific steps: under the condition of hydrogen atmosphere, firstly heating to 1150 ℃ within 3h, preserving heat for 5h, then heating to 1430 ℃ within 3h, preserving heat for 4h, and then cooling;
fifthly, performing internal quality ultrasonic flaw detection on the tungsten alloy sintered blank obtained in the fourth step mechanically according to the AA standard specified by the GJB1580A-2004 deformed metal ultrasonic inspection method, and enabling the detection result to be qualified;
sixthly, placing the tungsten alloy sintered blank qualified by the internal quality ultrasonic flaw detection in the step five in a vacuum heat treatment furnace for vacuum heat treatment to obtain the tungsten alloy with the internal porosity, cracks and other quality defects eliminated; the temperature of the vacuum heat treatment is 1190 ℃, and the vacuum degree is not more than 6.65 multiplied by 10-1Pa, the heat preservation time is 5h, and the furnace is cooled after the vacuum heat treatment.
Fig. 3b is a metallographic structure diagram of the tungsten alloy sintered compact obtained in this example, and it can be seen from fig. 3b that the structure of the tungsten alloy sintered compact is a typical tungsten alloy structure, i.e., hard phase tungsten particles are surrounded by a relatively soft solid solution of binder phase, and the binder phase is uniformly distributed, and the average diameter of the tungsten particles is grade 3 (23.42 μm).
Example 3
The embodiment comprises the following steps:
pouring iron powder, tungsten powder, nickel powder and cobalt powder into a mixer to be mixed for 10 hours to obtain mixed powder; the mass content of tungsten powder in the mixed powder is 40%, the mass content of nickel powder is 35.7%, the mass content of iron powder is 23.8%, the mass content of cobalt powder is 0.5%, manganese powder is added into the mixed powder, and the addition amount of the manganese powder is 2% of the mass of the mixed powder; the ball-material ratio adopted by mixing is 0.225: 1, adopting a grinding ball with the diameter of 16 mm;
step two, sieving the mixed powder obtained in the step one by a 140-mesh sieve, then putting the powder into a latex sleeve, pressing the powder into a green compact by adopting isostatic cool pressing, and then finishing the green compact by a lathe; the pressure of the cold isostatic pressing is 180MPa, and the pressure maintaining time is 10 min;
thirdly, placing the pressed blank trimmed in the second step into a muffle furnace for sintering for pre-alloying treatment to prepare a sticky lump; the temperature for pre-alloying treatment in the sintering process is 1450 ℃, and the heat preservation time is 60 min;
step four, machining the top end of the 95WNiFe base material with the quality defect inside to form a circular groove, wherein the wall thickness of the circular groove is 8mm, the depth of the circular groove is 15mm, machining the contact position of the bonding block obtained in the step three and the top end of the 95WNiFe base material with the quality defect inside until the bonding block is exposed to light, the size of the bonding block is matched with that of the circular groove, then placing the bonding block into the circular groove at the top end of the 95WNiFe base material with the quality defect inside, and then placing the bonding block into an intermediate frequency furnace for sintering to obtain a tungsten alloy sintering blank, wherein the tungsten alloy sintering blank is shown in figure 4 a; the 95WNiFe base material with the defect inside is obtained by performing internal quality ultrasonic flaw detection on an AA-grade standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method; the sintering process comprises the following specific steps: under the condition of hydrogen atmosphere, firstly heating to 1200 ℃ within 4h and preserving heat for 7h, then heating to 1460 ℃ within 4h and preserving heat for 5h, and then cooling;
fifthly, carrying out internal quality ultrasonic flaw detection on the tungsten alloy sintered compact obtained in the fourth step according to the AA standard specified by the GJB1580A-2004 deformed metal ultrasonic inspection method, and enabling the detection result to be qualified;
sixthly, placing the tungsten alloy sintered blank qualified by the internal quality ultrasonic flaw detection in the step five in a vacuum heat treatment furnace for vacuum heat treatment to obtain the tungsten alloy with the internal porosity, cracks and other quality defects eliminated; the temperature of the vacuum heat treatment is 1200 ℃, and the vacuum degree is not more than 6.65 multiplied by 10-1Pa, the heat preservation time is 10h, and the furnace is cooled after the vacuum heat treatment.
Fig. 4b is a metallographic structure diagram of the tungsten alloy sintered compact obtained in this example, and it can be seen from fig. 4b that the structure of the tungsten alloy sintered compact is a typical tungsten alloy structure in which hard phase tungsten particles are surrounded by a relatively soft solid solution of binder phase, and the binder phase is uniformly distributed, and the mean diameter of the tungsten particles is grade 5 (29.25 μm).
Example 4
The embodiment comprises the following steps:
pouring copper powder, nickel powder and cobalt powder into a mixer to be mixed for 8 hours to obtain mixed powder; the mass content of the nickel powder, the mass content of the copper powder and the mass content of the cobalt powder in the mixed powder are respectively 65.5%, 34% and 0.5%; the ball-material ratio adopted by mixing is 0.225: 1, adopting a grinding ball with the diameter of 12mm as a steel ball;
step two, sieving the mixed powder obtained in the step one by a 140-mesh sieve, then putting the powder into a latex sleeve, pressing the powder into a green compact by adopting isostatic cool pressing, and then finishing the green compact by a lathe; the pressure of the cold isostatic pressing is 120MPa, and the pressure maintaining time is 6 min;
thirdly, placing the pressed blank trimmed in the second step into a muffle furnace for sintering for pre-alloying treatment to prepare a sticky lump; the temperature for pre-alloying treatment in the sintering process is 1300 ℃, and the heat preservation time is 45 min;
step four, machining the top end of the 93WNiCu base material with the quality defect inside to form a circular groove, wherein the wall thickness of the circular groove is 3mm, the depth of the circular groove is 5mm, machining the contact position of the bonding block obtained in the step three and the top end of the 93WNiCu base material with the quality defect inside until the bonding block reaches the visible light, the size of the bonding block is matched with that of the circular groove, then placing the bonding block into the circular groove at the top end of the 93WNiCu base material with the quality defect inside, and then placing the bonding block into a muffle furnace for sintering to obtain a tungsten alloy sintering blank, wherein the tungsten alloy sintering blank is shown in figure 5 a; the 93WNiCu base material with quality defects inside is obtained by performing internal quality ultrasonic flaw detection on an AA-grade standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method; the sintering process comprises the following specific steps: under the condition of ammonia decomposition atmosphere, firstly heating to 950 ℃ within 4h and preserving heat for 5h, then heating to 1390 ℃ within 3h and preserving heat for 3h, and then cooling;
fifthly, carrying out internal quality ultrasonic flaw detection on the tungsten alloy sintered compact obtained in the fourth step according to the AA standard specified by the GJB1580A-2004 deformed metal ultrasonic inspection method, and enabling the detection result to be qualified;
sixthly, placing the tungsten alloy sintered blank qualified by the internal quality ultrasonic flaw detection in the step five into a vacuum heat treatment furnace for quenching treatment to obtain the tungsten alloy with the internal porosity, cracks and other quality defects eliminated; the quenching treatment temperature is 1320 ℃, the heat preservation time is 50min, and nitrogen gas is blown for cooling after quenching.
Fig. 5b is a metallographic structure diagram of the tungsten alloy sintered compact obtained in this example, and it can be seen from fig. 5b that the structure of the tungsten alloy sintered compact is a typical tungsten alloy structure, i.e., hard phase tungsten particles are surrounded by a relatively soft solid solution of binder phase, and the binder phase is uniformly distributed, and the average diameter of the tungsten particles is grade 3 (23.42 μm).
Example 5
This embodiment is different from embodiment 4 in that: and in the fourth step, the bonding block obtained in the third step is placed at the top end of a 93WNiCu base material with quality defects inside, then zirconium sand is adopted for paving and burying, and then the bonding block is placed in a muffle furnace for sintering to obtain a tungsten alloy sintering blank.
The tungsten alloy with the internal porosity, cracks and other quality defects eliminated, which is obtained in the embodiments 1 to 4 of the invention, is subjected to linear cutting sampling and performance detection, and the results are shown in the following table 1.
TABLE 1
As can be seen from Table 1, the tungsten alloy with internal porosity, cracks and other quality defects eliminated, which is obtained in the embodiments 1 to 4, of the invention has the yield strength, tensile strength, elongation and density meeting the requirements of the standard of the tungsten-based high-density alloy B777-15; as can be seen from the combination of FIGS. 2b to 5b, the distribution of the binder phase in the tungsten alloy structure is relatively uniform, and the tungsten crystal grains do not grow abnormally even in the range of 20.91 to 29.25. mu.m, which shows that the method of the present invention effectively eliminates the quality defects of the tungsten alloy such as internal porosity and cracks, improves the internal quality of the tungsten alloy, and ensures the performance of the tungsten alloy.
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 (9)
1. A method for eliminating internal quality defects of tungsten alloy is characterized by comprising the following steps:
pouring the powder A, tungsten powder, nickel powder and cobalt powder into a mixer for mixing to obtain mixed powder; the mass content of tungsten powder in the mixed powder is 0-40%, the mass content of nickel powder is 35.7-70%, the mass content of cobalt powder is 0-0.5%, the mass content of A powder is 23.8-34%, and the A powder is iron powder or copper powder;
step two, sieving the mixed powder obtained in the step one, then putting the sieved mixed powder into a latex sleeve, pressing the mixed powder into a pressed blank by adopting isostatic cool pressing, and then finishing the pressed blank by a wire saw or a lathe;
thirdly, placing the pressed blank trimmed in the second step into a muffle furnace for sintering for pre-alloying treatment to prepare a sticky lump;
placing the bonding block obtained in the third step on the top end of the tungsten alloy base material with quality defects inside, and then sending the tungsten alloy base material into a muffle furnace or an intermediate frequency furnace for sintering to obtain a tungsten alloy sintering blank; the tungsten alloy base material with quality defects inside is obtained by performing internal quality ultrasonic flaw detection on an AA-grade standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method;
fifthly, carrying out internal quality ultrasonic flaw detection on the tungsten alloy sintered compact obtained in the fourth step according to an AA standard specified by a GJB1580A-2004 deformed metal ultrasonic inspection method;
sixthly, placing the qualified tungsten alloy sintered blank subjected to the internal quality ultrasonic flaw detection in the step five into a vacuum heat treatment furnace, and performing vacuum heat treatment or quenching treatment to obtain a tungsten alloy with the internal quality defects eliminated; the temperature of the vacuum heat treatment is 1000-1200 ℃, and the vacuum degree is not more than6.65×10-1Pa, keeping the temperature for 3-10 h, and cooling along with the furnace after vacuum heat treatment; the quenching treatment temperature is 1320 ℃, the heat preservation time is 50min, and nitrogen blowing is adopted for cooling after heat preservation.
2. The method for eliminating the internal quality defect of the tungsten alloy as claimed in claim 1, wherein the mixing time in the step one is 6-10 h, and the ball-to-material ratio for mixing is 0.225: 1, the adopted grinding balls are steel balls with the diameter of 12 mm-16 mm.
3. The method for eliminating internal quality defects of the tungsten alloy according to claim 1, wherein the mass ratio of the nickel powder to the powder A in the mixed powder in the first step is (1.5-2.33): 1.
4. the method for eliminating the internal quality defects of the tungsten alloy as claimed in claim 1, wherein manganese powder is added to the mixed powder in the first step, and the adding mass of the manganese powder is 0.05-2% of the mass of the mixed powder before the manganese powder is added.
5. The method for eliminating the internal quality defect of the tungsten alloy according to claim 1, wherein the mixed powder in the second step is sieved by a 140-mesh sieve, then is put into a latex sleeve, and then is put into a cold isostatic press to be kept for 2-10 min under the condition that the pressing pressure is 120-180 MPa.
6. The method for eliminating the internal quality defects of the tungsten alloy according to claim 1, wherein the temperature for pre-alloying treatment in the sintering in the third step is 1300-1450 ℃, and the heat preservation time is 30-60 min.
7. The method for eliminating the internal quality defect of the tungsten alloy as claimed in claim 1, wherein the top end of the tungsten alloy base material in the fourth step is machined to form a circular groove, the sticky lump is placed in the circular groove, and the size of the sticky lump is matched with the size of the circular groove.
8. The method for eliminating the internal quality defect of the tungsten alloy as claimed in claim 1, wherein in the fourth step, the bonding block is placed on the top end of the tungsten alloy base material with the internal quality defect and then is buried and sintered by zirconium sand.
9. The method for eliminating the internal quality defects of the tungsten alloy as claimed in claim 1, wherein the sintering in the fourth step is carried out by the following specific processes: under the reducing atmosphere condition, firstly heating to 950-1200 ℃ within 2-4 h, preserving heat for 4-7 h, then heating to 1390-1460 ℃ within 2-4 h, preserving heat for 3-5 h, and then cooling.
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| CN116475422A (en) * | 2023-05-19 | 2023-07-25 | 福建国福中亚电气机械有限公司 | Preparation method and equipment of copper-tungsten alloy electrical contact |
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