CN112011711A - Method for manufacturing novel tungsten-copper alloy material - Google Patents
Method for manufacturing novel tungsten-copper alloy material Download PDFInfo
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- CN112011711A CN112011711A CN202010894794.6A CN202010894794A CN112011711A CN 112011711 A CN112011711 A CN 112011711A CN 202010894794 A CN202010894794 A CN 202010894794A CN 112011711 A CN112011711 A CN 112011711A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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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
- B22F3/1021—Removal of binder or filler
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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
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
Abstract
The novel tungsten-copper alloy material is prepared by using tungsten oxide as a raw material instead of tungsten powder and through a forming process, and the raw blank is subjected to degumming reduction, presintering, infiltration sintering and sintering to form the tungsten-copper alloy material. The manufacturing method of the novel tungsten-copper alloy material improves the tissue uniformity of the tungsten-copper alloy material and improves the mechanical property of tungsten-copper alloy material products.
Description
Technical Field
The invention relates to the field of novel material manufacturing, in particular to a manufacturing method of a novel tungsten-copper alloy material.
Background
In the prior art, the manufacturing process of the tungsten-copper alloy shaped charge liner adopts tungsten powder tungsten framework steel die pressing or isostatic pressing molding. The density difference of the tungsten skeleton blank is caused by the friction resistance of the tungsten skeleton powder and the mold wall in the steel mold pressing, and the density of the manufactured tungsten-copper alloy material is not uniform. Although the isostatic pressing blank is relatively uniform compared with a steel die pressing blank, closed holes caused by tungsten powder agglomeration cannot be eliminated. Both of these processes have the disadvantage that a uniform density and one hundred percent open porosity of the tungsten matrix material cannot be achieved. Because the normal distribution of the tungsten powder particle size of the framework material is uneven and the tungsten powder particles are agglomerated, the aperture ratio of the formed tungsten framework is less than one hundred percent, and the closed pore infiltration agent cannot be filled, so that the tungsten-copper alloy has uneven structure and reduced mechanical property. The liner is easy to break when the initiating explosive device forms a metal jet after exerting power, and the maximum power of the penetration and damage of the metal jet cannot be exerted. In addition, steel die pressing or isostatic pressing has extremely low blank utilization rate (only about 10 percent), high manufacturing cost and the like.
Disclosure of Invention
The invention aims to provide a novel tungsten-copper alloy material manufacturing method, which improves the structural uniformity of a tungsten-copper alloy material and improves the mechanical property of a tungsten-copper alloy material product.
In order to achieve the purpose, the invention provides a novel tungsten-copper alloy material manufacturing method, which comprises the steps of using tungsten oxide to replace tungsten powder as a raw material, preparing a green blank through a forming process, and carrying out degumming reduction, presintering, infiltration sintering on the green blank to generate the tungsten-copper alloy material.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps of: 70-75% of tungsten, 30-25% of copper and 2-3% of nickel, wherein the weight of tungsten oxide is calculated by the content of tungsten, and the weight of basic nickel carbonate is calculated by the content of nickel.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps of adding basic nickel carbonate and tungsten oxide into a high-energy ball mill to be wet-milled for 3-4 hours; feeding the mixture of the basic nickel carbonate and the tungsten oxide subjected to the high-energy ball milling into an internal mixer, adding 7-8 wt% of PEG (polyethylene glycol) glue, and carrying out internal mixing to obtain glue-infiltrated granules; the glue-infiltrated granular material is made into a green body by a forming process.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps of: copper is arranged around the green blank, and then the copper and the green blank are embedded into the alumina powder material boat together; and pushing the alumina powder boat embedded with copper and the green blank into a reducing atmosphere dewaxing furnace, heating to 550 ℃ from room temperature, and preserving heat for 2.5 hours to carry out first degumming reduction.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps of adding basic nickel carbonate powder, tungsten oxide powder and copper powder into a double-cone mixer to mix for 6-8 hours; feeding the mixture into an internal mixer, adding 7-8 wt% of PEG (polyethylene glycol) rubber for internal mixing to prepare rubber-infiltrated granules; the glue-infiltrated granular material is made into a green body by a forming process.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps of: burying the green blank in an alumina powder boat; and pushing the alumina powder boat embedded with the green blank into a reducing atmosphere dewaxing furnace, heating to 550 ℃ from room temperature, and preserving heat for 2.5 hours to carry out first degumming reduction.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps: after the first degumming and reduction, raising the temperature from 550 ℃ to 830 ℃, and preserving the heat for 1.5 hours to carry out second high-temperature reduction; heating from 830 ℃ to 950 ℃, presintering, preserving heat for 30 minutes, cooling to below 200 ℃ along with the furnace, and discharging.
The manufacturing method of the novel tungsten-copper alloy material comprises the following steps: and directly pushing the pre-sintered blank and the alumina powder boat into a two-belt type high-temperature molybdenum wire furnace for solution infiltration sintering, heating to 1350 +/-5 ℃, preserving the temperature for 30-40 minutes, and continuously pushing into a cooling water jacket for cooling.
The manufacturing method of the novel tungsten-copper alloy material further comprises a blank flaw detection step, wherein the tungsten-copper alloy blank subjected to infiltration sintering is subjected to flaw detection by coloring and then is transferred to a finish machining process after being free of defects.
Compared with the prior art, the invention has the beneficial technical effects that:
the manufacturing method of the novel tungsten-copper alloy material adopts tungsten oxide and copper as framework materials, oxygen atoms of the tungsten oxide are reduced by reducing atmosphere in a furnace in the processes of low-temperature degumming reduction and pre-sintering, oxygen atom hole acupuncture points which are uniformly distributed are left, and liquid metal copper and an infiltration agent are filled in the process of solution infiltration sintering, so that the tungsten-copper alloy material has good tissue uniformity, the problems of poor tissue uniformity and low material utilization rate of the tungsten-copper alloy material in the prior art are solved, compared with the prior art, the material utilization rate of the tungsten-copper alloy material reaches more than 80 percent, the prior art only has about 10 percent, and the open porosity of the tungsten framework can reach more than 98 percent;
the invention improves the density uniformity of the tungsten-copper alloy material structure, and ensures that the tungsten-copper alloy shaped charge liner forms metal jet which is not broken in the high-speed flight process; when the initiating explosive device exerts power, the phenomena of radial spalling, jet bending, local thickening and the like of the jet fluid are not generated in the process of crushing the tissues of the initiating explosive device.
Drawings
The manufacturing method of the novel tungsten-copper alloy material of the present invention is given by the following examples and the accompanying drawings.
FIG. 1 is a schematic view of a green body according to a preferred embodiment of the present invention.
FIG. 2 is a schematic diagram of a tungsten-copper alloy liner finished product according to a preferred embodiment of the present invention.
Detailed Description
The method for manufacturing the novel tungsten-copper alloy material of the present invention will be described in further detail with reference to fig. 1 to 2.
According to the manufacturing method of the novel tungsten-copper alloy material, tungsten oxide is used as a framework raw material instead of tungsten powder, the process formula and the process conditions are improved, and the problem that the tungsten-copper alloy material in the prior art is poor in structural uniformity is solved.
The invention relates to a method for manufacturing a novel tungsten-copper alloy material, which uses tungsten oxide to replace tungsten powder as a raw material, prepares a green blank through a forming process, and generates the tungsten-copper alloy material through degumming reduction, presintering, infiltration sintering and the like of the green blank.
Example one
In this example, the method for manufacturing a tungsten-copper alloy material according to the present invention will be described in detail by taking the manufacturing of a tungsten-copper alloy liner as an example.
The process flow of the embodiment is as follows: batching → high-energy ball milling → gum mixing and granulating → injection molding → degumming and reduction → presintering → solution infiltration and sintering → blank flaw detection → fine processing → inspection → packaging → finished product.
1) Ingredients
The raw materials are tungsten oxide, copper and basic nickel carbonate, wherein nickel is used as an infiltration agent; preferably, all the raw materials are in powder form;
the weight ratio of each component is as follows: 70-75% of tungsten, 30-25% of copper and 2-3% of nickel, wherein the weight of tungsten oxide is calculated by the content of tungsten, and the weight of basic nickel carbonate is calculated by the content of nickel;
2) high-energy ball mill
Adding the basic nickel carbonate powder and the tungsten oxide powder into a high-energy ball mill for wet milling for 3-4 hours;
3) granulating by mixing with glue
Feeding the mixture of the basic nickel carbonate and the tungsten oxide subjected to the high-energy ball milling into an internal mixer, adding 7-8% (weight percentage) of PEG (polyethylene glycol) glue, and carrying out internal mixing to obtain glue-doped granules;
4) injection molding
The glue-doped granules are subjected to injection molding to obtain a green body (namely a tungsten skeleton blank), and parameters of an injection molding process, such as injection temperature and injection pressure, are adjusted according to the shape and size of a product as shown in figure 1; specifically, the weight of the required glue-doped granulating material is calculated according to the design of the liner, the glue-doped granulating material is filled into a designed conical die cavity for heating and static pressure, and a green blank (tungsten skeleton blank) is removed after the glue-doped granulating material in the die cavity is completely compacted and cooled;
the raw blank prepared by the glue-infiltrated granulating material is not limited to injection molding, and other molding methods can also be adopted;
5) reduction of degumming
Inverting the green blank (i.e. with the cone opening upward); pressing copper powder into copper powder blocks, placing the copper powder blocks on the inverted green blanks, and embedding the copper powder blocks and the green blanks into an alumina powder material boat; pushing the alumina powder boat embedded with the copper powder blocks and the green blanks into a reducing atmosphere dewaxing furnace, heating the alumina powder boat from room temperature to 550 ℃, and preserving heat for 2.5 hours to carry out primary degumming reduction;
the copper powder block can be arranged at any position around the green blank and is not limited above the green blank; copper powder can be directly sprayed on the periphery of the green body, namely the copper powder can be in a block shape or a powder shape, and only the copper powder and the green body are embedded into an alumina powder material boat;
preferably, the embodiment further manufactures a conical alumina spacer, the outer surface of the conical alumina spacer is matched with the inner profile of a green blank (tungsten skeleton blank), the green blank is buckled on the conical alumina spacer and inverted, and then the copper powder block and the green blank are embedded into the alumina powder boat together, so that the technical problems of deformation and collapse of the tungsten skeleton blank in degumming reduction, pre-sintering and solution infiltration sintering of the tungsten skeleton during batch production are solved;
6) pre-firing
After the first degumming and reduction, raising the temperature from 550 ℃ to 830 ℃, and preserving the heat for 1.5 hours to carry out second high-temperature reduction; heating from 830 ℃ to 950 ℃, presintering, preserving heat for 30 minutes, cooling to below 200 ℃ along with the furnace, and discharging;
7) sintering by infiltration
Directly pushing the presintered blank and the alumina powder boat into a two-belt type high-temperature molybdenum wire furnace for solution infiltration sintering; in the embodiment, the temperature of one belt of the two-belt type high-temperature molybdenum wire furnace is controlled at 900 +/-5 ℃, the temperature of the two belts is controlled at 1350 +/-5 ℃, and the two belts are continuously pushed into a cooling water jacket for cooling after being kept at the high temperature section (1350 +/-5 ℃) for 30-40 minutes;
because the nickel serving as an introduction agent is added in the form of basic nickel carbonate, when the dewaxing furnace is in a reducing atmosphere at a medium temperature, the reducing atmosphere (hydrogen) can finely and dispersedly uniformly distribute the active metal nickel with a catalytic action on tungsten skeleton particles, and because the nickel serving as the introduction agent is uniformly distributed and the tungsten nickel and the nickel copper are mutually dissolved, the copper is uniformly distributed in the solution infiltration sintering process;
8) flaw detection of blank
And (3) transferring the tungsten-copper shaped charge liner blank subjected to infiltration sintering to a finish machining process after dye penetrant inspection is carried out on the blank without defects, wherein a finished product is shown in figure 2.
Because tungsten oxide and copper are used as framework materials, oxygen atoms of the tungsten oxide are reduced by reducing atmosphere in the furnace in the processes of low-temperature degumming reduction and presintering, uniformly distributed oxygen atom hole acupuncture points are left, and the liquid metal copper and an infiltration agent are filled in the process of solution infiltration sintering. The aperture ratio of the tungsten skeleton prepared by the invention can reach more than 98 percent, the copper distribution of the infiltration agent is very uniform, the tungsten-copper alloy shaped charge liner is stable and complete when the target test metal is jetted, and the stability of multiple test shots is consistent.
Example two
The process flow of the embodiment is as follows: batching → mixing → granulating by mixing with glue → injection molding → reduction by degumming → presintering → infiltration and sintering → flaw detection of blank → fine processing → inspection → packaging → finished product.
1) Ingredients
The raw materials are tungsten oxide, copper and basic nickel carbonate, wherein nickel is used as an infiltration agent; preferably, all the raw materials are in powder form;
the weight ratio of each component is as follows: 70-75% of tungsten, 30-25% of copper and 2-3% of nickel, wherein the weight of tungsten oxide is calculated by the content of tungsten, and the weight of basic nickel carbonate is calculated by the content of nickel;
2) mixing material
Adding the basic nickel carbonate powder, the tungsten oxide powder and the copper powder into a double-cone mixer to mix for 6-8 hours;
3) granulating by mixing with glue
Feeding the mixture into an internal mixer, adding 7-8% (weight percent) of PEG (polyethylene glycol) glue for internal mixing to prepare glue-infiltrated and granular materials;
4) injection molding
Performing injection molding on the glue-infiltrated granules to obtain a green body (namely a tungsten skeleton green body); the injection molding process parameters such as injection temperature, injection pressure and the like are adjusted according to the shape and the size of the product;
the raw blank prepared by the glue-infiltrated granulating material is not limited to injection molding, and other molding methods can also be adopted;
5) reduction of degumming
The green body is inverted (i.e. the cone opening is upward) and is buried in the alumina powder boat; pushing the alumina powder boat embedded with the green blank into a reducing atmosphere dewaxing furnace, heating the alumina powder boat from room temperature to 550 ℃, and preserving heat for 2.5 hours to carry out primary degumming reduction;
6) pre-firing
After the first degumming and reduction, raising the temperature from 550 ℃ to 830 ℃, and preserving the heat for 1.5 hours to carry out second high-temperature reduction; heating from 830 ℃ to 950 ℃, presintering, preserving heat for 30 minutes, cooling to below 200 ℃ along with the furnace, and discharging;
7) sintering by infiltration
Directly pushing the presintered blank and the alumina powder boat into a two-belt type high-temperature molybdenum wire furnace for solution infiltration sintering; in the embodiment, the temperature of one belt of the two-belt type high-temperature molybdenum wire furnace is controlled at 900 +/-5 ℃, the temperature of the two belts is controlled at 1350 +/-5 ℃, and the two belts are continuously pushed into a cooling water jacket for cooling after being kept at the high temperature section (1350 +/-5 ℃) for 30-40 minutes;
8) flaw detection of blank
And (4) transferring the tungsten-copper shaped charge liner blank subjected to infiltration sintering to a finish machining process after the blank is subjected to dye penetrant inspection and is free of defects.
The difference between the second embodiment and the first embodiment is that the second embodiment mixes tungsten oxide, copper and nickel to prepare a green body, and degumms and reduces together, while the first embodiment mixes tungsten oxide and nickel to prepare a green body, and adds copper in the degummed reduction step. When the tungsten content is lower, example two is used.
Claims (9)
1. The novel tungsten-copper alloy material is characterized in that tungsten oxide is used as a raw material to replace tungsten powder, a green body is prepared through a forming process, and the green body is subjected to degumming reduction, pre-sintering, infiltration sintering and sintering to generate the tungsten-copper alloy material.
2. The manufacturing method of the novel tungsten-copper alloy material according to claim 1, wherein the raw materials comprise tungsten oxide, copper and basic nickel carbonate, and the weight ratio of each component is as follows: 70-75% of tungsten, 30-25% of copper and 2-3% of nickel, wherein the weight of tungsten oxide is calculated by the content of tungsten, and the weight of basic nickel carbonate is calculated by the content of nickel.
3. The manufacturing method of the novel tungsten-copper alloy material according to claim 2, wherein basic nickel carbonate and tungsten oxide are added into a high-energy ball mill to be wet-milled for 3-4 hours; feeding the mixture of the basic nickel carbonate and the tungsten oxide subjected to the high-energy ball milling into an internal mixer, adding 7-8 wt% of PEG (polyethylene glycol) glue, and carrying out internal mixing to obtain glue-infiltrated granules; the glue-infiltrated granular material is made into a green body by a forming process.
4. The method for manufacturing a novel tungsten-copper alloy material according to claim 3, wherein the degumming reduction comprises: copper is arranged around the green blank, and then the copper and the green blank are embedded into the alumina powder material boat together; and pushing the alumina powder boat embedded with copper and the green blank into a reducing atmosphere dewaxing furnace, heating to 550 ℃ from room temperature, and preserving heat for 2.5 hours to carry out first degumming reduction.
5. The manufacturing method of the novel tungsten-copper alloy material according to claim 2, wherein the basic nickel carbonate powder, the tungsten oxide powder and the copper powder are added into a double-cone mixer and mixed for 6-8 hours; feeding the mixture into an internal mixer, adding 7-8 wt% of PEG (polyethylene glycol) rubber for internal mixing to prepare rubber-infiltrated granules; the glue-infiltrated granular material is made into a green body by a forming process.
6. The method for manufacturing a novel tungsten-copper alloy material according to claim 5, wherein the degumming reduction comprises: burying the green blank in an alumina powder boat; and pushing the alumina powder boat embedded with the green blank into a reducing atmosphere dewaxing furnace, heating to 550 ℃ from room temperature, and preserving heat for 2.5 hours to carry out first degumming reduction.
7. The method for manufacturing a novel tungsten-copper alloy material according to claim 4 or 6, wherein the pre-firing comprises: after the first degumming and reduction, raising the temperature from 550 ℃ to 830 ℃, and preserving the heat for 1.5 hours to carry out second high-temperature reduction; and raising the temperature from 830 ℃ to 950 ℃, presintering, preserving the heat for 30-40 minutes, cooling to below 200 ℃ along with the furnace, and discharging.
8. The method for manufacturing the novel tungsten-copper alloy material according to claim 7, wherein the infiltration sintering comprises: and directly pushing the pre-sintered blank and the alumina powder boat into a two-belt type high-temperature molybdenum wire furnace for infiltration sintering, heating to 1350 +/-5 ℃, preserving the heat for 30 minutes, and continuously pushing into a cooling water jacket for cooling.
9. The method for manufacturing the novel tungsten-copper alloy material according to claim 1, further comprising a blank flaw detection step, wherein the tungsten-copper alloy blank subjected to infiltration sintering is subjected to dye penetrant flaw detection and then is subjected to a finishing process after being free from defects.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114160787A (en) * | 2021-12-07 | 2022-03-11 | 沈阳金昌蓝宇新材料股份有限公司 | Manufacturing method of non-shrinkage tungsten framework |
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