CN114131026B - Process for producing molybdenum tube blank by mould pressing method - Google Patents
Process for producing molybdenum tube blank by mould pressing method Download PDFInfo
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- CN114131026B CN114131026B CN202111487319.8A CN202111487319A CN114131026B CN 114131026 B CN114131026 B CN 114131026B CN 202111487319 A CN202111487319 A CN 202111487319A CN 114131026 B CN114131026 B CN 114131026B
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 298
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 103
- 239000011733 molybdenum Substances 0.000 title claims abstract description 103
- 238000000034 method Methods 0.000 title claims abstract description 62
- 238000003825 pressing Methods 0.000 title claims abstract description 43
- 238000000227 grinding Methods 0.000 claims abstract description 71
- 239000001257 hydrogen Substances 0.000 claims abstract description 45
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 45
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 29
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 23
- 239000010959 steel Substances 0.000 claims abstract description 23
- 238000000748 compression moulding Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 25
- 238000004321 preservation Methods 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 10
- BDWFYHUDXIDTIU-UHFFFAOYSA-N ethanol;propane-1,2,3-triol Chemical compound CCO.OCC(O)CO BDWFYHUDXIDTIU-UHFFFAOYSA-N 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007723 die pressing method Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 27
- 239000000463 material Substances 0.000 abstract description 12
- 238000011068 loading method Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 235000011187 glycerol Nutrition 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 239000013077 target material Substances 0.000 description 6
- 238000009966 trimming Methods 0.000 description 6
- 238000009694 cold isostatic pressing Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 4
- 238000005242 forging Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
- B22F5/106—Tube or ring forms
-
- 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
-
- 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
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- 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
-
- 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
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a process for producing a molybdenum tube blank by a mould pressing method, which comprises the following steps: 1. reducing molybdenum powder by hydrogen to obtain reduced molybdenum powder; 2. preparing a molybdenum ring pressed compact from the reduced molybdenum powder by adopting a compression molding method; 3. pre-sintering the molybdenum ring pressed blank to obtain a molybdenum ring pre-sintered blank; 4. grinding two end faces of the molybdenum ring preform into visible light; 5. and cleaning the surfaces of a plurality of molybdenum ring pre-sintered blanks subjected to grinding visible light, sequentially loading into a steel sheath, vacuumizing and sealing, and performing hot isostatic pressing to obtain the molybdenum tube blank. The invention combines the compression molding method with the pre-sintering and the hot isostatic pressing, realizes the preparation of the molybdenum tube blank, improves the precision and the production efficiency of the molybdenum tube blank and the utilization rate of the molybdenum tube blank material and reduces the molybdenum metal loss through controlling the shape and the size of the molybdenum ring pressed blank and the connection process of the molybdenum ring pre-sintering, thereby reducing the production cost.
Description
Technical Field
The invention belongs to the technical field of molybdenum tube target material processing, and particularly relates to a process for producing a molybdenum tube blank by a mould pressing method.
Background
The molybdenum target material product has excellent high-temperature strength, good electric conduction and thermal conductivity, low specific impedance and good corrosion resistance, and is an indispensable key material in the industries of information storage, integrated circuit chips, in particular flat panel displays, thin film solar cells, sapphire manufacturing and the like at present.
The molybdenum tube target has high utilization rate and good coating uniformity, is suitable for large-area continuous magnetron sputtering production lines, and has become a new trend of future sputtering target development. The theoretical utilization rate of the tubular rotary target can reach 70% -80%, which is greatly higher than that of the planar target by 2% -30%, and the production cost of the coating is reduced, so that the tubular rotary target becomes the main direction of target development.
In addition, as the size of the liquid crystal screen is increased in recent years, the corresponding sputtering plate-shaped molybdenum target also increases the area of the sputtering plate-shaped molybdenum target, and the production difficulty of the molybdenum planar target is increased. The rotating molybdenum tube is used as a target, the width of the screen is determined by the length of the molybdenum tube, and the length of the screen is not limited. The outer diameter of the current molybdenum tube target is 120-160 mm, the inner diameter is 100-140 mm, and the length is 1500-4100 mm.
The production of the molybdenum tube target material generally takes a molybdenum tube blank as a raw material, and is generally obtained through processing means such as extrusion, forging, spinning and the like after induction heating, subsequent heat treatment and machining. Patent publication No. CN109746439A discloses a device for isostatic pressing and precise forming of a molybdenum thick-wall tube blank and a homogeneous sintering method, wherein a cold isostatic pressing method is adopted to compact, and then sintering is carried out to prepare a sintered thick-wall molybdenum tube blank, the material utilization rate of the sintered tube blank is about 85%, and the relative density is over 96%; the patent with publication number CN110000391A discloses a preparation method of a molybdenum tube for a rotary target, wherein a stainless steel sheath is manufactured, powder is packed and a hot isostatic pressing method is adopted to prepare a molybdenum tube blank; the patent with publication number CN104646929A discloses a method for manufacturing a molybdenum tube target material, wherein a molybdenum tube blank is prepared by adopting the methods of powder filling, cold isostatic pressing and hydrogen sintering; the patent with publication number CN112376022A discloses a preparation method of a rotary molybdenum tube target material, which adopts molybdenum powder to be filled into a rubber sleeve, and molybdenum tube blank is prepared by secondary isostatic cool pressing, high-temperature spraying of molybdenum powder slurry and high-temperature sintering. The main processes of blank pressing and forming in the above methods are all produced by adopting cold isostatic pressing or hot isostatic pressing processes, and the two methods have the characteristics of simple processes, short process flow, uniform structure and easy quality control. However, the molybdenum tube pressed compact prepared by adopting the cold isostatic pressing blank making process is irregular in shape, easy to form the phenomenon of waisting with big two ends and small middle and low in actual yield; the molybdenum powder is filled into a steel sheath to be directly produced by a hot isostatic pressing process, the deoxidization effect of the prepared molybdenum tube blank is relatively poor in the production process, and the molybdenum tube blank is easy to cause that the oxygen content of the molybdenum tube blank is relatively high and exceeds the requirements in YS/T1063-2015 molybdenum target.
How to prepare a high-precision molybdenum tube blank and how to realize a preparation process with less molybdenum metal loss, high production efficiency and low cost is a problem to be solved urgently in the industry.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a process for producing a molybdenum tube blank by a mould pressing method aiming at the defects in the prior art. The process combines the compression molding method with the pre-sintering and the hot isostatic pressing, realizes the preparation of the molybdenum tube blank, effectively improves the precision and the production efficiency of the molybdenum tube blank, and simultaneously improves the material utilization rate of the molybdenum tube blank and reduces the molybdenum metal loss through controlling the shape and the size of the molybdenum ring pressed blank and controlling the connecting process of the molybdenum ring pre-sintering, thereby reducing the production cost and ensuring that the produced molybdenum tube blank has better tissue compactness and uniformity.
In order to solve the technical problems, the invention adopts the following technical scheme: a process for producing molybdenum tube blanks by a compression molding method, comprising the steps of:
Firstly, putting molybdenum powder into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder;
Step two, filling the reduced molybdenum powder obtained in the step one into a molybdenum ring pressing mold, and preparing a molybdenum ring pressed compact by adopting a compression molding method;
Placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the step three to obtain visible light;
and fifthly, cleaning the surface of the molybdenum ring pre-sintered blank subjected to the grinding of the visible light in the fourth step until no foreign matters exist, sequentially filling the molybdenum ring pre-sintered blank into a steel sheath according to an arrangement mode that end faces are connected, vacuumizing and sealing, and performing hot isostatic pressing to obtain a molybdenum tube blank.
According to the invention, firstly, the molybdenum powder is subjected to hydrogen reduction to effectively reduce the oxygen content of harmful elements in the raw material molybdenum powder, and the oxygen content is generally controlled within the standard range of YS/T1063-2015 molybdenum target, so that the oxygen content in a molybdenum tube blank prepared by subsequent processing is ensured to reach the standard, and a foundation is laid for preparing the molybdenum tube target; and then preparing a molybdenum ring pressed blank by adopting a compression molding method, pre-sintering to obtain a molybdenum ring pre-sintered blank, grinding the two end faces of the molybdenum ring pre-sintered blank to obtain visible light, cleaning the surfaces of a plurality of molybdenum ring pre-sintered blanks, and then filling the cleaned surfaces into a sheath for hot isostatic pressing to obtain the molybdenum tube blank. The traditional cold isostatic pressing forming fills molybdenum powder in a soft rubber sleeve, the phenomena of uneven powder filling and poor shape inevitably exist, so that the problems of deviation such as waisting, poor roundness, big and small heads, eccentricity and the like of a pressed blank are caused, the pressed blank loss is more than 15 percent and more, and the precision of a molybdenum tube blank is limited; the invention adopts a compression molding method to press the molybdenum ring pressed compact, the shape and the size of the molybdenum ring pressed compact are completely controllable, the precision of a molybdenum tube blank is favorably improved, the compact loss of the pressed compact is not more than 2 percent, the compactness of the molybdenum ring pressed compact is improved by combining the pre-bonding, the solvent such as a binder in the molybdenum ring pressed compact is removed, and the molybdenum ring pressed compact is pressed by hot isostatic pressing after being stacked by combining a plurality of molybdenum ring pressed blanks. The invention improves the pressing precision and the pressing efficiency of the molybdenum tube blank, further improves the utilization rate of the molybdenum tube blank material to more than 95%, and reduces the raw material cost; meanwhile, the end faces of the molybdenum ring pre-sintered blanks are connected and arranged and sintered to prepare the molybdenum tube blank, so that the production efficiency is improved, the length of the molybdenum tube blank can be controlled by adjusting the number of the molybdenum ring pre-sintered blanks, the dimensional accuracy of the molybdenum tube blank is further controlled, the yield of the molybdenum tube blank is improved, and the comprehensive yield can reach more than 93%.
The molybdenum tube blank produced by the invention has more compact tissue structure and finer and more uniform grain size, is prepared by subsequent extrusion processing or forging, is simultaneously processed by combining a small extrusion ratio and a small forging ratio, reduces processing difficulty and risk, can obtain a large-specification molybdenum tube target, and improves the surface quality and the internal quality of the molybdenum tube target; or the molybdenum tube blank is machined and lathed to directly obtain the small-specification molybdenum tube target material.
The process for producing the molybdenum tube blank by the mould pressing method is characterized in that the Fisher particle size of the molybdenum powder in the first step is 6.0-8.0 mu m, and the mass purity is more than 99.95%. Compared with the conventional commercial molybdenum powder with the specification of 3-5 mu m, the molybdenum powder with the specification has better fluidity, the reduced molybdenum powder obtained after reduction is easier to be uniformly distributed in a molybdenum ring pressing mold in the compression molding process, and the pressed molybdenum ring pressed compact has good uniformity.
The process for producing the molybdenum tube blank by the mould pressing method is characterized in that the temperature of hydrogen reduction in the first step is 800-1000 ℃, the heat preservation time is 60-180 min, and the hydrogen pressure is 0.12-0.15 MPa. According to the invention, molybdenum powder is filled into a plurality of molybdenum boats, the molybdenum powder is placed in a hydrogen reduction furnace for hydrogen reduction, and the reduction efficiency is ensured by controlling the technological parameters of hydrogen reduction, so that the oxygen content in the molybdenum powder is reduced, and the purpose of controlling the oxygen content of a molybdenum tube blank is realized by reducing the oxygen content in raw materials.
The process for producing the molybdenum tube blank by the mould pressing method is characterized in that the specific process for preparing the molybdenum ring pressed blank by the mould pressing method in the second step comprises the following steps: adding glycerol and ethanol solution as a binder into the reduced molybdenum powder, uniformly mixing, then filling into a molybdenum ring pressing mold, and maintaining the pressure for 15-45 s by adopting the pressure of 250-350 MPa to obtain a molybdenum ring pressed compact; the glycerol-ethanol solution is prepared from glycerol and ethanol according to the volume ratio of 1:1, the added mass of the glycerol-ethanol solution is 0.2% -0.5% of the mass of the reduced molybdenum powder, and the ratio of the height to the diameter of the molybdenum ring pressed compact is not more than 1:2. the adhesive has the advantages that the adhesive is adopted to improve the bonding capability between molybdenum powders, so that the bonding performance of molybdenum ring pressed compacts is improved, the relative density of the molybdenum ring pressed compacts is improved, the defects of the molybdenum ring pressed compacts are reduced, and the powder spraying phenomenon in the pressing process is prevented; meanwhile, the compression molding method of the molybdenum ring compression mold for two-way compression by adopting the upper mold punch and the lower mold punch is combined, so that the quality of the molybdenum ring pressed compact is uniform and consistent, the bonding strength is improved, and the subsequent process is facilitated to be smoothly carried out.
The process for producing the molybdenum tube blank by the mould pressing method is characterized in that the temperature of the pre-junction in the step three is 1200-1400 ℃, and the heat preservation time is 60-120 min. The invention promotes the densification of the structure by controlling the pre-sintering process parameters of the molybdenum ring pressed blank, controls the relative density to be more than 70%, is beneficial to the follow-up hot isostatic pressing, simultaneously further reduces the oxygen content in the molybdenum ring pressed blank, promotes the solvent such as the binder added in the compression molding method to volatilize rapidly at high temperature, and improves the quality of the molybdenum tube blank.
The process for producing the molybdenum tube blank by the mould pressing method is characterized in that the single-sided grinding amount of grinding visible light in the fourth step is 0.2-0.5 mm, the grinding travel speed is 15-27 m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, and the feed rate is 0.01-0.02 mm; the roughness Ra of two end surfaces of the molybdenum ring preform after grinding the visible light is less than or equal to 0.8 mu m, the parallelism of the two end surfaces is not more than 0.1mm, and the concentricity is not more than 0.4mm. According to the invention, the dimensional accuracy of the two end faces of the molybdenum ring pre-sintered blank is controlled by limiting the process parameters of grinding visible light, so that the contact area of the adjacent end faces is enlarged, and a good contact surface state is provided for subsequent hot isostatic pressing.
The process for producing the molybdenum tube blank by using the mould pressing method is characterized in that the pressure of the hot isostatic pressing in the fifth step is 100 MPa-150 MPa, the temperature is 1200-1350 ℃, and the heat preservation time is 60-240 min. According to the invention, by controlling the technological parameters of hot isostatic pressing, high-temperature and high-pressure conditions are provided, so that the mutual diffusion of molybdenum atoms on adjacent contact surfaces in the end surfaces of the molybdenum ring pre-billets is promoted to realize effective connection, the depth of a bonding layer is increased, and the integral reliable connection of the molybdenum tube billets is realized.
The process for producing the molybdenum tube blank by the mould pressing method is characterized in that the density of the molybdenum tube blank in the fifth step is more than 99% of theoretical density, and the average grain size is not more than 50 mu m. The molybdenum tube blank prepared by the method has good tissue compactness and uniformity and wide application prospect.
Compared with the prior art, the invention has the following advantages:
1. The invention combines the compression molding method with the pre-bonding and the hot isostatic pressing, realizes the preparation of the molybdenum tube blank, effectively improves the precision and the production efficiency of the molybdenum tube blank, and simultaneously improves the material utilization rate of the molybdenum tube blank and reduces the molybdenum metal loss through controlling the shape and the size of the molybdenum ring pressed blank and the connection process of the molybdenum ring pre-bonding, thereby reducing the production cost and ensuring that the produced molybdenum tube blank has better tissue compactness and uniformity.
2. The invention adopts the mould pressing method to prepare the molybdenum ring pressed compact, the size and specification of the mould can be designed according to the specification of the target product, the shape and specification size of the molybdenum ring pressed compact can be completely controlled, the roundness and the size deviation of the molybdenum ring pressed compact are controlled to be not more than 0.5mm, the loss of molybdenum metal in the subsequent processing is reduced, the product rate of a molybdenum tube blank is improved, and the mould pressing method has simple technological operation and high production efficiency.
3. According to the invention, the molybdenum ring pressed blank is placed in the hydrogen molybdenum wire push rod furnace for pre-sintering, the device is simple, the operation is convenient, the density of the molybdenum ring pressed blank (which can reach 70% of theoretical density) is effectively improved, the oxygen content in the molybdenum ring pressed blank is further reduced, and the oxygen content in the molybdenum tube blank is ensured to be within the standard range of YS/T1063-2015 molybdenum target.
4. The invention grinds the two end faces of the molybdenum ring pre-bonded blank with visible light as a bonding surface for diffusion connection of molybdenum atoms in the subsequent hot isostatic pressing, thereby providing more favorable conditions for diffusion connection.
5. The connecting parts in the molybdenum tube blank prepared by the method are tightly combined, the strength is higher, the shape and the size of the molybdenum tube blank are uniform, the structure of the molybdenum tube is fine and uniform, the compactness is good, and the method is suitable for the subsequent extrusion, forging and other pressure processing.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is an assembly drawing of a molybdenum ring pressing mold used in the compression molding method of the present invention.
Fig. 2 is a schematic structural view of a combined female die in a molybdenum ring pressing die used in the compression molding method of the invention.
FIG. 3 is a schematic view of the structure of the molybdenum ring preform of the present invention after being encased in a steel sheath.
Fig. 4 is a metallographic structure diagram of a molybdenum tube blank prepared in example 1 of the present invention.
Reference numerals illustrate:
1-combining female die; 1-a ring module; 1-2-mounting a mark;
2, a female die outer ring 3 and a die frame; 4-upper die stamping;
5-lower stamping; 6-molybdenum ring pre-sintering; 7, steel sheath;
8-vacuumizing tube.
Detailed Description
As shown in fig. 1 and 2, a molybdenum ring pressing mold adopted by the compression molding method comprises a combined female mold 1 and an upper punch 4 arranged in the combined female mold 1, wherein a lower punch 5 matched with the upper punch 4 is arranged at the lower part of the combined female mold 1, a female mold outer ring 2 is coated on the outer side of the combined female mold 1, a mold frame 3 is arranged on the outer side of the female mold outer ring 2, the combined female mold in the molybdenum ring pressing mold is formed by splicing and combining 3 120-degree annular modules 1-1, and mounting marks 1-2 are arranged at two ends of each annular module 1-1.
As shown in fig. 3, the steel sheath after the molybdenum ring pre-formed body is filled in the steel sheath comprises a steel sheath 7 and a plurality of molybdenum ring pre-formed bodies 6 which are arranged in the steel sheath 7 and are stacked in an arrangement mode that the end faces are connected, and the end part of the steel sheath 7 is provided with a vacuumizing tube 8.
Example 1
The embodiment comprises the following steps:
firstly, putting molybdenum powder with the Fisher particle size of 7.2 mu m and the mass purity of 99.95% into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder; the temperature of hydrogen reduction is 800 ℃, the heat preservation time is 180min, and the hydrogen pressure is 0.12MPa;
Step two, adding 60g of a mixture of glycerin and ethanol according to a ratio of 1: the glycerol-ethanol solution prepared by the volume ratio of 1 is used as a binder and is uniformly mixed, then the mixture is put into a molybdenum ring pressing die, and the pressure of 350MP is used for maintaining the pressure for 30s, so that the height-diameter ratio of 1:1.53 molybdenum ring compact; the outer diameter of the combined female die in the molybdenum ring pressing die is 260mm, and the inner diameter is 165mm;
Placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact; the temperature of the pre-junction is 1200 ℃, and the heat preservation time is 120min; the outer diameter of the molybdenum ring preform is 235mm, the inner diameter is 150mm, and the height is 155mm;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the 10 steps by adopting a 7130 surface grinding machine respectively to obtain visible light; the grinding stroke speed of the grinding visible light is 20m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, the feeding amount is 0.01mm, the single-sided grinding amount is 0.4mm, 0.3mm, 0.5mm, 0.2mm, 0.3mm, 0.4mm, 0.2mm and 0.4mm respectively, the roughness Ra=0.65 mu m of the two end faces of the molybdenum ring preform after the grinding visible light is 0.6 kg, 29.6kg, 29.7kg, 29.5kg, 29.8kg, 29.7kg, 29.6kg, 29.8kg and 29.6kg respectively, and the parallelism of the two end faces is 0.05mm, and the concentricity is 0.2mm respectively;
Step five, cleaning the surfaces of the 10 molybdenum ring pre-blanks subjected to grinding and visible light until no foreign matters exist, sequentially loading the molybdenum ring pre-blanks into a Q235 steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, performing hot isostatic pressing, taking down the Q235 steel sheath, and performing turning and trimming to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 150MPa, the temperature is 1300 ℃, and the heat preservation time is 120min.
The detection shows that the molybdenum tube blank obtained in the embodiment has the mass of 292kg, the outer diameter of 220mm, the inner diameter of 140mm, the length of 1280mm, the density of 10.12g/cm 3, the average grain size of 45 mu m and the comprehensive utilization rate of materials of 97.3 percent.
FIG. 4 is a metallographic structure diagram of a molybdenum tube blank prepared in this example, and according to FIG. 4, the average grain size of the molybdenum tube blank was measured to be 45 μm by the intercept point method in GB/T6394-2017 method for measuring average grain size of metals.
Example 2
The embodiment comprises the following steps:
Firstly, putting molybdenum powder with the Fisher particle size of 7.5 mu m and the mass purity of 99.96% into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder; the temperature of hydrogen reduction is 1000 ℃, the heat preservation time is 60min, and the hydrogen pressure is 0.15MPa;
Step two, adding 60g of a mixture of glycerin and ethanol according to a ratio of 1: the glycerol-ethanol solution prepared by the volume ratio of 1 is used as a binder and is uniformly mixed, then the mixture is put into a molybdenum ring pressing die, and the pressure is maintained for 45 seconds by adopting the pressure of 300MPa, so that the high diameter ratio of 1:1.49 molybdenum ring compact; the outer diameter of the combined female die in the molybdenum ring pressing die is 260mm, and the inner diameter is 165mm;
Placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact; the temperature of the pre-junction is 1350 ℃, and the heat preservation time is 60min; the outer diameter of the molybdenum ring preform is 235mm, the inner diameter of the molybdenum ring preform is 148mm, and the height of the molybdenum ring preform is 160mm;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the 10 steps by adopting a 7130 surface grinding machine respectively to obtain visible light; the grinding stroke speed of the grinding visible light is 15m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, the feeding amount is 0.02mm, the single-sided grinding amount is 0.5mm, 0.4mm, 0.3mm, 0.5mm, 0.2mm, 0.3mm and 0.3mm respectively, the roughness Ra=0.58 mu m of the two end faces of the molybdenum ring preform after the grinding visible light is obtained, the mass of the 10 molybdenum ring preforms after the grinding visible light is 29.5kg, 29.6kg, 29.7kg, 29.5kg, 29.8kg, 29.7kg, the parallelism of the two end faces is 0.08mm, and the concentricity is 0.3mm respectively;
step five, cleaning the surfaces of the 10 molybdenum ring pre-blanks subjected to grinding and visible light until no foreign matters exist, sequentially loading the molybdenum ring pre-blanks into a Q235 steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, performing hot isostatic pressing, taking down the Q235 steel sheath, and performing turning and trimming to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 100MPa, the temperature is 1350 ℃, and the heat preservation time is 180min.
The detection shows that the molybdenum tube blank obtained in the embodiment has the mass of 290kg, the outer diameter of 218mm, the inner diameter of 138mm, the length of 1300mm, the density of 10.10g/cm 3, the average grain size of 47 mu m and the comprehensive utilization rate of materials of 96.7 percent.
Example 3
The embodiment comprises the following steps:
Firstly, putting molybdenum powder with the Fisher particle size of 6.5 mu m and the mass purity of 99.96% into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder; the temperature of hydrogen reduction is 800 ℃, the heat preservation time is 120min, and the hydrogen pressure is 0.15MPa;
Step two, adding 90g of a mixture of glycerol and ethanol according to a ratio of 1: the glycerol-ethanol solution prepared by the volume ratio of 1 is used as a binder and is uniformly mixed, then the mixture is put into a molybdenum ring pressing die, and the pressure of 250MPa is used for maintaining the pressure for 45s, so that the height-diameter ratio of 1:1.45 molybdenum ring compact; the outer diameter of the combined female die in the molybdenum ring pressing die is 260mm, and the inner diameter is 165mm;
Placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact; the temperature of the pre-junction is 1350 ℃, and the heat preservation time is 90min; the outer diameter of the molybdenum ring preform is 235mm, the inner diameter is 150mm, and the height is 165mm;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the 6 steps by adopting a 7130 surface grinding machine respectively to obtain visible light; the grinding stroke speed of the grinding visible light is 20m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, the feeding amount is 0.01mm, the single-sided grinding amount is 0.5mm, 0.4mm, 0.5mm, 0.3mm, 0.5mm and 0.3mm respectively, the roughness Ra=0.62 mu m of two end faces of the molybdenum ring preform after the grinding visible light, the quality of the 6 molybdenum ring preforms after the grinding visible light is 29.5kg, 29.6kg, 29.5kg, 29.7kg, 29.5kg and 29.7kg respectively, the parallelism of the two end faces is 0.05mm, and the concentricity is 0.4mm;
Step five, cleaning the surfaces of the 6 molybdenum ring pre-blanks subjected to grinding and visible light until no foreign matters exist, sequentially loading the molybdenum ring pre-blanks into a Q235 steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, performing hot isostatic pressing, taking down the Q235 steel sheath, and performing turning and trimming to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 130MPa, the temperature is 1350 ℃, and the heat preservation time is 180min.
The detection shows that the molybdenum tube blank obtained in the embodiment has the mass of 172kg, the outer diameter of 220mm, the inner diameter of 140mm, the length of 750mm, the density of 10.13g/cm 3, the average grain size of 43 μm and the comprehensive utilization rate of materials of 95.6%.
Example 4
The embodiment comprises the following steps:
Firstly, putting molybdenum powder with the Fisher particle size of 6.0 mu m and the mass purity of 99.97% into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder; the hydrogen reduction temperature is 900 ℃, the heat preservation time is 120min, and the hydrogen pressure is 0.15MPa;
Step two, 125g of a mixture of glycerin and ethanol according to 1: the glycerol-ethanol solution prepared by the volume ratio of 1 is used as a binder and is uniformly mixed, then the mixture is put into a molybdenum ring pressing die, and the pressure of 350MPa is used for maintaining the pressure for 30 seconds, so that the high diameter ratio of 1:1.53 molybdenum ring compact; the outer diameter of the combined female die in the molybdenum ring pressing die is 245mm, and the inner diameter is 165mm;
placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact; the temperature of the pre-junction is 1400 ℃, and the heat preservation time is 60min; the outer diameter of the molybdenum ring preform is 220mm, the inner diameter is 148mm, and the height is 145mm;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the 6 steps by adopting a 7130 surface grinding machine respectively to obtain visible light; the grinding stroke speed of the grinding visible light is 27m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, the feeding amount is 0.01mm, the single-sided grinding amount is 0.5mm, 0.4mm, 0.3mm and 0.4mm respectively, the roughness Ra=0.54 mu m of two end faces of the molybdenum ring preform after the grinding visible light, the quality of the 6 molybdenum ring preforms after the grinding visible light is 24.6kg, 24.7kg, 24.8kg and 24.7kg respectively, the parallelism of the two end faces is 0.1mm, and the concentricity is 0.2mm;
Step five, cleaning the surfaces of the 6 molybdenum ring pre-blanks subjected to grinding and visible light until no foreign matters exist, sequentially loading the molybdenum ring pre-blanks into a Q235 steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, performing hot isostatic pressing, taking down the Q235 steel sheath, and performing turning and trimming to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 130MPa, the temperature is 1200 ℃, and the heat preservation time is 240min.
The detection shows that the molybdenum tube blank obtained in the embodiment has the mass of 143kg, the outer diameter of 208mm, the inner diameter of 140mm, the length of 755mm, the density of 10.12g/cm 3, the average grain size of 40 μm and the comprehensive utilization rate of materials of 95.3 percent.
Example 5
The embodiment comprises the following steps:
Firstly, putting molybdenum powder with the Fisher particle size of 8.0 mu m and the mass purity of 99.95% into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder; the temperature of hydrogen reduction is 900 ℃, the heat preservation time is 90min, and the hydrogen pressure is 0.14MPa;
Step two, adding 100g of a mixture of glycerin and ethanol according to a ratio of 1: the glycerol-ethanol solution prepared by the volume ratio of 1 is used as a binder and is uniformly mixed, then the mixture is put into a molybdenum ring pressing die, and the pressure of 300MPa is used for maintaining the pressure for 30 seconds, so that the high diameter ratio of 1:1.48 molybdenum ring compact; the outer diameter of the combined female die in the molybdenum ring pressing die is 245mm, and the inner diameter is 165mm;
placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact; the temperature of the pre-junction is 1350 ℃, and the heat preservation time is 90min; the outer diameter of the molybdenum ring preform is 220mm, the inner diameter is 150mm, and the height is 145mm;
grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the 6 steps by adopting a 7130 surface grinding machine respectively to obtain visible light; the grinding stroke speed of the grinding visible light is 27m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, the feeding amount is 0.01mm, the single-sided grinding amount is 0.4mm, 0.3mm, 0.5mm, 0.4mm and 0.4mm respectively, the roughness Ra=0.70 mu m of two end faces of the molybdenum ring preform after the grinding visible light, the quality of the 6 molybdenum ring preforms after the grinding visible light is 24.7kg, 24.8kg, 24.6kg, 24.7kg and 24.7kg respectively, the parallelism of the two end faces is 0.08mm, and the concentricity is 0.3mm respectively;
Step five, cleaning the surfaces of the 6 molybdenum ring pre-blanks subjected to grinding and visible light until no foreign matters exist, sequentially loading the molybdenum ring pre-blanks into a Q235 steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, performing hot isostatic pressing, taking down the Q235 steel sheath, and performing turning and trimming to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 130MPa, the temperature is 1350 ℃, and the heat preservation time is 60min.
The test shows that the molybdenum tube blank obtained in the embodiment has the mass of 144kg, the outer diameter of 210mm, the inner diameter of 140mm, the length of 750mm, the density of 10.11g/cm 3, the average grain size of 42 μm and the comprehensive utilization rate of the material of 96%.
Example 6
The embodiment comprises the following steps:
Firstly, putting molybdenum powder with the Fisher particle size of 7.2 mu m and the mass purity of 99.955% into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder; the temperature of hydrogen reduction is 1000 ℃, the heat preservation time is 120min, and the hydrogen pressure is 0.12MPa;
Step two, adding 50g of a mixture of glycerin and ethanol according to a ratio of 1: the glycerol-ethanol solution prepared by the volume ratio of 1 is used as a binder and is uniformly mixed, then the mixture is put into a molybdenum ring pressing die, and the pressure of 250MPa is used for maintaining the pressure for 15s, so that the height-diameter ratio of 1:1.44 molybdenum ring compact; the outer diameter of the combined female die in the molybdenum ring pressing die is 245mm, and the inner diameter is 165mm;
Placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for pre-sintering to obtain a molybdenum ring pre-sintering compact; the temperature of the pre-junction is 1350 ℃, and the heat preservation time is 120min; the outer diameter of the molybdenum ring preform is 220mm, the inner diameter is 148mm, and the height is 155mm;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the third step by adopting a 7130 surface grinding machine to obtain visible light; the grinding travel speed of the grinding visible light is 27m/min, the adopted grinding wheel rotating speed is 1440 r/min, the feeding amount is 0.01mm, the single-sided grinding amount is 0.5mm, 0.4mm, 0.3mm, 0.5mm, 0.3mm and 0.4mm respectively, the roughness Ra=0.50 μm of the two end surfaces of the molybdenum ring pre-sintered blank after grinding the visible light, the mass of the 12 molybdenum ring pre-sintered blanks after grinding the visible light is 24.6kg, 24.7kg, 24.8kg, 24.6kg, 24.8kg and 24.7kg respectively, the parallelism of the two end surfaces is 0.1mm, and the concentricity is 0.2mm;
Step five, cleaning the surfaces of the molybdenum ring pre-sintered blanks subjected to the grinding visible light in the step four until no foreign matters exist, sequentially loading the molybdenum ring pre-sintered blanks into a Q235 steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, performing hot isostatic pressing, taking off the Q235 steel sheath, and performing turning and trimming to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 135MPa, the temperature is 1350 ℃, and the heat preservation time is 120min.
The detection shows that the molybdenum tube blank obtained in the embodiment has the mass of 290kg, the outer diameter of 208mm, the inner diameter of 140mm, the length of 1550mm, the density of 10.13g/cm 3, the average grain size of 47 mu m and the comprehensive utilization rate of materials of 96.7 percent.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (5)
1. A process for producing a molybdenum tube blank by a mould pressing method, which is characterized by comprising the following steps:
Firstly, putting molybdenum powder into a hydrogen reduction furnace for hydrogen reduction to obtain reduced molybdenum powder;
Step two, filling the reduced molybdenum powder obtained in the step one into a molybdenum ring pressing mold, and preparing a molybdenum ring pressed compact by adopting a compression molding method; the height-to-diameter ratio of the molybdenum ring pressed compact is 1:1.53, 1:1.49, 1:1.45, 1:1.53, 1:1.48 or 1:1.44, and the roundness and the dimensional deviation of the molybdenum ring pressed compact are controlled to be not more than 0.5mm;
Placing the molybdenum ring pressed compact obtained in the step two into a hydrogen molybdenum wire push rod furnace for presintering to obtain a molybdenum ring presintering compact; the presintering temperature is 1200-1400 ℃, and the heat preservation time is 60-90 min;
Grinding the two end faces of the molybdenum ring pre-sintered blank obtained in the step three to obtain visible light;
Step five, cleaning the surface of the molybdenum ring pre-sintered blank subjected to grinding visible light in the step four until no foreign matters exist, sequentially filling the molybdenum ring pre-sintered blank into a steel sheath according to an arrangement mode that end surfaces are connected, vacuumizing and sealing, and performing hot isostatic pressing to obtain a molybdenum tube blank; the pressure of the hot isostatic pressing is 100-150 MPa, the temperature is 1200-1350 ℃, and the heat preservation time is 60-240 min; the density of the molybdenum tube blank reaches more than 99% of theoretical density, and the average grain size is not more than 50 mu m.
2. The process for producing a molybdenum pipe blank by a compression molding method according to claim 1, wherein the Fisher size of the molybdenum powder in the first step is 6.0 μm to 8.0 μm, and the mass purity is 99.95% or more.
3. The process for producing a molybdenum tube blank by a die pressing method according to claim 1, wherein the hydrogen gas is reduced at 800-1000 ℃ for 60-180 min and at 0.12-0.15 MPa.
4. The process for producing a molybdenum pipe blank by a compression molding method according to claim 1, wherein the specific process for preparing the molybdenum ring compact by the compression molding method in the second step is as follows: adding glycerol and ethanol solution as a binder into the reduced molybdenum powder, uniformly mixing, then filling into a molybdenum ring pressing die, and maintaining the pressure for 15-45 s by adopting the pressure of 250-350 MPa to obtain a molybdenum ring pressed compact; the glycerol-ethanol solution is prepared from glycerol and ethanol according to a volume ratio of 1:1, and the added mass of the glycerol-ethanol solution is 0.2% -0.5% of the mass of the reduced molybdenum powder.
5. The process for producing a molybdenum pipe blank by a mould pressing method according to claim 1, wherein in the fourth step, the single-sided grinding amount of grinding visible light is 0.2 mm-0.5 mm, the grinding travel speed is 15 m/min-27 m/min, the adopted grinding wheel rotating speed is 1440 revolutions per minute, and the feeding amount is 0.01 mm-0.02 mm; the roughness Ra of two end surfaces of the molybdenum ring preform after grinding the visible light is less than or equal to 0.8 mu m, the parallelism of the two end surfaces is not more than 0.1mm, and the concentricity is not more than 0.4mm.
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