CN103769590A - Large-size high-density tungsten tube and preparing method thereof - Google Patents
Large-size high-density tungsten tube and preparing method thereof Download PDFInfo
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- CN103769590A CN103769590A CN201410010875.XA CN201410010875A CN103769590A CN 103769590 A CN103769590 A CN 103769590A CN 201410010875 A CN201410010875 A CN 201410010875A CN 103769590 A CN103769590 A CN 103769590A
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 108
- 239000010937 tungsten Substances 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 38
- 238000012545 processing Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000013461 design Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 230000007547 defect Effects 0.000 claims description 15
- 238000007493 shaping process Methods 0.000 claims description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 238000005056 compaction Methods 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract 2
- 239000011819 refractory material Substances 0.000 abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000006698 induction Effects 0.000 description 7
- 229910052594 sapphire Inorganic materials 0.000 description 7
- 239000010980 sapphire Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000004484 Briquette Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000007750 plasma spraying Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
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Abstract
The invention discloses a large-size high-density tungsten tube and a preparing method thereof. The method includes the step of mixing raw materials, wherein the raw materials, namely tungsten powder, are uniformly mixed in a mixer; the step of isostatic cool pressing forming, wherein design is carried out according to size requirements of a blank, a forming die is manufactured, then the uniformly mixed raw materials are placed in the forming die, and a tungsten tube blank is obtained through isostatic cool pressing forming processing; the step of high-temperature sintering, wherein the tungsten tube blank is sintered at a high temperature to obtain a sintered blank, and during sintering, a ball-shaped refractory material is placed below the tungsten tube blank. According to the preparing method, the difficult problems of edge breakage, edge failure, cracks, uniform density and the like are solved in the production process of the tungsten tube; compared with the prior art, the produced tungsten tube is large in size, high in density and suitable for large-scale production; a product can bear the high temperature of 2000-2300 DEG C for a long time under protection atmosphere, and the tungsten tube, as the refractory material, plays an important role in multiple industrial fields.
Description
Technical field
The invention belongs to refractory metal special processing technology field, relate to a kind of large scale high density tungsten pipe and preparation method thereof, tungsten pipe product of the present invention is mainly used in the industries such as the long crystalline substance of sapphire, quartz ware production.
Background technology
High density tungsten pipe is the core component of quartz ware continuous induction melting furnace, the long brilliant stove of sapphire, and along with the rapid growth of quartz glass output, the continuous induction melting furnace capacity of producing quartz glass needs further to expand, to improve single stove production capacity; Along with LED promotes to domestic lighting, require more large size sapphire crystal to make chip substrate material, increasing long brilliant stove size is to obtain the more effective ways of large-size crystals.Increasing continuous induction melting furnace capacity all needs production major diameter high density tungsten pipe supporting with it with long brilliant stove size, requires the external diameter of tungsten pipe to be greater than Ф 500mm.Current production technology seldom has can produce that external diameter exceedes Ф 500mm, density is greater than 18.0g/cm
3tungsten pipe, can not meet industrial development demand, therefore the production of large scale high density tungsten pipe becomes a difficult problem to be solved.
At present, the production technology of tungsten pipe has plasma spraying method, spinning method, powder metallurgic method and chemical deposition.The people such as Wu Zijian, Zhang Huyin has made external diameter with plasma spraying Forming Technique and has been greater than Ф 500mm tungsten pipe, but finds aborning, and plasma spraying method is produced tungsten pipe and easily produced longitudinal crack, and relative density only reaches 83%, has affected the mechanical property of goods.With plasma spraying Forming Technique make tungsten pipe be not suitable for quartz glass industry.
The people such as Yin Guoping, Xing Zongyue uses powder metallurgic method base, make sample with spinning method processing Seamless W pipe, measure the hardness of tungsten pipe in process, density, tissue variation and recrystallization temperature, and prepared the high accuracy seamless thin wall tungsten pipe of demarcating stove for Wolfram rhenium heat electric couple.The people such as Ma Jie, Wei Jianzhong is with WF
6, H
2for raw material, adopt chemical vapour deposition technique deposition to prepare small diameter refractory metals tungsten pipe; Publication number is CN102242347A, within open day, is that the patent " a kind of preparation method of the tungsten pipe for heater " on November 16th, 2011 is take red copper as matrix, at substrates chemical vapour deposition (CVD) W element, then dissolves matrix, finally obtains tungsten pipe.The tungsten pipe size less (diameter is less than Ф 50mm) that present stage prepares with spinning method and chemical vapour deposition technique, is not suitable for the long brilliant industry of quartz glass industry and sapphire.
Summary of the invention
For the defect of prior art; the object of the present invention is to provide a kind of large scale high density tungsten pipe and preparation method thereof; this technique is suitable for large-scale production; its tungsten pipe finished product has that relative density is high, size large (maximum outside diameter Ф 760mm, length 1800mm), size adaptability and high conformity, yield rate advantages of higher; and under protective atmosphere, can bear the high temperature of 2000-2300 ℃, have advantages of under high temperature not and quartz raw material, sapphire raw material reaction.
To achieve these goals, the present invention has adopted following technical scheme:
A preparation method for large scale high density tungsten pipe, comprises the steps:
Raw material blending step is evenly mixed raw material tungsten powder in batch mixer;
Cold isostatic compaction step, according to pressed compact, charging requires size design and makes shaping dies, then even mixed raw material is packed in described mould and carries out cold isostatic compaction processing to obtain tungsten pipe pressed compact;
High temperature sintering step, carries out high temperature sintering to obtain sintering blank by described tungsten pipe pressed compact, wherein, when sintering described in tungsten pipe pressed compact below be placed with spherical fireproof material.
In above-mentioned preparation method, when high temperature sintering, tungsten pipe pressed compact is positioned over to the deflation resistance that can reduce tungsten pipe pressed compact lower end on one deck spherical fireproof material, promote the upper and lower synchronous of tungsten pipe pressed compact, concrete principle is as follows: in sintering process, tungsten pipe pressed compact lower end because and loading platform between there is rubbing action, tungsten pipe lower end shrink compared with tungsten pipe upper end shrink little; After the upper spherical fireproof material of tungsten pipe below pad, the suffered friction in tungsten pipe lower end becomes rolling friction from sliding friction, and coefficient of friction diminishes relatively, and friction resistance reduces, thereby reduces tungsten pipe pressed compact lower end deflation resistance, guarantees tungsten pipe density uniformity.As a kind of preferred embodiment, the material of described spherical fireproof material can be zirconia.
In above-mentioned preparation method, as a kind of preferred embodiment, in described high temperature sintering step, described spherical fireproof material is that one deck particle mean size is the spherical fireproof material of Φ 1-3mm.
In above-mentioned preparation method, as a kind of preferred embodiment, in described high temperature sintering step, the maximum temperature of described high temperature sintering is 2300-2380 ℃, and maximum temperature temperature retention time is 4-8 hour, and heating rate is 30-70 ℃/h.Exemplarily, described heating rate is 35 ℃/h, 40 ℃/h, 55 ℃/h, 60 ℃/h, 65 ℃/h or 68 ℃/h; Described maximum temperature is 2310 ℃, 2325 ℃, 2335 ℃, 2345 ℃, 2360 ℃ or 2375 ℃, and maximum temperature temperature retention time is 4.5 hours, 5 hours, 6 hours, 7 hours or 8 hours.More preferably, described high temperature sintering carries out under hydrogen or vacuum atmosphere.In the method, high temperature sintering adopts lower heating rate can further promote tungsten pipe to shrink up and down unanimously, guarantees that tungsten pipe sintered density improves.
In above-mentioned preparation method, as a kind of preferred embodiment, in described raw material blending step, described raw material tungsten powder is that the tungsten powder of 1.8～2.2 microns and average Fisher particle size are that the tungsten powder of 3.8～4.2 microns forms by average Fisher particle size, and wherein average Fisher particle size is the 40%-45% that the tungsten powder consumption of 1.8～2.2 microns accounts for described raw material tungsten powder gross mass.More preferably, described raw material tungsten powder is the Fw-1 type tungsten powder that meets GB.Use the tungsten powder of above-mentioned two kinds of specifications carry out raw material proportioning and mix and can improve raw material uniformity and compact strength.
In above-mentioned preparation method, as a kind of preferred embodiment, in described raw material blending step, the time of described mixing is 5-6 hour, and more preferably, described mixing is to mix in V-type batch mixer.
In above-mentioned preparation method, as a kind of preferred embodiment, in described cold isostatic compaction step, shaping pressure is 280-300Mpa, and the dwell time is 0.5-2 hour, then pressure release.More preferably, described pressure release total time was controlled in 45-60 minute.Adopt above cold isostatic compaction technique, the pressed compact obtaining approaches and requires size, without collapsing limit, misrun, defects i.e.cracks.
In above-mentioned preparation method, as a kind of preferred embodiment, in described cold isostatic compaction step, described shaping dies comprises: cylindrical steel core rod, be set in the heavy wall gum cover of described cylindrical steel core rod outside and both ends open and be covered on the plug at described heavy wall gum cover two ends, described even mixed raw material is loaded in the space between described cylindrical steel core rod and described heavy wall gum cover.Adopt pressed compact prepared by this mould to approach and require size, pressed compact shaping amount is little.
In above-mentioned preparation method, as a kind of preferred embodiment, described preparation method also comprises:
Sintering blank detecting step, detects sintering blank presentation quality and measures global density;
Accessory processing step, carries out accessory processing according to drawing requirement to detecting qualified sintering blank, in the time of described accessory processing, adopts the mode that is installed of multiple spot chuck, can alleviate single-point so stressed, reduces tungsten pipe crack risk.Preferably, described multiple spot chuck refers to or 24 chucks at 16;
Crack-detecting step, adopts the method for penetrant inspection to detect the tungsten pipe crack defect after accessory processing.
A large scale high density tungsten pipe that adopts said method to prepare, preferably, the global density of described tungsten pipe is 18.0-18.6g/cm
3(drainage mensuration), size range is: external diameter Ф 500-760mm, height 1200-1800mm.
The present invention compared with prior art has following beneficial effect:
1) adopt above-mentioned explained hereafter large scale high density tungsten pipe, realized serialization, the mass produced, be suitable for large-scale production.
2) in the time that the diameter of pure tungsten goods exceedes Φ 500mm, pressed compact is prone to and collapses limit, defects i.e.cracks, and this difficult problem is the bottleneck that large scale pure tungsten is produced.The present invention adopts raw material blending technique to improve compact strength, adopts high-pressure forming technique (cold isostatic compaction technology) to guarantee pressed compact quality, and pressed compact is without collapsing the defects such as limit, crackle, misrun.
3) large scale pure tungsten is difficult to reach densified sintering product, shrinks inconsistent requirement up and down, and this problem is also a great problem that tungsten pipe is produced.The present invention adds by reduction heating rate and pressed compact bottom the technique that exotic material is spherical fireproof material, has promoted tungsten pipe to shrink up and down unanimously, improves tungsten pipe sintered density.
4) technique that the present invention adopts multiple spot chuck to be installed in the time of accessory processing, reduces the risk that crackle occurs.
5) can the production size large high tungsten pipe product of (maximum outside diameter Ф 760mm, maximum height 1800mm) relative density of technique of the present invention; this process yield is high; and the tungsten pipe of producing can bear the high temperature of 2000-2300 ℃ under protective atmosphere, have advantages of under high temperature not and quartz raw material, sapphire raw material reaction.
6) sintering briquette of tungsten pipe, through machining, can obtain the finished size of demand, size accuracy and high conformity.
Accompanying drawing explanation
Fig. 1 is the tungsten tube section schematic diagram that the present invention produces.
The specific embodiment
The present invention uses above-mentioned technique successfully to produce the highly dense tungsten pipe of major diameter, and its global density is greater than 18.0g/cm
3, external diameter Ф 500-Ф 760mm, height 800-1800mm, wherein have Ф 500*1800 type tungsten pipe, Ф 760mm*1200 type tungsten pipe etc.These tungsten pipes can be used to quartz glass continuous induction melting furnace and the long brilliant stove of sapphire, thereby promote the device upgrade of these two industries.In order to make the features and advantages of the present invention clearer, the present invention has adopted following examples to be elaborated.
Embodiment 1
Tungsten tube section schematic diagram prepared by the present embodiment is referring to Fig. 1, wherein OD1=500mm, and OD2=460mm, OD3=440mm, ID=400mm, H=1800mm, h1=90mm, h2=100mm, referred to as Ф 500*1800mm type tungsten pipe.
Concrete preparation method is as follows:
1) selecting the average Fisher particle size of Fw-1 type that meets GB is that the tungsten powder of 1.8 microns and average Fisher particle size are that the tungsten powder of 4 microns is as tungsten pipe raw material; wherein; the mass ratio of the tungsten powder of the tungsten powder of 1.8 microns and 4 microns is 4:6; purity is 99.9%, above-mentioned tungsten pipe raw material is placed in to V-type batch mixer and under high-purity argon gas protection, mixes 5 hours.
2) according to pressed compact, charging requires set of dimensions to dress up mould, mixed raw material is loaded in the space between cylindrical steel core rod and heavy wall gum cover, after charging with sealing again behind plug jam-pack heavy wall gum cover two ends, then charged shaping grinding apparatus is hung in cold isostatic press cylinder body and suppressed, by cold isostatic press equipment regulation suppress, pressurize and pressure release operate to obtain tungsten pipe pressed compact, wherein, shaping pressure is 280Mpa, pressurize 1 hour, the pressure release time is 45 minutes.
3) under hydrogen atmosphere, to be placed in high temperature induction sintering furnace sintering through tungsten pipe pressed compact, heating rate is 70 ℃/h, and maximum temperature is 2300 ℃, high-temperature holding time is 4 hours, and when sintering, placement particle mean size in tungsten pipe pressed compact below is the zirconia exotic material of Φ 2mm.
4) sintering briquette presentation quality is detected, the equal zero defect of 30 cover sintering blank after testing, the global density that then adopts drainage to measure 30 cover tungsten pipe sintering briquettes is 18.05-18.20g/cm
3; Choosing density is 18.2g/cm
3a tungsten pipe, tungsten pipe diverse location is sampled to (short transverse is a sampling height every 100mm, co-altitude interval 45
°get 20*20*5mm sample, obtain altogether 144 samples), survey the density of every sample, find that sample density scope is 18.15-18.25g/cm
3, upper strata density and lower floor's density difference are little.
5) adopt the mode of being installed of 16 chucks to carry out accessory processing according to drawing requirement, after Vehicle Processing, carry out again surperficial rubbing down.16 chucks of the present embodiment are compared with three-jaw or chuck, and each active force being installed a little reduces, thereby reduce the generation possibility risk of tungsten pipe crack.
30 crack defects that overlap Ф 500*1800mm type tungsten pipes that adopt the method for penetrant inspection to produce the present embodiment are tested, and through checking the equal flawless defect of 30 cover tungsten pipe, yield rate is 100%.
Embodiment 2
Tungsten tube section schematic diagram prepared by the present embodiment is referring to Fig. 1, wherein OD1=760mm, and OD2=740mm, OD3=700mm, ID=640mm, H=1200mm, h1=90mm, h2=100mm, referred to as Ф 760*1200mm type tungsten pipe.
Concrete preparation method is as follows:
1) selecting the average Fisher particle size of Fw-1 type that meets GB is that the tungsten powder of 2 microns and average Fisher particle size are that the tungsten powder of 4 microns is as tungsten pipe raw material; wherein; the mass ratio of the tungsten powder of the tungsten powder of 2 microns and 4 microns is 45:55; purity is 99.9%, above-mentioned tungsten pipe raw material is placed in to V-type batch mixer and under high-purity argon gas protection, mixes 6 hours.
2) according to pressed compact, charging requires set of dimensions to dress up mould, mixed raw material is loaded in the space between cylindrical steel core rod and heavy wall gum cover, after charging with sealing again behind plug jam-pack heavy wall gum cover two ends, then charged shaping grinding apparatus is hung in cold isostatic press cylinder body and suppressed, by cold isostatic press equipment regulation suppress, pressurize and pressure release operate to obtain tungsten pipe pressed compact, wherein, shaping pressure is 290Mpa, pressurize 1 hour, the pressure release time is 50 minutes.
3) under hydrogen atmosphere, tungsten pipe pressed compact is placed in to high temperature induction sintering furnace sintering, and heating rate is 30 ℃/h, and maximum temperature is 2380 ℃, high-temperature holding time is 8 hours, and when sintering, placement particle mean size in tungsten pipe pressed compact below is the zirconia exotic material of Φ 1mm.
4) sintering briquette presentation quality is detected, the equal zero defect of 6 cover sintering blank after testing, the global density that then adopts drainage to measure 6 cover tungsten pipe sintering briquettes is 18.02-18.15g/cm
3.Choosing density is 18.10g/cm
3a tungsten pipe, tungsten pipe diverse location is sampled to (short transverse is a sampling height every 100mm, and co-altitude is every 45
°get 20*20*5mm sample), survey the density of every sample, find that sample density scope is 18.08-18.13g/cm
3, upper strata density and lower floor's density difference are little.
5) adopt the mode of being installed of 24 chucks to carry out accessory processing according to drawing requirement, after Vehicle Processing, carry out again surperficial rubbing down.
6 crack defects that overlap Ф 760*1200mm type tungsten pipes that adopt the method for penetrant inspection to produce the present embodiment are tested, and through checking the equal flawless defect of 6 cover tungsten pipe, yield rate is 100%.
Embodiment 3
Tungsten tube section schematic diagram prepared by the present embodiment is referring to Fig. 1, wherein OD1=600mm, and OD2=560mm, OD3=540mm, ID=500mm, H=1200mm, h1=90mm, h2=100mm, referred to as Ф 600*1200mm type tungsten pipe.
Concrete preparation method is as follows:
1) selecting the average Fisher particle size of Fw-1 type that meets GB is that the tungsten powder of 2.2 microns and average Fisher particle size are that the tungsten powder of 3.8 microns is as tungsten pipe raw material; wherein; the mass ratio of the tungsten powder of the tungsten powder of 2.2 microns and 3.8 microns is 45:55; purity is 99.9%, above-mentioned tungsten pipe raw material is placed in to V-type batch mixer and under high-purity argon gas protection, mixes 6 hours.
2) according to pressed compact, charging requires set of dimensions to dress up mould, mixed raw material is loaded in the space between cylindrical steel core rod and heavy wall gum cover, after charging with sealing again behind plug jam-pack heavy wall gum cover two ends, then charged shaping grinding apparatus is hung in cold isostatic press cylinder body and suppressed, by cold isostatic press equipment regulation suppress, pressurize and pressure release operate to obtain tungsten pipe pressed compact, wherein, shaping pressure is 300Mpa, pressurize 1 hour, the pressure release time is 60 minutes.
3) under hydrogen atmosphere, tungsten pipe pressed compact is placed in to high temperature induction sintering furnace sintering, and heating rate is 50 ℃/h, and maximum temperature is 2350 ℃, high-temperature holding time is 6 hours, and when sintering, placement particle mean size in tungsten pipe pressed compact below is the zirconia exotic material of Φ 3mm.
4) sintering briquette presentation quality is detected, the equal zero defect of 15 cover sintering blank after testing, the global density that then adopts drainage to measure 15 cover tungsten pipe sintering briquettes is 18.10-18.25g/cm
3, choosing density is 18.15g/cm
3a tungsten pipe, tungsten pipe diverse location is sampled to (short transverse is a sampling height every 100mm, and co-altitude is every 45
°get 20*20*5mm sample), survey the density of every sample, find that sample density scope is 18.13-18.20g/cm
3, upper strata density and lower floor's density difference are little.
5) adopt the mode of being installed of 24 chucks to carry out accessory processing according to drawing requirement, after Vehicle Processing, carry out again surperficial rubbing down.
15 crack defects that overlap Ф 600*1200mm type tungsten pipes that adopt the method for penetrant inspection to produce the present embodiment are tested, and through checking the equal flawless defect of 15 cover tungsten pipe, yield rate is 100%.
The purposes that should be appreciated that these embodiment only limits the scope of the invention for the present invention being described but not being intended to.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various changes, modification and/or modification to the present invention, within these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (10)
1. a preparation method for large scale high density tungsten pipe, is characterized in that, comprises the steps:
Raw material blending step is evenly mixed raw material tungsten powder in batch mixer;
Cold isostatic compaction step, according to pressed compact, charging requires size design and makes shaping dies, then even mixed raw material is packed in described mould and carries out cold isostatic compaction processing to obtain tungsten pipe pressed compact;
High temperature sintering step, carries out high temperature sintering to obtain sintering blank by described tungsten pipe pressed compact, wherein, when sintering described in tungsten pipe pressed compact below be placed with spherical fireproof material.
2. preparation method according to claim 1, is characterized in that, in described high temperature sintering step, described spherical fireproof material is that one deck particle mean size is the spherical fireproof material of Φ 1-3mm; Preferably, the material of described spherical fireproof material is zirconia.
3. preparation method according to claim 1, is characterized in that, in described high temperature sintering step, the maximum temperature of described high temperature sintering is 2300-2380 ℃, and maximum temperature temperature retention time is 4-8 hour, and heating rate is 30-70 ℃/h; Preferably, described high temperature sintering carries out under hydrogen or vacuum atmosphere.
4. preparation method according to claim 1, it is characterized in that, in described raw material blending step, described raw material tungsten powder is that the tungsten powder of 1.8～2.2 microns and average Fisher particle size are that the tungsten powder of 3.8～4.2 microns forms by average Fisher particle size, and wherein average Fisher particle size is the 40%-45% that the tungsten powder consumption of 1.8～2.2 microns accounts for described raw material tungsten powder gross mass; Preferably, described raw material tungsten powder is the Fw-1 type tungsten powder that meets GB.
5. preparation method according to claim 1, is characterized in that, in described raw material blending step, the time of described mixing is 5-6 hour, and preferably, described mixing is to mix in V-type batch mixer.
6. preparation method according to claim 1, is characterized in that, in described cold isostatic compaction step, shaping pressure is 280-300Mpa, and the dwell time is 0.5-2 hour, then pressure release; Preferably, described pressure release total time was controlled in 45-60 minute.
7. preparation method according to claim 1, it is characterized in that, in described cold isostatic compaction step, described shaping dies comprises: cylindrical steel core rod, be set in the heavy wall gum cover of described cylindrical steel core rod outside and both ends open and be covered on the plug at described heavy wall gum cover two ends, described even mixed raw material is loaded in the space between described cylindrical steel core rod and described heavy wall gum cover.
8. preparation method according to claim 1, is characterized in that, described preparation method also comprises:
Sintering blank detecting step, detects sintering blank presentation quality and measures global density;
Accessory processing step, carries out accessory processing according to drawing requirement to detecting qualified sintering blank, in the time of described accessory processing, adopts the mode that is installed of multiple spot chuck; Preferably, described multiple spot chuck is 16 or 24 chucks;
Crack-detecting step, adopts the method for penetrant inspection to detect the tungsten pipe crack defect after accessory processing.
9. a large scale high density tungsten pipe that adopts the arbitrary described method of claim 1-8 to prepare.
10. tungsten pipe according to claim 9, is characterized in that, the global density of described tungsten pipe is 18.0-18.6g/cm
3, be of a size of: external diameter Ф 500-760mm, height 1200-1800mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107009093A (en) * | 2017-01-12 | 2017-08-04 | 厦门虹鹭钨钼工业有限公司 | A kind of preparation method of rear-earth-doped tungsten pipe |
| CN114951661A (en) * | 2022-06-10 | 2022-08-30 | 西安华力装备科技有限公司 | Preparation method of tungsten alloy large product with through holes or blind holes |
| CN115109977A (en) * | 2021-03-23 | 2022-09-27 | 安泰科技股份有限公司 | Ultra-large-specification high-performance tungsten alloy pipe and preparation method thereof |
| CN115415526A (en) * | 2021-05-13 | 2022-12-02 | 安泰天龙钨钼科技有限公司 | Oversized tungsten tube and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107009093A (en) * | 2017-01-12 | 2017-08-04 | 厦门虹鹭钨钼工业有限公司 | A kind of preparation method of rear-earth-doped tungsten pipe |
| CN107009093B (en) * | 2017-01-12 | 2019-01-29 | 厦门虹鹭钨钼工业有限公司 | A kind of production method of rear-earth-doped tungsten pipe |
| CN115109977A (en) * | 2021-03-23 | 2022-09-27 | 安泰科技股份有限公司 | Ultra-large-specification high-performance tungsten alloy pipe and preparation method thereof |
| CN115415526A (en) * | 2021-05-13 | 2022-12-02 | 安泰天龙钨钼科技有限公司 | Oversized tungsten tube and preparation method thereof |
| CN114951661A (en) * | 2022-06-10 | 2022-08-30 | 西安华力装备科技有限公司 | Preparation method of tungsten alloy large product with through holes or blind holes |
| CN114951661B (en) * | 2022-06-10 | 2024-01-30 | 西安华力装备科技有限公司 | Preparation method of large tungsten alloy product with through holes or blind holes |
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