CN103769590B - Large-size high-density tungsten pipe and preparation method thereof - Google Patents
Large-size high-density tungsten pipe and preparation method thereof Download PDFInfo
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- CN103769590B CN103769590B CN201410010875.XA CN201410010875A CN103769590B CN 103769590 B CN103769590 B CN 103769590B CN 201410010875 A CN201410010875 A CN 201410010875A CN 103769590 B CN103769590 B CN 103769590B
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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 110
- 239000010937 tungsten Substances 0.000 title claims abstract description 110
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000012545 processing Methods 0.000 claims abstract description 20
- 238000007493 shaping process Methods 0.000 claims abstract description 12
- 238000005056 compaction Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims description 16
- 230000007547 defect Effects 0.000 claims description 14
- 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
- 238000002156 mixing Methods 0.000 claims description 7
- 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
- 238000001514 detection method Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 208000037656 Respiratory Sounds Diseases 0.000 abstract description 6
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 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 5
- 230000006698 induction Effects 0.000 description 5
- 239000004484 Briquette Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000010586 diagram Methods 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
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000013022 venting Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009471 action 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
- 238000011161 development Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 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
- 235000009566 rice Nutrition 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Abstract
The invention discloses a kind of large-size high-density tungsten pipe and preparation method thereof.This method includes raw material admixing step, and raw material tungsten powder is uniformly mixed in batch mixer；Cold isostatic compaction step, designed according to pressed compact charging desired size and make shaping dies, then uniformly mixed raw material is loaded in the mould and carries out cold isostatic compaction processing to obtain tungsten pipe pressed compact；High temperature sintering step, the tungsten pipe pressed compact is subjected to high temperature sintering to obtain sintering blank, wherein, spherical fireproof material is placed with below the tungsten pipe pressed compact during sintering.The inventive method solves the problem such as chipping, arrisdefect, crackle, Density inhomogeneity in tungsten pipe production process, and the tungsten pipe size produced compared with prior art is big, density is high, suitable for large-scale production；And product can bear 2,000 2300 DEG C of high temperature for a long time under protective atmosphere, there is important use in many industrial circles as exotic material.
Description
Technical field
The invention belongs to refractory metal technical field, is related to a kind of large-size high-density tungsten pipe and its preparation side
Method, tungsten pipe product of the present invention are mainly used in the industries such as sapphire crystallization, quartz ware production.
Background technology
High density tungsten pipe is quartz ware continuous induction melting furnace, the core component of sapphire crystallization furnace, with quartz glass yield
Rapid growth, producing the continuous smelting heat size of quartz glass needs further to expand, to improve single stove production capacity；As LED is to civilian
Illumination is promoted, it is desirable to which more large size sapphire crystal makes chip substrate material, and increase long crystal furnace size is to obtain more large scale
The effective ways of crystal.Increase continuous smelting heat size and long crystal furnace size are required for production major diameter high density tungsten pipe matched,
It is required that the external diameter of tungsten pipe is more than Ф 500mm.The few external diameters that can produce of current production technology are more than more than Ф 500mm, density
18.0g/cm3Tungsten pipe, it is impossible to meet industrial development demand, therefore the production of large-size high-density tungsten pipe turns into difficulty to be solved
Topic.
At present, the production technology of tungsten pipe has plasma spraying method, spinning process, powder metallurgic method and chemical deposition.Wu Zi
Strong, Zhang Huyin et al. has made external diameter with plasma spraying Forming Technique and has been more than Ф 500mm tungsten pipes, but sends out in production
Existing, plasma spraying method production tungsten tube capacity is also easy to produce longitudinal crack, and relative density have impact on the mechanical property of product only up to 83%.
The tungsten pipe made of plasma spraying Forming Technique is not suitable for quartz glass industry.
Yin Guoping, Xing Zongyue et al. powder metallurgic method base, sample is made with spinning process processing Seamless W pipe, determines and adds
The hardness of tungsten pipe, density, tissue change and recrystallization temperature during work, and it is prepared for the height for Wolfram rhenium heat electric couple demarcation stove
Precision seamless thin wall tungsten pipe.Ma Jie, Wei Jianzhong et al. are with WF6、H2For raw material, using chemical vapor deposition prepare compared with
Minor diameter refractory metals tungsten pipe；Publication No. CN102242347A, publication date are the patent on November 16th, 2011《One kind is used for
The preparation method of the tungsten pipe of heater》It is using red copper as matrix, in substrates chemical vapor deposition W elements, then dissolves base
Body, finally give tungsten pipe.The tungsten pipe size prepared at this stage with spinning process and chemical vapour deposition technique is smaller（Diameter is less than Ф
50mm）, be not suitable for quartz glass industry and sapphire crystallization industry.
The content of the invention
The defects of for prior art, it is an object of the invention to provide a kind of large-size high-density tungsten pipe and its preparation side
Method, the technique are suitable to large-scale production, and its tungsten pipe finished product has relative density height, size big（Maximum outside diameter Ф 760mm, length
Spend 1800mm), size adaptability and the advantages that uniformity is good, high yield rate, and 2000-2300 can be born under protective atmosphere
DEG C high temperature, have high temperature under not with quartz raw material, sapphire raw material react the advantages of.
To achieve these goals, present invention employs following technical scheme：
A kind of preparation method of large-size high-density tungsten pipe, comprises the following steps：
Raw material admixing step, raw material tungsten powder is uniformly mixed in batch mixer；
Cold isostatic compaction step, designed according to pressed compact charging desired size and make shaping dies, then will uniformly mixed
Raw material after conjunction loads in the mould and carries out cold isostatic compaction processing to obtain tungsten pipe pressed compact；
High temperature sintering step, the tungsten pipe pressed compact is subjected to high temperature sintering to obtain sintering blank, wherein, described in during sintering
Spherical fireproof material is placed with below tungsten pipe pressed compact.
Tungsten pipe pressed compact is positioned on one layer of spherical fireproof material and can be reduced in above-mentioned preparation method, during high temperature sintering
The deflation resistance of tungsten pipe pressed compact lower end, promoting tungsten pipe pressed compact, synchronous, concrete principle are as follows up and down：In sintering process, tungsten
Because rubbing action between loading platform be present, tungsten pipe lower end is shunk small compared with the contraction of tungsten pipe upper end for pipe pressed compact lower end；Below tungsten pipe
On pad after spherical fireproof material, the suffered friction in tungsten pipe lower end is changed into rolling friction from sliding friction, and coefficient of friction is relative to diminish, institute
Reduced by friction resistance force, so as to reduce tungsten pipe pressed compact lower end deflation resistance, ensure tungsten pipe density uniformity.As a kind of preferred
Embodiment, the material of the spherical fireproof material can be zirconium oxide.
It is described spherical resistance in the high temperature sintering step as a kind of preferred embodiment in above-mentioned preparation method
Fiery material is the spherical fireproof material that one layer of particle mean size is Φ 1-3mm.
In above-mentioned preparation method, as a kind of preferred embodiment, in the high temperature sintering step, the high temperature burns
The maximum temperature of knot is 2300-2380 DEG C, and maximum temperature soaking time is 4-8 hours, and heating rate is 30-70 DEG C/h.Example
Property, the heating rate is 35 DEG C/h, 40 DEG C/h, 55 DEG C/h, 60 DEG C/h, 65 DEG C/h or 68 DEG C/h；The maximum temperature is
2310 DEG C, 2325 DEG C, 2335 DEG C, 2345 DEG C, 2360 DEG C or 2375 DEG C, maximum temperature soaking time be 4.5 hours, 5 hours, 6
Hour, 7 hours or 8 hours.It is highly preferred that the high temperature sintering is carried out under hydrogen or vacuum atmosphere.It is high in this method
Temperature sintering can further promote contraction above and below tungsten pipe consistent using relatively low heating rate, ensure that tungsten pipe sintered density improves.
In above-mentioned preparation method, as a kind of preferred embodiment, in the raw material admixing step, the raw material tungsten
Powder is made up of the tungsten powder that average Fisher particle size is 1.8~2.2 microns and the tungsten powder that average Fisher particle size is 3.8~4.2 microns, its
In average Fisher particle size be that 1.8~2.2 microns of tungsten powder dosage accounts for the 40%-45% of the raw material tungsten powder gross mass.It is highly preferred that
The raw material tungsten powder is the Fw-1 type tungsten powders for meeting national standard.Raw material proportioning is carried out using the tungsten powder of above two specification and mixing can
To improve raw material uniformity and compact strength.
In above-mentioned preparation method, as a kind of preferred embodiment, in the raw material admixing step, the mixing
Time is 5-6 hours, it is highly preferred that the mixing is mixed in V-type batch mixer.
In above-mentioned preparation method, as a kind of preferred embodiment, in the cold isostatic compaction step, shaping pressure
Strong is 280-300Mpa, and the dwell time is 0.5-2 hours, then pressure release.It is highly preferred that the pressure release total time control is in 45-
In 60 minutes.Using above cold isostatic compaction technique, obtained pressed compact lacks close to desired size, no chipping, misrun, crackle etc.
Fall into.
In above-mentioned preparation method, as a kind of preferred embodiment, in the cold isostatic compaction step, it is described into
Shape mould includes：Cylindrical steel core rod, it is set in outside the cylindrical steel core rod and the heavy wall gum cover of both ends open and is covered on
The plug at the heavy wall gum cover both ends, the uniformly mixed raw material loaded on the cylindrical steel core rod and the heavy wall gum cover it
Between space in.The pressed compact prepared using the mould is small close to desired size, pressed compact shaping amount.
In above-mentioned preparation method, as a kind of preferred embodiment, the preparation method also includes：
Blank detecting step is sintered, detection sintering blank presentation quality simultaneously determines global density；
Accessory processing step, accessory processing is carried out to detecting qualified sintering blank according to drawing requirement, described supporting
During processing, it using the mode that is loaded of multiple spot chuck, can so mitigate single-point stress, reduce tungsten pipe crack risk.Preferably, institute
State multiple spot chuck and refer to or 24 chucks at 16 points；
Crack-detecting step, using the tungsten pipe crack defect after the method detection accessory processing of penetrant inspection.
A kind of large-size high-density tungsten pipe prepared using the above method, it is preferable that the global density of the tungsten pipe is
18.0-18.6g/cm3（Drainage determines）, size range is：External diameter Ф 500-760mm, height 1200-1800mm.
The present invention has the advantages that compared with prior art：
1）Using above-mentioned technique productions large-size high-density tungsten pipe, serialization, the mass of production are realized, suitable for scale
Metaplasia is produced.
2）When the diameter of pure tungsten product is more than Φ 500mm, easily there is the defects of chipping, crackle in pressed compact, and this problem is
The bottleneck of large scale pure tungsten production.The present invention improves compact strength using raw material blending technique, using high-pressure forming technique（It is cold etc.
Hydrostatic profile technology）Pressed compact quality is ensure that, the defects of pressed compact is without chipping, crackle, misrun.
3）Large scale pure tungsten is extremely difficult to densified sintering product, shrinks inconsistent requirement up and down, and this problem is also tungsten Guan Sheng
The a great problem of production.The present invention adds the exotic material i.e. work of spherical fireproof material by reducing heating rate and pressed compact bottom
Skill, promote tungsten pipe and shrink consistent, raising tungsten pipe sintered density up and down.
4）The technique that the present invention is loaded in accessory processing using multiple spot chuck, reduce the risk that crackle occurs.
5）It is big that the technique of the present invention can produce size（Maximum outside diameter Ф 760mm, maximum height 1800mm) relative density height
Tungsten pipe product, the process yield is high, and the tungsten pipe produced can bear 2000-2300 DEG C of high temperature under protective atmosphere,
The advantages of with not reacted under high temperature with quartz raw material, sapphire raw material.
6）The sintering briquette of tungsten pipe can obtain the finished size of demand, dimensioning accuracy and uniformity are good through over mechanical processing.
Brief description of the drawings
Fig. 1 is tungsten tube section schematic diagram produced by the invention.
Embodiment
The present invention successfully produces the highly dense tungsten pipe of major diameter with above-mentioned technique, and its global density is more than 18.0g/cm3, it is outer
Footpath Ф 500- Ф 760mm, height 800-1800mm, wherein having Ф 500*1800 type tungsten pipe, Ф 760mm*1200 type tungsten pipes etc..This
A little tungsten pipes can be used for quartz glass continuous induction melting furnace and sapphire crystallization furnace, so as to promote the device upgrade of the two industries.
In order that the features and advantages of the present invention are clearer, present invention employs following examples to be described in detail.
Embodiment 1
Tungsten tube section schematic diagram manufactured in the present embodiment referring to Fig. 1, wherein OD1=500mm, OD2=460mm, OD3=
440mm, ID=400mm, H=1800mm, h1=90mm, referred to as h2=100mm, Ф 500*1800mm types tungsten pipe.
Specific preparation method is as follows：
1）The tungsten powder and average Fisher particle size for being 1.8 microns from the average Fisher particle size of Fw-1 types for meeting national standard are 4 micro-
The tungsten powder of rice as tungsten pipe raw material, wherein, the mass ratio of 1.8 microns of tungsten powder and 4 microns of tungsten powder is 4：6, purity is
99.9%, above-mentioned tungsten pipe raw material is placed in V-type batch mixer under high-purity argon gas protection and mixed 5 hours.
2）According to pressed compact charging desired size assembled formation mould, mixed raw material is loaded on cylindrical steel core rod and heavy wall
In space between gum cover, sealed again after stoppering heavy wall gum cover both ends with plug after charging, then charged shaping
Grinding tool hangs in cold isostatic press cylinder body and suppressed, and is suppressed by cold isostatic press equipment regulation, pressurize and pressure release
Operate to obtain tungsten pipe pressed compact, wherein, shaping pressure is 280Mpa, and pressurize 1 hour, venting duration is 45 minutes.
3）In a hydrogen atmosphere, will be placed in high temperature induction sintering furnace and sinter by tungsten pipe pressed compact, heating rate be 70 DEG C/
H, maximum temperature are 2300 DEG C, and high-temperature holding time is 4 hours, and it is Φ 2mm to place particle mean size below tungsten pipe pressed compact during sintering
Zirconium oxide exotic material.
4）Sintering briquette presentation quality is detected, 30 sets of sintering equal zero defects of blank, are then surveyed using drainage after testing
The global density of fixed 30 sets of tungsten pipe sintering briquettes is 18.05-18.20g/cm3；Selection density is 18.2g/cm3A tungsten pipe, to tungsten
Pipe diverse location is sampled（Short transverse is a sampling height every 100mm, with vertical separation 45°20*20*5mm is taken to try
Sample, 144 samples are obtained altogether）, the density of every sample is surveyed, it is found that sample density scope is 18.15-18.25g/cm3, upper strata
Density and lower layer density difference are small.
5）Accessory processing is carried out using the mode of being loaded of 16 chucks according to drawing requirement, carries out surface throwing after Vehicle Processing again
Mill.16 chucks of the present embodiment are compared with three-jaw or chuck, and the active force being each loaded a little reduces, so as to reduce tungsten pipe
The generation of crackle may risk.
The crack defect of the 30 sets of Ф 500*1800mm type tungsten pipes produced using the method for penetrant inspection to the present embodiment is entered
Performing check, through examining the equal flawless defect of 30 sets of tungsten pipes, yield rate 100%.
Embodiment 2
Tungsten tube section schematic diagram manufactured in the present embodiment referring to Fig. 1, wherein OD1=760mm, OD2=740mm, OD3=
700mm, ID=640mm, H=1200mm, h1=90mm, referred to as h2=100mm, Ф 760*1200mm types tungsten pipe.
Specific preparation method is as follows：
1）The tungsten powder and average Fisher particle size for being 2 microns from the average Fisher particle size of Fw-1 types for meeting national standard are 4 microns
Tungsten powder as tungsten pipe raw material, wherein, the mass ratio of 2 microns of tungsten powder and 4 microns of tungsten powder is 45：55, purity is
99.9%, above-mentioned tungsten pipe raw material is placed in V-type batch mixer under high-purity argon gas protection and mixed 6 hours.
2）According to pressed compact charging desired size assembled formation mould, mixed raw material is loaded on cylindrical steel core rod and heavy wall
In space between gum cover, sealed again after stoppering heavy wall gum cover both ends with plug after charging, then charged shaping
Grinding tool hangs in cold isostatic press cylinder body and suppressed, and is suppressed by cold isostatic press equipment regulation, pressurize and pressure release
Operate to obtain tungsten pipe pressed compact, wherein, shaping pressure is 290Mpa, and pressurize 1 hour, venting duration is 50 minutes.
3）In a hydrogen atmosphere, tungsten pipe pressed compact is placed in high temperature induction sintering furnace and sintered, heating rate is 30 DEG C/h, most
High-temperature is 2380 DEG C, and high-temperature holding time is 8 hours, places the oxygen that particle mean size is Φ 1mm during sintering below tungsten pipe pressed compact
Change zirconium exotic material.
4）Sintering briquette presentation quality is detected, 6 sets of sintering equal zero defects of blank, are then determined using drainage after testing
The global density of 6 sets of tungsten pipe sintering briquettes is 18.02-18.15g/cm3.Selection density is 18.10g/cm3A tungsten pipe, to tungsten pipe
Diverse location is sampled（Short transverse is a sampling height every 100mm, with height every 45°20*20*5mm is taken to try
Sample）, the density of every sample is surveyed, it is found that sample density scope is 18.08-18.13g/cm3, upper layer density is poor with lower layer density
It is not small.
5）Accessory processing is carried out using the mode of being loaded of 24 chucks according to drawing requirement, carries out surface throwing after Vehicle Processing again
Mill.
The crack defect of the 6 sets of Ф 760*1200mm type tungsten pipes produced using the method for penetrant inspection to the present embodiment is carried out
Examine, through examining the equal flawless defect of 6 sets of tungsten pipes, yield rate 100%.
Embodiment 3
Tungsten tube section schematic diagram manufactured in the present embodiment referring to Fig. 1, wherein OD1=600mm, OD2=560mm, OD3=
540mm, ID=500mm, H=1200mm, h1=90mm, referred to as h2=100mm, Ф 600*1200mm types tungsten pipe.
Specific preparation method is as follows：
1）The tungsten powder and average Fisher particle size for being 2.2 microns from the average Fisher particle size of Fw-1 types for meeting national standard are 3.8
The tungsten powder of micron as tungsten pipe raw material, wherein, the mass ratio of 2.2 microns of tungsten powder and 3.8 microns of tungsten powder is 45：55, purity
It is 99.9%, above-mentioned tungsten pipe raw material is placed in V-type batch mixer under high-purity argon gas protection and mixed 6 hours.
2）According to pressed compact charging desired size assembled formation mould, mixed raw material is loaded on cylindrical steel core rod and heavy wall
In space between gum cover, sealed again after stoppering heavy wall gum cover both ends with plug after charging, then charged shaping
Grinding tool hangs in cold isostatic press cylinder body and suppressed, and is suppressed by cold isostatic press equipment regulation, pressurize and pressure release
Operate to obtain tungsten pipe pressed compact, wherein, shaping pressure is 300Mpa, and pressurize 1 hour, venting duration is 60 minutes.
3）In a hydrogen atmosphere, tungsten pipe pressed compact is placed in high temperature induction sintering furnace and sintered, heating rate is 50 DEG C/h, most
High-temperature is 2350 DEG C, and high-temperature holding time is 6 hours, places the oxygen that particle mean size is Φ 3mm during sintering below tungsten pipe pressed compact
Change zirconium exotic material.
4）Sintering briquette presentation quality is detected, 15 sets of sintering equal zero defects of blank, are then surveyed using drainage after testing
The global density of fixed 15 sets of tungsten pipe sintering briquettes is 18.10-18.25g/cm3, selection density is 18.15g/cm3A tungsten pipe, to tungsten
Pipe diverse location is sampled（Short transverse is a sampling height every 100mm, with height every 45°20*20*5mm is taken to try
Sample）, the density of every sample is surveyed, it is found that sample density scope is 18.13-18.20g/cm3, upper layer density is poor with lower layer density
It is not small.
5）Accessory processing is carried out using the mode of being loaded of 24 chucks according to drawing requirement, carries out surface throwing after Vehicle Processing again
Mill.
The crack defect of the 15 sets of Ф 600*1200mm type tungsten pipes produced using the method for penetrant inspection to the present embodiment is entered
Performing check, through examining the equal flawless defect of 15 sets of tungsten pipes, yield rate 100%.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to the protection model of the limitation present invention
Enclose.In addition, it should also be understood that, after the technology contents of the present invention have been read, those skilled in the art can make each to the present invention
Kind change, modification and/or variation, all these equivalent form of values equally fall within the guarantor that the application appended claims are limited
Within the scope of shield.
Claims (11)
1. a kind of preparation method of large-size high-density tungsten pipe, it is characterised in that comprise the following steps：
Raw material admixing step, raw material tungsten powder is uniformly mixed in batch mixer；In the raw material admixing step, the original
Expect tungsten powder by the tungsten powder that average Fisher particle size is 1.8~2.2 microns and the tungsten powder group that average Fisher particle size is 3.8~4.2 microns
Into wherein averagely Fisher particle size is that 1.8~2.2 microns of tungsten powder dosage accounts for the 40%-45% of the raw material tungsten powder gross mass；
Cold isostatic compaction step, designed according to pressed compact charging desired size and make shaping dies, after then uniformly mixing
Raw material load in the mould and carry out cold isostatic compaction processing to obtain tungsten pipe pressed compact；The isostatic cool pressing into
In type step, shaping pressure is 280-300Mpa, and the dwell time is 0.5-2 hours, then pressure release, is controlled the pressure release total time
Within 45-60 minutes；
High temperature sintering step, the tungsten pipe pressed compact is subjected to high temperature sintering to obtain sintering blank, wherein, tungsten pipe during sintering
Spherical fireproof material is placed with below pressed compact, in the high temperature sintering step, the maximum temperature of the high temperature sintering is 2300-
2380 DEG C, maximum temperature soaking time is 4-8 hours, and heating rate is 30-70 DEG C/h；The spherical fireproof material is one layer flat
The spherical fireproof material that equal granularity is Φ 1-3mm；
Wherein, the external diameter of large-size high-density tungsten pipe is Ф 500-760mm, height 1200-1800mm.
2. preparation method according to claim 1, it is characterised in that described spherical resistance in the high temperature sintering step
The material of fiery material is zirconium oxide.
3. preparation method according to claim 1, it is characterised in that the high temperature sintering is under hydrogen or vacuum atmosphere
Carry out.
4. preparation method according to claim 1, it is characterised in that in the raw material admixing step, the raw material tungsten
Powder is the Fw-1 type tungsten powders for meeting national standard.
5. preparation method according to claim 1, it is characterised in that in the raw material admixing step, the mixing
Time is 5-6 hours.
6. preparation method according to claim 5, it is characterised in that the mixing is mixed in V-type batch mixer.
7. preparation method according to claim 1, it is characterised in that in the cold isostatic compaction step, it is described into
Shape mould includes：Cylindrical steel core rod, it is set in outside the cylindrical steel core rod and the heavy wall gum cover of both ends open and is covered on
The plug at the heavy wall gum cover both ends, the uniformly mixed raw material loaded on the cylindrical steel core rod and the heavy wall gum cover it
Between space in.
8. preparation method according to claim 1, it is characterised in that the preparation method also includes：
Blank detecting step is sintered, detection sintering blank presentation quality simultaneously determines global density；
Accessory processing step, accessory processing is carried out to detecting qualified sintering blank according to drawing requirement, in the accessory processing
When, using the mode that is loaded of multiple spot chuck；
Crack-detecting step, using the tungsten pipe crack defect after the method detection accessory processing of penetrant inspection.
9. preparation method according to claim 8, it is characterised in that the multiple spot chuck is 16 points or 24 chucks.
A kind of 10. large-size high-density tungsten pipe prepared using any methods describeds of claim 1-9.
11. tungsten pipe according to claim 10, it is characterised in that the global density of the tungsten pipe is 18.0-18.6g/cm3。
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| 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 |
| CN115415526B (en) * | 2021-05-13 | 2023-05-19 | 安泰天龙钨钼科技有限公司 | Oversized tungsten tube and preparation method thereof |
| 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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