CN107867690B - A kind of high temperature base WC powder and its preparation method and application - Google Patents
A kind of high temperature base WC powder and its preparation method and application Download PDFInfo
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- CN107867690B CN107867690B CN201711240464.XA CN201711240464A CN107867690B CN 107867690 B CN107867690 B CN 107867690B CN 201711240464 A CN201711240464 A CN 201711240464A CN 107867690 B CN107867690 B CN 107867690B
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention discloses the preparation method of high temperature base WC powder, comprising the following steps: by WO3Pretreatment matches carbon with primary; obtain the mixture one of total phosphorus content 13.8% ~ 15.5%; re-compacted molding carries out hydrogen-free carbonization treatment; it is sieved after broken, progress is secondary to match carbon, obtains the mixture two that total phosphorus content is 6.08%~6.15%; under the protection of hydrogen; secondary carbonization treatment is carried out, be sieved after being crushed, high temperature base WC powder is made.The present invention provides stable high temperature base WC powder preparation process, and the crystal grain tungsten powder defect produced is few, and completely, the WC crystalline perfection being prepared is good for powder grain development, and transgranular distortion is smaller.Energy effective protection carbonizing apparatus, prevents from generating steam in carbonisation, has saved cost of equipment maintenance in production process.
Description
Technical field
The present invention relates to the preparation method fields of hard alloy, more particularly, to a kind of high temperature base WC powder and its system
Preparation Method and application.
Background technique
In recent years, with the continuous extension of hard alloy application field, hard alloy material is towards super thick and two ultra-fine
Direction is developed, and super thick hard alloy is widely used to mining drilling tool, roll and stamping die field.
Hard alloy has very high hardness, intensity, wearability and corrosion resistance, is known as " industrial tooth ", answers extensively
For fields such as military project, space flight and aviation, machining, metallurgy, oil drilling, mine tool, telecommunications, buildings.With work
The continuous promotion of industry level, people propose requirements at the higher level to the performance of hard alloy.Main raw material(s) as hard alloy
WC powder, importance are self-evident.The process of the WC powder of traditional handicraft preparation are as follows: WO3In reduction furnace lower than 700 DEG C~
1000 DEG C of progress H2Reduction obtains W powder, then by its with C is black is uniformly mixed, carried out at 1450 DEG C~1900 DEG C in carbide furnace
High temperature cabonization obtains WC powder.It being restricted by apparatus factor, reduction temperature is lower, obtained W powder often ateliosis, and this
Kind feature can not be changed in carbonation stage.Therefore the WC crystalline perfection of traditional handicraft preparation is general, transgranular distortion is larger.It is existing
With the presence of the deficiencies of technology process is many and diverse, process control needs are high, unstable product quality.
And high temperature base WC has good moulding characteristic, has positive effect for the enough toughness for improving hard alloy, by
In its good crystallization property, the comprehensive performance of hard alloy is also significantly improved.But high temperature base WC powder preparation process
It is not sufficiently stable, the crystal grain tungsten powder defect produced is more, and crystallization is bad, and distortion crystal grain is more；It is difficult to meet production needs.
Summary of the invention
The technical problem to be solved by the present invention is in view of the shortcomings of the prior art, providing a kind of high temperature base WC powder and its preparation
Methods and applications.By WO3It carries out matching carbon and twice carbonization treatment twice, carbonisation can be prevented with effective protection carbonizing apparatus
Middle generation steam, protects carbonizing apparatus；And as twice match carbon and twice carbonization treatment make made from WC powder developed
Entirely, the WC crystalline perfection being prepared is good, and transgranular distortion is smaller.
The purpose of the present invention is achieved by the following technical programs:
There is provided a kind of preparation method of high temperature base WC powder, comprising the following steps: by WO3Pretreatment matches carbon with primary, obtains
To the mixture one of total phosphorus content 13.8%~15.5%, re-compacted molding carries out hydrogen-free carbonization treatment, is sieved after broken, carries out
It is secondary to match carbon, it obtains the mixture two that total phosphorus content is 6.08%~6.15% and is carried out at secondary carbonization under the protection of hydrogen
Reason be sieved after being crushed, high temperature base WC powder is made.
Specific steps are as follows:
S1. by WO3It carries out pre-grinding and handles 1~4h, carbon black is added and carries out once matching carbon；After mixing, by quality point
Number meter, obtains the mixture one of total carbon content 13.8%~15.5%；
S2. by one compression moulding of mixture described in step S1, hydrogen-free carbonization treatment is carried out, embryo material one is made；
S3. embryo material one obtained by step S2 is carried out after being crushed, crosses 80~150 mesh metallic sieves, gained mixture is carried out
Sampling measurement total carbon, oxygen content；
S4. mixture described in step S3 is carried out secondary with carbon；After mixing, as mass fraction, total carbon is obtained to contain
The mixture two that amount is 6.08%~6.15%；
S5. mixture two described in step S4 is subjected to secondary carbonization treatment, embryo material two carries out ball mill crushing by treated
Afterwards, 100~180 mesh metallic sieves are crossed, the high temperature base WC powder that carbonization FSSS granularity is 0.8 μm~5.0 μm is made.
The preparation method of high temperature base WC powder of the invention passes through to WO3Pretreatment, compression moulding, the hydrogen-free carbonization of raw material
Processing, it is secondary scientifically define charging rate with secondary carbonization under carbon and protective atmosphere, primary hydrogen-free carbonization is to reacting furnace
Protective atmosphere is adjusted, and is played a protective role to consersion unit.The adjustment of the technique can be accurately obtained the target WC powder of needs
End, completely, the WC crystalline perfection being prepared is good for obtained WC powder development, and transgranular distortion is smaller.
Further, hydrogen-free carbonization treatment described in step S2 is reacted in hydrogen-free carbide furnace, and the temperature of reaction is
1500~1800 DEG C, the fltting speed of the mixture one is 15~40min/boat.
Further, secondary carbonization treatment described in step S5,1600 DEG C~1900 DEG C of temperature, protective atmosphere H2, dew point-
60 DEG C, the fltting speed of the mixture two is 15~40min/boat.
The preparation method of high temperature base WC powder of the invention considers equipment and production cycle in production, and it is raw to be suitable for industry
It producing, science defines the fltting speed of charging, and pushing away boat speed can control reaction speed, so that different reaction products is obtained,
The WC powder of different FSSS granularities.
It is further preferred that the WO3For national standard zero level WO3, the tungsten carbide impurity content of this kind of grade is few, is conducive to oxygen
Change the production of tungsten powder.
Another object of the present invention is to disclose high temperature base made from a kind of preparation method as above-mentioned high temperature base WC powder
WC powder.
Another object of the present invention is to disclose high temperature base made from a kind of preparation method as above-mentioned high temperature base WC powder
WC powder is in ground mine alloy and hard alloy cutter product.
Compared with prior art, beneficial effects of the present invention:
The process flow of the preparation method of high temperature base WC powder of the invention is less, simple to operate, is significantly reduced
The investment of equipment, energy-saving and emission-reduction have good social and economical benefits.
The WC powder of the preparation method preparation of high temperature base WC powder of the invention has crystallization completely, close to theory WC powder
Lattice constant, transgranular distortion is minimum, and powder size uniformity is preferable；The WC-Co hard alloy of powder preparation has good
Performance.
In production, energy effective protection equipment extends equipment and uses the longevity preparation method of high temperature base WC powder of the invention
Life has biggish economic benefit.
WC powder preparation controllability of the invention is high, and structure is uniform, good combination property.
Detailed description of the invention
The SEM picture of the high temperature base WC powder of the technique preparation of Fig. 1 embodiment of the present invention 2.
The SEM picture of the WC powder of the traditional handicraft preparation of Fig. 2 comparative example 1.
Specific embodiment
Present invention be described in more detail in the following with reference to the drawings and specific embodiments.Unless stated otherwise, the present invention is implemented
The various raw materials that example uses can be obtained by regular market purchase, or be prepared according to the conventional method of this field, used to set
Standby is experiment commonly used equipment.Unless otherwise defined or described herein, all professional and scientific terms used herein and this field
Meaning known to person skilled in the art is identical.
The preparation method of high temperature base WC powder of the invention, comprising the following steps: by WO3Pretreatment matches carbon with primary, obtains
To the mixture one of total phosphorus content 13.8%~15.5%, re-compacted molding carries out hydrogen-free carbonization treatment, is sieved after broken, carries out
It is secondary to match carbon, it obtains the mixture two that total phosphorus content is 6.08%~6.15% and is carried out at secondary carbonization under the protection of hydrogen
Reason be sieved after being crushed, high temperature base WC powder is made.
Embodiment 1
The preparation method of the high temperature base WC powder of the present embodiment, specific steps are as follows:
S1. by 12 μm of national standard zero level WO of FSSS granularity3It is carried out in the double cone blender equipped with line with rubber stainless steel ball pre-
Milled processed 4h is added carbon black and carries out once matching carbon；After mixing, as mass fraction, total carbon content 15.5% is obtained
Mixture one；
S2. the mixture one of step S1 is pressed on press machine, reacted in hydrogen-free carbide furnace into
The hydrogen-free carbonization treatment of row, the temperature of reaction are 1500 DEG C, and the fltting speed of mixture one is 15min/boat；Embryo material one is made；
S3. embryo material one obtained by step S2 is carried out after being crushed, crosses 100 mesh metallic sieves, gained mixture is sampled
Measure total carbon, oxygen content；Gained mixture total carbon 6.01%, oxygen content 0.12%；
S4. according to testing result, mixture described in step S3 is carried out in double cone blender secondary with carbon；By total carbon
It is adjusted to 6.15%；
S5. mixture two described in step S4 is subjected to secondary carbonization treatment, 1600 DEG C of the temperature of secondary carbonization treatment, protection
Atmosphere is H2, -60 DEG C of dew point, the fltting speed of mixture two is 15min/boat.By treated, embryo material two is carried out after being crushed,
150 mesh metallic sieves are crossed, carbonization FSSS granularity obtained by the technique is 0.8 μm, total carbon 6.15%, free carbon≤0.08%, oxygen
Content 0.08%.
Embodiment 2
The preparation method of the high temperature base WC powder of the present embodiment, specific steps are as follows:
S1. by 14 μm of national standard zero level WO of FSSS granularity3It is carried out in the double cone blender equipped with line with rubber stainless steel ball pre-
Milled processed 2h is added carbon black and carries out once matching carbon；After mixing, as mass fraction, total carbon content 14.8% is obtained
Mixture one；
S2. by one compression moulding of mixture described in step S1, reaction is carried out in hydrogen-free carbide furnace and is carried out at hydrogen-free carbonization
Reason, the temperature of reaction are 1650 DEG C, and the fltting speed of mixture one is 30min/boat；Embryo material one is made；
S3. embryo material one obtained by step S2 is carried out after being crushed, crosses 100 mesh metallic sieves, gained mixture is sampled
Measure total carbon, oxygen content；Gained mixture total carbon 5.82%, oxygen content 0.09%；
S4. according to testing result, mixture described in step S3 is carried out in double cone blender secondary with carbon；By total carbon
It is adjusted to 6.13%；
S5. mixture two described in step S4 is subjected to secondary carbonization treatment, 1700 DEG C of the temperature of secondary carbonization treatment, protection
Atmosphere is H2, -60 DEG C of dew point, the fltting speed of mixture two is 25min/boat.By treated, embryo material two is carried out after being crushed,
150 mesh metallic sieves are crossed, carbonization FSSS granularity obtained by the technique is 2.5 μm, and total carbon 6.12%, free carbon 0.05%, oxygen contains
Amount 0.06%.
Embodiment 3
The preparation method of the high temperature base WC powder of the present embodiment, specific steps are as follows:
S1. by 17.5 μm of national standard zero level WO of FSSS granularity3It is carried out in the double cone blender equipped with line with rubber stainless steel ball
Pre-grinding handles 2h, and carbon black is added and carries out once matching carbon；After mixing, as mass fraction, total carbon content 13.8% is obtained
Mixture one；
S2. by one compression moulding of mixture described in step S1, reaction is carried out in hydrogen-free carbide furnace and is carried out at hydrogen-free carbonization
Reason, the temperature of reaction are 1800 DEG C, and the fltting speed of mixture one is 40min/boat；Embryo material one is made；
S3. embryo material one obtained by step S2 is carried out after being crushed, crosses 100 mesh metallic sieves, gained mixture is sampled
Measure total carbon, oxygen content；Gained mixture total carbon 5.63%, oxygen content 0.09%；
S4. according to testing result, mixture described in step S3 is carried out in double cone blender secondary with carbon；By total carbon
It is adjusted to 6.13%；
S5. mixture two described in step S4 is subjected to secondary carbonization treatment, 1900 DEG C of the temperature of secondary carbonization treatment, protection
Atmosphere is H2, -60 DEG C of dew point, the fltting speed of mixture two is 40min/boat.By treated, embryo material two is carried out after being crushed,
120 mesh metallic sieves are crossed, carbonization FSSS granularity obtained by the technique is 5.0 μm, and total carbon 6.12%, free carbon 0.05%, oxygen contains
Amount 0.05%.
Comparative example 1
This comparative example is current universal 2-3umWC powder process, technique are as follows:
W powder addition carbon black is obtained into the mixture that total phosphorus content is 6.10%~6.13%, then in blender mixing 4h,
Then gained mixture being subjected to carburizing reagent in carbide furnace, the protective atmosphere of this carburizing reagent is H2, -60 DEG C of dew point, H2
Flow 0.5-1m3/h, boat charge 6-8kg/boat, 1600 DEG C of carburizing temperature push away speed, push away fast 15min/boat.
Gained WC block carries out rolling ball milling and is crushed, technique: inventory 200kg/ batches, ratio of grinding media to material 2:1 is crushed time 40min,
Broken material crosses 120 mesh metallic sieves.
High temperature base WC powder made from the preparation method of the high temperature base WC powder of 1~embodiment of the present embodiment 3 is for ground mine
In alloy and hard alloy cutter product.
X is carried out in order to verify high temperature based powders and the traditional handicraft WC powder (comparative example 1) of embodiment 2 prepared by this technique
X ray diffraction analysis x and scanning electron microscope, specific data are shown in Table 1, Fig. 1 and Fig. 2.The high temperature base WC powder of embodiment 2 is from picture
The crystal grain of WC powder is spherical, single crystal grain, and powder crystallization is complete, even particle size distribution, and degree of aggregation is relatively low.Comparative example 1
Method preparation 2-2.5 μm of WC powder, as shown in Figure 2, which is mostly polycrystalline particle, and assembles more serious, and granularity
Unevenly.
Table 1
By table 1 the result shows that the WC powder distortion of lattice of this technique only has the 1/5 of ordinary powder, powder crystallization integrality is higher.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should be included within scope of the invention.
Claims (4)
1. a kind of preparation method of high temperature base WC powder, which comprises the following steps:
S1. by 14 μm of FSSS granularity of WO3It carries out pre-grinding and handles 2h, carbon black is added and carries out once matching carbon；After mixing, it presses
Mass fraction meter obtains the mixture one of total carbon content 14.8%；
S2. by one compression moulding of mixture described in step S1, hydrogen-free carbonization treatment is carried out at 1650 DEG C, and embryo material one is made；
S3. embryo material one obtained by step S2 is carried out after being crushed, crosses 100 mesh metallic sieves, gained mixture is sampled measurement
Total carbon, oxygen content；
S4. mixture described in step S3 is carried out secondary with carbon；After mixing, as mass fraction, obtaining total carbon content is
6.13% mixture two；
S5. mixture two described in step S4 is carried out secondary carbonization treatment: 1700 DEG C of the temperature of secondary carbonization treatment protects gas
Atmosphere is H2, and -60 DEG C of dew point, the fltting speed of mixture two is 25min/boat, and by treated, embryo material two is carried out after being crushed, mistake
The high temperature base WC powder that carbonization FSSS granularity is 2.5 μm is made in 150 mesh metallic sieves.
2. the preparation method of high temperature base WC powder according to claim 1, which is characterized in that the WO3For national standard zero level WO3。
3. high temperature base WC powder made from a kind of preparation method of high temperature base WC powder as described in claim 1 ~ 2 any one.
4. high temperature base WC powder made from a kind of preparation method of the high temperature base WC powder as described in claim 3 is for ground mine alloy
And in hard alloy cutter product.
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| CN108892141A (en) * | 2018-09-06 | 2018-11-27 | 北京科技大学 | A kind of high-purity, ultrafine tungsten carbide preparation method |
| CN110668444A (en) * | 2019-11-12 | 2020-01-10 | 株洲硬质合金集团有限公司 | Preparation method of tungsten carbide powder |
| CN112342449B (en) * | 2020-10-16 | 2021-11-23 | 株洲明日硬质合金有限公司 | Hard alloy and preparation method and application thereof |
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| CN1597510A (en) * | 2004-07-30 | 2005-03-23 | 自贡硬质合金有限责任公司 | Production method of needle-shaped tungsten carbide powder |
| CN1907604A (en) * | 2006-08-18 | 2007-02-07 | 谭天翔 | Direct reduction carbonization manufacture method for tungsten carbide or tungsten carbide-cobalt ultrafine particle powder |
| CN101664809A (en) * | 2009-10-09 | 2010-03-10 | 株洲硬质合金集团有限公司 | Uniform macromeritic tungsten powder and method for preparing tungsten carbide powder |
| CN102649571A (en) * | 2012-05-07 | 2012-08-29 | 株洲硬质合金集团有限公司 | Production method for superfine tungsten carbide powder |
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| ITUB20151362A1 (en) * | 2015-05-26 | 2016-11-26 | F I L M S S P A Fabbrica Italiana Leghe Metalliche Sinterizzate | PROCEDURE FOR THE DIRECT PRODUCTION OF TUNGSTEN CARBIDE POWDERS OF VARIOUS GRANULOMETRIES STARTING FROM SCHEELITE MINERALS. |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1597510A (en) * | 2004-07-30 | 2005-03-23 | 自贡硬质合金有限责任公司 | Production method of needle-shaped tungsten carbide powder |
| CN1907604A (en) * | 2006-08-18 | 2007-02-07 | 谭天翔 | Direct reduction carbonization manufacture method for tungsten carbide or tungsten carbide-cobalt ultrafine particle powder |
| CN101664809A (en) * | 2009-10-09 | 2010-03-10 | 株洲硬质合金集团有限公司 | Uniform macromeritic tungsten powder and method for preparing tungsten carbide powder |
| CN102649571A (en) * | 2012-05-07 | 2012-08-29 | 株洲硬质合金集团有限公司 | Production method for superfine tungsten carbide powder |
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