CN1310244A - Preparation of composite hard alloy powder of tungsten carbide and titanium cobalt carbide - Google Patents
Preparation of composite hard alloy powder of tungsten carbide and titanium cobalt carbide Download PDFInfo
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- CN1310244A CN1310244A CN 00110137 CN00110137A CN1310244A CN 1310244 A CN1310244 A CN 1310244A CN 00110137 CN00110137 CN 00110137 CN 00110137 A CN00110137 A CN 00110137A CN 1310244 A CN1310244 A CN 1310244A
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- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 15
- 239000000956 alloy Substances 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- NNSIWZRTNZEWMS-UHFFFAOYSA-N cobalt titanium Chemical compound [Ti].[Co] NNSIWZRTNZEWMS-UHFFFAOYSA-N 0.000 title claims description 8
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 25
- 238000003763 carbonization Methods 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 150000001721 carbon Chemical group 0.000 claims description 2
- 238000007908 dry granulation Methods 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 abstract description 9
- 239000002245 particle Substances 0.000 description 18
- 239000000203 mixture Substances 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- 238000000889 atomisation Methods 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910000531 Co alloy Inorganic materials 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 6
- 235000019241 carbon black Nutrition 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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Abstract
The composite hard alloy powder contains WC 55-75 wt%, and TiC 15-35 wt% other than Co. The preparation features that soluble salts of W, Co and Ti in certain proportion are first dissolved in water through stirring; the solution is atomized into small drops of 1 micron less size and hot air dried and pelletized at air inlet temperature 200-300 deg.c and air outlet temperature 100-200 deg.c; and the gathered powder is roasted at 600-800 deg.c for 1-5 hr and carbonized to obtain WC-TiC-Co hard alloy powder. The preparation process of the present invention is simple and can prepare powder with homogeneous component and structure and nanometer level size.
Description
The present invention relates to the Wimet technology, a kind of preparation method of composite hard alloy powder of tungsten carbide and titanium cobalt carbide is provided especially.
The WC-TiC-Co Wimet has higher anti-crescent moon hole, wearing and tearing ability, is applicable to the cutter that the continuous chip material is arranged as cutting.In China, the turnout of WC-TiC-Co alloy is only second to the WC-Co alloy, is mainly used in the machining of steel.Tungsten is the basic constituent element of Wimet, belong to rare metal, yet China's tungsten ore resource is very abundant, and reserves are about half of world's total reserves, so the hard carbide industry of China fully develops talents.Fig. 1 is the process flow sheet of traditional production WC-TiC-Co alloy.The method technology more complicated of traditional as seen from the figure production WC-TiC-Co need batch mixing and shattering process through repeatedly, and batch mixing each time and shattering process all can cause the introducing of the inhomogeneous and impurity of composition.And the preparation of raw material needs the long reaction process of high temperature.This all makes the increase of making energy consumption and cost.In addition, the control of carbon amount and the control of weave construction are also very difficult, the therefore normal alloy that two kinds of different trades mark occur but having obtained with a kind of technology fully.
The object of the present invention is to provide a kind of preparation method of composite hard alloy powder of tungsten carbide and titanium cobalt carbide, it is the economization existing processes greatly, and prepared powder composition and the homogeneous microstructure that goes out, and granularity can reach nano-scale.
The invention provides a kind of preparation method of composite hard alloy powder of tungsten carbide and titanium cobalt carbide, the weight item scope of composite powder is in WC55-75%, TiC15-35%, Co surplus, it is characterized in that: at first that the soluble salt of tungstenic, cobalt, titanium is soluble in water in proportion, stir; Above-mentioned solution mist is changed into small droplets, and drop size is used the hot-air dry granulation simultaneously less than 1 μ m, and inlet air temperature 200-300 ℃, air outlet temperature 100-200 ℃; The powder of collecting was accompanied burning 1-5 hour at 600-800 ℃, carry out carbonization again and promptly get the WC-Co-TiC cemented carbide powder.
Adopt the inventive method synthetic nano level WC-Co-TiC composite powder to prepare the concrete technology of Wimet referring to Fig. 2.At first be the salt of selecting to contain tungsten, cobalt, titanium, the requirement of this selection is: 1) these salt can be water-soluble.2) chemical reaction not taking place, do not form the segregation of composition, does not preferably form precipitation yet between the aqueous solution of each salt.3) can not produce poisonous, deleterious material between each salt.4) price is cheap as far as possible.After selecting suitable salt, just can they are soluble in water respectively, mix mutually then, form the aqueous solution, salt and water weight ratio should be about 30%, so that the flour extraction rate in the raising atomization drying process should carry out original salt raw material weighing by resulting alloy particle composition during preparation.The aqueous solution for preparing is carried out atomization drying, the schematic diagram of atomization drying equipment used is seen shown in Figure 3, the powder of collecting is put in the loft drier, the powder of collecting is for green, mean particle size is about 40 μ m, particle surface is slick sphere, as controls improperly, can produce fracture, subsides, swollenly particle in irregular shape such as split.
The particle of collecting behind the atomization drying is put into temperature control furnace carry out the deionization processing, accompanying in this stage and the general ceramic preparation process burnt similar, and deionized purpose is the unnecessary ion remaval that will be mixed in the salt, to reduce the disadvantageous effect that these impurity bring.Deionization is handled and can be carried out in air, also can in hydrogen, oxygen or rare gas element, carry out, accompanying the particle after the burning is Ti, W, Co hopcalite, this process can be monitored this reaction process with TGA, accompany the burning temperature and time with what determine to be fit to, accompany after the burning particle morphology as shown in Figure 4.
With accompany after the burning particle with carry out carbonization after carbon mixes, this is that a routine techniques can adopt several different methods, as directly mixing carbon high temperature cabonization or with the gas that contains carbon atom, as CO, C then with ball milling
2H
2, CH
4Deng the gas carbonization, in industrial production, preferably adopt ball milling to mix carbon, and carry out carbonization with gas control carbon potential method.List is used the gas carbonization, and the reaction times is very long, and may cause uneven components.Some processing parameters in the necessary choose reasonable carbonization process, otherwise can cause the carbonization deficiency, produce defectives such as uncombined carbon, these processing parameters comprise the add-on of carbon black, the ball milling time of carbon black and oxide compound, carbonization temperature and carbonization time, the flow of atmosphere selection, gas etc.
The SEM of the particle that the process above-mentioned steps obtains schemes as shown in Figure 5, and resultant articles can directly be suppressed or sinter into to the powder after the carbonization.Because each composition mixes in molecular level, therefore reduced temperature of reaction, shorten the reaction times greatly, thereby can access nano level WC-TiC-Co particle, this Wimet performance is improved a lot.
The feedstock production WC-TiC-Co cemented carbide powder that employing of the present invention is different with traditional method.Can save preparation WC, TiC, a series of processes of Co raw material powder.Directly, not only save cost, and reduced many links with replacing to salt.
Because selected Ti, W, Co is soluble salt, this can make by the particle composition that obtains behind the atomization drying very even, experiment shows this even, can reach the uniform mixing of molecular level, this homogeneity of ingredients also makes particle that the segregation of composition does not take place in aftertreatment, but form nano level fine particle, thereby can under lower temperature, carbonization become nano level WC-TiC-Co particle.
Creatively used the atomization drying technology to come the uniform progenitor of prepared composition among the present invention, and usually the atomization drying technology only is suitable for and carry out drying treatment.This makes that producing the WC-TiC-Co alloy becomes very easy, greatly reduces cost, very likely replaces traditional technology.
In a word, the present invention has many advantages:
1) technical process is simplified greatly, and equipment is simple.
2) because each component uniform mixing in solution, so the control of composition is more prone to, and homogeneity of ingredients improves greatly.
3) with the powder process of atomization drying technology, the production efficiency height, the particle composition that makes is even, has substituted ball-milling technology and has brought various disadvantageous effects.
4) use the carbonization technology, only need a step to handle and can make the WC-Co-TiC alloy, temperature of reaction is low, and the reaction times is short, has reduced cost.
5) can be made into nano-scale, mixed uniformly WC-TiC-Co composite particles will help improving WC-TiC-Co Wimet performance.
Below by embodiment in detail the present invention is described in detail.
Accompanying drawing 1 is the process flow sheet of traditional production WC-TiC-Co alloy.
Accompanying drawing 2 is the process flow sheet of production WC-TiC-Co alloy of the present invention.
Accompanying drawing 3 is the schematic diagram of atomization drying equipment used.
Accompanying drawing 4 burns the back particle morphology for accompanying.
Accompanying drawing 5 is a) atomization drying b of the SEM photo of different steps particle) accompany and burn c) carbonization d) thermal treatment
Embodiment 1: preparation WC
65-TiC
25-Co
10Powdered alloy
With AMT powder that contains tungsten and titaniferous TiCl
3Solution and the Co (NO that contains cobalt
3)
2Come obtain solution, after the weighing according to a certain percentage of each raw material, blunge and evenly do not produce any precipitation, carry out powder process with atomization drying equipment then, the starting powder that obtains is for spherical, see Fig. 5,, obtain required alloying constituent so can mix in any ratio because raw material is the aqueous solution of solubility.
The powder of atomization drying is handled through deionization, obtains containing W, Ti, Co hopcalite.This mixture is at 750 ℃, accompanies in the air in 2 hours to obtain after the burning.Atmosphere can be decided according to selected raw material.
This then hopcalite mixes with carbon black.Be blended on the ball mill commonly used and carry out, the add-on of carbon black is calculated with reference to traditional mode of production, and adjusts according to the purity of reacting the carbon black that is added and the purity of oxide compound.
With the carbonization in graphite furnace or other tube furnace of these powder, carbonization is carried out in the atmosphere of CO at last, and carbonization temperature is at 1100-1300 ℃.The preparation particle morphology as shown in Figure 5, XRD is diffracted to WC, TiC, Co peak.
Embodiment 2:
With the APT powder and the TiCl that contain tungsten
3Solution and the CoCl that contains Co
2Prepare original solution, undertaken also can obtaining the WC-TiC-Co alloy powder by embodiment 1 then.
Embodiment 3:
Press embodiment 1 or 2, the particle through atomization drying obtains when deionization is handled, at 750 ℃ * 2hr, carries out in the rare gas elementes such as Ar.
Embodiment 4:
Mix the also available airflow milling method of carbon process and carry out, carry out carbonization then.
Embodiment 5:
Carbonization process need not mix the carbon process, directly carries out in carbonaceous atmosphere, as directly carrying out carbonization with CO, may produce uncombined carbon after the carbonization, uses CO/CO then
2Mixed gas produce different carbon potentials and remove the free carbon blacks.
Claims (3)
1, a kind of preparation method of composite hard alloy powder of tungsten carbide and titanium cobalt carbide, the weight item scope of composite powder is in WC55-75%, TiC15-35%, Co surplus, it is characterized in that: at first that the soluble salt of tungstenic, cobalt, titanium is soluble in water in proportion, stir; Above-mentioned solution mist is changed into small droplets, and drop size is used the hot-air dry granulation simultaneously less than 1 μ m, and inlet air temperature 200-300 ℃, air outlet temperature 100-200 ℃; The powder of collecting was accompanied burning 1-5 hour at 600-800 ℃, carry out carbonization again and promptly get the WC-TiC-Co cemented carbide powder.
2, by the preparation method of the described composite hard alloy powder of tungsten carbide and titanium cobalt carbide of claim 1, it is characterized in that: described carbonization process adopts directly and mixes the carbon method of high temperature cabonization then with ball milling.
3, by the preparation method of the described composite hard alloy powder of tungsten carbide and titanium cobalt carbide of claim 1, it is characterized in that: described carbonization process adopts gas CO, the C that contains carbon atom
2H
2, CH
4Carbonization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110137 CN1114709C (en) | 2000-02-23 | 2000-02-23 | Preparation of composite hard alloy powder of tungsten carbide and titanium cobalt carbide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110137 CN1114709C (en) | 2000-02-23 | 2000-02-23 | Preparation of composite hard alloy powder of tungsten carbide and titanium cobalt carbide |
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| Publication Number | Publication Date |
|---|---|
| CN1310244A true CN1310244A (en) | 2001-08-29 |
| CN1114709C CN1114709C (en) | 2003-07-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732766A (en) * | 2012-07-06 | 2012-10-17 | 四川大学 | Coarse grain hard alloy material and preparation method thereof |
| CN103820694A (en) * | 2014-01-27 | 2014-05-28 | 湖南海云冶金材料有限公司 | Method for preparing WC (Wolfram Carbide)-TiC (Titanium Carbide) solid solution powder for tungsten-titanium-cobalt hard alloy |
| CN109280838A (en) * | 2018-11-30 | 2019-01-29 | 宇龙精机科技（浙江）有限公司 | A kind of titanium-cobalt alloy and preparation method thereof |
-
2000
- 2000-02-23 CN CN 00110137 patent/CN1114709C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732766A (en) * | 2012-07-06 | 2012-10-17 | 四川大学 | Coarse grain hard alloy material and preparation method thereof |
| CN103820694A (en) * | 2014-01-27 | 2014-05-28 | 湖南海云冶金材料有限公司 | Method for preparing WC (Wolfram Carbide)-TiC (Titanium Carbide) solid solution powder for tungsten-titanium-cobalt hard alloy |
| CN103820694B (en) * | 2014-01-27 | 2015-11-25 | 湖南海云冶金材料有限公司 | The preparation method of a kind of tungsten-titanium-cobalt series hard metal WC-TiC solid-solution powder |
| CN109280838A (en) * | 2018-11-30 | 2019-01-29 | 宇龙精机科技（浙江）有限公司 | A kind of titanium-cobalt alloy and preparation method thereof |
| CN109280838B (en) * | 2018-11-30 | 2020-11-06 | 宇龙精机科技（浙江）有限公司 | Titanium-cobalt alloy and preparation method thereof |
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| Publication number | Publication date |
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| CN1114709C (en) | 2003-07-16 |
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