CN103658670A - Ultrafine titanium powder and preparation method thereof - Google Patents
Ultrafine titanium powder and preparation method thereof Download PDFInfo
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- CN103658670A CN103658670A CN201410019195.4A CN201410019195A CN103658670A CN 103658670 A CN103658670 A CN 103658670A CN 201410019195 A CN201410019195 A CN 201410019195A CN 103658670 A CN103658670 A CN 103658670A
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- titanium powder
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Abstract
The invention belongs to the technical field of the preparation of titanium powder, and particularly relates to ultrafine titanium powder and a preparation method thereof. The method comprises the steps of heating sponge titanium particles inn a hydrogen reduction furnace, preserving the heat under the vacuum state, and reducing the titanium particles; heating the obtained titanium particles until the metal titanium is gasified, and condensating the titanium into spheres by suddenly reducing the temperature so as to obtain the ultrafine titanium powder. The oxygen content of the prepared ultrafine titanium powder is 1 to 5000ppm, the purity is 99 to 99.999 percent, the granularity D50 is 0.1 to 5 micrometers, the granularity D97 is 0.1 to 10 micrometers, and the ultrafine titanium powder is in an aspheric shape. An aero-engine blade coating produced by adopting the prepared ultrafine metal titanium powder has the advantages of large binding force, uniformity in thickness, small granularity, compaction, smooth surface, better corrosion resistance and the like. The ultrafine titanium powder has high crystallinity and good sintering property.
Description
Technical field
The invention belongs to titanium valve preparing technical field, be specifically related to a kind of purification ultrafine titanium powder and preparation method thereof.
Background technology
Titanium is a kind of argenteous transition metal, it is characterized by lightweight, intensity is high, tool metallic luster, also has good resistance to corrosion (comprising seawater, chloroazotic acid and chlorine).Due to its stable chemical property, good high temperature resistant, low temperature resistant, anti-strong acid, anti-highly basic, and high strength, low-density, by good reputation be " space metal ".
The method that obtains super-fine metal powder on general industry has:
(1) hydrogenation-disproportionation--method of dehydrogenating: the method is generally used for the powder process that production can be inhaled the metal of hydrogen, inhales hydrogen by high temperature, the lattice particle disproportionation of arranging after temperature reduces, metal bond energy reduces, easily broken, thereby reaches object prepared by powder.
(2) comminution by gas stream: the method is generally used for produces oxide-based powder, if produce metal-powder, generally uses the mode of nitrogen protection, and the powder of production can reach submicron order.
(3) ball-milling method: the method is a kind of method of more general production submicron particle, the method production efficiency is low, easily introduce impurity.
(4) physical vapor method: the method is a kind of method of emerging super-fine metal powder, and the particle diameter of powder can reach 100nm-5um.
Titanium valve hot-spraying technique, through development for many years, can be applied to incrustation, anti-corrosion coating, seal coating etc. for the production of various coatings, also can be for the production of sputtering target material pipe target, and thickness is the thickest can be sprayed into 5mm.For blade of aviation engine, require coating layer thickness 1-100 μ m, and excellent bonding performance, use the modes such as magnetron sputtering, plating all can not obtain the coating of desired properties, only have the mode by thermal spraying purification ultrafine titanium powder (particle diameter is 0.1-1 μ m) to obtain.
Summary of the invention
The object of this invention is to provide a kind of purification ultrafine titanium powder, there is higher degree of crystallinity and good sintering character; The present invention provides the preparation method of purification ultrafine titanium powder simultaneously, scientific and reasonable, simple.
The oxygen content of purification ultrafine titanium powder of the present invention is 1-5000ppm, and purity is 99-99.999%, and particle diameter D50 is 0.1-5 micron, and D97 is 0.1-10 micron.
Described purification ultrafine titanium powder to be shaped as class spherical.
The preparation method of purification ultrafine titanium powder of the present invention, step is as follows:
(1) select titanium sponge particle, use hydrogen reducing furnace, heating is incubated under vacuum, and titanium particle is reduced;
(2) titanium particle step (1) being obtained is heated to Titanium gasification, and then that titanium is condensed into is spherical in quenching, obtains.
The purity of the titanium sponge particle described in step (1) is 99.5-99.999%.
Heating-up temperature described in step (1) is 1000-1400 ℃, preferably 1100-1300 ℃.
Vacuum described in step (1) is 6.67 * 10
-2-1.0 * 10
-4pa.
Temperature retention time described in step (1) is 2-10 hour.
Heating-up temperature described in step (2) is 3500-20000 ℃.
Heat time described in step (2) is 0.5-3 hour.
Quench temperature described in step (2) is 20-500 ℃.
It is 0.1-1 μ m that the purification ultrafine titanium powder purity that the present invention prepares is more than or equal to 99%, D50 particle diameter, and D97 is less than 10 microns, and oxygen content is less than 5000ppm, is shaped as class spherical.
The purification ultrafine titanium powder that the present invention prepares is for the production of blade of aviation engine coating.
The present invention compared with prior art, has following beneficial effect:
1, the blade of aviation engine coating that adopts superfine metal titanium valve prepared by the present invention to produce, has adhesion large, and coating layer thickness is even, crystal grain is tiny, fine and close, smooth surface and have the advantages such as better corrosion resistance.
2, superfine metal titanium valve of the present invention has higher degree of crystallinity and good sintering character.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the superfine metal titanium valve of embodiment 1 preparation.
Fig. 2 is the SEM figure of embodiment 1 coating layer thickness direction.
Fig. 3 is the surperficial SEM figure after embodiment 1 coating surface corrosion.
Fig. 4 is the SEM figure of the superfine metal titanium valve of embodiment 2 preparations.
Fig. 5 is the surperficial SEM figure after embodiment 2 coating surface corrosion.
Fig. 6 is the SEM figure of the superfine metal titanium valve of embodiment 3 preparations.
Fig. 7 is the surperficial SEM figure after embodiment 3 coating surface corrosion.
Fig. 8 is the SEM figure of comparative example 1 coating layer thickness direction.
Fig. 9 is the SEM figure of comparative example 2 coating layer thickness directions.
The specific embodiment
Below in conjunction with embodiment, the present invention is described further.
(1) selecting purity is 99.5% titanium sponge particle, uses hydrogen reducing furnace, is heated to 1200 ℃, keeps vacuum 10
-2pa, is incubated 4 hours titanium particle is reduced;
(2) adopt physical vaporous deposition: the titanium particle that step (1) is obtained is heated to Titanium gasification, and heating-up temperature is 5000 ℃, and the heat time is 1 hour, and then 60 ℃ of quenchings make it to be condensed into spherical metallic titanium powder, obtain, and its D50 is 0.77 μ m.
Purification ultrafine titanium powder is carried out to SEM test, the results are shown in Figure 1.
Further, adopt the method for plasma spraying that the purification ultrafine titanium powder of embodiment 1 is sprayed on to plain steel surface, prepare surperficial corrosion-inhibiting coating, coating layer thickness scanning direction Electronic Speculum is as Fig. 2; Then by modes such as surface observation, SEM observation, brine corrosions, detect coating performance, the results are shown in Table 1 and Fig. 3.
Embodiment 2
(1) selecting purity is 99.999% titanium sponge particle, uses hydrogen reducing furnace, is heated to 1300 ℃, keeps vacuum 6.67 * 10
-2pa, is incubated 2 hours titanium particle is reduced;
(2) adopt physical vaporous deposition: the titanium particle that step (1) is obtained is heated to Titanium gasification, and heating-up temperature is 5000 ℃, and the heat time is 1.5 hours, and then 20 ℃ of quenchings make it to be condensed into spherical metallic titanium powder, obtain, and its D50 is 5.77 μ m.
Purification ultrafine titanium powder is carried out to SEM test, the results are shown in Figure 4.
Further, adopt the method for plasma spraying that the purification ultrafine titanium powder of embodiment 2 is sprayed on to plain steel surface, prepare surperficial corrosion-inhibiting coating; Then by modes such as surface observation, SEM observation, brine corrosions, detect coating performance, the results are shown in Table 1 and Fig. 5.
Embodiment 3
(1) selecting purity is 99.9% titanium sponge particle, uses hydrogen reducing furnace, is heated to 1400 ℃, keeps vacuum 1.0 * 10
-3pa, is incubated 10 hours titanium particle is reduced;
(2) adopt physical vaporous deposition: the titanium particle that step (1) is obtained is heated to Titanium gasification, and heating-up temperature is 15000 ℃, and the heat time is 2 hours, and then 400 ℃ of quenchings make it to be condensed into spherical metallic titanium powder, obtain, and its D50 is 6.65 μ m.
Purification ultrafine titanium powder is carried out to SEM test, the results are shown in Figure 6.
Further, adopt the method for plasma spraying that the purification ultrafine titanium powder of embodiment 3 is sprayed on to plain steel surface, prepare surperficial corrosion-inhibiting coating; Then by modes such as surface observation, SEM observation, brine corrosions, detect coating performance, the results are shown in Table 1 and Fig. 7.
Comparative example 1
The D50 that the method for employing plasma spraying is prepared ball-milling method is that the common metal titanium valve (purity is greater than 99.5%, and oxygen content is less than 1000ppm) of 22.5 μ m is sprayed on plain steel surface, prepares surperficial corrosion-inhibiting coating; Then by modes such as surface observation, SEM observation, brine corrosions, detect coating performance, the results are shown in Table 1 and Fig. 8.
Comparative example 2
The D50 that the method for employing plasma spraying is prepared ball-milling method is that the common metal titanium valve (purity is greater than 99.5%, and oxygen content is less than 1000ppm) of 4.88 μ m is sprayed on plain steel surface, prepares surperficial corrosion-inhibiting coating; Then by modes such as surface observation, SEM observation, brine corrosions, detect coating performance, the results are shown in Table 1 and Fig. 9.
Table 1 coating performance result
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (10)
1. a purification ultrafine titanium powder, is characterized in that the oxygen content of described purification ultrafine titanium powder is 1-5000ppm, and purity is 99-99.999%, and particle diameter D50 is 0.1-5 micron, and D97 is 0.1-10 micron.
2. purification ultrafine titanium powder according to claim 1, it is characterized in that described purification ultrafine titanium powder to be shaped as class spherical.
3. a preparation method for the purification ultrafine titanium powder described in claim 1 or 2, is characterized in that step is as follows:
(1) select titanium sponge particle, use hydrogen reducing furnace, heating is incubated under vacuum, and titanium particle is reduced;
(2) titanium particle step (1) being obtained is heated to Titanium gasification, and then that titanium is condensed into is spherical in quenching, obtains.
4. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the purity of the titanium sponge particle described in step (1) is 99.5-99.999%.
5. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the heating-up temperature described in step (1) is 1000-1400 ℃.
6. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the vacuum described in step (1) is 6.67 * 10
-2-1.0 * 10
-4pa.
7. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the temperature retention time described in step (1) is 2-10 hour.
8. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the heating-up temperature described in step (2) is 3500-20000 ℃.
9. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the heat time described in step (2) is 0.5-3 hour.
10. the preparation method of purification ultrafine titanium powder according to claim 3, is characterized in that the quench temperature described in step (2) is 20-500 ℃.
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| CN106334791A (en) * | 2016-10-24 | 2017-01-18 | 贵州省钛材料研发中心有限公司 | Production method for spherical titanium powder for 3D printing |
| CN109622943A (en) * | 2019-01-08 | 2019-04-16 | 成都先进金属材料产业技术研究院有限公司 | Purification ultrafine titanium powder and preparation method thereof |
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