CN104084594A - Method for preparing microfine spherical niobium powder - Google Patents
Method for preparing microfine spherical niobium powder Download PDFInfo
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- CN104084594A CN104084594A CN201410246608.2A CN201410246608A CN104084594A CN 104084594 A CN104084594 A CN 104084594A CN 201410246608 A CN201410246608 A CN 201410246608A CN 104084594 A CN104084594 A CN 104084594A
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Abstract
The invention relates to a method for preparing microfine spherical niobium powder. The method comprises the following steps: firstly, forming stable argon plasmas and adjusting all parameters to control the distribution of the plasmas in a reactor; feeding raw niobium powder, enabling the niobium powder to pass through a plasma region, and heating and melting particles; after the niobium powder leaves from the plasma region, quickly cooling and solidifying to obtain the microfine spherical niobium powder. Compared with irregular particular raw powder, most of the powder particles are spherical, the flowability, the particle density and the purity are higher, the particle surface is smooth, and the particle porosity is low. According to the method disclosed by the invention, the niobium powder particles are changed in shape, the rate of spheroidization is high, the apparent density of the powder is increased, the flowability and the physical property of the niobium powder are improved, the phase of the niobium powder cannot be changed, application in certain fields is facilitated, and the cost is low.
Description
Technical field
The present invention relates to a kind of method of preparing minute spherical niobium powder, belong to powder preparation field.
Background technology
Do thermal source aspect the spheroidising of micron-submicron and some nano material with plasma, there is larger technical advantage.Radio frequency plasma torch arc body is very large, arc stream is stablized, be easy to adjusting controls, and makes it to be easily applied to superfines material processed technical field.At present, overseas utilization plasma is processed powder technology and has been possessed certain technical merit.Canadian Tyke receive the plasma powder handling system of (TEKNA) company exploitation aspect induction plasma technology in first place in the world, realized metal dust and the SiO such as W, Mo, Re, Ta, Ni, Cu
2, ZrO
2, YSZ, Al
2o
3deng the spheroidising of oxide ceramic powder.Domestic Xinan Nuclear Physics Research Academy adopts self-built plasma spheroidization system, has realized W, Al
2o
3deng the nodularization of powder, nodularization rate is high, and size reaches 0.5～45 μ m, and powder, for thermal spraying and powder metallurgy, has good performance.
Because the good application of nodularization powder in some fields, the nodularization of the especially high refractory powder of various powder becomes the demand of powder preparation.Metal niobium is a kind of high refractory metal, and fusing point, up to 2740 DEG C, can absorb gas, as degasifier, is also a kind of good superconductor, is applied to many high-tech sectors.As in high-energy physics field, need to obtain high-performance, large-sized niobium goods, prepare niobium goods if print technique with laser 3D, compare traditional handicraft, likely obtain performance more excellent, the product that size is larger.But, in the time adopting laser 3D to print fine and close high-performance niobium goods, adopt the irregular powder of grain shape, in the time printing stone, mobility is bad, cause printing speed slow, and bulk density is little, easily forms hole, not fine and close; If adopting spherical powder is raw material niobium powder, in the time printing stone, good fluidity, bulk density is large, and laser sintered rear shrink of product is even, can realize comparatively accurate size Control, extrudate density is even, and the porosity is low, finer and close, preparation process is consuming time greatly to be reduced, and laser sintered power also will reduce; And by the powder of radio frequency plasma nodularization, impurity content can further reduce, and especially reduces micro amount of oxygen impurity content, thereby further optimizes the superconduct performance of niobium goods.
Under this context request, need to there is a kind of truly feasible, method with certain production capacity, carry out the preparation of minute spherical niobium powder.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, nodularization rate is high, possess the method for preparing minute spherical niobium powder of certain production capacity.
The present invention is achieved through the following technical solutions:,
A method of preparing minute spherical niobium powder, the method comprises the following steps:
1) form stable argon plasma torch;
2) by carrying gas, former metal niobium powder is sent to the high-temperature region of plasma torch, niobium powder is heated, and forms particle drop;
3) niobium powder particles drop leaves after plasma area, and cooling curing forms spheric granules powder;
4) collect spherical niobium powder.
According to the present invention, step 1) in, in high frequency plasma reactor, forming the needed reacting gas of argon plasma torch (preferably Ar) input flow rate is 40～60slpm, the high voltage loading on induction coil is 6～8KV.Reacting gas (preferably Ar) input flow rate when described argon plasma stable operation is 20～50slpm, and protective gas (Ar) input flow rate is 30～120slpm, and internal system air pressure is 0.03～0.06MPa.
According to the present invention, step 2) in, described in carry gas can use argon gas, hydrogen etc. in hot environment not with the gas of metal-powder generation chemical reaction.The average grain diameter of the former powder of metal niobium adding is 0.5～45 μ m, and carrying gas control flow is 0.5～5slpm, and niobium powder feeding control flow is 5～50g/min.
According to the present invention, step 3) in, niobium powder particles drop leaves after plasmatorch, in high thermograde (10
-6) under rapidly cooling, enter heat-exchanging chamber quenching and solidify, under capillary effect, form spherical particle.
According to the present invention, step 4) in, spherical niobium powder collected with collector.
Advantage of the present invention is, compares with the former powder of irregular particle shape, and powder granule is most of spherical in shape, and mobility, grain density, purity are higher, and particle surface is bright and clean, and particle porosity is low.The method that the present invention proposes has changed the shape of niobium powder particles, nodularization rate is high, improved the purity of niobium powder simultaneously, and increase the apparent density of powder, increased niobium powder mobility, improved the physical property of niobium powder, can not change the thing phase of niobium powder simultaneously, be conducive to the application that powder is compact formed and sintering, 3D print high-performance niobium goods, dense coating etc., and with low cost, can obtain very high technical value added.Compare with other patent about niobium alloy powder nodularization, the pure niobium powder fusing point that the present invention adopts is very high, has improved purity, and have certain spheroidizing of powder productivity when the niobium sphere of powder.
Brief description of the drawings
Fig. 1 is the process chart of the spherical niobium powder of preparation.
Fig. 2 is the scanning electron microscope (SEM) photograph that adopts the former powder of-200 order niobium in embodiment 1.
Fig. 3 adopts the scanning electron microscope (SEM) photograph after the former sphere of powder of-200 order niobium in embodiment 1.
Fig. 4 is the contrast of the XRD diffraction spectra before and after spheroidizing of powder in embodiment 1.
Fig. 5 adopts the scanning electron microscope (SEM) photograph after the former sphere of powder of-300 order niobium in embodiment 2.
Detailed description of the invention
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail.But those skilled in the art understand, and the present invention is not limited thereto.Any improvement of making on basis of the present invention and variation, all within protection scope of the present invention.
Prepare a method for minute spherical niobium powder, as shown in Figure 1, it carries out flow process in the steps below successively:
1, set up the argon plasma torch of stable operation: 40～60slpm continues argon gas stream to plasma reactor input, induction coil loads high voltage, voltage can be 6～8KV, igniter electric discharge simultaneously, coil inductively coupled and the igniter corona of high-voltage line triggers, and makes argon gas ionization produce argon plasma torch.Now make to keep negative pressure state in whole plasma reactor, can ensure plasma torch stable operation.
2, utilize and carry gas by the core high-temperature region heating of metal niobium powder (former powder) injection argon plasma torch.Carry gas can use argon gas, hydrogen etc. in hot environment not with the gas of metal-powder generation chemical reaction.Niobium pruinescence is sent into the core high-temperature region of plasma torch, absorbs a large amount of heats, and particle surface starts fusing, due to capillary effect, forms the very high niobium powder particles of sphericity.
3, the niobium powder particles drop cooling curing after heating and melting is formed to spherical niobium powder.Niobium powder particles drop leaves after plasmatorch, in high thermograde (10
-6) under rapidly cooling, enter heat-exchanging chamber quenching and solidify, thereby form spherical particle.
4, gas is detached, collect spherical niobium powder.After nodularization process completes, gas is detached, processes discharge, nodularization powder enters collection storage tank, and automatic gauge is collected.Finally carry out vacuum packaging.
Embodiment 1:
Taking 200 object niobium powder as raw material, when the operation of nodularization process stabilization, the high voltage loading on induction coil is 7.8KV, and Ar reacting gas input flow rate is 40slpm, protection gas 75slpm, and system internal gas pressure is 0.04MPa; Carrying gas control flow is 1slpm, and niobium powder feeding control flow is 19g/min.After nodularization, obtain the spherical niobium powder of 200 object.
Fig. 2 is the irregular particle microstructure of raw material niobium powder, and particle has polygon corner angle.
Fig. 3 is spherical niobium powder microstructure figure prepared by embodiment 1.As shown in Figure 3, the niobium powder particles nodularization rate of preparation is high, good sphericity, any surface finish.
Fig. 4 is that spherical niobium powder thing prepared by embodiment 1 is tested (XRD) mutually, with former powder contrast.As shown in Figure 4, (Fig. 4 a) mates with Nb powder standard diffraction maximum the front powder of spheroidising, there is no other material diffraction maximums.The characteristic diffraction peak of (b), the X-ray diffraction position of Nb powder does not change Fig. 4, is still (110), (200), (211)) after plasma nodularization is processed, crystal structure is single Nb phase.In this explanation the present invention, the high temperature of plasma does not affect the thing phase of powder.
Embodiment 2:
Taking 300 object niobium powder as raw material, when the operation of nodularization process stabilization, the high voltage loading on induction coil is 11.5KV, and Ar reacting gas input flow rate is 25slpm, protection gas 120slpm, and system internal gas pressure is 0.05MPa; Carrying gas control flow is 1slpm, and niobium powder feeding control flow is 30g/min.After nodularization, obtain the spherical niobium powder of 300 object, ESEM is as Fig. 5.
Fig. 5 is spherical niobium powder microstructure figure prepared by embodiment 2.As shown in Figure 5, the niobium powder particles nodularization rate of preparation is high, good sphericity, any surface finish.
The raw material niobium powder using in the microstructure of the raw material niobium powder using in embodiment 2 and embodiment 1 is similar, is irregular particle, and particle has polygon corner angle.
Claims (8)
1. a preparation method for spherical niobium powder, the method comprises the following steps:
1) form stable argon plasma torch;
2) by carrying gas, former metal niobium powder is sent to the high-temperature region of plasma torch, niobium powder is heated, and forms particle drop;
3) niobium powder particles drop leaves after plasma area, and cooling curing forms spheric granules powder;
4) collect spherical niobium powder.
2. preparation method as claimed in claim 1, wherein, step 1) described in argon plasma torch in high frequency plasma reactor, form.
3. preparation method as claimed in claim 2, wherein, forming the needed reacting gas of argon plasma torch (Ar) input flow rate is 40～60slpm, the high voltage loading on induction coil is 6～8KV.
4. preparation method as claimed in claim 2; wherein; reacting gas (Ar) input flow rate when described argon plasma stable operation is 20～50slpm, and protective gas (Ar) input flow rate is 30～120slpm, and internal system air pressure is 0.03～0.06MPa.
5. the preparation method as described in claim 1-4 any one, wherein said step 2) in, described in carry gas can use argon gas, hydrogen etc. in hot environment not with the gas of metal-powder generation chemical reaction.
6. the preparation method as described in claim 1-5 any one, wherein said step 2) in, the average grain diameter of the former powder of metal niobium adding is 0.5～45 μ m, and carrying gas control flow is 0.5～5slpm, and niobium powder feeding control flow is 5～50g/min.
7. the preparation method as described in claim 1-6 any one, wherein said step 3) in, niobium powder particles drop leaves after plasma torch, rapidly cooling, enter heat-exchanging chamber quenching and solidify, under capillary effect, form spherical particle.
8. the preparation method as described in claim 1-7 any one, wherein said step 4) in, spherical niobium powder collected with collector.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105522161A (en) * | 2015-12-25 | 2016-04-27 | 中国科学院重庆绿色智能技术研究院 | Rapid large-scale preparing method for small-grain-size spherical powder for 3D printing |
| CN105537602A (en) * | 2015-12-25 | 2016-05-04 | 中国科学院重庆绿色智能技术研究院 | Rapid large-scale preparing method for spherical ultra-high-temperature alloy powder for 3D printing |
| CN108247072A (en) * | 2016-12-29 | 2018-07-06 | 江民德 | A kind of method that spherical 3D printing powder is prepared using plasma |
| CN108500281A (en) * | 2018-05-03 | 2018-09-07 | 宁夏东方钽业股份有限公司 | Spherical tantalum, niobium and tantalum-niobium alloy powder, and preparation method thereof and its purposes in 3D printing and medical instrument |
| CN109092514A (en) * | 2018-07-25 | 2018-12-28 | 信阳核工业新材料有限公司 | A kind of preparation method of high fluidity silica flour |
| WO2020123265A1 (en) * | 2018-12-12 | 2020-06-18 | Global Advanced Metals Usa, Inc. | Spherical niobium alloy powder, products containing the same, and methods of making the same |
| CN111545766A (en) * | 2020-06-23 | 2020-08-18 | 柯良节 | Equipment and method for preparing high-purity spherical metal powder |
| CN113800522A (en) * | 2021-09-27 | 2021-12-17 | 星尘科技(广东)有限公司 | Method for preparing high-purity compact tungsten carbide-cobalt composite spherical powder material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105522161A (en) * | 2015-12-25 | 2016-04-27 | 中国科学院重庆绿色智能技术研究院 | Rapid large-scale preparing method for small-grain-size spherical powder for 3D printing |
| CN105537602A (en) * | 2015-12-25 | 2016-05-04 | 中国科学院重庆绿色智能技术研究院 | Rapid large-scale preparing method for spherical ultra-high-temperature alloy powder for 3D printing |
| CN108247072A (en) * | 2016-12-29 | 2018-07-06 | 江民德 | A kind of method that spherical 3D printing powder is prepared using plasma |
| CN108500281A (en) * | 2018-05-03 | 2018-09-07 | 宁夏东方钽业股份有限公司 | Spherical tantalum, niobium and tantalum-niobium alloy powder, and preparation method thereof and its purposes in 3D printing and medical instrument |
| CN109092514A (en) * | 2018-07-25 | 2018-12-28 | 信阳核工业新材料有限公司 | A kind of preparation method of high fluidity silica flour |
| WO2020123265A1 (en) * | 2018-12-12 | 2020-06-18 | Global Advanced Metals Usa, Inc. | Spherical niobium alloy powder, products containing the same, and methods of making the same |
| CN113165066A (en) * | 2018-12-12 | 2021-07-23 | 全球先进金属美国股份有限公司 | Spherical niobium alloy powder, product containing same, and method for producing same |
| CN111545766A (en) * | 2020-06-23 | 2020-08-18 | 柯良节 | Equipment and method for preparing high-purity spherical metal powder |
| CN113800522A (en) * | 2021-09-27 | 2021-12-17 | 星尘科技(广东)有限公司 | Method for preparing high-purity compact tungsten carbide-cobalt composite spherical powder material |
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Application publication date: 20141008 |