CN86107657A - The production method of purification of spherical Niobium Pentxoxide - Google Patents
The production method of purification of spherical Niobium Pentxoxide Download PDFInfo
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- CN86107657A CN86107657A CN 86107657 CN86107657A CN86107657A CN 86107657 A CN86107657 A CN 86107657A CN 86107657 CN86107657 CN 86107657 CN 86107657 A CN86107657 A CN 86107657A CN 86107657 A CN86107657 A CN 86107657A
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Abstract
A kind of production purification process of Niobium Pentxoxide specifically is applicable to the production method of the Niobium Pentxoxide that monolithic ceramic capacitor is used.Industrial standards level niobium hydroxide after pickling, washing, more than 0.5 hour, is preferably in 550～650 ℃ of calcinings 2.5～4.0 hours in 500～750 ℃ temperature lower calcinations.The apparent particle form of the Niobium Pentxoxide of producing is globular-Nb
2O
5, be applicable to raw material as niobium-containing monolith ceramic capacitor.The electrical property of the monolithic ceramic capacitor that produces with this kind Niobium Pentxoxide is good.The flow process and the equipment of this processing method are simple, less investment, and constant product quality, cost is low.
Description
The present invention relates to the production purification process of Niobium Pentxoxide, more specifically saying so is applicable to the producing and manufacturing technique of the spherical Niobium Pentxoxide of using as the monolithic ceramic capacitor raw material.
Development along with circuit integration, for " outer paste " element in miniaturization, the requirement of high reliability aspect is more and more higher, and wherein electrical condenser is the main positions that accounts for composed component, is element likely at monolithic ceramic capacitor aspect the realization miniaturization, and its volume is 1/200～1/1000 of a monolithic ceramic capacitor, the characteristics of monolithic ceramic capacitor are that volume is little, capacity is big, insulativity is high, and nonpolarity, can be used in high frequency, can make the product of all temps coefficient.Because of electrode in ceramic dielectic inside, wet fastness is good, reliability is high, low price.Therefore, monolithic ceramic capacitor is a rising kind, and it has obtained using widely as the peripheral product of unicircuit.Both at home and abroad all at a large amount of development monolithic ceramic capacitors, particularly niobium-containing monolith ceramic capacitor.Niobium Pentxoxide is one of main raw material of making niobium-containing monolith ceramic capacitor.
The existing processing method of producing Niobium Pentxoxide is with tantalum-niobium concentrate, under the temperature about 100 ℃, decompose with hydrofluoric acid, sulfuric acid as ildefonsite, the aqueous solution that contains the tantalum niobium after the decomposition or contain the ore pulp organic solvent of tantalum niobium, as methyl iso-butyl ketone (MIBK), secondary octanol, dibutyl acetamide the fluoro complex of niobium tantalum is extracted in the organic phase and with other impurity element, as separation such as iron, manganese, aluminium, tungsten, molybdenum, silicon, tin.In order to remove the small amount of impurities element of bringing in the extraction process in the organic solvent, wash organic phase with sulphuric acid soln, make a spot of impurity element change aqueous phase again over to.The organic phase that contains tantalum niobium fluoro complex after washing is stripped into water with dilute sulphuric acid with the niobium fluoro complex in the organic phase.But when reextraction niobium fluoro complex, a spot of tantalum fluoro complex also enters and contains the niobium aqueous phase, uses the organic solvent extraction little tantalum for this reason again, and separates fully with niobium.Through precipitating with ammoniacal liquor or ammonia with the complete isolating niobium fluoro complex aqueous solution that contains of tantalum, control PH7～8 when precipitating, the moisture niobium hydroxide that is precipitated out makes the solid hydrogen niobium oxides separate with its mother liquor with filter methods such as vacuum filtration or filter presss.The moisture niobium hydroxide of separating is calcined more than 6 hours with pure water washing back in 800～1000 ℃.Niobium Pentxoxide after the calcining generally is sheet β-Nb2O5 or sheet β+γ ' Nb2O5 crystal, the foreign matter content height, this Niobium Pentxoxide is that tabular crystal is unfavorable for the contact between the various raw materials of monolithic ceramic capacitor porcelain, influence the sosoloidization of ceramics, not good with the monolithic ceramic capacitor electrical property that this kind Niobium Pentxoxide is made as raw material, often do not meet the specification standards of monolithic ceramic capacitor, and cause waste.
Russian patent document 552296 has been introduced the method for purified hydrogen niobium oxides, tantalum hydroxide, can remove impurity fluorine wherein.This method is with the solution washing niobium hydroxide that contains aluminium salt, and the aqueous solution of aluminium salt contains aluminium 10～20 grams per liters, and the solid-to-liquid ratio during washing is 1: 5-15 can make that fluorine content is reduced to 0.03～0.04% in the niobium hydroxide.
Another piece russian patent document 891566 has been introduced the processing method of producing high-purity Niobium Pentxoxide, its method is that niobium hydroxide is placed pure water, adding oxalic acid again is heated to niobium hydroxide and dissolves fully, filtered while hot, cooling separates the crystallization of solid niobium oxalate with its mother liquor, wash above-mentioned crystallization with the ethanolic soln of oxalic acid after, carried out thermolysis 1～3 hour in 800～900 ℃, the Niobium Pentxoxide that this explained hereafter goes out can be used as the raw material of opticglass.
А. И. Н и к о л а e в etc. proposed the pyrohydrolytic method purify niobium and tantalum oxyhydroxide method (А. И. Н и к о л а e в, Ж у р н а л п р и к л а д н-о й х и м и и, No7,1631～1634,1983), this method is to calcine in 300～800 ℃ in the presence of water vapour, and the content of impurity such as fluorine, phosphorus, sulphur, carbon in the oxyhydroxide of niobium and tantalum is reduced.
The Japanese documentation spy opens clear 58-156537 and has proposed to feed water vapor in 500～1200 ℃ temperature range, and the fluorine niobium oxides is carried out the processing method that thermal hydrolysis is produced Niobium Pentxoxide.
The method technology of the purified hydrogen niobium oxides that russian patent document 552296 proposes is simple, can reduce the fluorine content in the Niobium Pentxoxide, but will consume a large amount of aluminium salt, has increased the cost of product, makes again that the content of impurity aluminum increases in the product.Russian patent document 891566 can make foreign matter contents such as iron in the Niobium Pentxoxide, manganese, copper, cobalt, calcium reduce greatly, but consume a large amount of expensive oxalic acid and alcohol, increased cost, the temperature of calcining Niobium Pentxoxide is higher, consumed power is big, and the rate of recovery of niobium is very low.The purify technology of oxyhydroxide of niobium and tantalum of pyrohydrolytic method can be removed fluorine effectively, has reduced impurity such as fluorine, phosphorus, sulphur, carbon, but can not reduce the content of impurity such as heavy metal, calcium, magnesium, and needed comparatively complex apparatus.
In order to work out the producing and manufacturing technique that is applicable to the Niobium Pentxoxide of using as monolithic ceramic capacitor, studied the influence of the crystalline phase, appearance of foreign matter content in the Niobium Pentxoxide and Niobium Pentxoxide, found to meet following standard: manganese＜0.015%, aluminium＜0.014%, iron＜1.0%, carbon＜0.1% as the foreign matter content in the Niobium Pentxoxide of monolithic ceramic capacitor raw material to the monolithic ceramic capacitor electrical property; The crystal of Niobium Pentxoxide is pseudo-hexagonal system (being commonly called as alpha-crystal), apparent particle form with spherical be good.With the Niobium Pentxoxide that meets above-mentioned specification is that the electrical property of the monolithic ceramic capacitor made of raw material is good, and stable.
The objective of the invention is to work out a producing and manufacturing technique that is fit to do the Niobium Pentxoxide that the monolithic ceramic capacitor raw material uses, foreign matter content, crystalline form, apparent particulate form in the Niobium Pentxoxide of producing with this processing method meet the requirement as the raw material of monolithic ceramic capacitor, and steady quality.Good with it as the monolithic ceramic capacitor electrical property.Another object of the present invention is the processing method of this production Niobium Pentxoxide of working out, and it is simple that flow process and equipment thereof are wanted, and the cost of product is low.
The present invention is a kind of processing method of producing the purification Niobium Pentxoxide, is raw material with the niobium hydroxide, and with the niobium hydroxide diluted mineral acid, pure water with after its pickling, the washing, is calcined successively, and the incinerating temperature is 500～750 ℃, and the incinerating time was greater than 0.5 hour.
For the number of times that reduces pickling preferably method be to be raw material with industrial standards level niobium hydroxide, the content of Niobium Pentxoxide＞84.0% in the niobium hydroxide.At first, under the situation of heat tracing, carry out pickling with diluted mineral acid in proportion,, accelerate removing of impurity element, reduce the pickling number of times to increase the efficient of pickling.Use known filtration method of person of ordinary skill in the field or siphonage with solid-liquid separation after the pickling.Because the niobium hydroxide after the solid-liquid separation still contains small amounts of inorganic acid, so must use pure water, for example distilled water or deionized water wash, to remove the small amounts of inorganic acid in the niobium hydroxide.For washing is carried out smoothly, increase washing efficiency, in water washing process, be good with heat tracing.
Used diluted mineral acid can be any acid in nitric acid, hydrochloric acid, the sulfuric acid during pickling.When niobium hydroxide carried out pickling with any diluted mineral acid in nitric acid, hydrochloric acid, the sulfuric acid, its concentration was controlled at 3～8%(percent by volume) for good.Used 3～8%(percent by volume during pickling) acid solution amount for the per kilogram niobium hydroxide with 5～10 liters, for well.
Preferably under heat tracing, stir during pickling, the temperature of heat tracing is 60～100 ℃, the time that heat tracing stirs is 20～50 minutes, after the pickling with the known filtration method of affiliated technical field technician or siphonage with solid-liquid separation, the number of times of pickling is by content, the kind of the used acid of pickling, the concentration of impurity in the niobium hydroxide raw material, whether factor decision such as heated and stirred and filtering mode during pickling.Niobium hydroxide after pickling needs to use pure water, and for example distilled water or deionized water are washed niobium hydroxide, and the per kilogram niobium hydroxide need the pure water amount be 5～10 liters during washing.Pure water can be distilled water or deionized water.Heat tracing stirs 20～50 fens better in water washing process, and the temperature of heat tracing is 60～100 ℃.The purpose of washing mainly is to remove the adsorbed acid of niobium hydroxide in the acid cleaning process.The pH value that is washed to the suspension of niobium hydroxide reaches 7～8.Niobium hydroxide after the washing carries out solid-liquid separation with known filter method of person of ordinary skill in the field or siphonage.
In acid cleaning process, in the used mineral acid, be best with nitric acid.Carry out the number of times that pickling can reduce washing with nitric acid, often make with hydrochloric acid, when sulfuric acid carries out pickling that impurity such as chlorine, sulphur increases in the Niobium Pentxoxide.The concentration of used nitric acid is 4～7%(percent by volume preferably), the amount of the salpeter solution used 4～7%(percent by volume of per kilogram niobium hydroxide) is 6～8 liters, preferably 25～35 minutes time that heat tracing stirs during pickling, the temperature of heat tracing is preferably 85～95 ℃.
During washing, it is 6～8 liters that the per kilogram niobium hydroxide needs the pure water amount, and pure water can be distilled water or deionized water, and preferably 25～35 minutes time that heat tracing stirs, the temperature during heat tracing is preferably 85～95 ℃.The mode that how much depends on solid-liquid separation of number of times of washing and the degree of solid-liquid separation, solid-liquid separation must be good more, and washing times is few more, and washing times is three times usually, all adopts the identical operations condition three times.
Niobium hydroxide after overpickling, washing are handled is calcined, the incinerating temperature is controlled at 500～750 ℃, calcining temperature is lower than 500 ℃, can not generate the Niobium Pentxoxide of α-crystal formation, and major part still exists with the form of niobium hydroxide and amorphous Niobium Pentxoxide.Calcining temperature is higher than 750 ℃, then generates β-Nb2O5 crystal formation or β+γ '-Nb2O5 crystal formation.Calcining the required time is more than 0.5 hour, and calcination time was less than 0.5 hour, and the composition brought into play in the Niobium Pentxoxide can not be got rid of fully; Long for example 8 hours of calcination time, the waste that will inevitably bring the energy.Calcining temperature during calcining preferably is controlled at 550～650 ℃, forges to be preferably 2.5～4.0 hours combustion time.
The crystalline phase of the Niobium Pentxoxide of producing with production purification process of the present invention is pseudo-hexagonal system (being commonly called as alpha-crystal), apparent particulate form is spherical, not only being suitable for as lead magnoniobate is the raw material of ceramic condenser, equally also is applicable to as niobium iron acid lead system and other to contain the raw material of niobium ceramic condenser system.
The observation photographic means of the apparent particulate form of crystal is that the Niobium Pentxoxide powder is put in the spirit solvent, with ultrasonic dispersing about 20～30 minutes, get the spirituous solution of a Niobium Pentxoxide powder then, drop on the copper seat of polishing, alcohol volatilization back Niobium Pentxoxide powder is dispersed on the copper seat, with ion sputtering instrument metal spraying on the copper seat that has Niobium Pentxoxide, thickness is hundreds of to one thousand dusts again, is placed at last to observe on the JSM-840 scanning electron microscope and photograph.The observation of the apparent particulate form of the Niobium Pentxoxide powder of producing with production purification process of the present invention the results are shown in Figure 1.
Fig. 1. the apparent particulate form of the Niobium Pentxoxide powder of producing with method of the present invention
The JSM-840 scanning electron microscope
Acceleration voltage: 15KV
Magnification: 8500(* 0.6)
Fig. 2. the X diffractogram of the Niobium Pentxoxide of the pseudo-hexagonal system of producing with method of the present invention (being commonly called as alpha-crystal)
The full-automatic diffractometer of APD-10, target: CuK α voltage: 40KV electric current: 20MA
Chart speed: 1mm/1 °
Fig. 3. the mode of appearance of the Niobium Pentxoxide powder among the comparative example
The JSM-840 scanning electron microscope
Acceleration voltage 15KV, magnification: 720
The Niobium Pentxoxide of producing with production purification process of the present invention is carried out the X diffraction analysis, and its diffractogram is seen Fig. 2, and the Niobium Pentxoxide that production purifying technique as can be seen from Figure 2 of the present invention is produced is pseudo-hexagonal system (being commonly called as α-crystal formation)
The content chemical gauging of impurity element in the Niobium Pentxoxide, wherein the content of carbon, sulphur is measured with burning-infra-red method.
Advantage of the present invention is: the first, the Niobium Pentxoxide of being produced with production purification process of the present invention is pseudo-hexagonal system, and apparent particulate form is spherical, and the content of its impurity meets the ingredient requirement of making monolithic ceramic capacitor fully; The apparent particulate form of Niobium Pentxoxide powder is spherical, helps the contact between each raw material in the porcelain of monolithic ceramic capacitor and the solutionizing of ceramics; Each batch of Niobium Pentxoxide constant product quality of producing with production purification process of the present invention, with this Niobium Pentxoxide is that the electrical property of the monolithic ceramic capacitor that comes out of raw material production is good, specific inductivity is between 7300～8200, reached the desired index of low frequency monolithic ceramic capacitor fully, insulation resistance, normal temperature dielectric loss tg δ and tide back dielectric loss tg δ H
2The index of O has all surpassed set quota.The Niobium Pentxoxide of producing with producing and manufacturing technique of the present invention is that the concrete data of the electrical property of the monolithic ceramic capacitor made of raw material see Table one.
The second, the flow process and the equipment of production purification process of the present invention are all simple, and facility investment is little, and the industrial chemicals consumption is little, low price, and the incinerating time is short, and temperature is low, saves energy in a large number, product cost is low, and quality is high and stablize the rate of recovery height of niobium.
More specifically describe the present invention with following non-limiting examples, protection scope of the present invention is not subjected to the qualification of these embodiment.
Embodiment 1.
With 0.1 kilogram of (Ningxia Non-Ferrous Metal Smeltery of industrial standards level niobium hydroxide, down with) and 5% salpeter solution (percent by volume, the Beijing Chemical Plant, chemical pure, down with) 0.8 liter, put into 1 liter glass beaker,, filter after 25 minutes in 90 ℃ of heated and stirred, add 0.7 liter of deionized water, in 90 ℃ of heated and stirred 25 minutes, filter.Carry out three washings with above-mentioned same formality, the niobium hydroxide of washing after three times places evaporating dish, puts into the retort furnace calcining, and calcining temperature is 600 ℃, calcines two hours.The Niobium Pentxoxide that generates is an alpha-crystal, and apparent particulate form is spherical, and the lead magnoniobate made from this Niobium Pentxoxide is that the electrical property of low frequency monolithic ceramic capacitor sees Table one.Foreign matter content in the Niobium Pentxoxide is as follows: Fe0.40%, Si＜0.05%, Al＜0.01%, Sn＜0.001%, Ti＜0.01%, W＜0.01%, Mo＜0.01%, the content of the Nb2O5 in the Niobium Pentxoxide＞98.0%.
Embodiment 2.
With 0.7 liter of the salpeter solution of 0.1 kilogram of industrial standards level niobium hydroxide and 4%, put into 1 liter glass beaker,, filter after 30 minutes in 90 ℃ of heated and stirred.Add 0.8 liter of distilled water, after 30 minutes, filter in 85 ℃ of heated and stirred.Carry out three washings with above-mentioned same formality.The niobium hydroxide of washing after three times places evaporating dish, put into the retort furnace calcining, calcining temperature is 580 ℃, calcined 3 hours, the Niobium Pentxoxide that generates is an alpha-crystal, apparent particulate form is spherical, and the lead magnoniobate made from this Niobium Pentxoxide is that the electrical property of low frequency monolithic ceramic capacitor sees Table one.
Embodiment 3.
Salpeter solution (percent by volume) 0.64 lifting of 0.08 kilogram of industrial standards level niobium hydroxide and 7% gone in 1 liter the glass beaker, after 30 minutes, filter in 85 ℃ of heated and stirred.Add 0.6 liter of deionized water,, filter in 85 ℃ of heated and stirred 30 minutes.Carry out three washings with above-mentioned same formality.The niobium hydroxide of washing after three times places evaporating dish, put into the retort furnace calcining, calcining temperature is 650 ℃, calcined 2.5 hours, the Niobium Pentxoxide that generates is an alpha-crystal, apparent particulate form is spherical, and the lead magnoniobate made from this Niobium Pentxoxide is that the electrical property of low frequency monolithic ceramic capacitor sees Table one.
Embodiment 4.
With 0.7 liter of the hydrochloric acid soln (percent by volume, Beijing Chemical Plant, chemical pure) of 0.080 kilogram of industrial standards level niobium hydroxide and 5%,, filter in 90 ℃ of heated and stirred 25 minutes.Add 0.8 liter of deionized water,, filter in 85 ℃ of heated and stirred 30 minutes.Carry out four washings with above-mentioned same formality, the niobium hydroxide of washing after four times places evaporating dish, puts into the retort furnace calcining, and calcining temperature is 600 ℃, calcination time 3.0 hours.Calcining back gained Niobium Pentxoxide is an alpha-crystal, and apparent particulate form is spherical, and the lead magnoniobate made from this Niobium Pentxoxide is that the electrical property of low frequency monolithic ceramic capacitor sees Table one.
Embodiment 5.(comparative example)
With industrial standards level niobium hydroxide, at 900 ℃, to calcine 4 hours, the Niobium Pentxoxide that obtains is β+γ ' crystal, mode of appearance is a sheet, sees Fig. 3.
The lead magnoniobate made from this Niobium Pentxoxide is that the electrical property of low frequency monolithic ceramic capacitor sees Table one.
Table one. the lead magnoniobate that the Niobium Pentxoxide that obtains among each embodiment is made
It is the electrical property of low frequency monolithic ceramic capacitor
Claims (8)
1, a kind of processing method of producing the purification Niobium Pentxoxide is a raw material with the niobium hydroxide, and feature of the present invention is, niobium hydroxide diluted mineral acid, pure water successively with its pickling, after the washing, are calcined, the incinerating temperature is 500～750 ℃, and the incinerating time was greater than 0.5 hour.
According to a kind of processing method of producing the purification Niobium Pentxoxide of claim 1, it is characterized in that 2, said diluted mineral acid is any acid in nitric acid, hydrochloric acid, the sulfuric acid.
According to a kind of processing method of producing the purification Niobium Pentxoxide of claim 1, it is characterized in that 3, the pure water of said washing usefulness is distilled water or deionized water.
4, according to a kind of processing method of producing the purification Niobium Pentxoxide of claim 2, it is characterized in that, the concentration of any acid in nitric acid, hydrochloric acid, the sulfuric acid is 3～8%(percent by volume) temperature of pickling is 60～100 ℃, the per kilogram niobium hydroxide is 5～10 liters with the acid solution amount.
According to a kind of processing method of producing the purification Niobium Pentxoxide of claim 1, it is characterized in that 5, the temperature that washing keeps is 60～100 ℃, the per kilogram niobium hydroxide is 5～10 liters with the pure water amount.
6, according to a kind of processing method of producing the purification Niobium Pentxoxide of claim 4, it is characterized in that, the concentration of said nitric acid is 4～7%(percent by volume), the temperature of pickling is 85～95 ℃, the per kilogram niobium hydroxide is 6～8 liters with 4～7% salpeter solution amount.
According to a kind of processing method of producing the purification Niobium Pentxoxide of claim 5, it is characterized in that 7, the temperature during washing is 85～95 ℃, per kilogram hydroxide two niobiums are 6～8 liters with the pure water amount.
According to a kind of processing method of producing the purification Niobium Pentxoxide of claim 1, it is characterized in that 8, said calcining temperature is 550～650 ℃, calcination time is 2.5～4.0 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86107657A CN86107657B (en) | 1986-11-11 | 1986-11-11 | Production for sphare niobium pentoxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86107657A CN86107657B (en) | 1986-11-11 | 1986-11-11 | Production for sphare niobium pentoxide |
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| Publication Number | Publication Date |
|---|---|
| CN86107657A true CN86107657A (en) | 1987-12-09 |
| CN86107657B CN86107657B (en) | 1988-01-13 |
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ID=4803631
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86107657A Expired CN86107657B (en) | 1986-11-11 | 1986-11-11 | Production for sphare niobium pentoxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336439A (en) * | 2011-08-30 | 2012-02-01 | 宜春市金洋稀有金属有限公司 | Production method and device for tantalum niobium oxides |
| CN102424420A (en) * | 2011-09-15 | 2012-04-25 | 宜春市金洋稀有金属有限公司 | Method for preparing niobium pentoxide by using ferrocolumbium as raw material |
| CN102465204A (en) * | 2010-11-16 | 2012-05-23 | 肇庆多罗山蓝宝石稀有金属有限公司 | Method for preparing niobium pentoxide with high apparent density |
| CN102603002A (en) * | 1998-09-16 | 2012-07-25 | 卡伯特公司 | Methods to partially reduce a niobium metal oxide and oxygen reduced niobium oxides |
| CN107055613A (en) * | 2017-02-27 | 2017-08-18 | 湖南工业大学 | One kind is without substrate niobium pentoxide nano chip arrays negative material and its preparation method and application |
| CN110697775A (en) * | 2019-11-08 | 2020-01-17 | 广东广晟稀有金属光电新材料有限公司 | Preparation method of low-nitrogen niobium hydroxide |
| CN116102065A (en) * | 2023-02-20 | 2023-05-12 | 河北东同光电科技有限公司 | Preparation method of high-purity niobium pentoxide superfine powder |
-
1986
- 1986-11-11 CN CN86107657A patent/CN86107657B/en not_active Expired
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603002A (en) * | 1998-09-16 | 2012-07-25 | 卡伯特公司 | Methods to partially reduce a niobium metal oxide and oxygen reduced niobium oxides |
| CN102465204A (en) * | 2010-11-16 | 2012-05-23 | 肇庆多罗山蓝宝石稀有金属有限公司 | Method for preparing niobium pentoxide with high apparent density |
| CN102336439A (en) * | 2011-08-30 | 2012-02-01 | 宜春市金洋稀有金属有限公司 | Production method and device for tantalum niobium oxides |
| CN102424420A (en) * | 2011-09-15 | 2012-04-25 | 宜春市金洋稀有金属有限公司 | Method for preparing niobium pentoxide by using ferrocolumbium as raw material |
| CN102424420B (en) * | 2011-09-15 | 2013-07-31 | 宜春市金洋稀有金属有限公司 | Method for preparing niobium pentoxide by using ferrocolumbium as raw material |
| CN107055613A (en) * | 2017-02-27 | 2017-08-18 | 湖南工业大学 | One kind is without substrate niobium pentoxide nano chip arrays negative material and its preparation method and application |
| CN110697775A (en) * | 2019-11-08 | 2020-01-17 | 广东广晟稀有金属光电新材料有限公司 | Preparation method of low-nitrogen niobium hydroxide |
| CN116102065A (en) * | 2023-02-20 | 2023-05-12 | 河北东同光电科技有限公司 | Preparation method of high-purity niobium pentoxide superfine powder |
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| Publication number | Publication date |
|---|---|
| CN86107657B (en) | 1988-01-13 |
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