CN108689422A - A kind of large-specific surface area nano gadolinium oxide raw powder's production technology - Google Patents
A kind of large-specific surface area nano gadolinium oxide raw powder's production technology Download PDFInfo
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- CN108689422A CN108689422A CN201810568422.7A CN201810568422A CN108689422A CN 108689422 A CN108689422 A CN 108689422A CN 201810568422 A CN201810568422 A CN 201810568422A CN 108689422 A CN108689422 A CN 108689422A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01P2004/01—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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention belongs to Nano Rare-earth Materials preparation fields, specifically provide a kind of large-specific surface area nano gadolinium oxide raw powder's production technology.Steps are as follows:Inorganic salt solution containing gadolinium is uniformly mixed with surfactant, precursor solution is made, precursor solution pH value is adjusted to 3.5-4 with sodium carbonate liquor, the pH value of precursor solution is adjusted to 8.5-9.5 with deployed high purity sodium hydroxide solution again, pass through filtration washing, dry, the gadolinium oxide particle diameter of nanometer powder obtained after 700-850 DEG C of high-temperature calcination is 30-60nm, BET:50-60 is evenly distributed.
Description
Technical field
The invention belongs to Nano Rare-earth Materials preparation field, more particularly to a kind of large-specific surface area nano gadolinium oxide powder
Preparation method.
Background technology
The preparation of nano-ceramic powder is the matter of utmost importance of nano ceramic material nanometer material industry related to other, main
Preparation method is wanted to have solid phase method, liquid phase method and vapor phase method.Since the 1990s, nano-ceramic powder enters industrialization hair
The exhibition stage.China mainly uses wet chemistry method and vapour deposition process to carry out the preparation of industrialized nano ceramic powder at present, mainly
Product includes CaCO3,ZnO,Al2O3,SiOx,TiO2,Si3N4With SiC etc..
Nano oxidized gadolinium powder can be used for various fluorescent powders, the neutron absorber material in atomic pile, and magnetic bubble material increases
Feel screen material.Also there is certain application in optical glass, electronics industry etc., it is also possible to make Gd-Ga garnet material.
The technique for preparing nano oxidized gadolinium powder at present all has that the common precipitation method need to use ammonium salt
As precipitating reagent, ammonium ion has pollution to environment, to ammonium ion handle and can increase cost, while easily being made when high-temperature calcination
Become larger at particle, specific surface area is less than normal, easy there are the second equal dephasigns;The methods of hydro-thermal method, sol-gal process, product has
Chemical composition is accurate, even particle distribution, but yield is less than normal, cannot accomplish to produce in batches.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation sides of large-specific surface area nano gadolinium oxide powder
Method.Specific technical solution is as follows:
A kind of large-specific surface area nano gadolinium oxide raw powder's production technology, including steps are as follows:
(1) inorganic salt solution containing gadolinium is prepared:It is prepared deionized water is added in high-purity inorganic salt solution containing gadolinium
At the inorganic salt solution containing gadolinium of 0.2-0.4mol/l concentration;
(2) surfactant is added in the inorganic salt solution containing gadolinium in step (1), is fully mixed to uniformly, system
Obtain precursor solution;Wherein, surfactant is by absolute ethyl alcohol, polyethylene glycol 2000 and neopelex group in proportion
At.
The present invention is using absolute ethyl alcohol as decentralized medium, and polyethylene glycol 2000, neopelex are as main
Dispersant can pass through hydrogen due to containing a large amount of ehter bonds and hydroxyl in polyethylene glycol with the hydroxyl on nano oxidized gadolinium hydrate surface
Key is connected, and makes nano oxidized one layer of PEG protective layer of gadolinium hydrate adsorption, to improve the space bit between nano-particle
Resistance alleviates agglomeration dry, between calcination stage nano-particle;Neopelex can improve reaction emulsion
In it is various constitute phases between surface tension, be allowed to form uniform and stable dispersion;In polyethylene glycol 2000 and dodecane
Under the synergistic effect of base benzene sulfonic acid sodium salt, help to prepare bigger serface gadolinium oxide powder.
(3) precursor solution pH value is adjusted to 3.5-4 with deployed sodium carbonate liquor;
(4) pH value of precursor solution 8.5-9.5 is adjusted to deployed high purity sodium hydroxide solution again fully to stir
After mixing, ageing obtains the presoma gadolinium hydroxide gel of gadolinium oxide;
(5) after plate compression, the gadolinium hydroxide gel that step (4) obtains is washed by deionized water, in vacuum
Under the conditions of it is dry;
Free water and the crystallization water can have an impact the uniformity of particle in calcination process, while crystal grain can be made to grow up,
Defect is formed therefore first to be dried in vacuo before being calcined to remove free water and the crystallization water.
(6) it the product after drying is put into high-temperature electric resistance furnace 700 DEG C~850 DEG C calcines and keeps the temperature 3-5h and obtain Large ratio surface
The nano oxidized gadolinium powder of product.
As a preference of the present invention, the inorganic salts containing gadolinium described in step (1), can be in gadolinium chloride or gadolinium nitrate
A kind of or gadolinium chloride and gadolinium nitrate are with 1:The mixture of 1 mass ratio mixing;
As a preference of the present invention, the mass ratio of the surfactant and gadolinium oxide described in step (2) is mass ratio is
0.075-0.085:1, absolute ethyl alcohol in surfactant, polyethylene glycol 2000, neopelex mass ratio be 1:
0.3-0.4:0.2-0.3。
This ratio is to be characterized by what test of many times obtained as a result, passing through:Pattern, the BET of particle are attained by expection,
It cannot achieve the effect that dispersion if the amount of surfactant is on the low side, can lead to diameter of particle if the amount of surfactant is on the high side
It increased dramatically, spontaneously form second particle, keep the powder granule finally obtained larger.
As a preference of the present invention, the preferred 0.5-1mol/l of sodium carbonate liquor concentration in step (3);
As a preference of the present invention, the preferred 0.3-0.6mol/l of high purity sodium hydroxide solution in step (4);
The present invention is to balance YCl to 3.5-4 with sodium carbonate liquor adjusting precursor solution pH value3The acid value of solution,
YCl3H when solution pH value < (3.5-4)+On the high side, if not adjusting PH, sodium hydroxide solution can elder generation and H after being added+Reaction, without
It is and YCl3Solution reaction causes sodium hydroxide solution dosage insufficient, keeps reaction incomplete, granular grows can be made uneven, shape
At defect.Then it is to make crystal grain uniform growth to make system react completely to adjust pH value again to 8.5-9.5.If directly added
Entering excessive sodium hydroxide solution prevents sodium hydroxide solution dosage deficiency from reaction system PH can be made higher, is easy to make particle in life
Particle agglomeration is caused in growth process.
As a preference of the present invention, digestion time is 3-5 hours in step (4);
As a preference of the present invention, deionized water water temperature is 50-60 DEG C in step (5);
As a preference of the present invention, being dried 4-6 hours under vacuum in step (5), drying temperature is 100 DEG C, very
Reciprocal of duty cycle is 90.5-95.8KPa;
As a preference of the present invention, 700 DEG C~850 DEG C of step (6) calcination temperature, soaking time 3-5h;
Advantageous effect:
(1) complexed surfactant that the present invention uses is made of a variety of dispersants, can be acted synergistically between each other, from
And the dispersibility of particle is improved, particle agglomeration is prevented, the control of final products grain size and particle diameter distribution is conducive to;
(2) use sodium carbonate, sodium hydroxide pellets not can cause environmental pollution, solve with ammonium salt sealed Belt come ring
The problem of border pollution and high expensive;
(3) vacuum drying is taken before high-temperature calcination, can reduce the moisture in material, makes material powder in calcination process
Particle is not susceptible to reunite, and improves the uniformity of particle;
(4) the nano oxidized gadolinium diameter of particle that the present invention synthesizes is between 30~60nm, BET:50-60, be evenly distributed powder
Body granularity is smaller and is uniformly dispersed.
Description of the drawings
Fig. 1 is the SEM figures for the gadolinium oxide nano-powder that embodiment 1 obtains.
Fig. 2 is the SEM figures for the gadolinium oxide nano-powder that embodiment 2 obtains.
Fig. 3 is the SEM figures for the gadolinium oxide nano-powder that embodiment 3 obtains.
Fig. 4 is the SEM figures for the gadolinium oxide nano-powder that embodiment 4 obtains.
Fig. 5 is the SEM figures for the gadolinium oxide nano-powder that embodiment 5 obtains.
Fig. 6 is the SEM figures for the gadolinium oxide nano-powder that comparative example 1 obtains.
Fig. 7 is the SEM figures for the gadolinium oxide nano-powder that comparative example 2 obtains.
Fig. 8 is the SEM figures for the gadolinium oxide nano-powder that comparative example 3 obtains.
Fig. 9 is the SEM figures for the gadolinium oxide nano-powder that comparative example 4 obtains.
Figure 10 is the SEM figures for the gadolinium oxide nano-powder that comparative example 5 obtains.
Specific implementation mode
Embodiment 1
A kind of large-specific surface area nano gadolinium oxide raw powder's production technology, including steps are as follows:
(1) inorganic salt solution containing gadolinium is prepared:1.6mol/L gadolinium chloride solution 68.97L (gadolinium oxide 20kg) are taken to be put into
In retort, 482.8L deionized waters are added, are configured to the gadolinium chloride solution of 0.2mol/L concentration;
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.3kg, neopelex:0.3kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
(3) deployed surfactant is added in gadolinium chloride solution, is fully mixed to uniformly;
(4) after taking sodium carbonate 0.8kg, addition 7.55L deionized waters fully to dissolve, the sodium carbonate for being configured to 1mol/L is molten
Sodium carbonate liquor is added with the flow of 0.5L/min in gadolinium chloride solution, adjusts pH value to 4 by liquid;
(5) after taking high purity sodium hydroxide powder 7.2kg, addition 300L deionized waters fully to dissolve, it is configured to 0.6mol/l
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 2L/min in retort, it is 9.5 to adjust pH value, fully
After stirring, it is aged 4 hours;
(6) it is washed, is dried 5 hours under vacuum, drying temperature 100 by deionized water with plate and frame filter press
DEG C, vacuum degree 90.3-95.6KPa;
(7) product after drying is put into 850 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 3h, obtains nano oxidized gadolinium powder.
The gadolinium oxide nano-powder that the present embodiment obtains is as shown in Figure 1, as seen from the figure, gadolinium oxide particle diameter of nanometer powder is
30-60nm is evenly distributed, and detects BET:54m2/g。
Embodiment 2
(1) inorganic salt solution containing gadolinium is prepared:1.6mol/L gadolinium chloride solution 68.97L (gadolinium oxide 20kg) are taken to be put into
In retort, 298.9L deionized waters are added, are configured to 0.3mol/L gadolinium chloride solution;
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.4kg, neopelex:0.2kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
(3) deployed surfactant is added in gadolinium chloride solution, is fully mixed to uniformly;
(4) after taking sodium carbonate 0.8kg, addition 15.1L deionized waters fully to dissolve, the sodium carbonate for being configured to 0.5mol/L is molten
Sodium carbonate liquor is added with the flow of 0.5L/min in gadolinium chloride solution, adjusts pH value to 4 by liquid;
(5) after taking high purity sodium hydroxide powder 7.2kg, addition 600L deionized waters fully to dissolve, it is configured to 0.3mol/l
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 3L/min in retort, it is 9 to adjust pH value, is fully stirred
After mixing, it is aged 3 hours;
(6) plate compression being washed by deionized water, is dried 4 hours under vacuum, drying temperature is 100 DEG C,
Vacuum degree is 90.3-95.6KPa;
(7) product after drying is put into 800 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 5h, obtains nano oxidized gadolinium powder.
The gadolinium oxide particle diameter of nanometer powder that the present embodiment obtains is 30-60nm, is evenly distributed, and BET is detected:56m2/g。
Embodiment 3
(1) inorganic salt solution containing gadolinium is prepared:1.6mol/L gadolinium nitrate solution 68.97L (gadolinium oxide 20kg) are taken to be put into
In retort, 551.7L deionized waters are added, are configured to 0.2mol/L gadolinium chloride solution;
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.3kg, neopelex:0.2kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
(3) deployed surfactant is added in gadolinium chloride solution, is fully mixed to uniformly;
(4) after taking sodium carbonate 0.8kg, addition 9.43L deionized waters fully to dissolve, the sodium carbonate for being configured to 0.8mol/L is molten
Sodium carbonate liquor is added with the flow of 0.5L/min in gadolinium chloride solution, adjusts pH value to 4 by liquid;
(5) after taking high purity sodium hydroxide powder 7.2kg, addition 600L deionized waters fully to dissolve, it is configured to 0.5mol/l
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 3L/min in retort, it is 9.5 to adjust pH value, fully
After stirring, it is aged 3 hours;
(6) plate compression being washed by deionized water, is dried 4 hours under vacuum, drying temperature is 100 DEG C,
Vacuum degree is 90.3-95.6KPa;
(7) product after drying is put into 750 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 5h, obtains nano oxidized gadolinium powder.
The gadolinium oxide particle diameter of nanometer powder that the present embodiment obtains is 30-60nm, is evenly distributed, and BET is detected:58m2/g。
Embodiment 4
(1) inorganic salt solution containing gadolinium is prepared:1.6mol/L gadolinium chloride solution 68.97L (gadolinium oxide 20kg) are taken to be put into
In retort, 207L deionized waters are added, are configured to 0.4mol/L gadolinium chloride solution;
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.4kg, neopelex:0.2kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
(3) deployed surfactant is added in gadolinium chloride solution, is fully mixed to uniformly;
(4) after taking sodium carbonate 0.8kg, addition 7.55L deionized waters fully to dissolve, the sodium carbonate for being configured to 1mol/L is molten
Sodium carbonate liquor is added with the flow of 0.5L/min in gadolinium chloride solution, adjusts pH value to 3.5 by liquid;
(5) after taking high purity sodium hydroxide powder 7.2kg, addition 300L deionized waters fully to dissolve, it is configured to 0.6mol/l
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 2L/min in retort, it is 8.5 to adjust pH value, fully
After stirring, it is aged 4 hours;
(6) plate compression being washed by deionized water, is dried 5 hours under vacuum, drying temperature is 100 DEG C,
Vacuum degree is 90.3-95.6KPa;
(7) product after drying is put into 850 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 3h, obtains nano oxidized gadolinium powder.
The gadolinium oxide particle diameter of nanometer powder that the present embodiment obtains is 30-60nm, is evenly distributed, and BET is detected:53m2/g。
Embodiment 5
(1) inorganic salt solution containing gadolinium is prepared:Take the mixed solution 68.97L (oxygen of 1.6mol/L gadolinium chlorides and gadolinium nitrate
Change gadolinium 20kg) it is put into retort, 551.7L deionized waters are added, is configured to 0.2mol/L gadolinium chlorides and gadolinium nitrate mixing is molten
Liquid;
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.3kg, neopelex:0.3kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
(3) deployed surfactant is added in gadolinium chloride solution, is fully mixed to uniformly;
(4) after taking sodium carbonate 0.8kg, addition 7.55L deionized waters fully to dissolve, the sodium carbonate for being configured to 1mol/L is molten
Sodium carbonate liquor is added with the flow of 0.5L/min in gadolinium chloride solution, adjusts pH value to 4 by liquid;
(5) after taking high purity sodium hydroxide powder 7.2kg, addition 450L deionized waters fully to dissolve, it is configured to 0.4mol/l
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 2.5L/min in retort, it is 9 to adjust pH value, fully
After stirring, it is aged 4 hours;
(6) plate compression being washed by deionized water, is dried 6 hours under vacuum, drying temperature is 100 DEG C,
Vacuum degree is 90.3-95.6KPa;
(7) product after drying is put into 750 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 5h, obtains nano oxidized gadolinium powder.
The gadolinium oxide particle diameter of nanometer powder that the present embodiment obtains is 30-60nm, is evenly distributed, and BET is detected:58.5m2/g。
Comparative example 1
Step (2) in embodiment 1 is changed to:
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.1kg, neopelex:0.1kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
Other conditions are constant, and gadolinium oxide nano-powder obtained is as shown in Figure 6.Grain size is 30-60nm, but reunites and compare
Seriously, dispersibility is poor, detects BET:25m2/g。
Comparative example 2
Step (2) in embodiment 1 is changed to:
(2) absolute ethyl alcohol is taken respectively:1kg, polyethylene glycol 2000:0.6kg, neopelex:0.5kg will gather
Ethylene glycol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
Other conditions are constant, and gadolinium oxide nano-powder obtained is as shown in Figure 7.Grain size is 100-200nm, and particle obviously increases
Greatly, BET is detected:34m2/g。
Comparative example 3
Step (2) in embodiment 1 is changed to:
(2) absolute ethyl alcohol is taken respectively:1kg, polyvinyl alcohol:0.3kg, neopelex:0.3kg, by poly- second two
Alcohol 2000 and neopelex, which are separately added into absolute ethyl alcohol, to be sufficiently stirred, and surfactant is allocated;
Other conditions are constant, and gadolinium oxide nano-powder obtained is as shown in Figure 8.Grain size is 30-60nm, but reunites and compare
Seriously, dispersibility is poor, detects BET:31m2/g。
Comparative example 4
Step (1)~step (3) with embodiment 1,
(4) after taking high purity sodium hydroxide powder 7.2kg, addition 300L deionized waters fully to dissolve, it is configured to 0.6mol/l
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 2L/min in retort, it is 9.5 to adjust pH value, fully
After stirring, it is aged 4 hours;
(5) it is washed, is dried 5 hours under vacuum, drying temperature 100 by deionized water with plate and frame filter press
DEG C, vacuum degree is 90.3~95.6KPa;
(6) product after drying is put into 850 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 5h, obtains nano oxidized gadolinium powder.System
The gadolinium oxide particle diameter of nanometer powder obtained is totally bigger than normal, as shown in figure 9, detection BET:24m2/g。
Comparative example 5
Step (1)~step (4) with embodiment 1,
(5) after taking high purity sodium hydroxide powder 8kg, addition 333L deionized waters fully to dissolve, it is configured to 0.6mol/l hydrogen
Then sodium hydroxide solution sodium hydroxide solution is added with the flow of 2L/min in retort, it is 11 to adjust pH value, is sufficiently stirred
Afterwards, it is aged 4 hours;
(6) plate compression being washed by deionized water, is dried 5 hours under vacuum, drying temperature is 100 DEG C,
Vacuum degree is 90.3~95.6KPa;
(7) product after drying is put into 850 DEG C of calcinings in high-temperature electric resistance furnace, keeps the temperature 5h, obtains nano oxidized gadolinium powder.System
The case where gadolinium oxide nano-powder obtained is as shown in Figure 10, and grain size is very uneven, and particle significantly increases detects BET:
28m2/g。
Claims (8)
1. a kind of large-specific surface area nano gadolinium oxide raw powder's production technology, it is characterised in that:Steps are as follows for the preparation method:
(1) addition deionized water in high-purity inorganic salt solution containing gadolinium is configured to the nothing containing gadolinium of 0.2-0.4mol/l concentration
Machine saline solution;
(2) surfactant is added in the inorganic salt solution containing gadolinium in step (1), is fully mixed to uniformly, before being made
Drive liquid solution;Wherein, surfactant is made of absolute ethyl alcohol, polyethylene glycol 2000 and neopelex;
(3) precursor solution pH value is adjusted to 3.5-4 with deployed sodium carbonate liquor;
(4) pH value of precursor solution is adjusted to 8.5-9.5 with deployed high purity sodium hydroxide solution again, be sufficiently stirred
Afterwards, ageing obtains gadolinium hydroxide gel;
(5) after plate compression, gadolinium hydroxide gel is washed by deionized water, is dried under vacuum;
(6) product after drying is put into high-temperature electric resistance furnace and calcines and keeps the temperature to obtain large-specific surface area nano gadolinium oxide powder.
2. large-specific surface area nano gadolinium oxide raw powder's production technology as described in claim 1, it is characterised in that:Step (1)
Described in the inorganic salts containing gadolinium be gadolinium chloride or gadolinium nitrate or gadolinium chloride and gadolinium nitrate with 1:The mixing of 1 mass ratio mixing
Object.
3. large-specific surface area nano gadolinium oxide raw powder's production technology as described in claim 1, it is characterised in that:Step (2)
Described in surfactant and the mass ratio of gadolinium oxide be 0.075-0.085:1, absolute ethyl alcohol, poly- second two in surfactant
Alcohol 2000, neopelex mass ratio be 1:0.3-0.4:0.2-0.3.
4. large-specific surface area nano gadolinium oxide raw powder's production technology as described in claim 1, it is characterised in that:Step (3)
Described in a concentration of 0.5-1mol/l of sodium carbonate liquor.
5. large-specific surface area nano gadolinium oxide raw powder's production technology as described in claim 1, it is characterised in that:Step (4)
Described in a concentration of 0.3-0.6mol/l of high purity sodium hydroxide solution, digestion time be 3-5 hours.
6. large-specific surface area nano gadolinium oxide raw powder's production technology as described in claim 1, it is characterised in that:Step (5)
Described in 50-60 DEG C of deionized water water temperature;Vacuum condition lower drying time is:4-6 hours, drying temperature was 100 DEG C, vacuum degree
For 90.5-95.8KPa.
7. large-specific surface area nano gadolinium oxide raw powder's production technology as described in claim 1, it is characterised in that:Step (6)
The calcination temperature is 700 DEG C -850 DEG C, soaking time 3-5h.
8. large-specific surface area nano gadolinium oxide powder made from a kind of method as described in claim 1, it is characterised in that:It is described to receive
Rice gadolinium oxide diameter of particle is 30-60nm, BET:50-60.
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| CN110217806A (en) * | 2019-07-04 | 2019-09-10 | 中国科学院青海盐湖研究所 | A kind of salt lake richness lithium making from brine for bulky grain lithium carbonate method |
| CN111018527A (en) * | 2019-12-26 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano gadolinium oxide for dielectric ceramic capacitor |
| CN112010338A (en) * | 2020-07-27 | 2020-12-01 | 常州市卓群纳米新材料有限公司 | Method for preparing low-sodium nanometer ytterbium oxide with good monodispersity by sodium salt precipitation |
| CN112028105A (en) * | 2020-08-06 | 2020-12-04 | 常州市卓群纳米新材料有限公司 | Method for preparing nanometer praseodymium oxide by fused salt coprecipitation method |
| CN112846173A (en) * | 2021-02-08 | 2021-05-28 | 南通大学 | Preparation method of core-shell structure tungsten/gadolinium oxide powder for X, gamma ray protection |
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| CN110217806A (en) * | 2019-07-04 | 2019-09-10 | 中国科学院青海盐湖研究所 | A kind of salt lake richness lithium making from brine for bulky grain lithium carbonate method |
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| CN111018527A (en) * | 2019-12-26 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano gadolinium oxide for dielectric ceramic capacitor |
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| CN112028105A (en) * | 2020-08-06 | 2020-12-04 | 常州市卓群纳米新材料有限公司 | Method for preparing nanometer praseodymium oxide by fused salt coprecipitation method |
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