CN1289631C - Rare earth red fluorescent powder and method for making same - Google Patents
Rare earth red fluorescent powder and method for making same Download PDFInfo
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- CN1289631C CN1289631C CN 200310110328 CN200310110328A CN1289631C CN 1289631 C CN1289631 C CN 1289631C CN 200310110328 CN200310110328 CN 200310110328 CN 200310110328 A CN200310110328 A CN 200310110328A CN 1289631 C CN1289631 C CN 1289631C
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- fluorescent powder
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- 239000000843 powder Substances 0.000 title claims abstract description 64
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 34
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims description 12
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 7
- -1 rare earth metal ion salts Chemical class 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 3
- 229940039790 sodium oxalate Drugs 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 6
- 229910052771 Terbium Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 21
- 239000000126 substance Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 230000032683 aging Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 229910052693 Europium Inorganic materials 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- AWIMWGGXVCAWEM-UHFFFAOYSA-N europium(3+) gadolinium(3+) oxygen(2-) yttrium(3+) Chemical compound [O-2].[Eu+3].[Gd+3].[Y+3] AWIMWGGXVCAWEM-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The present invention belongs to the technical field of rare earth luminescent materials, and particularly relates to red fluorescent powder of rare earth tricolor fluorescent powder and a preparation method thereof. Rare earth red lamp powder whose luminous intensity is similar to or higher than that of the existing commercial rare earth red fluorescent powder is prepared by changing the composition of traditional rare earth red luminescent materials. Solution A of rare earth metal ion salts is prepared by mixing raw materials according to the molar ratio of the composition of the red fluorescent powder which is expressed as the following molecular formula: (Y<a>Gd<1-A-B-C>Eu<b>M<c>)2O3, wherein the a is at least 0.1 and at most 0.9, the b is at least 0.01 and at most 0.2, the c is more than 0 and at most 0.1, and the M is selected from one or several kinds of La, Sm and Tb. The molar ratio of Y<3+>, Eu<3+>, Gd<3+> and M<3+> contained in the solution A is a: (1-a-b-c): b: c.
Description
Technical field
The invention belongs to rare earth luminescent material field, particularly red fluorescence powder in the rare-earth trichromatic fluorescent powder and preparation method thereof.
Technical background
The advantage of fluorescent RE powder mainly contains: emitted energy concentrates on specific wavelength, emissive porwer and good stability.Rare earth red fluorescent powder Y wherein
2O
3: Eu
3+Its quantum yield is near 100%, and it is very good that the mercury line of excitation band and 254nm coincide, and the sharp line that is positioned at 613nm is its main emission peak, therefore be main commercial red fluorescence powder so far from finding, but the shortcoming of this fluorescent material is that price is higher always.
U.S. Pat P6097146 has reported a kind of novel yttrium europium oxide gadolinium plasma flat and has shown (PDP) rouge and powder, and its chemical formula is (Y
1-a-bGd
aEu
b)
2O
3, 0≤a≤0.9,0.01≤b≤0.2 is to use the high-temperature solid phase reaction method synthetic.This method mainly is to improve the brightness and the purity of color of rouge and powder by the ratio of content that increases europium and gadolinium.But the content of europium is than higher in the prescription that it provided, and its mol ratio has reached 0.1~0.2, and the cost of fluorescent material is higher.
U.S. Pat P6042747 has also reported a kind of novel borate rouge and powder, and its chemical formula is (Y
1-a-b-cGd
cM
bEu
a) BO
3, 0.01≤a≤0.1,0.1≤b≤0.5, c≤0.1, M is one or more among Mg, Ca, Sr, the Ba.Its synthetic method is a sol-gel method, can prepare the fluorescent material of thin (0.1 μ m~2 μ m) of granularity down at lesser temps (800 ℃~950 ℃).But the problem of this method is a complicated operation, the production cost height, and efficient is low.
Other has the red fluorescence powder chemical constitution of one piece of Chinese patent, 02155323.8 report to be: aMO:bRE
2O
3: 3B
2O
3: cEu
2O
3, wherein: a=6~8, b=0~0.999, c=0.001~2.0, M is Mg
2+, Ca
2+, Sr
2+, Ba
2+In one or more, RE is La
3+, Y
3+Or/and Gd
3-Its synthetic method is a high temperature solid-state method, and the main purpose of this method is to introduce the lower alkaline-earth metal ions of price to replace original rare earth ion and reduce cost.But find in our experiment that the light decay of this red fluorescence powder is bigger, is not suitable for practical application.
Summary of the invention
A purpose of the present invention provides the red fluorescence powder in a kind of rare-earth trichromatic fluorescent powder, by changing the composition of traditional rare earth red fluorescence powder, with rare earth oxide Gd
2O
3Replace the higher rare earth oxide Y of price
2O
3, realize that the rare earth red fluorescent powder luminescent properties of preparation is not less than existing commercial red fluorescence powder, and cost reduces.
Another object of the present invention provides a kind of preparation method of rare earth red fluorescent powder.
The molecular formula of rare earth red fluorescent powder of the present invention is:
(Y
aGd
1-a-b-cEu
bM
c)
2O
3, 0.1≤a≤0.9,0.01≤b≤0.2,0<c≤0.1 wherein, M is selected from one or more among La, Sm, the Tb.
The preparation method of the red fluorescence powder in the rare-earth trichromatic fluorescent powder of the present invention may further comprise the steps:
(1) with La
2O
3, Sm
2O
3, Tb
4O
7Or their any mixture is dissolved in nitric acid or the hydrochloric acid soln, and obtaining GOLD FROM PLATING SOLUTION, to belong to ionic concn be 0.0001~2mol/L, and pH is 1~4;
(2) with Y
2O
3, Gd
2O
3And Eu
2O
3Be dissolved in respectively in nitric acid or the hydrochloric acid soln, obtain GOLD FROM PLATING SOLUTION and belong to ionic concn and be respectively 0.1~1.5mol/L, pH is respectively 1~4;
(3) 3 kinds of solution of solution that step (1) is obtained and step (2) acquisition according to the mixed in molar ratio in the molecular formula, are formulated as rare earth ion salts solution A;
(Y
aGd
1-a-b-cEu
bM
c)
2O
3, 0.1≤a≤0.9,0.01≤b≤0.2,0<c≤0.1 wherein, M is selected from one or more among La, Sm, the Tb;
A: 1-a-b-c: b: c is by being contained Y in the solution A
3+, Eu
3+, Gd
3+, M
3+The ionic mol ratio.
(4) solution A is mixed between the room temperature to 90 ℃, add precipitation agent, precipitation agent is selected from one or more in oxalic acid solution, sodium oxalate solution, the ammonium oxalate solution, and wherein the concentration of precipitation agent is 1wt%~30wt%, obtains white depositions B;
(5) sediment B continues to stir ageing 1~5 hour, and sediment B is filtered, and washing is decomposed sediment B 0.5~4 hour at 800~1000 ℃ of constant temperature, obtains rare-earth oxide C;
(6) add fusing assistant in rare-earth oxide C, make fusing assistant account for the 0.01wt%~2wt% of rare earth oxide and fusing assistant total mass, be positioned over then and carry out batch mixing in the blender, obtain mixture D, fusing assistant is selected from NH
4F, Al
2O
3, NH
4Cl, HBO
3, (NH
4)
2SO
4, BaCl
2, Li
2CO
3In one or more.
(7) with mixture D 1000~1350 ℃ of constant temperature calcinations 1~4 hour, obtain red fluorescence powder in the rare-earth trichromatic fluorescent powder through step such as wash powder, sieve.Or
(1) with La
2O
3, Sm
2O
3, Tb
4O
7Or their any mixture is according to mol ratio in the molecular formula and Y
2O
3, Gd
2O
3And Eu
2O
3Mix, obtain mixture A ';
(Y
aGd
1-a-b-cEu
bM
c)
2O
3, 0.1≤a≤0.9,0.01≤b≤0.2,0<c≤0.1 wherein, M is selected from one or more among La, Sm, the Tb;
A: 1-a-b-c: b: c is by being contained Y among the mixture A '
2O
3, Gd
2O
3, Eu
2O
3, M
2O
3Mol ratio.
(2) add fusing assistant in mixture A ', make fusing assistant account for the 0.01wt%~2wt% of rare earth oxide and fusing assistant total mass, be positioned over then and carry out batch mixing in the blender, obtain mixture B ', fusing assistant is selected from NH
4F, Al
2O
3, NH
4Cl, HBO
3, (NH
4)
2SO
4, BaCl
2, Li
2CO
3In one or more.
(3) with mixture B ' 1000~1350 ℃ of constant temperature calcinations 1~4 hour, obtain red fluorescence powder in the rare-earth trichromatic powder through step such as wash powder, sieve.
The rare earth red fluorescent powder that the present invention obtains, by changing the composition of traditional rare earth red fluorescence powder, the luminous intensity of prepared rare earth red fluorescent powder is close to or higher than existing commercial rare earth red fluorescent powder.
Embodiment
Embodiment 1
Chemical formula (the Y of rare-earth trichromatic red fluorescence powder product
0.20Gd
0.7Eu
0.04Sm
0.006)
2O
3With Y
2O
3, Gd
2O
3, Eu
2O
3, Sm
2O
3After dissolving fully with nitric acid, pH value of solution is 3~4, every kind of strength of solution of titration, wherein Y
2O
3, Gd
2O
3, Eu
2O
3Dissolving back gained solution concentration of metal ions is 0.1mol/L, Sm
2O
3Dissolving back gained solution concentration of metal ions is 0.0001mol/L.In the ratio in the above-mentioned chemical formula, accurately pipette above solution respectively.Mixing solutions stirs the oxalic acid solution that adds 10wt% down under 60 ℃ of water bath condition, drip complete back and stir ageing 1 hour.Topple over and fall supernatant liquid and, be deposited in 100 ℃ of oven dry 4 hours, the powder after the oven dry is put into the high purity aluminium oxide crucible, 850 ℃ of constant temperature calcinations 2 hours with washing of precipitate 3 times.Take by weighing the oxide compound 100g and the 0.6g H of gained
3BO
3Together put into blender, mixing time is 4 hours, then it is transferred in the high purity aluminium oxide crucible, and 1250 ℃ of calcinings 3 hours, step obtained red fluorescence powder through washing powder, sieve etc.It is 1.03 times of commercial red fluorescence powder that Hitachi F-850 fluorescence spectrophotometer is tested its luminous intensity.
Embodiment 2
Chemical formula (the Y of rare-earth trichromatic red fluorescence powder product
0.20Gd
0.7Eu
0.04Tb
0.002)
2O
3With Y
2O
3, Gd
2O
3, Eu
2O
3, Tb
4O
7After dissolving fully with nitric acid, pH value of solution is 3~4, every kind of strength of solution of titration, wherein Y
2O
3, Gd
2O
3, Eu
2O
3Dissolving back gained solution concentration of metal ions is 1.5mol/L, Tb
4O
7Dissolving back gained solution concentration of metal ions is 2mol/L.In the ratio in the above-mentioned chemical formula, accurately pipette above solution respectively.Mixing solutions stirs the sodium oxalate solution that adds 10wt% down under 80 ℃ of water bath condition, drip complete back and stir ageing 3 hours.Topple over and fall supernatant liquid and, be deposited in 100 ℃ of oven dry 4 hours, the powder after the oven dry is put into the high purity aluminium oxide crucible, 850 ℃ of constant temperature calcinations 2 hours with washing of precipitate 3 times.Take by weighing the oxide compound 50g and the 0.4g Li of gained
2CO
3Together put into blender, mixing time is 4 hours, then it is transferred in the high purity aluminium oxide crucible, and 1050 ℃ of calcinings 3 hours, step obtained red fluorescence powder through washing powder, sieve etc.It is 1.00 times of commercial red fluorescence powder that Hitachi F-850 fluorescence spectrophotometer is tested its luminous intensity.
Embodiment 3
Chemical formula (the Y of rare-earth trichromatic red fluorescence powder product
0.20Gd
0.7Eu
0.04Tb
0.001Sm
0.002)
2O
3With Y
2O
3, Gd
2O
3, Eu
2O
3, Tb
4O
7, Sm
2O
3After dissolving fully with nitric acid, pH value of solution is 3~4, every kind of strength of solution of titration, wherein Y
2O
3, Gd
2O
3, Eu
2O
3Dissolving back gained solution concentration of metal ions is 1.0mol/L, Sm
2O
3, Tb
4O
7Dissolving back gained solution concentration of metal ions is 0.02mol/L.In the ratio in the above-mentioned chemical formula, accurately pipette above solution respectively.Mixing solutions stirs the oxalic acid solution that adds 10wt% down under normal temperature condition, drip complete back and stir ageing 2.5 hours.Topple over and fall supernatant liquid and, be deposited in 100 ℃ of oven dry 4 hours, the powder after the oven dry is put into the high purity aluminium oxide crucible, 850 ℃ of constant temperature calcinations 2 hours with washing of precipitate 3 times.Take by weighing the oxide compound 100g and the 0.2g H of gained
3BO
3With 0.6g BaCl
2Together put into blender, mixing time is 4 hours, then it is transferred in the high purity aluminium oxide crucible, and 1350 ℃ of calcinings 3 hours, step obtained red fluorescence powder through washing powder, sieve etc.It is 1.05 times of commercial red fluorescence powder that Hitachi F-850 fluorescence spectrophotometer is tested its luminous intensity.
Embodiment 4
Accurately take by weighing Y respectively
2O
316.91g, Gd
2O
356.99g, Eu
2O
34.39g, Sm
2O
30.87g, La
2O
30.81g.With the BaCl that accounts for its total mass 0.1wt%
2Li with 0.2wt%
2CO
3Together put into blender, mixing time is 6 hours, then it is transferred in the high purity aluminium oxide crucible, and 1150 ℃ of calcinings 2 hours, step obtained red fluorescence powder through washing powder, sieve etc.It is 0.99 times of commercial red fluorescence powder that Hitachi F-850 fluorescence spectrophotometer is tested its luminous intensity.
Claims (8)
1. rare earth red fluorescent powder, it is characterized in that: described red fluorescence powder molecular formula is:
(Y
aGd
1-a-b-cEu
bM
c)
2O
3, 0.1≤a≤0.9,0.01≤b≤0.2,0<c≤0.1 wherein, M is selected from one or more among La, Sm, the Tb.
2. the preparation method of a rare earth red fluorescent powder as claimed in claim 1, it is characterized in that: described method steps comprises:
(1) with La
2O
3, Sm
2O
3, Tb
4O
7Or their any mixture is dissolved in nitric acid or the hydrochloric acid soln, and obtaining GOLD FROM PLATING SOLUTION, to belong to ionic concn be 0.0001~2mol/L;
(2) with Y
2O
3, Gd
2O
3And Eu
2O
3Be dissolved in respectively in nitric acid or the hydrochloric acid soln, obtain GOLD FROM PLATING SOLUTION and belong to ionic concn and be respectively 0.1~1.5mol/L;
(3) 3 kinds of solution of solution that step (1) is obtained and step (2) acquisition according to the mixed in molar ratio in the molecular formula, are formulated as rare earth ion salts solution A;
(Y
aGd
1-a-b-cEu
b-M
c)
2O
3, 0.1≤a≤0.9,0.01≤b≤0.2,0<c≤0.1 wherein, M is selected from one or more among La, Sm, the Tb;
A: 1-a-b-c: b: c is by being contained Y in the solution A
3+, Eu
3+, Gd
3+, M
3+The ionic mol ratio;
(4) solution A is mixed, add precipitation agent, obtain sediment B;
(5) sediment B is filtered, and washing is decomposed at 800~1000 ℃ of constant temperature, obtains rare-earth oxide C;
(6) in rare-earth oxide C, add fusing assistant, make fusing assistant account for the 0.01wt%~2wt% of rare earth oxide and fusing assistant total mass, be positioned over then and carry out batch mixing in the blender, obtain mixture D;
(7) with mixture D 1000~1350 ℃ of constant temperature calcinations, through washing powder, sieving, obtain the red fluorescence powder in the rare-earth trichromatic fluorescent powder.
3. method as claimed in claim 2 is characterized in that: the pH of described step (1) solution is 1~4; The pH of described step (2) solution is 1~4.
4. method as claimed in claim 2 is characterized in that: the concentration of described precipitation agent is 1wt%~30wt%.
5. as claim 2 or 4 described methods, it is characterized in that: described precipitation agent is selected from one or more in oxalic acid solution, sodium oxalate solution, the ammonium oxalate solution.
6. method as claimed in claim 2 is characterized in that: described fusing assistant is selected from NH
4F, Al
2O
3, NH
4Cl, HBO
3, (NH
4)
2SO
4, BaCl
2, Li
2CO
3In one or more.
7. the preparation method of a rare earth red fluorescent powder as claimed in claim 1, it is characterized in that: described method steps comprises:
(1) with La
2O
3, Sm
2O
3, Tb
4O
7Or their any mixture is according to mol ratio in the molecular formula and Y
2O
3, Gd
2O
3And Eu
2O
3Mix, obtain mixture A ';
(Y
aGd
1-a-b-cEu
b-M
c)
2O
3, 0.1≤a≤0.9,0.01≤b≤0.2,0<c≤0.1 wherein, M is selected from one or more among La, Sm, the Tb;
A: 1-a-b-c: b: c is by being contained Y among the mixture A '
2O
3, Gd
2O
3, Eu
2O
3, M
2O
3Mol ratio;
(2) in mixture A ', add fusing assistant, make fusing assistant account for the 0.01wt%~2wt% of rare earth oxide and fusing assistant total mass, be positioned over then and carry out batch mixing in the blender, obtain mixture B ';
(3) with mixture B ' 1000~1350 ℃ of constant temperature calcinations, through washing powder, sieving, obtain the red fluorescence powder in the rare-earth trichromatic powder.
8. method as claimed in claim 7 is characterized in that: described fusing assistant is selected from NH
4F, Al
2O
3, NH
4Cl, HBO
3, (NH
4)
2SO
4, BaCl
2, Li
2CO
3In one or more.
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CN100575451C (en) * | 2008-01-24 | 2009-12-30 | 同济大学 | A kind of red nano-fluorescent powder and preparation method thereof |
CN101417788B (en) * | 2008-09-24 | 2010-06-23 | 陕西师范大学 | Method for preparing tetragonal Eu-doped LaOF red nano fluorescent powder |
CN102260501B (en) * | 2011-05-17 | 2013-12-04 | 内蒙古大学 | Method for preparing red nano-fluorescent material |
CN102766457A (en) * | 2012-06-29 | 2012-11-07 | 彩虹集团电子股份有限公司 | Preparation method for yttrium gadolinium europium oxide red fluorescent powder applicable to 3D PDP |
CN104371721B (en) * | 2014-10-17 | 2017-03-29 | 乐山东承新材料有限公司 | rare earth red fluorescent powder and preparation method thereof |
CN108408757B (en) * | 2018-03-15 | 2020-06-23 | 益阳鸿源稀土有限责任公司 | Preparation method of high-purity superfine scandium oxide powder |
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