CN1228392C - Nano silicon dioxide/ferroferric oxide composite particle material and preparation method thereof - Google Patents
Nano silicon dioxide/ferroferric oxide composite particle material and preparation method thereof Download PDFInfo
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- CN1228392C CN1228392C CN 02155203 CN02155203A CN1228392C CN 1228392 C CN1228392 C CN 1228392C CN 02155203 CN02155203 CN 02155203 CN 02155203 A CN02155203 A CN 02155203A CN 1228392 C CN1228392 C CN 1228392C
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- iron salt
- silicon dioxide
- particulate material
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 27
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 18
- 239000011246 composite particle Substances 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 44
- 150000002505 iron Chemical class 0.000 claims description 25
- 239000011238 particulate composite Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 22
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical group Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 18
- 239000011790 ferrous sulphate Substances 0.000 claims description 17
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 17
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 17
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 17
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 17
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- 239000011247 coating layer Substances 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 4
- 238000009388 chemical precipitation Methods 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229960001866 silicon dioxide Drugs 0.000 description 13
- 206010013786 Dry skin Diseases 0.000 description 8
- 239000000203 mixture Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention belongs to the field of inorganic functional composite materials and preparation methods thereof, and particularly relates to a nano silicon dioxide/ferroferric oxide composite particle material and a preparation method thereof. The generated ferroferric oxide nanocrystalline is compositely assembled on the surface of spherical nano silicon dioxide particles in the reaction process by adopting a chemical precipitation method to form a spherical/shell-shaped composite particle material. The invention is characterized in that the nanometer ferroferric oxide is coated with the silicon dioxide, and the characteristics of the nanometer silicon dioxide and the ferroferric oxide are combined together, so that the nanometer ferroferric oxide has the functionalized characteristics of light weight, magnetism and low radiance, and can be applied to the fields of manufacturing transparent pigments, stealth materials and the like.
Description
Technical field
The invention belongs to inorganic functional matrix material and preparation method field, particularly a kind of nano silicon/Z 250 composite particulate material and preparation method thereof.
Background technology
The matrix material of lightweight, low-E is the focus and the difficult point of stealth material research.The nanometer clad composite material since it to have structure variation, composition and performance adjustable, easily process characteristics such as compound, can be used as the novel stealth material of excellent property.Nano silicon density is low, specific surface area is big, thermal conductivity is little, is a kind of good lightweight, heat insulation, soundproof material.The metal composite structure that coats infrared transparent pigment at silica sphere designs low-launch-rate gradient pigment, is the assembling of camouflage coating material, and the development research of novel material provides a compound modulation novelty, wide space.
At existing more reports of preparation composite particles such as silica sphere coated with silver, cobalt oxide, zinc oxide, zinc sulphide.Langmuir, 18,2001,3352 have reported with the sonochemistry sedimentation and have prepared silicon-dioxide/silver-colored composite particles.J.Mater.Res., 9,1994,436 reported with the precipitation surface reaction method and successfully prepared silicon-dioxide/basic carbonate yttrium and basic carbonate yttrium/silica composite granules.Chem.Mater., 11,1999,806 reports have successfully prepared silicon-dioxide/zinc sulphide composite particles with the sonochemistry method.J.Colloid Interface Sci., 160,1993,288 are reported in the Virahol and coat alpha-type ferric oxide by the hydrolysis tetraethoxysilane and prepare alpha-type ferric oxide/silica composite granules.But, also do not see the relevant report for preparing nano silicon/Z 250 composite particles at silica sphere clad nano Z 250 so far as yet.
Summary of the invention
One of purpose of the present invention provides a kind of nano silicon/Z 250 composite particulate material.
A further object of the present invention is to propose a kind of employing surface chemistry precipitator method in reaction process the brilliant complex group of ferriferrous oxide nano to be contained on the spheric nanometer silicon dioxide particle surface, forms the nano silicon/Z 250 composite particulate material of a kind of ball/hull shape shape.
Nano silicon of the present invention/Z 250 composite particulate material is the composite particulate material of ball/hull shape shape, and described is spherical nano-silicon dioxide by coating the base material ball, and it is the ferriferrous oxide nano crystalline substance that described shell coats material; Described even coating shell is approximately 5~40 nanometer thickness; The diameter of composite particles is 50~1500 nanometers.
The preparation method of nano silicon of the present invention/Z 250 composite particulate material, this method steps comprises:
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 0.5%~5%;
(2). divalent iron salt and trivalent iron salt are mixed with the aqueous solution of proper concn respectively, by divalent iron salt: the volume ratio of trivalent iron salt is 1: 0.5~2 to mix, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of divalent iron salt and trivalent iron salt, the initial volumetric molar concentration of divalent iron salt in the mixed solution and trivalent iron salt reaches 5 * 10 respectively
-5Mol/L~5.5 * 10
-3Mol/L and 5 * 10
-5Mol/L~5.5 * 10
-3Mol/L; The consumption of iron salt solutions is determined according to the thickness requirement of required Z 250 coating layer;
(3). sodium hydroxide or ammonia soln are added drop-wise to step (2) contain in the mixed solution of divalent iron salt and trivalent iron salt, make pH value of solution remain on 8~10, under 60~90 ℃ of conditions, stir simultaneously, react after 0.5~2 hour ageing 0.5~2 hour; With resultant washing, separation, after 60~100 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material (structure of composite particulate material is seen accompanying drawing 1) of ball/hull shape shape.
Described divalent iron salt is iron protochloride or ferrous sulfate.
Described trivalent iron salt is iron(ic) chloride or ferric sulfate.
The present invention adopts chemical precipitation method the brilliant complex group of the ferriferrous oxide nano that generates can be contained on the silica particles in reaction process, forms the even coating layer of Z 250 of about 5~40 nanometer thickness.Nano silicon/Z 250 composite particulate material light weight has the functional performance of ferromagnetism and low-E.
A kind of nano silicon of the present invention/preparation method is easy for the Z 250 composite particulate material, and cost is low, and the product purity height can be applicable to make fields such as transparent pigment, stealth material.
Description of drawings
Fig. 1. the ball of the nano silicon of the embodiment of the invention 4/Z 250 composite particulate material/shell structure synoptic diagram.
Embodiment
Embodiment 1
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 0.5%;
(2). iron protochloride and iron(ic) chloride are mixed with the aqueous solution of proper concn respectively, press iron protochloride: the volume ratio of iron(ic) chloride is mixed at 1: 1.5, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of iron protochloride and iron(ic) chloride, the initial volumetric molar concentration of iron protochloride and iron(ic) chloride reaches 5 * 10 respectively
-5Mol/L and 7.5 * 10
-5Mol/L;
(3). certain density aqueous sodium hydroxide solution is added drop-wise to step (2) contains in the mixed solution of iron protochloride and iron(ic) chloride, make pH value of solution remain on 8, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 80 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 5~15 nanometer thickness; The diameter of composite particles is 50~60 nanometers.
Embodiment 2
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 1%;
(2). iron protochloride and iron(ic) chloride are mixed with the aqueous solution of proper concn respectively, press iron protochloride: the volume ratio of iron(ic) chloride is mixed at 1: 2, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of iron protochloride and iron(ic) chloride, the initial volumetric molar concentration of iron protochloride and iron(ic) chloride reaches 1.0 * 10 respectively
-3Mol/L and 2.0 * 10
-3Mol/L;
(3). certain density ammonia soln is added drop-wise to step (2) contains in the mixed solution of iron protochloride and iron(ic) chloride, make pH value of solution remain on 9, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 80 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 15~25 nanometer thickness; The diameter of composite particles is 285~295 nanometers.
Embodiment 3
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 2%;
(2). iron protochloride and iron(ic) chloride are mixed with the aqueous solution of proper concn respectively, press iron protochloride: the volume ratio of iron(ic) chloride is mixed at 1: 1.7, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of iron protochloride and iron(ic) chloride, the initial volumetric molar concentration of iron protochloride and iron(ic) chloride reaches 1.0 * 10 respectively
-3Mol/L and 1.7 * 10
-3Mol/L;
(3). certain density aqueous sodium hydroxide solution is added drop-wise to step (2) contains in the mixed solution of iron protochloride and iron(ic) chloride, make pH value of solution remain on 9, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 80 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 20~35 nanometer thickness; The diameter of composite particles is 520~535 nanometers.
Embodiment 4
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 5%;
(2). iron protochloride and iron(ic) chloride are mixed with the aqueous solution of proper concn respectively, press iron protochloride: the volume ratio of iron(ic) chloride is mixed at 1: 2, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of iron protochloride and iron(ic) chloride, the initial volumetric molar concentration of iron protochloride and iron(ic) chloride reaches 2.75 * 10 respectively
-3Mol/L and 5.5 * 10
-3Mol/L;
(3). certain density aqueous sodium hydroxide solution is added drop-wise to step (2) contains in the mixed solution of iron protochloride and iron(ic) chloride, make pH value of solution remain on 10, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 80 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 30~40 nanometer thickness; The diameter of composite particles is 1485~1500 nanometers.
Embodiment 5
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 2%;
(2). ferrous sulfate and ferric sulfate partition are not made the aqueous solution of proper concn, press ferrous sulfate: the volume ratio of ferric sulfate is mixed at 1: 0.5, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of ferrous sulfate and ferric sulfate, the initial volumetric molar concentration of ferrous sulfate and ferric sulfate reaches 2.0 * 10 respectively
-3Mol/L and 1.0 * 10
-3Mol/L;
(3). certain density aqueous sodium hydroxide solution slowly is added drop-wise to step (2) contains in the mixed solution of ferrous sulfate and ferric sulfate, make pH value of solution remain on 9, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 80 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 15~30 nanometer thickness; The diameter of composite particles is 245~260 nanometers.
Embodiment 6
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 0.5%;
(2). ferrous sulfate and ferric sulfate are mixed with the aqueous solution of proper concn respectively, press ferrous sulfate: the volume ratio of ferric sulfate is mixed at 1: 1, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of ferrous sulfate and ferric sulfate, the initial volumetric molar concentration of ferrous sulfate and ferric sulfate reaches 5.5 * 10 respectively
-5Mol/L and 5.5 * 10
-5Mol/L;
(3). certain density ammonia soln is added drop-wise to step (2) contains in the mixing solutions of ferrous sulfate and ferric sulfate, make pH value of solution remain on 8, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 85 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 5~10 nanometer thickness; The diameter of composite particles is 250~255 nanometers.
Embodiment 7
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 5%;
(2). ferrous sulfate and ferric sulfate are mixed with the aqueous solution of proper concn, press ferrous sulfate: the volume ratio of ferric sulfate is mixed at 1: 0.9, and be added drop-wise in the suspension of (1) step, obtain containing the mixture of ferrous sulfate and ferric sulfate, the initial volumetric molar concentration of ferrous sulfate and ferric sulfate reaches 2.5 * 10 respectively
-3Mol/L and 2.3 * 10
-3Mol/L;
(3). certain density aqueous sodium hydroxide solution is added drop-wise to step (2) contains in the mixture of ferrous sulfate and ferric sulfate, make pH value of solution remain on 9, average rate stirs under 85 ℃ of conditions simultaneously, reacts after 1 hour ageing 0.5 hour; With resultant washing, separation, after 80 ℃ of dryings, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape.Evenly coating layer is approximately 25~35 nanometer thickness; The diameter of composite particles is 275~285 nanometers.
Claims (6)
1. nano silicon/Z 250 composite particulate material, it is characterized in that: this composite particulate material is the composite particulate material of ball/hull shape shape, described is spherical nano-silicon dioxide by coating the base material ball, and it is the ferriferrous oxide nano crystalline substance that described shell coats material; Described even coating shell is 5~40 nanometers; The diameter of composite particles is 50~1500 nanometers.
2. the preparation method of nano silicon as claimed in claim 1/Z 250 composite particulate material, it is characterized in that: this method steps comprises:
(1). nanometer silicon dioxide particle is distributed in the aqueous solution, and the weight percent concentration that makes suspension is 0.5%~5%;
(2). divalent iron salt and trivalent iron salt are mixed with the aqueous solution respectively, by divalent iron salt: the volume ratio of trivalent iron salt is 1: 0.5~2 to mix, and be added drop-wise in the suspension of step (1), obtain containing the mixed solution of divalent iron salt and trivalent iron salt, the initial volumetric molar concentration of divalent iron salt in the mixed solution and trivalent iron salt reaches 5 * 10 respectively
-5Mol/L~5.5 * 10
-3Mol/L and 5 * 10
-5Mol/L~5.5 * 10
-3Mol/L;
(3). sodium hydroxide or ammonia soln are added drop-wise to step (2) contain in the mixed solution of divalent iron salt and trivalent iron salt, make pH value of solution remain on 8~10, under 60~90 ℃ of conditions, stir simultaneously, reaction back ageing; With resultant washing, separation, obtain the nano silicon/Z 250 composite particulate material of ball/hull shape shape after the drying.
3. method as claimed in claim 2 is characterized in that: described divalent iron salt is iron protochloride or ferrous sulfate.
4. method as claimed in claim 2 is characterized in that: described trivalent iron salt is iron(ic) chloride or ferric sulfate.
5. method as claimed in claim 2 is characterized in that: described shell coating layer is 5~40 nanometers.
6. method as claimed in claim 2 is characterized in that: the diameter of described composite particles is 50~1500 nanometers.
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