CN110835474B - Low-absorption-ratio pigment particles for star and preparation method thereof - Google Patents
Low-absorption-ratio pigment particles for star and preparation method thereof Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 146
- 239000000049 pigment Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 89
- 239000010410 layer Substances 0.000 claims abstract description 52
- 238000010521 absorption reaction Methods 0.000 claims abstract description 44
- 239000011159 matrix material Substances 0.000 claims abstract description 36
- 239000002346 layers by function Substances 0.000 claims abstract description 31
- 230000007704 transition Effects 0.000 claims abstract description 29
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 28
- 239000011258 core-shell material Substances 0.000 claims abstract description 17
- 229910052844 willemite Inorganic materials 0.000 claims abstract description 16
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 38
- 239000002243 precursor Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 18
- 230000007062 hydrolysis Effects 0.000 claims description 18
- 238000006460 hydrolysis reaction Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 15
- 238000004381 surface treatment Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 229910052909 inorganic silicate Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- 239000000413 hydrolysate Substances 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000009471 action Effects 0.000 abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 82
- 239000011787 zinc oxide Substances 0.000 description 35
- 229910052681 coesite Inorganic materials 0.000 description 10
- 229910052906 cristobalite Inorganic materials 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 229910052682 stishovite Inorganic materials 0.000 description 10
- 229910052905 tridymite Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- ZOIVSVWBENBHNT-UHFFFAOYSA-N dizinc;silicate Chemical group [Zn+2].[Zn+2].[O-][Si]([O-])([O-])[O-] ZOIVSVWBENBHNT-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000012686 silicon precursor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/04—Compounds of zinc
- C09C1/043—Zinc oxide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention provides a low-absorption-ratio pigment particle for a satellite and a preparation method thereof, wherein the pigment particle comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the particle matrix is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The low absorption ratio pigment prepared by the invention is pure white, the particle size distribution range is about 0.9-1.8 mu m, the solar absorption ratio is less than or equal to 0.08, and the proton irradiation energy 90keV dose is 5 multiplied by 1015cm‑2The variation of the solar absorption ratio after the action is less than or equal to 0.1, and the requirement of the electron irradiation energy of 90keV dosage of 1 multiplied by 10 is met16cm‑2The variation of the solar absorption ratio after the action is less than or equal to 0.09.
Description
Technical Field
The invention relates to the technical field of thermal control materials, in particular to a low-absorption-ratio pigment particle for a satellite and a preparation method thereof.
Background
With the development of multifunctional satellites, a large number of high-performance electronic products are used on the satellites, the power is high, the integration level is high, the heat flux density is high, most of the high-performance electronic products are temperature sensitive devices, and the effective control of the internal temperature of the satellites becomes the basis for realizing the functions of the high-performance electronic products. Thermal control coatings are surface materials specially used for changing the thermal radiation property of solid surfaces, and are widely applied in the field of satellite thermal control. Solar absorptivity of thermal control coatings on satellite surfaces is an important controllable thermal performance parameter. The thermal control coating with different solar absorptance alphas is adopted to determine the surface thermal equilibrium temperature level of the spacecraft exposed in the space environment. The thermal equilibrium temperature of the surface of the object is proportional to the solar absorptance as. Therefore, the satellite model development provides urgent demands for low-absorption and high-reflection thermal control coating pigments, and the development and preparation of the low-absorption thermal control coating pigments are realized by technical improvement on the basis of the existing thermal control coating pigments (such as zinc oxide, calcium oxide, titanium dioxide and the like), so that support is provided for the application of subsequent models.
Disclosure of Invention
The invention provides a low-absorption-ratio pigment particle for a satellite and preparation thereof, aiming at the defects of the prior art, and provides an in-situ hydrolysis growth method, wherein an optical performance enhancing unit is implanted in the preparation process of a thermal control coating pigment, a layer of compact core-shell structure and surface functional structure is subjected to hydrolysis growth on the surface of a pigment matrix zinc oxide, the surface functional design of a low-absorption-ratio filler, a low-absorption pigment preparation technology and the like are broken through, the preparation of the thermal control coating pigment with low absorption ratio performance is realized, the mass preparation of the low-absorption-ratio high-performance pigment with stable performance is realized, and the preparation method is applied to the preparation of the thermal control coating for the satellite. The solar absorption ratio is less than or equal to 0.08 and the proton irradiation energy 90keV dose is 5 multiplied by 10 through the tests and the evaluation of pigment basic performance and space environment stability15cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.1, and the requirement of the electron irradiation energy of 90keV dosage of 1 multiplied by 10 is met16cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.09.
The purpose of the invention is realized by the following technical scheme:
the invention provides a low-absorption-ratio pigment particle for a satellite, which comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the particle matrix is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer.
Preferably, the preparation method of the modified ZnO particles comprises the following steps:
grinding chemical pure ZnO powder, drying at 40-60 deg.C for 0.5-3h, and performing surface treatment.
Preferably, the temperature of the surface treatment is 120-200 ℃ and the time is 1.5-4 hours.
Preferably, in the transition layer, the mass ratio of Si-O-Si to ZnO is 25-35: 65-75.
Preferably, the particle matrix has a particle diameter of 0.6 to 1.6 μm, the transition layer has a thickness of 0.05 to 0.25 μm, and the surface functional layer has a thickness of 0.05 to 0.25 μm.
The invention also provides a preparation method of the low-absorption-ratio pigment particles for the star, which comprises the following steps:
A. preparing a particle matrix material: grinding chemical pure ZnO powder, drying at 40-60 ℃ for 0.5-3h, and then carrying out surface treatment to obtain modified ZnO particles;
B. coating the surface of the particle substrate: dissolving the modified ZnO particles in absolute ethyl alcohol to prepare a mixed solution, and dispersing a silicon dioxide precursor in the mixed solution by adopting stirring and ultrasonic treatment;
C. hydrolysis of the surface structure of the particle matrix: b, hydrolyzing and drying the ZnO-silicon dioxide precursor mixed solution prepared in the step B to ensure that nano SiO with a certain thickness is attached to the surface of ZnO2A layer;
D. high-temperature post-treatment: the ZnO-SiO obtained after the treatment of the step C2The mixed powder is subjected to high-temperature heat treatment to form a layer of Zn on the surface of the particle matrix of the pigment2SiO4And (4) obtaining the low-absorption-ratio pigment particles for the star by a core-shell structure.
Preferably, in step a, the surface treatment conditions include: the temperature is 120 ℃ and 200 ℃, and the time is 1.5-4 hours.
Preferably, in the step B, the mass ratio of the modified ZnO particles to the silica precursor is: 75-90: 10-25; the stirring time is 2-6 hours, and the ultrasonic treatment time is 0.2-3 hours.
Preferably, in step C, the conditions of the hydrolysis treatment include: the pH value of the hydrolysate is less than 5.5, and the hydrolysis time is 0.2 to 1 hour at the room temperature; the conditions of the drying treatment include: the drying temperature is 100-150 ℃ and the drying time is 4-10 hours.
Preferably, in step D, the conditions of the high temperature heat treatment include: the temperature is 300 ℃ and 450 ℃, and the time is 3-5 hours.
Preferably, in the step B, the silicon dioxide precursor is silicate, and the silicon dioxide precursor accounts for 10-25 wt% of the ZnO-silicon dioxide precursor mixed liquid system.
Preferably, the silicate substances comprise at least one of TEOS and TBOS.
The surface functional structure of the coating pigment is realized through the core-shell structure, the subsequent modification work is more effective after the surface treatment of ZnO is carried out, the stability of the zinc silicate structure formed on the surface of ZnO is ensured in the hydrolysis process of the silicon dioxide precursor, and the optical performance of the pigment is improved through the silicon dioxide structure on the surface layer.
Compared with the prior art, the invention has the following beneficial effects:
the novel star-used low-absorption-ratio pigment has better optical performance and good space environment stability on the basis of ensuring that the pigment has good dissolving performance and spraying performance.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic representation of the low absorption ratio pigment particles for stars prepared in accordance with the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment relates to a low-absorption-ratio pigment particle for a star and a preparation method thereof.
The structure of the low-absorption-ratio pigment particle for star prepared in the embodiment is shown in fig. 1, and the three structures (from left to right) are respectively an initial state, an intermediate state and a finished state in the preparation process. The three-layer structure sequentially comprises a particle substrate, a transition layer and a surface functional layer; the particle substrate is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The core-shell structure is formed by taking a ZnO particle structure as a core body and forming Zn on the surface of ZnO particles2SiO4The cladding structure is referred to as a shell structure.
The specific preparation method of the low-absorption-ratio pigment particles for the star of the embodiment comprises the following steps:
1) the star is prepared by using a particle matrix of the low-absorption ratio pigment: grinding chemical pure ZnO powder, placing the powder into an oven (the temperature is 40 ℃ and the time is 1h) to carry out primary pigment surface treatment operation, removing air, water and other impurities absorbed on the particle surface, and then carrying out surface treatment on the particle surface by adopting a vacuum sintering furnace (the temperature is 120 ℃ and the time is 1.5h) to obtain modified ZnO particles;
2) coating the surface of the pigment particle substrate: slowly adding the modified ZnO particles into absolute ethyl alcohol, stirring by using a magnetic stirrer, uniformly dispersing to prepare a ZnO solution, adding a silicon dioxide precursor (TEOS) into the ZnO solution which is stirred by magnetic stirring, dispersing for 3 hours, and performing ultrasonic treatment for 0.5 hour to uniformly disperse the silicon dioxide precursor into the ZnO solution (the mass ratio of the modified ZnO particles to the TEOS is 90: 10);
3) hydrolysis of the surface structure of the pigment particle matrix: for the ZnO-silicon dioxide precursor mixed solution (wherein, the oxide is generated) prepared in the step BThe silicon precursor accounts for 10 wt% of the mixed solution system), and hydrolyzing and drying (hydrolysis conditions are: the PH value of the hydrolysate is 5.2, and the hydrolysis time is 0.2 hour; the conditions of the drying treatment include: drying at 100 deg.C for 4 hours), hydrolyzing the silica precursor at high temperature under acidic condition to obtain SiO2Nano SiO with a certain thickness can be formed on the surface of ZnO2A layer;
4) high-temperature post-treatment: the ZnO-SiO obtained after the treatment of the step C is treated2Placing the mixed powder in a clean alumina crucible, carrying out high-temperature heat treatment (at 300 ℃ for 3 hours) in a sintering furnace, and forming a layer of Zn on the surface of a pigment particle matrix in the sintering process2SiO4And (4) obtaining the low-absorption-ratio pigment particles for the star by a core-shell structure.
The low-absorption-ratio pigment obtained in the embodiment comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the pigment particle substrate is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to Zn2SiO4:SiO2＝8:1:1。
The performance of the novel low absorption ratio pigment for star prepared in this example was tested as follows:
a) appearance: pure white particles;
b) particle size: particle size distribution in the range of about 0.9 to about 1.8 μm; wherein the particle size of the particle matrix is 0.7-1.6 μm, the thickness of the transition layer is 0.05-0.1 μm, and the thickness of the surface functional layer is 0.05-0.1 μm.
c) Solar absorption ratio: less than or equal to 0.08;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.1;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.09.
Example 2
The embodiment relates to a novel low-absorption-ratio pigment for a star and a preparation method thereof, which are basically the same as the embodiment 1 except that:
the low-absorption-ratio pigment particles obtained in the embodiment comprise a particle substrate, a transition layer and a surface functional layer which are sequentially arranged; the pigment particle substrate is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to Zn2SiO4:SiO2＝7:1:2。
The properties of the low-absorptance pigment granules for stars prepared in this example were tested as follows:
a) appearance: pure white particles;
b) particle size: particle size distribution in the range of about 0.9 to about 1.8 μm; wherein the particle size of the particle matrix is 0.6-1.5 μm, the thickness of the transition layer is 0.1-0.15 μm, and the thickness of the surface functional layer is 0.1-0.15 μm.
c) Solar absorption ratio: less than or equal to 0.08;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.1;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.09.
Example 3
The embodiment relates to a novel low-absorption-ratio pigment for a star and a preparation method thereof, which are basically the same as the embodiment 1 except that:
the silica precursor used in this example was TBOS.
The low-absorption-ratio pigment obtained in the embodiment comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the pigment particle substrate is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to Zn2SiO4:SiO2＝6:2:2。
The properties of the low-absorptance pigment granules for stars prepared in this example were tested as follows:
a) appearance: pure white particles;
b) particle size: particle size distribution in the range of about 0.9 to about 1.8 μm; wherein the particle size of the particle matrix is 0.6-1.4 μm, the thickness of the transition layer is 0.1-0.15 μm, and the thickness of the surface functional layer is 0.1-0.25 μm.
c) Solar absorption ratio: less than or equal to 0.08;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.1;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.09.
Example 4
The specific preparation method of the low-absorption-ratio pigment particles for the star of the embodiment comprises the following steps:
1) the star is prepared by using a particle matrix of the low-absorption ratio pigment: grinding chemical pure ZnO powder, placing the powder into an oven (the temperature is 60 ℃ and the time is 0.5h) to carry out primary pigment surface treatment operation, removing air, water and other impurities absorbed on the particle surface, and then carrying out surface treatment on the particle surface by adopting a vacuum sintering furnace (the temperature is 150 ℃ and the time is 4h) to obtain modified ZnO particles;
2) coating the surface of the pigment particle substrate: slowly adding the modified ZnO particles into absolute ethyl alcohol, stirring by using a magnetic stirrer, uniformly dispersing to prepare a ZnO solution, adding a silicon dioxide precursor (TEOS) into the ZnO solution which is stirred by magnetic stirring, dispersing for 2 hours, and performing ultrasonic treatment for 3 hours to uniformly disperse the silicon dioxide precursor into the ZnO solution (the mass ratio of the modified ZnO particles to the TEOS is 75: 25);
3) hydrolysis of the surface structure of the pigment particle matrix: b, hydrolyzing and drying the ZnO-silicon dioxide precursor mixed solution (wherein the silicon dioxide precursor accounts for 25 wt% of the mixed solution system) prepared in the step B (the hydrolysis conditions are that the pH of the hydrolysate is 5.4, and the hydrolysis time is0.6 hour; the conditions of the drying treatment include: drying temperature of 150 ℃ for 10 hours), hydrolyzing the silicon dioxide precursor under high temperature and acidic conditions to generate SiO2Nano SiO with a certain thickness can be formed on the surface of ZnO2A layer;
4) high-temperature post-treatment: the ZnO-SiO obtained after the treatment of the step C is treated2Placing the mixed powder in a clean alumina crucible, carrying out high-temperature heat treatment (at 400 ℃ for 5 hours) in a sintering furnace, and forming a layer of Zn on the surface of a pigment particle matrix in the sintering process2SiO4And (4) obtaining the low-absorption-ratio pigment particles for the star by a core-shell structure.
The low-absorption-ratio pigment obtained in the embodiment comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the pigment particle substrate is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to Zn2SiO4:SiO2＝6:1:3。
The performance of the novel low absorption ratio pigment for star prepared in this example was tested as follows:
a) appearance: pure white particles;
b) particle size: particle size distribution in the range of about 0.9 to about 1.8 μm; wherein the particle size of the particle matrix is 0.6-1.4 μm, the thickness of the transition layer is 0.05-0.15 μm, and the thickness of the surface functional layer is 0.15-0.25 μm.
c) Solar absorption ratio: less than or equal to 0.09;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.1;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.1.
Example 5
The specific preparation method of the low-absorption-ratio pigment particles for the star of the embodiment comprises the following steps:
1) the star is prepared by using a particle matrix of the low-absorption ratio pigment: grinding chemical pure ZnO powder, placing the powder into an oven (the temperature is 50 ℃ and the time is 3 hours) to carry out primary pigment surface treatment operation, removing air, water and other impurities absorbed on the particle surface, and then carrying out surface treatment (the temperature is 200 ℃ and the time is 2 hours) by adopting a vacuum sintering furnace to obtain modified ZnO particles;
2) coating the surface of the pigment particle substrate: slowly adding the modified ZnO particles into absolute ethyl alcohol, stirring by using a magnetic stirrer, uniformly dispersing to prepare a ZnO solution, adding a silicon dioxide precursor (TEOS) into the ZnO solution which is stirred by magnetic stirring, dispersing for 6 hours, and performing ultrasonic treatment for 0.2 hour to uniformly disperse the silicon dioxide precursor into the ZnO solution (the mass ratio of the modified ZnO particles to the TEOS is 85: 15);
3) hydrolysis of the surface structure of the pigment particle matrix: b, hydrolyzing and drying the ZnO-silicon dioxide precursor mixed solution (wherein the silicon dioxide precursor accounts for 15 wt% of the mixed solution system) prepared in the step B (the hydrolysis condition is that the pH of the hydrolyzed solution is 5.2, the hydrolysis time is 1 hour, and the drying condition comprises that the drying temperature is 120 ℃ and the drying time is 6 hours), hydrolyzing the silicon dioxide precursor under high temperature and acidic conditions, and generating SiO2Nano SiO with a certain thickness can be formed on the surface of ZnO2A layer;
4) high-temperature post-treatment: the ZnO-SiO obtained after the treatment of the step C is treated2Placing the mixed powder in a clean alumina crucible, carrying out high-temperature heat treatment (the temperature is 450 ℃ and the time is 4 hours) in a sintering furnace, and forming a layer of Zn on the surface of a pigment particle matrix in the sintering process2SiO4And (4) obtaining the low-absorption-ratio pigment particles for the star by a core-shell structure.
The low-absorption-ratio pigment obtained in the embodiment comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the pigment particle substrate is modified ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to Zn2SiO4:SiO2＝5:3:1。
The performance of the novel low absorption ratio pigment for star prepared in this example was tested as follows:
a) appearance: pure white particles;
b) particle size: particle size distribution in the range of about 0.9 to about 1.8 μm; wherein the particle size of the particle matrix is 0.6-1.4 μm, the thickness of the transition layer is 0.15-0.25 μm, and the thickness of the surface functional layer is 0.05-0.15 μm.
c) Solar absorption ratio: less than or equal to 0.09;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.11;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.12.
Comparative example 1
This comparative example is essentially the same as the process of example 1, except that: this comparative example does not perform the treatment of step 1), and directly employs the treatment of chemically pure ZnO powder to step 2).
The pigment prepared by the comparative example comprises a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the pigment particle substrate is chemical pure ZnO particles; the transition layer is Zn2SiO4A core-shell structure; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to Zn2SiO4:SiO2＝8:1:1。
The performance of the novel low absorption ratio pigment for star prepared in this example was tested as follows:
a) appearance: pure white particles;
b) particle size: particle size distribution in the range of about 0.9 to about 1.8 μm; wherein the particle size of the particle matrix is 0.7-1.6 μm, the thickness of the transition layer is 0.05-0.1 μm, and the thickness of the surface functional layer is 0.05-0.1 μm.
c) Solar absorption ratio: less than or equal to 0.12;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2Function ofThe variation of the rear solar absorption ratio is less than or equal to 0.2;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.12.
Comparative example 2
This comparative example is essentially the same as the process of example 1, except that: this comparative example did not carry out the treatment of step 4).
The pigment prepared by the comparative example comprises a particle matrix and a surface functional layer which are sequentially arranged; the pigment particle substrate is chemical pure ZnO particles; the surface functional layer is a nano silicon dioxide layer. The mass ratio of the pigment system is ZnO to SiO2＝8:2。
The performance of the novel low absorption ratio pigment for star prepared in this example was tested as follows:
a) appearance: pure white particles;
b) particle size: 0.8-1.8 μm; wherein the particle size of the particle matrix is 0.6-1.5 μm, and the thickness of the surface functional layer is 0.2-1.3 μm.
c) Solar absorption ratio: less than or equal to 0.5;
d) proton irradiation stability: proton irradiation energy 90keV dose 5X 1015cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.12;
e) electron irradiation stability: electron irradiation energy 90keV dose 1X 1016cm-2The variation of the solar absorption ratio after the action is less than or equal to 0.12.
The performance test method comprises the following steps:
the low absorption ratio pigment particles prepared in the above examples and comparative examples were subjected to a performance test as follows:
1) optical Performance testing
The test uses a UV-visible-near-IR Spectrophotometer model LAMBDA950 (UV/VIS/NIR Spectrophotometer) manufactured by Perkin-Elmer, USA, to measure the solar absorptance of the antistatic white thermal control coating. The measurable wavelength range of the device is 200nm to 2500nm, the resolution of the device is 0.1nm, the bandwidth is less than or equal to 0.05nm, the stray light is less than or equal to 0.00008 percent T, the noise is less than 0.0008A, the repeatability of the photometer is less than 0.0001A, the baseline drift is less than 0.0002A/h, and the baseline is straight: +/-0.001A, high stability, high base line straightness and low stray light. In the experiment, the step size was set to 5nm and the slit width was set to 4 nm.
2) Space proton irradiation environment test
The test is based on the sixth part of the GJB2502.6-2006 spacecraft thermal control coating test method: the standard file requirements of vacuum-proton irradiation test, etc., the proton irradiation energy is 90keV, and the irradiation flux is 1 x 1010cm-2s, cumulative dose of radiation of 5X 1015cm-2(ii) a The vacuum chamber should have no oil pollution and the background vacuum degree should be better than 1.3X 10-3Pa。
3) Space electron irradiation environment test
The test is based on the seventh part of the GJB2502.7-2006 spacecraft thermal control coating test method: the standard file requirements of vacuum-electron irradiation test, etc., proton irradiation energy is 90keV, and irradiation flux is 1 x 1011cm-2s, cumulative dose of radiation of 1X 1016cm-2(ii) a The vacuum chamber should have no oil pollution and the background vacuum degree should be better than 1.3X 10-3Pa。
In conclusion, the low-absorption-ratio pigment particles for the star have better optical performance and good space environment stability on the basis of ensuring that the pigment has good dissolving performance and spraying performance.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (8)
1. The low-absorption-ratio pigment particles for the star are characterized by comprising a particle matrix, a transition layer and a surface functional layer which are sequentially arranged; the particle matrix is modified ZnO particles; the transition layer is Zn2SiO4Core-shellStructure; the surface functional layer is a nano silicon dioxide layer;
the preparation method of the modified ZnO particles comprises the following steps:
grinding chemical pure ZnO powder, drying at 40-60 deg.C for 0.5-3h, and performing surface treatment;
the temperature of the surface treatment is 120-200 ℃, and the time is 1.5-4 hours.
2. The low absorption ratio pigment particles for a satellite according to claim 1, wherein the particle base particle diameter is 0.6 to 1.6 μm, the thickness of the transition layer is 0.05 to 0.25 μm, and the thickness of the surface functional layer is 0.05 to 0.25 μm.
3. A method for preparing a low-absorptance pigment particle for a satellite according to any one of claims 1 to 2, comprising the steps of:
A. preparing a particle matrix material: grinding chemical pure ZnO powder, drying at 40-60 ℃ for 0.5-3h, and then carrying out surface treatment to obtain modified ZnO particles;
B. coating the surface of the particle substrate: dissolving the modified ZnO particles in absolute ethyl alcohol to prepare a mixed solution, and dispersing a silicon dioxide precursor in the mixed solution by adopting stirring and ultrasonic treatment;
C. hydrolysis of the surface structure of the particle matrix: b, hydrolyzing and drying the ZnO-silicon dioxide precursor mixed solution prepared in the step B to ensure that nano SiO with a certain thickness is attached to the surface of ZnO2A layer;
D. high-temperature post-treatment: the ZnO-SiO obtained after the treatment of the step C2The mixed powder is subjected to high-temperature heat treatment to form a Zn layer on the surface of the particle matrix2SiO4And (4) obtaining the low-absorption-ratio pigment particles for the star by a core-shell structure.
4. The method for preparing a low-absorptivity pigment particle for a satellite according to claim 3, wherein in the step A, the surface treatment conditions include: the temperature is 120 ℃ and 200 ℃, and the time is 1.5-4 hours.
5. The method for preparing the star low absorption ratio pigment particles according to claim 3, wherein in the step B, the modified ZnO particles and the silica precursor are mixed according to the mass ratio of: 75-90: 10-25; the stirring time is 2-6 hours, and the ultrasonic treatment time is 0.2-3 hours.
6. The method for producing a low-absorptance pigment particle for a satellite according to claim 3, wherein the conditions of the hydrolysis treatment in the step C include: the pH value of the hydrolysate is less than 5.5, and the hydrolysis time is 0.2 to 1 hour at the room temperature; the conditions of the drying treatment include: the drying temperature is 100-150 ℃ and the drying time is 4-10 hours.
7. The method for preparing a low-absorptance pigment particle for a satellite according to claim 3, wherein the conditions of the high-temperature heat treatment in step D include: the temperature is 300 ℃ and 450 ℃, and the time is 3-5 hours.
8. The method for preparing the star-used low-absorption-ratio pigment particles according to claim 3, wherein in the step B, the silicon dioxide precursor is a silicate substance, and the silicon dioxide precursor accounts for 10-25 wt% of the ZnO-silicon dioxide precursor mixed liquid system.
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