CN114905186A - SiO with inertia 2 Preparation method and application of negative expansion particles of protective layer - Google Patents
SiO with inertia 2 Preparation method and application of negative expansion particles of protective layer Download PDFInfo
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- CN114905186A CN114905186A CN202210396183.8A CN202210396183A CN114905186A CN 114905186 A CN114905186 A CN 114905186A CN 202210396183 A CN202210396183 A CN 202210396183A CN 114905186 A CN114905186 A CN 114905186A
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- 239000002245 particle Substances 0.000 title claims abstract description 85
- 239000011241 protective layer Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 239000000376 reactant Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 239000007790 solid phase Substances 0.000 claims abstract description 4
- 238000005219 brazing Methods 0.000 claims description 19
- 239000000945 filler Substances 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 229910001220 stainless steel Inorganic materials 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 206010067484 Adverse reaction Diseases 0.000 abstract description 3
- 230000006838 adverse reaction Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010406 interfacial reaction Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Silicon Compounds (AREA)
Abstract
SiO with inertia 2 The invention discloses a preparation method and application of negative expansion particles of a protective layer, and aims to solve the problems of high chemical activity and uncontrollable interface reaction of the conventional negative expansion particles. The preparation method comprises the following steps: adding negative expansion particle powder into a mixed solution of deionized water and alcohol, and performing ultrasonic vibration to obtain a suspension; secondly, adding concentrated ammonia water into the suspension, uniformly stirring, then adding tetraethoxysilane, and stirring for reaction; thirdly, after stirring, centrifugally separating and collecting solid-phase substances; fourthly, placing the particle reactant into a muffle furnace for sintering treatment to obtain inert SiO 2 Negative expansion particles of the protective layer. The invention constructs uniform and compact inert SiO on the surface of the negative expansion particles 2 And a protective layer for preventing the negative expansion particles from directly contacting the base material. On one hand, adverse reaction of the negative expansion particles and the parent material is inhibited, and on the other hand, retention rate of the negative expansion particles in the parent material is improved.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to inert SiO 2 A preparation method and application of negative expansion particles of a protective layer.
Background
For a component or member of dissimilar materials, the difference in linear expansion coefficients between the different components can lead to the generation of large residual stresses, thereby reducing the mechanical properties of the component/member and shortening its useful life. One solution commonly used today is to reduce the coefficient of linear expansion by adding negative coefficient of expansion particles to a material with a high coefficient of linear expansion, thereby reducing the thermal mismatch between the components and relieving residual stress.
However, this approach has major limitations: the negative expansion particles generally have high chemical activity and are easy to have violent chemical reaction with the parent material. On one hand, the reaction consumes a large amount of negative expansion particles, so that the retention rate of the particles is reduced, and the negative expansion effect cannot be fully exerted. On the other hand, the reaction may generate a large amount of brittle compounds, resulting in a severe degradation of the mechanical properties of the component/member. Therefore, there is a need to develop a new method to obtain negative expansion particles with stable chemistry and controllable interfacial reactions.
Disclosure of Invention
The invention provides inert SiO for solving the problems of higher chemical activity and uncontrollable interface reaction of the existing negative expansion particles 2 A preparation method and application of negative expansion particles of a protective layer.
The invention has inert SiO 2 The preparation method of the negative expansion particles of the protective layer is realized according to the following steps:
adding negative expansion particle powder into a mixed solution of deionized water and alcohol (absolute ethyl alcohol), and obtaining a suspension after ultrasonic vibration;
secondly, adding concentrated ammonia water into the suspension, uniformly stirring, then adding tetraethoxysilane, and stirring for reaction;
after stirring, centrifugally separating and collecting solid phase matters, and washing to obtain a particle reactant;
fourthly, sintering the particle reactant in a muffle furnace at the heat preservation temperature of 100-600 ℃, and naturally cooling to room temperature after heat preservation to obtain inert SiO 2 Negative expansion particles of the protective layer;
wherein the negative expansion particle powder in the step one is ZrW 2 O 8 、HfW 2 O 8 、ZrMo 2 O 8 、ZrV 2 O 8 、ThP 2 O 8 、CeP 2 O 8 、Sc 2 W 3 O 12 、Dy 2 W 3 O 12 、Y 2 W 3 O 12 、Er 2 W 3 O 12 、Yb 2 W 3 O 12 、Lu 2 W 3 O 12 、Y 2 Mo 3 O 12 、Er 2 Mo 3 O 12 、Yb 2 Mo 3 O 12 、Lu 2 Mo 3 O 12 、Sc 2 Mo 3 O 12 、TaVO 5 、NbVO 5 、CaZrF 6 、MgZrF 6 、FeZrF 6 、CaNbF 6 、TiZrF 6 、LiAlSiO 4 One or more of mixed powders.
The invention has inert SiO 2 The application of the negative expansion particles of the protective layer is to apply the negative expansion particles as an auxiliary material to the brazing filler metal.
The invention provides a SiO with inertia 2 The preparation method of the negative expansion particles of the protective layer is characterized in that uniform and compact inert SiO is constructed on the surface of the negative expansion particles 2 And a protective layer for preventing the negative expansion particles from directly contacting the base material. On one hand, adverse reaction of the negative expansion particles and the parent material is inhibited, and on the other hand, retention rate of the negative expansion particles in the parent material is improved.
Having an inert S as described in the inventioniO 2 The preparation method of the negative expansion particles of the protective layer mainly comprises the following beneficial effects:
1. SiO prepared by the invention 2 The protective layer prevents the negative expansion particles from directly contacting with the parent metal, inhibits adverse interface reaction, avoids the generation of brittle compounds, and improves the strength of the joint.
2、SiO 2 The protective layer greatly reduces the reaction loss of the negative expansion particles, improves the retention rate of the negative expansion particles, can fully exert the negative expansion capacity of the negative expansion particles and reduces the residual stress.
3. The preparation method has low cost and simple operation, and the SiO is 2 The thickness of the layer is controllable, and the method is suitable for most negative expansion particles.
Drawings
FIG. 1 shows a schematic view of the first embodiment at Y 2 W 3 O 12 Inert SiO prepared on the surface of particles 2 High resolution transmission electron microscopy of the protective layer;
FIG. 2 shows the results obtained in example one, wherein Y is 5 wt.% 2 W 3 O 12 Granular Ag-based solder joint BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And a back-scattered photograph of the joint obtained with AISI 441 stainless steel;
FIG. 3 shows a sample of one embodiment using a SiO-containing film containing 20 wt.% of SiO 2 Y of the protective layer 2 W 3 O 12 Granular Ag-based solder joint BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And AISI 441 stainless steel.
Detailed Description
The first embodiment is as follows: this embodiment has inert SiO 2 The preparation method of the negative expansion particles of the protective layer is implemented according to the following steps:
adding negative expansion particle powder into a mixed solution of deionized water and alcohol, and performing ultrasonic vibration to obtain a suspension;
secondly, adding concentrated ammonia water into the suspension, uniformly stirring, then adding tetraethoxysilane, and stirring for reaction;
after stirring, centrifugally separating and collecting solid phase matters, and washing to obtain a particle reactant;
fourthly, sintering the particle reactant in a muffle furnace at the heat preservation temperature of 100-600 ℃, and naturally cooling to room temperature after heat preservation to obtain inert SiO 2 Negative expansion particles of the protective layer;
wherein the negative expansion particle powder in the step one is ZrW 2 O 8 、HfW 2 O 8 、ZrMo 2 O 8 、ZrV 2 O 8 、ThP 2 O 8 、CeP 2 O 8 、Sc 2 W 3 O 12 、Dy 2 W 3 O 12 、Y 2 W 3 O 12 、Er 2 W 3 O 12 、Yb 2 W 3 O 12 、Lu 2 W 3 O 12 、Y 2 Mo 3 O 12 、Er 2 Mo 3 O 12 、Yb 2 Mo 3 O 12 、Lu 2 Mo 3 O 12 、Sc 2 Mo 3 O 12 、TaVO 5 、NbVO 5 、CaZrF 6 、MgZrF 6 、FeZrF 6 、CaNbF 6 、TiZrF 6 、LiAlSiO 4 One or more of mixed powders.
The embodiment adopts the inert SiO with uniform and compact structure on the surface of the negative expansion particles 2 And a protective layer for preventing the negative expansion particles from directly contacting the base material. On one hand, adverse reaction of the negative expansion particles and the parent material is inhibited, and on the other hand, retention rate of the negative expansion particles of the parent material is improved.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the average particle diameter of the negative expansion particle powder in the first step is 0.1 to 10 μm.
The third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the mixed solution in the first step is prepared from absolute ethyl alcohol and deionized water in a mass ratio of 60: 40-90: 10.
The fourth concrete implementation mode: the difference between the present embodiment and one of the first to third embodiments is that the mass ratio of the negative expansion particle powder to the mixed solution in the first step is (0.2-2): 100.
The fifth concrete implementation mode: the difference between the present embodiment and one of the first to the fourth embodiments is that the ultrasonic vibration time in the first step is 2-15 min.
The sixth specific implementation mode: the embodiment is different from one of the first to fifth embodiments in that the volume ratio of the concentrated ammonia water used in the second step to the mixed solution is (1-5): 100, and the mass concentration of the concentrated ammonia water is 25%.
The seventh embodiment: the difference between the present embodiment and one of the first to sixth embodiments is that the volume ratio of the tetraethoxysilane to the mixed solution in the second step is (1-5): 100.
The specific implementation mode is eight: the difference between this embodiment and the first to seventh embodiments is that the stirring time in the second step is 1 to 10 hours.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is that in the fourth step, the temperature is maintained at 500 ℃ for 2-3 h.
The detailed implementation mode is ten: this embodiment has inert SiO 2 The application of the negative expansion particles of the protective layer is to apply the negative expansion particles as an auxiliary material to the brazing filler metal.
The concrete implementation mode eleven: the embodiment applies the SiO having inertia 2 Negative expansion particle brazing of protective layers to BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And stainless steel as follows:
the mass ratio of (15-25): (75-85) adding inert SiO 2 Mixing the negative expansion particles of the protective layer with Ag powder, pressing the mixed powder into an Ag-based brazing filler metal sheet, and clamping the Ag-based brazing filler metal sheet in BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And applying 0.3-0.6 MPa pressure between the stainless steel and the stainless steel, and performing brazing connection at 900-950 ℃.
Example (b): this example has inert SiO 2 The preparation method of the negative expansion particles of the protective layer comprises the following stepsThe implementation steps are as follows:
firstly, preparing 84g of mixed solution from absolute ethyl alcohol and deionized water according to the mass ratio of 76:24, and mixing the negative expansion particles Y 2 W 3 O 12 Adding the powder into the mixed solution, and performing ultrasonic vibration for 5min to obtain a suspension;
adding 2mL of concentrated ammonia water (the mass concentration is 25%) into the suspension, uniformly stirring, then adding 2mL of ethyl orthosilicate, and carrying out stirring reaction at room temperature for 3 hours;
thirdly, after stirring, separating out particles through a centrifugal machine (3000r/min), and washing the particles for three times through alcohol to obtain a particle reactant;
fourthly, placing the particle reactant into a muffle furnace for sintering, keeping the temperature at 500 ℃ for 2 hours, and naturally cooling to room temperature after the temperature is kept, so as to obtain inert SiO 2 Negative expansion particles of the protective layer.
This example is at Y 2 W 3 O 12 Preparation of dense SiO on the surface of powder 2 Coating, the coating subsequently suppressing Y 2 W 3 O 12 Reaction of the powder with the parent material.
As can be seen from FIG. 1, at Y 2 W 3 O 12 A layer of SiO is generated on the surface of the powder 2 Protective layer, SiO obtained by the method of this example 2 The thickness of the protective layer is about 35nm, and the protective layer is compact, uniform and has the same thickness as Y 2 W 3 O 12 The bonding was good.
To verify SiO 2 The protective layer is used for firstly removing Y without the protective layer 2 W 3 O 12 Mixing the particles and Ag powder according to the mass ratio of 5:95 to obtain the material containing Y 2 W 3 O 12 The Ag-based brazing filler metal particles are pressed into Ag-based brazing filler metal sheets (the thickness of the brazing filler metal sheets is 100 microns), and the Ag-based brazing filler metal sheets are clamped in the BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ Applying 0.4MPa pressure between the stainless steel and the stainless steel, performing braze welding connection of BaZr at a connection temperature of 950 ℃ and a heat preservation time of 30min (the temperature rise and reduction rate is 3 ℃/min) 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And AISI 441 stainless steel. As can be seen from FIG. 2, there is no SiO 2 Protective layer Y 2 W 3 O 12 The powder will react with BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ The violent reaction produces a brittle compound layer, directly leading to cracking and failure of the joint.
The product obtained in this example was then treated with SiO 2 Y of the protective layer 2 W 3 O 12 Mixing the particles and Ag powder according to the mass ratio of 20:80 to obtain corresponding Ag-based brazing filler metal, pressing into Ag-based brazing filler metal sheets (the thickness of the brazing filler metal sheets is 100 microns), and clamping the Ag-based brazing filler metal sheets in BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ Applying 0.4MPa pressure between the stainless steel and the stainless steel, performing braze welding connection of BaZr at a connection temperature of 950 ℃ and a heat preservation time of 30min (the temperature rise and reduction rate is 3 ℃/min) 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And AISI 441 stainless steel. As can be seen from fig. 3, the joint was well formed and no cracks were generated. Description of inert SiO 2 Protective layer avoids Y 2 W 3 O 12 Powder and BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ The violent interfacial reaction is suppressed and the formation of a brittle compound layer is avoided.
Claims (10)
1. With inert SiO 2 The preparation method of the negative expansion particles of the protective layer is characterized by comprising the following steps:
adding negative expansion particle powder into a mixed solution of deionized water and alcohol, and performing ultrasonic vibration to obtain a suspension;
secondly, adding concentrated ammonia water into the suspension, uniformly stirring, then adding tetraethoxysilane, and stirring for reaction;
after stirring, centrifugally separating and collecting solid phase matters, and washing to obtain a particle reactant;
fourthly, sintering the particle reactant in a muffle furnace at the heat preservation temperature of 100-600 ℃, and naturally cooling to room temperature after heat preservation to obtain inert SiO 2 Negative expansion particles of the protective layer;
wherein the negative expansion particle powder in the step one is ZrW 2 O 8 、HfW 2 O 8 、ZrMo 2 O 8 、ZrV 2 O 8 、ThP 2 O 8 、CeP 2 O 8 、Sc 2 W 3 O 12 、Dy 2 W 3 O 12 、Y 2 W 3 O 12 、Er 2 W 3 O 12 、Yb 2 W 3 O 12 、Lu 2 W 3 O 12 、Y 2 Mo 3 O 12 、Er 2 Mo 3 O 12 、Yb 2 Mo 3 O 12 、Lu 2 Mo 3 O 12 、Sc 2 Mo 3 O 12 、TaVO 5 、NbVO 5 、CaZrF 6 、MgZrF 6 、FeZrF 6 、CaNbF 6 、TiZrF 6 、LiAlSiO 4 One or more of mixed powders.
2. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that the average particle size of the negative expansion particle powder in the step one is 0.1-10 mu m.
3. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that the mass ratio of the negative expansion particle powder to the mixed solution in the step one is (0.2-2): 100.
4. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that the ultrasonic vibration time in the step one is 2-15 min.
5. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that the concentrated ammonia water used in the step two is mixed with the mixed solutionThe volume ratio of the mixed solution is (1-5): 100, and the mass concentration of the concentrated ammonia water is 25%.
6. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that the volume ratio of the tetraethoxysilane to the mixed solution in the step two is (1-5): 100.
7. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that the stirring time in the second step is 1-10 hours.
8. Inert SiO to claim 1 2 The preparation method of the negative expansion particles of the protective layer is characterized in that in the fourth step, the temperature is kept at 500 ℃ for 2-3 h.
9. Inert SiO as claimed in claim 1 2 Use of negatively expanded particles for protective layers, characterized in that they are provided with inert SiO 2 The negative expansion particles of the protective layer are used as auxiliary materials in the brazing filler metal.
10. Use according to claim 9, characterized in that the inert SiO is used 2 Negative expansion particle brazing of protective layers to BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And stainless steel as follows:
the mass ratio of (15-25): (75-85) adding inert SiO 2 Mixing the negative expansion particles of the protective layer with Ag powder, pressing the mixed powder into Ag-based brazing filler metal sheets, and clamping the Ag-based brazing filler metal sheets in BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3-δ And applying 0.3-0.6 MPa pressure between the stainless steel and the stainless steel, and performing brazing connection at 900-950 ℃.
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2022
- 2022-04-15 CN CN202210396183.8A patent/CN114905186A/en active Pending
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