CN116002960A - Preparation method of heat-conducting flexible glass substrate - Google Patents
Preparation method of heat-conducting flexible glass substrate Download PDFInfo
- Publication number
- CN116002960A CN116002960A CN202211663330.XA CN202211663330A CN116002960A CN 116002960 A CN116002960 A CN 116002960A CN 202211663330 A CN202211663330 A CN 202211663330A CN 116002960 A CN116002960 A CN 116002960A
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- CN
- China
- Prior art keywords
- heat
- glass
- conductivity
- flexible glass
- filler
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000011521 glass Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000758 substrate Substances 0.000 title description 4
- 239000000945 filler Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000006066 glass batch Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims 3
- 239000011256 inorganic filler Substances 0.000 claims 2
- 229910003475 inorganic filler Inorganic materials 0.000 claims 2
- 239000005347 annealed glass Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical group Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 238000005530 etching Methods 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 230000003813 thin hair Effects 0.000 description 1
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention relates to a preparation method of heat-conducting flexible glass, which is characterized by comprising two aspects of adding heat-conducting filler and chemically thinning; the heat-conducting filler is nano-particle size, glass batch is melted at high temperature, a certain amount of glass liquid is poured into a mold, then a layer of nano-level heat-conducting filler is rapidly and uniformly covered on the surface of the glass liquid, and the rest glass liquid is poured on the surface for molding and annealing; the flexible glass with the middle filled with the nano-level heat conducting filler is prepared by using a chemical thinning method. According to the invention, the high-heat-conductivity flexible glass is prepared by adding the heat-conducting filler and a chemical thinning method, so that the heat conductivity of the flexible glass can be effectively increased.
Description
Technical Field
The invention relates to the technical field of electronic glass manufacturing, in particular to a preparation method of heat-conducting flexible glass.
Background
With the rapid development of electronic technology, the performance of substrate materials such as high thermal conductivity, low dielectric constant, and good thermal stability are required. The flexible glass is a common substrate material, and has high chemical strength, good mechanical property and the like, and has high potential application value in the electronic fields of mobile phones, computers and the like. However, glass is used as a thermal bad body, the thermal conductivity of the glass is generally between 0.712 and 1.340W/(m.K), and the lower thermal conductivity can influence the heat dissipation efficiency of the device, so that the service life of the device is influenced, and therefore, the improvement of the thermal conductivity of the flexible glass is important.
Currently, common methods for increasing thermal conductivity are filling with thermally conductive fillers and the like. Common heat conducting fillers include nitrides, carbides and the like, and nanoscale heat conducting fillers have better heat conducting performance than common heat conducting fillers due to the size specificity of the nanoscale heat conducting fillers. For flexible glass, the glass batch is melted at a high temperature of 1550-1600 ℃, the filler is added into the glass batch, alkaline substances in the glass batch can corrode the filler at a high temperature, the filler performance is changed, the thickness of the flexible glass is less than 0.1mm, and the common filler size reaches the micron level and can also influence the preparation of the flexible glass.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of heat-conducting flexible glass, which is characterized in that nano-level heat-conducting filler is added in the glass pouring process, and the required heat-conducting flexible glass is thinned by a chemical thinning method, so that the reaction of glass batch and the heat-conducting filler in the high-temperature process is avoided, the influence of the filler size on the size of the flexible glass is reduced, and meanwhile, a flexible glass layer with the heat-conducting filler can be effectively prepared.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of heat-conducting flexible glass comprises the following steps:
1) Melting the glass batch material into glass liquid at high temperature, pouring part of the glass liquid into a mold, uniformly covering the surface of the glass liquid with nano heat-conducting filler, pouring the rest glass liquid into the mold, and performing molding annealing;
2) And preparing the formed glass into the heat-conducting flexible glass with the middle containing the heat-conducting filler and the thickness less than 0.1mm by using a chemical thinning method.
Further, the particle size of the heat conducting filler is in the nanometer level, and the mass fraction is more than 10%.
Further, the glass batch comprises 60-75% by mass of SiO2; 1-4% of Al2O3; 5-10% of Na2O; 0-2% of K2O; 10-12% of CaO; 0-1% MgO;
further, the chemical thinning hair is wiped on the surface of the glass by strong acid such as HF and the like, and then is cleaned by distilled water for 3 times;
further, placing the weighed glass batch into a high-temperature furnace, melting at a high temperature of 1550-1600 ℃, pouring part of glass liquid in a mold, then rapidly and uniformly spraying high-heat-conductivity filler on the surface, and finally pouring the rest glass liquid; since glass is molded in a short time, chemical reaction between the molten glass and the filler is extremely difficult.
Further, chemically thinning the glass after casting molding by using HF and the like to prepare flexible glass with the thickness of less than 0.1mm, wherein the flexible glass contains high heat conduction filler in the middle.
The invention has the advantages that:
the method has the advantages of simple steps and convenient operation, and the heat-conducting filler is added in the glass pouring process, so that the reaction of the filler and the glass batch is avoided; the flexible glass with the middle containing the heat conducting filler is prepared by using a chemical thinning method, the nano-level high heat conducting filler is selected, the influence of the filler size on the flexible glass is reduced, and the heat conducting property of the flexible glass is better improved.
The specific embodiment is as follows:
example 1: a preparation method of heat-conducting flexible glass is characterized by comprising the following steps: it comprises the following steps:
(a) Preparing heat-conducting flexible glass:
the flexible glass batch comprises 75 mass percent of SiO2;3% Al2O3;10% Na2O;2% of K2O;9% CaO;1% MgO;
placing the flexible glass batch in a high-temperature furnace, melting at a high temperature of 1550 ℃, pouring about 50% of glass liquid into a copper mold, uniformly spraying AlN nano filler which accounts for about 20% of the glass liquid in mass and has a particle size of 40nm on the surface of the poured glass liquid within 5 seconds, and ensuring that the glass liquid is in a softened state; pouring the rest about 50% of glass liquid into a mould, and performing forming annealing at 550 ℃;
(b) Preparing heat-conducting flexible glass: cooling the annealed flexible glass to room temperature, etching the surface of the flexible glass by using HF, and repeatedly cleaning the flexible glass with distilled water for 3 times; and then etching by HF, cleaning by distilled water, and repeatedly etching until the thickness reaches 70 mu m to prepare the heat-conducting flexible glass with the middle containing nano heat-conducting filler.
Example 2:
the flexible glass batch comprises 71 mass percent of SiO2;4% Al2O3;10% Na2O;2% of K2O;12% CaO;1% MgO;
placing the flexible glass batch in a high-temperature furnace, melting at a high temperature of 1550 ℃, pouring about 50% of glass liquid into a copper mold, uniformly spraying hexagonal boron nitride nano filler which accounts for about 20% of the glass liquid in mass and has a particle size of 100nm on the surface of the poured glass liquid within 5 seconds, and ensuring that the glass liquid is in a softened state. Pouring the rest about 50% of glass liquid into a mould, and performing forming annealing at 600 ℃;
(b) Preparing heat-conducting flexible glass: etching the surface of the flexible glass by using HF, and repeatedly cleaning the flexible glass by using distilled water for 3 times; and then etching by HF, cleaning by distilled water, and repeatedly etching until the thickness reaches 70 mu m to prepare the heat-conducting flexible glass with the middle containing nano heat-conducting filler.
Example 3:
the flexible glass batch comprises 72 mass percent of SiO2;3% Al2O3;10% Na2O;2% of K2O;12% CaO;1% MgO;
placing the flexible glass batch in a high-temperature furnace, melting at a high temperature of 1550 ℃, pouring about 50% of glass liquid into a copper mold, uniformly spraying silicon carbide nano filler which accounts for about 20% of the glass liquid in mass and has a particle size of 50nm on the surface of the poured glass liquid within 5 seconds, and ensuring that the glass liquid is kept in a softened state. Pouring the rest about 50% of glass liquid into a mould, and performing forming annealing at 550 ℃;
(b) Preparing heat-conducting flexible glass: etching the surface of the flexible glass by using HF, and repeatedly cleaning the flexible glass by using distilled water for 3 times; and then etching by HF, cleaning by distilled water, and repeatedly etching until the thickness is 50 mu m, thus preparing the heat-conducting flexible glass with the middle containing nano heat-conducting filler.
According to the methods of examples 1-3, flexible glass was obtained, and the heat conductivity was measured for each of the flexible glass and the common flexible glass, and the measurement results were as follows:
| thermal conductivity/W.m -1 K -1 | CS（MPa） | DOL（μm） | |
| Flexible glass | 1.25 | 253 | 17 |
| Example 1 | 1.75 | 259 | 16 |
| Example 2 | 1.90 | 248 | 17 |
| Example 3 | 1.54 | 251 | 19 |
Claims (6)
1. The preparation method of the high-heat-conductivity flexible glass is characterized by comprising the following steps of:
1) Melting the glass batch at high temperature, pouring part of glass liquid in a mold, uniformly covering the surface of the glass liquid with nano-level heat conducting filler, pouring the rest glass liquid on the surface of the glass liquid, and annealing and forming;
2) Thinning the annealed glass by a chemical thinning method, wiping two sides of the glass by using HF strong acid, and cleaning the glass with distilled water for more than 3 times to prepare the flexible glass with the filler layer with high heat conductivity in the middle.
2. The preparation method of the high-heat-conductivity flexible glass according to claim 1, wherein the particle size of the high-heat-conductivity filler of the flexible glass is nano-scale, the high-heat-conductivity filler is high-heat-conductivity inorganic filler, and the mass percentage of the high-heat-conductivity filler is more than 10% of the mass of the flexible glass.
3. The method for preparing the high-heat-conductivity flexible glass according to claim 2, wherein the high-heat-conductivity inorganic filler is aluminum nitride or h-BN.
4. The method for preparing high-heat-conductivity flexible glass according to claim 2 or 3, wherein the glass batch comprises 60-75% by mass of SiO2; 1-4% of Al2O3; 5-10% of Na2O; 0-2% of K2O; 10-12% of CaO; 0-1% MgO.
5. The preparation method of the high-heat-conductivity flexible glass according to claim 4, wherein after the glass batch is fired at a high temperature, part of glass liquid is poured into a mold, when the glass liquid is kept in a softened state, the surface is uniformly covered with high-heat-conductivity filler by means of coating, spraying or the like, and finally the rest of glass liquid is poured and annealed at 550-600 ℃ for molding.
6. The method for preparing the high-heat-conductivity flexible glass according to claim 5, wherein the glass after casting molding is subjected to chemical thinning by using HF (hydrogen fluoride) and the like, so that the flexible glass with the thickness of less than 0.1mm is prepared, and the flexible glass contains a high-heat-conductivity filler in the middle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211663330.XA CN116002960B (en) | 2022-12-23 | 2022-12-23 | Preparation method of heat-conducting flexible glass substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211663330.XA CN116002960B (en) | 2022-12-23 | 2022-12-23 | Preparation method of heat-conducting flexible glass substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116002960A true CN116002960A (en) | 2023-04-25 |
| CN116002960B CN116002960B (en) | 2024-03-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211663330.XA Active CN116002960B (en) | 2022-12-23 | 2022-12-23 | Preparation method of heat-conducting flexible glass substrate |
Country Status (1)
| Country | Link |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3997314A (en) * | 1975-02-28 | 1976-12-14 | Asahi Glass Co., Ltd. | Process and apparatus for manufacturing a wire reinforced float glass |
| US20100028689A1 (en) * | 2008-07-31 | 2010-02-04 | Kam-Chuen Yung | B-stage thermal conductive dielectric coated metal-plate and method of making same |
| CN102336523A (en) * | 2011-06-01 | 2012-02-01 | 武汉理工大学 | High thermal conductivity rare earth/AIN/microcrystalline glass composite material and its preparation method |
| JP2012111665A (en) * | 2010-11-25 | 2012-06-14 | Tokyo Univ Of Science | Heat conductive glass, and method for manufacturing the same |
| CN114664501A (en) * | 2022-03-29 | 2022-06-24 | 中国人民解放军海军工程大学 | Mica tape with high heat conductivity coefficient and preparation method thereof |
| CN115286241A (en) * | 2022-08-09 | 2022-11-04 | 中建材玻璃新材料研究院集团有限公司 | Ultrathin flexible glass with high fracture toughness and preparation method thereof |
-
2022
- 2022-12-23 CN CN202211663330.XA patent/CN116002960B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3997314A (en) * | 1975-02-28 | 1976-12-14 | Asahi Glass Co., Ltd. | Process and apparatus for manufacturing a wire reinforced float glass |
| US20100028689A1 (en) * | 2008-07-31 | 2010-02-04 | Kam-Chuen Yung | B-stage thermal conductive dielectric coated metal-plate and method of making same |
| JP2012111665A (en) * | 2010-11-25 | 2012-06-14 | Tokyo Univ Of Science | Heat conductive glass, and method for manufacturing the same |
| CN102336523A (en) * | 2011-06-01 | 2012-02-01 | 武汉理工大学 | High thermal conductivity rare earth/AIN/microcrystalline glass composite material and its preparation method |
| CN114664501A (en) * | 2022-03-29 | 2022-06-24 | 中国人民解放军海军工程大学 | Mica tape with high heat conductivity coefficient and preparation method thereof |
| CN115286241A (en) * | 2022-08-09 | 2022-11-04 | 中建材玻璃新材料研究院集团有限公司 | Ultrathin flexible glass with high fracture toughness and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN116002960B (en) | 2024-03-12 |
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