CN112694266A - High-strength reliable-sealing quartz glass and preparation method thereof - Google Patents
High-strength reliable-sealing quartz glass and preparation method thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 238000007789 sealing Methods 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 110
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 40
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000006004 Quartz sand Substances 0.000 claims abstract description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 20
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 20
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 20
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 20
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 20
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims abstract description 20
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 20
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 20
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000010453 quartz Substances 0.000 claims description 53
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910000831 Steel Inorganic materials 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000010959 steel Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 19
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000001856 Ethyl cellulose Substances 0.000 claims description 18
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 18
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 18
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 18
- 229920001249 ethyl cellulose Polymers 0.000 claims description 18
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 18
- 229940116411 terpineol Drugs 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000006060 molten glass Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000011368 organic material Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 2
- 231100001240 inorganic pollutant Toxicity 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 231100000719 pollutant Toxicity 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000005394 sealing glass Substances 0.000 abstract description 17
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 abstract description 10
- 239000003566 sealing material Substances 0.000 abstract description 6
- 239000002241 glass-ceramic Substances 0.000 abstract description 2
- 239000012046 mixed solvent Substances 0.000 abstract description 2
- 238000009736 wetting Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 53
- 239000010410 layer Substances 0.000 description 32
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- 239000011247 coating layer Substances 0.000 description 8
- 239000000356 contaminant Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000010292 electrical insulation Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002070 germicidal effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002470 thermal conductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/20—Uniting glass pieces by fusing without substantial reshaping
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
Abstract
The invention discloses a high-strength reliable-sealing quartz glass and a preparation method thereof, wherein the preparation method comprises the following steps: preparing glass powder, cleaning quartz glass, coating a glass layer and heating for sealing, taking low-melting-point glass ceramics prepared from quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate and molybdenum oxide as sealing glass of the quartz glass, and adjusting the components of the sealing glass and the heat treatment process to obtain the purpose of matching with the thermal expansion coefficient of the quartz glass; the influence of internal stress on the sealing of the quartz glass is fully reduced, the sealing strength is greatly enhanced, the mixed solvent and the glass powder are mixed when the glass layer is coated, the wetting angle of the sealing material and the quartz glass is reduced, so that the sealing material can be better extended on the quartz glass, the thickness of the sealed glass layer is more uniform, and the sealing material is combined with the fine treatment of the quartz glass to ensure that the air tightness of a sealed product is good.
Description
Technical Field
The invention relates to a preparation method of sealing glass, in particular to high-strength reliable-sealing quartz glass and a preparation method thereof.
Background
The quartz glass is special industrial technical glass composed of silicon dioxide single component, and is praised as 'king of glass' by experts in the field of new materials because the quartz glass has a series of special physical and chemical properties. The quartz glass has very low thermal expansion coefficient, good thermal shock resistance, poor thermal conductor, excellent optical performance, excellent electrical insulation and good chemical stability. In the case of electric light sources, quartz glass is used for manufacturing gas discharge lamps such as energy saving lamps, germicidal lamps, mercury lamps, sodium lamps, metal halide lamps, Light Emitting Diodes (LEDs), infrared lamps, ultraviolet germicidal lamps, and the like. The quartz glass is mainly applied to the production of prefabricated rods in the manufacture of optical fibers, such as deposition tubes, head tubes, tail tubes, holding rods, tail rods and the like used in the rod manufacturing process of MCVD, PCVD, OVD and VAD technologies. Quartz glass is widely used in the semiconductor industry because of its excellent properties such as high purity, high temperature resistance, low thermal expansion, etc. Such as: a quartz glass diffusion tube used in key processes of doping, diffusing, oxidizing, annealing and the like of a monocrystalline silicon wafer; a quartz bell jar used in the silicon wafer epitaxial process; a flower basket and a bracket used in the silicon chip acid washing and ultrasonic cleaning procedures; a silicon wafer carrier used in the silicon wafer diffusion process; a quartz crucible used in a step of pulling a silicon single crystal. In the electronic information industry, "high precision glass masks" made of high purity quartz glass are one of the key materials for producing cathode ray tubes, thin film transistor displays, field emission displays, vacuum fluorescent displays, organic light emitting displays. The quartz glass also has unique function in the aerospace industry at the front end, and can participate in manufacturing space astronomical telescopes, space laser reflectors, spaceship rotary window windows and space cameras.
Along with the development of science and technology, the application conditions of the quartz glass are also more strict, and how to obtain good sealing between the quartz glassBecomes a technical problem to be solved. The sealing glass is an intermediate glass for sealing glass, ceramics, metals, composite materials, and the like. The sealing between glass and glass is usually carried out by sintering and melting in a flame of gas or a mixture of natural gas and oxygen. In order to ensure reliable sealing, the coefficients of thermal expansion of the sealing glasses must be very similar, otherwise the glasses will break due to internal stresses generated during sealing. The thermal expansion coefficient of quartz glass is extremely small and is only 5X 10 at high temperature-7/° c, the coefficient of thermal expansion of the sealing glass must also be small enough to match the effect. Experience proves that: if the difference in linear expansion coefficient is not more than 7X 10-7At/° c, internal stress generated at the weld does not cause cracking. Annealing is preferably used to eliminate internal stress at the sealed position, otherwise the sealed position is easy to crack.
The quartz glass has unique application in military aerospace, and the excellent performance of the quartz glass is important. In aerospace planes and space ships, there are many structures where multiple layers of quartz glass are required, such as: each visible window needs three layers of glass for composite use, and the outermost layer and the innermost layer are both made of quartz glass. The surface of the space shuttle can also be composed of a large number of quartz glass tiles, and how to have better connectivity is also a problem to be solved. Most of the existing documents and patents are about the research and application of sealing between quartz glass and metal, and it is only mentioned how to seal between quartz glass. Therefore, it is necessary to develop a technique for sealing silica glass with high strength.
Disclosure of Invention
The invention aims to provide high-strength and reliable-sealing quartz glass and a preparation method thereof, and the prepared quartz glass sealing system has the advantages of small thermal expansion coefficient, excellent electrical insulation performance, high sealing strength, excellent chemical stability and small internal stress.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of high-strength reliable-sealing quartz glass specifically comprises the following steps:
first, preparation of glass frit
(1.1) weighing 36-40 wt% of quartz sand, 18-22 wt% of alumina, 3-5 wt% of lithium carbonate, 26-30 wt% of germanium oxide, 1.5-3 wt% of zinc oxide, 2-3 wt% of titanium dioxide, 1.5-2.5 wt% of zirconium dioxide, 0.5-1.2 wt% of barium nitrate and 2-3 wt% of molybdenum oxide according to mass percentage;
(1.2) fully mixing the materials weighed in the step (1.1), adding the mixture into a quartz crucible, and keeping the temperature at 1500-1600 ℃ for 3-5 hours to obtain glass liquid;
(1.3) pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 550-600 ℃ for annealing for 3-5 h, and then cooling along with the furnace;
(1.4) crushing the cooled glass, and sieving to obtain glass powder;
second, cleaning the quartz glass
Cleaning quartz glass to remove surface pollutants;
third, coating a glass layer
Taking ethyl cellulose, butyl carbitol and terpineol according to the weight ratio of (1-3) to (3-6) to obtain an organic material, mixing the glass material prepared in the first step and the organic material according to the weight ratio of (2-4) to (1-3), and coating the mixture on the surface of quartz glass to form a glass layer;
fourthly, heating and sealing
(4.1) aligning and sticking the quartz glass with the coated glass layer on one surface and the other piece of quartz glass together, and putting the quartz glass and the other piece of quartz glass into a mould to keep the temperature for 20-50 min at 1100-1200 ℃;
and (4.2) transferring the mold into a muffle furnace, heating to 800-900 ℃, preserving heat for 1-2 h, and turning off the muffle furnace to cool along with the furnace to obtain the sealing quartz glass.
Further, the materials weighed in the step (1.2) are placed into a V-shaped mixer to be mixed for 40-60 min to form a mixture.
Further, in the step (1.4), the cooled glass is placed into a cylindrical die, and the glass is crushed by a hydraulic tablet press and then sieved to obtain glass powder.
Further, in the step (1.4), the glass is crushed and then sieved by a 200-300-mesh standard sieve to obtain glass powder.
Further, the specific process of cleaning the quartz glass in the second step is as follows:
further, the step of cleaning the quartz glass specifically comprises the following steps:
(2.1) firstly, soaking quartz glass in acetone, ethanol and deionized water respectively, and carrying out ultrasonic cleaning for five minutes respectively;
and (2.2) cleaning by using sulfuric acid and RCA solution respectively to remove organic and inorganic pollutants on the surface.
The invention provides a novel quartz sealing system, which solves the problem of explosion caused by internal stress generated after quartz glass is sealed, and aims to obtain the aim of matching with the thermal expansion coefficient of quartz glass by taking low-melting microcrystalline glass prepared from quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate and molybdenum oxide as the sealing glass of the quartz glass through adjusting the components of the sealing glass and the heat treatment process. The influence of internal stress on the sealing of the quartz glass is fully reduced, the sealing strength is greatly enhanced, the mixed solvent and the glass powder are mixed when the glass layer is coated, the wetting angle of the sealing material and the quartz glass is reduced, so that the sealing material can be better extended on the quartz glass, the thickness of the sealed glass layer is more uniform, and the sealing material is combined with the fine treatment of the quartz glass to ensure that the air tightness of a sealed product is good.
The quartz glass sealing system obtained by the preparation method has the advantages of small thermal expansion coefficient, excellent electrical insulation performance, high sealing strength, good air tightness, excellent chemical stability, small internal stress, stable service performance under high temperature, good thermal shock resistance, extremely low thermal expansion coefficient and uniform stress distribution, and can adapt to various extreme conditions.
The product of the invention has excellent performance and can be applied to the fields of electronics, aerospace, semiconductors and the like. And the preparation process has the advantages of simple operation process, simple equipment, less investment and low cost, and is suitable for batch production of enterprises.
Drawings
FIG. 1 is a thermal expansion diagram of a quartz glass sealing system prepared in example 1 of the present invention;
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1:
first step, preparation of microcrystalline glass powder
(1) First, 36 wt% of quartz sand, 20 wt% of alumina, 4 wt% of lithium carbonate, 30 wt% of germanium oxide, 3 wt% of zinc oxide, 2 wt% of titanium dioxide, 2 wt% of zirconium dioxide, 1 wt% of barium nitrate, and 2 wt% of molybdenum oxide were weighed, respectively, by mass percentage.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 45min to form a mixture.
(3) Mixing uniformly, adding into a quartz crucible, and keeping the temperature at 1580 ℃ for 5 h.
(4) And pouring molten glass on a steel plate, sending the steel plate into a 600 ℃ muffle furnace for annealing for 3h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And (4) crushing, and screening by a 250-mesh standard sieve to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 2: 1. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 2:5: 5.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold was held at 1150 ℃ for 40 min.
(3) And (4) transferring the mould into a muffle furnace, heating to 800 ℃, preserving heat for 2 hours, then closing the muffle furnace, and cooling the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
The linear expansion of the quartz glass sealing system is tested by NETZSCH DIL 402PC, referring to figure 1, the abscissa is the sample temperature, the ordinate is the elongation of the sample, and as can be seen from figure 1, the linear expansion of the prepared quartz sealing system is 1.001 multiplied by 10-7The material has extremely low coefficient of thermal expansion per DEG C (room temperature to 700 ℃), has an expansion transition temperature of 686 ℃, and can be used for a long time at high temperature.
Example 2:
first step, preparation of microcrystalline glass powder
(1) First, 38 wt% of quartz sand, 20 wt% of alumina, 3 wt% of lithium carbonate, 29 wt% of germanium oxide, 2 wt% of zinc oxide, 3 wt% of titanium dioxide, 2 wt% of zirconium dioxide, 1 wt% of barium nitrate, and 2 wt% of molybdenum oxide were weighed, respectively, by mass percentage.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 55min to form a mixture.
(3) Mixing uniformly, adding into a quartz crucible, and keeping the temperature at 1600 ℃ for 4 h.
(4) And pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 590 ℃ for annealing for 3h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And sieving the crushed glass powder by a standard sieve of 200 meshes to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 3: 1. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 2:6: 5.
Fourthly, heating and sealing
(1) Aligning and sticking the quartz plate with the coated glass layer on one surface and the other one together, and putting the quartz plate and the other one into a special die;
(2) the mold was held at 1160 deg.C for 30 min.
(3) And (3) transferring the mould into a muffle furnace, heating to 900 ℃, preserving heat for 1h, then closing the muffle furnace, and cooling the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
The linear expansion of the quartz glass sealing system is tested by NETZSCH DIL 402PC, and the linear expansion of the prepared quartz sealing system is 1.230 multiplied by 10-7/° c (room temperature to 700 ℃).
Example 3:
first step, preparation of microcrystalline glass powder
(1) First, 37 wt% of quartz sand, 21 wt% of alumina, 3 wt% of lithium carbonate, 28 wt% of germanium oxide, 2.5 wt% of zinc oxide, 2.5 wt% of titanium dioxide, 2 wt% of zirconium dioxide, 1 wt% of barium nitrate, and 3 wt% of molybdenum oxide were weighed, respectively, in mass percent.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 50min to form a mixture.
(3) Mixing uniformly, adding into quartz crucible, and keeping temperature at 1590 deg.C for 4.5 h.
(4) And pouring molten glass on a steel plate, sending the steel plate into a 600 ℃ muffle furnace for annealing for 3h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And (4) grinding the mixture, and screening the mixture by a standard sieve of 300 meshes to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 4: 1. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 2:6: 6.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold is placed at 1200 ℃ and kept warm for 30 min.
(3) And (4) transferring the mould into a muffle furnace, heating to 850 ℃, preserving heat for 1.5h, then closing the muffle furnace, and cooling the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
The linear expansion of the quartz glass sealing system is tested by NETZSCH DIL 402PC, and the prepared quartz sealing system has the linear expansion of 1.175 multiplied by 10-7/° c (room temperature to 700 ℃).
Example 4:
first step, preparation of microcrystalline glass powder
(1) First, 40 wt% of quartz sand, 20 wt% of alumina, 3 wt% of lithium carbonate, 28 wt% of germanium oxide, 2 wt% of zinc oxide, 2 wt% of titanium dioxide, 2 wt% of zirconium dioxide, 1 wt% of barium nitrate, and 2 wt% of molybdenum oxide were weighed, respectively, by mass percentage.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 60min to form a mixture.
(3) Mixing, adding into quartz crucible, and keeping temperature at 1570 deg.C for 3.5 h.
(4) And pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 550 ℃ for annealing for 3h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And (4) grinding the mixture, and screening the mixture by a standard sieve of 300 meshes to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 4: 3. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 3:5: 5.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold was placed at 1100 ℃ for 40 min.
(3) And (4) transferring the mould into a muffle furnace, heating to 850 ℃, preserving heat for 1.5h, then closing the muffle furnace, and cooling the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
Through NETThe linear expansion of the quartz glass sealing system is tested by ZSCH DIL 402PC, and the prepared quartz sealing system has the linear expansion of 1.306 multiplied by 10-7/° c (room temperature to 700 ℃).
Example 5:
first step, preparation of microcrystalline glass powder
(1) First, 40 wt% of quartz sand, 21 wt% of alumina, 4 wt% of lithium carbonate, 27 wt% of germanium oxide, 2 wt% of zinc oxide, 2 wt% of titanium dioxide, 1.5 wt% of zirconium dioxide, 0.5 wt% of barium nitrate, and 2 wt% of molybdenum oxide were weighed in mass percentage, respectively.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 45min to form a mixture.
(3) Mixing uniformly, adding into a quartz crucible, and keeping the temperature at 1600 ℃ for 4 h.
(4) Pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 570 ℃ for annealing for 3h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And sieving the crushed glass powder by a standard sieve of 200 meshes to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer is prepared according to the weight ratio of the glass material to the organic material of 1: 1. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 3:5: 6.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold was held at 1140 ℃ for 30 min.
(3) And (4) transferring the mould into a muffle furnace, heating to 800 ℃, preserving heat for 1h, then closing the muffle furnace, and cooling the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
The linear expansion of the quartz glass sealing system is tested by NETZSCH DIL 402PC, and the linear expansion of the prepared quartz sealing system is 1.241 multiplied by 10-7/° c (room temperature to 700 ℃).
Example 6:
first step, preparation of microcrystalline glass powder
(1) First, 37 wt% of quartz sand, 20 wt% of alumina, 4 wt% of lithium carbonate, 30 wt% of germanium oxide, 2 wt% of zinc oxide, 3 wt% of titanium dioxide, 1.5 wt% of zirconium dioxide, 0.5 wt% of barium nitrate, and 2 wt% of molybdenum oxide were weighed, respectively, in mass percent.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 50min to form a mixture.
(3) Mixing uniformly, adding into a quartz crucible, and keeping the temperature at 1600 ℃ for 5 h.
(4) And pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 550 ℃ for annealing for 3.5h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And (4) crushing, and screening by a 250-mesh standard sieve to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 2: 1. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 3:4: 5.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold was held at 1160 deg.C for 35 min.
(3) And (4) transferring the mould into a muffle furnace, heating to 860 ℃ and preserving heat for 1.5h, and then closing the muffle furnace to cool the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
The linear expansion of the quartz glass sealing system is tested by NETZSCH DIL 402PC, and the linear expansion of the prepared quartz sealing system is 1.181 multiplied by 10-7/° c (room temperature to 700 ℃).
Example 7:
first step, preparation of microcrystalline glass powder
(1) First, 40 wt% of quartz sand, 18 wt% of alumina, 5 wt% of lithium carbonate, 26 wt% of germanium oxide, 1.5 wt% of zinc oxide, 3 wt% of titanium dioxide, 2.5 wt% of zirconium dioxide, 1.2 wt% of barium nitrate, and 2.8 wt% of molybdenum oxide were weighed in mass percentage, respectively.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 50min to form a mixture.
(3) Mixing uniformly, adding into a quartz crucible, and keeping the temperature at 1600 ℃ for 3 h.
(4) And pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 550 ℃ for annealing for 5h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And (4) crushing, and screening by a 250-mesh standard sieve to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 4: 3. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 3:5: 5.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold was placed at 1100 ℃ and held for 50 min.
(3) And (4) transferring the mould into a muffle furnace, heating to 860 ℃ and preserving heat for 1.5h, and then closing the muffle furnace to cool the mould along with the furnace. Thus obtaining the sealed transparent quartz glass product.
Example 8:
first step, preparation of microcrystalline glass powder
(1) First, 36 wt% of quartz sand, 22 wt% of alumina, 5 wt% of lithium carbonate, 26 wt% of germanium oxide, 1.5 wt% of zinc oxide, 3 wt% of titanium dioxide, 2.5 wt% of zirconium dioxide, 1.0 wt% of barium nitrate, and 3.0 wt% of molybdenum oxide were weighed in mass percentage, respectively.
(2) And then putting the weighed quartz sand, aluminum hydroxide, lithium carbonate, germanium oxide, zinc oxide, titanium dioxide, zirconium dioxide, barium nitrate, molybdenum oxide and the like into a V-shaped mixer to mix for 50min to form a mixture.
(3) Mixing uniformly, adding into quartz crucible, and keeping temperature at 1500 deg.C for 5 h.
(4) Pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 560 ℃ for annealing for 5h, and then cooling along with the furnace.
(5) And (4) putting the cooled glass into a customized cylindrical die, and crushing the glass by using a hydraulic tabletting primary machine. And (4) crushing, and screening by a 250-mesh standard sieve to obtain the glass powder.
Second, cleaning the quartz plate
(1) Firstly, the surface of quartz is cleaned by ultrasonic waves, and the quartz is soaked in acetone, ethanol and deionized water and cleaned by ultrasonic waves for about five minutes.
(2) The surface is cleaned by using sulfuric acid and RCA solution to remove organic and inorganic contaminants.
Third, coating a glass layer
(1) In order to make the sealing glass layer more uniform, terpineol, organic ethyl cellulose and butyl carbitol are required to be uniformly mixed with glass powder and coated on the surface of quartz glass. The coating layer was formulated with a glass frit to organic frit weight ratio of 2: 1. The three organic reagents were mixed in a weight ratio of ethyl cellulose, butyl carbitol and terpineol of 1:3: 3.
Fourthly, heating and sealing
(1) The quartz plate with the coated glass layer on one side is aligned with the other plate and put into a special mould.
(2) The mold was held at 1200 ℃ for 20 min.
(3) The mould is transferred into a muffle furnace, heated to 870 ℃ and kept warm for 1.5h, then the muffle furnace is closed, and the mould is cooled along with the furnace. Thus obtaining the sealed transparent quartz glass product.
The quartz glass sealing system prepared by the invention can be applied to the field of military aviation, can be used for sealing the quartz glass used for the aerospace windows of space shuttles and spaceships, can adapt to the extreme conditions of the space, cannot generate the electrostatic shielding effect, and fully exerts the excellent performance of the quartz glass. The ceramic tile can be used for sealing quartz glass ceramic tiles on the outer shell of a space plane, can resist high temperature after sealing, and cannot generate overlarge stress at a sealing part due to heating because of good thermal expansion coefficient matching, so that the sealing is cracked or separated. The excellent thermal shock resistance can also ensure that the sealing system has long service life, can be used for many times and reduces the cost. The sealing system has uniform stress distribution, so that the sealing system has good three-dimensional uniformity and meets the application requirement in the laser reflector.
The present invention is described in detail with reference to the above embodiments, and those skilled in the art will understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (6)
1. A preparation method of high-strength reliable sealed quartz glass is characterized by comprising the following steps: the method specifically comprises the following steps:
first, preparation of glass frit
(1.1) weighing 36-40 wt% of quartz sand, 18-22 wt% of alumina, 3-5 wt% of lithium carbonate, 26-30 wt% of germanium oxide, 1.5-3 wt% of zinc oxide, 2-3 wt% of titanium dioxide, 1.5-2.5 wt% of zirconium dioxide, 0.5-1.2 wt% of barium nitrate and 2-3 wt% of molybdenum oxide according to mass percentage;
(1.2) fully mixing the materials weighed in the step (1.1), adding the mixture into a quartz crucible, and keeping the temperature at 1500-1600 ℃ for 3-5 hours to obtain glass liquid;
(1.3) pouring molten glass on a steel plate, sending the steel plate into a muffle furnace at 550-600 ℃ for annealing for 3-5 h, and then cooling along with the furnace;
(1.4) crushing the cooled glass, and sieving to obtain glass powder;
second, cleaning the quartz glass
Cleaning quartz glass to remove surface pollutants;
third, coating a glass layer
Taking ethyl cellulose, butyl carbitol and terpineol according to the weight ratio of (1-3) to (3-6) to obtain an organic material, mixing the glass material prepared in the first step and the organic material according to the weight ratio of (2-4) to (1-3), and coating the mixture on the surface of quartz glass to form a glass layer;
fourthly, heating and sealing
(4.1) aligning and sticking the quartz glass with the coated glass layer on one surface and the other piece of quartz glass together, and putting the quartz glass and the other piece of quartz glass into a mould to keep the temperature for 20-50 min at 1100-1200 ℃;
and (4.2) transferring the mold into a muffle furnace, heating to 800-900 ℃, preserving heat for 1-2 h, and turning off the muffle furnace to cool along with the furnace to obtain the sealing quartz glass.
2. A method of producing a high strength, reliable sealed quartz glass according to claim 1, characterized in that: and (3) putting the weighed materials into a V-shaped mixer to mix for 40-60 min in the step (1.2) to form a mixture.
3. A method of producing a high strength, reliable sealed quartz glass according to claim 1, characterized in that: and (1.4) putting the cooled glass into a cylindrical die, crushing the glass by using a hydraulic tablet press, and sieving to obtain glass powder.
4. A method of producing a high strength, reliable sealed quartz glass according to claim 1, characterized in that: and (1.4) crushing the glass, and screening the crushed glass by a standard sieve of 200-300 meshes to obtain glass powder.
5. The method for preparing a high-strength and reliable sealed quartz glass according to claim 1, wherein the second step of cleaning the quartz glass comprises the following specific steps:
(2.1) firstly, soaking quartz glass in acetone, ethanol and deionized water respectively, and carrying out ultrasonic cleaning for five minutes respectively;
and (2.2) cleaning by using sulfuric acid and RCA solution respectively to remove organic and inorganic pollutants on the surface.
6. A sealed quartz glass produced by the production method according to any one of claims 1 to 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114988703A (en) * | 2022-06-28 | 2022-09-02 | 陕西科技大学 | Sealing glass compound and preparation method and application method thereof |
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