WO2015196537A1 - 真空玻璃的制备方法 - Google Patents

真空玻璃的制备方法 Download PDF

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Publication number
WO2015196537A1
WO2015196537A1 PCT/CN2014/084161 CN2014084161W WO2015196537A1 WO 2015196537 A1 WO2015196537 A1 WO 2015196537A1 CN 2014084161 W CN2014084161 W CN 2014084161W WO 2015196537 A1 WO2015196537 A1 WO 2015196537A1
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WIPO (PCT)
Prior art keywords
glass
vacuum
piece
sheet
melting point
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PCT/CN2014/084161
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English (en)
French (fr)
Inventor
滕少波
滕腾
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滕少波
滕腾
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Publication of WO2015196537A1 publication Critical patent/WO2015196537A1/zh

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Classifications

    • 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
    • C03B23/24—Making hollow glass sheets or bricks
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
    • 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
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A30/00—Adapting or protecting infrastructure or their operation
    • Y02A30/24—Structural elements or technologies for improving thermal insulation
    • Y02A30/249—Glazing, e.g. vacuum glazing
    • 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
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
    • Y02B80/22—Glazing, e.g. vaccum glazing
    • 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

Definitions

  • the present invention relates to the field of vacuum glass, and in particular to a method of preparing vacuum glass.
  • the vacuum layer of vacuum glass can effectively block indoor and outdoor heat conduction, significantly reduce indoor air-conditioning computer machine pollutants and greenhouse gas emissions, has good thermal insulation performance, can reduce the transmission of noise, vacuum glass because of its superiority
  • the performance of the application is very extensive.
  • the application number is 2013106090473, and the publication date is March 19, 2014.
  • the invention patent application entitled the preparation process of vacuum glass discloses a method for preparing vacuum glass, and the lead-free glass powder is dispersed on the surface of the glass to form The fulcrum with the designed height and area is sent to the tempering furnace for tempering to obtain tempered glass.
  • the flat glass with the suction hole is placed on one side of the tempered glass belt fulcrum, and the vent hole is sealed by vacuuming after sealing.
  • the vacuum glass prepared by the method has two defects: First, the preparation time is relatively long, generally it takes eight hours to obtain vacuum glass, such as the setting of the fulcrum, the height, area and diameter of the pointing point are strictly controlled, which is time consuming and laborious; Second, the surface of the vacuum glass has air venting holes, and the vacuum glass surface has different pressure bearing capacities and is not aesthetically pleasing.
  • the application number is 2012103740367, and the publication date is March 6, 2013.
  • the invention is a patent application for vacuum glass and a preparation method thereof.
  • the vacuum glass is prepared by vacuuming in a vacuum furnace while heating.
  • the method produces vacuum glass, and the low melting point sealing glass powder is easy to foam and carbonize under high temperature and high negative pressure, and the solubility of lead and tin in the low melting point sealing glass powder is low, and the lead tin is easy to seal the glass from the low melting point.
  • the powder is detached to form a carbonized black line, thereby affecting the gelation property of the low-melting sealing glass powder and affecting the sealing property of the vacuum glass.
  • the present invention provides a method for preparing a vacuum glass which has a short preparation time, a low energy consumption, a good sealing property, and a uniform load carrying capacity.
  • a method for preparing vacuum glass comprising the following steps:
  • step 2 Place the glass: no glue, less glue or glazed glass piece and a piece of glued glass piece processed in step 1 to form a glass group, at least one set of glass groups are arranged above and below the high temperature heating piece, and at least Use a piece of high temperature heating sheet, the glass of each group should be placed in the absence of glue, less glue or glazed glass and direct contact with the high temperature heating sheet.
  • the placed glass group and the high temperature heating sheet are placed in the preheating box.
  • 3 Heating in the kiln Place the pre-heating box in the vacuum kiln, and quickly evacuate the pressure to a pressure of 10 - 1 ⁇ 10 - 3 pa.
  • the high temperature heating sheet is heated by electricity, and the high temperature heating sheet is glued, less glued or Direct contact between the glazed glass sheets, the heat is transferred from the non-adhesive, less glue or glazed glass sheet to the rubber surface with the glue glass sheet, and heated to a low melting point sealing glass powder in a gel form during heating At the same time, the glass sheet is pressed and pressed, and when the thickness between the two glass sheets reaches the thickness standard of the vacuum glass, the high temperature heating sheet stops heating;
  • the hot gas is introduced into the vacuum kiln.
  • the purpose of injecting hot air is to prevent the glass in the kiln from being damaged at high temperature, destroying the vacuum environment in the vacuum kiln and canceling the vacuum. After the piece pressure, remove the pre-heating box.
  • the glass piece coated with the low melting point sealing glass powder is placed in a tempering furnace and heated to 650 to 750, and heated for 2 to 3 minutes to make the low melting point sealing glass powder gelatinous, blasting. Purging and cooling, the low melting point sealing glass powder is solidified on the glass piece, the glass is tempered to become tempered glass, and the upper surface of the low melting point sealing glass powder forms a concave and convex point for supporting action, and the glass is combined by step 2 A suction port is formed after the sheet.
  • the blast purging makes the surface of the low melting point sealing glass adhesive uneven, and the glueless, less glued or glazed glass piece and the laminated glass piece are placed in a group of glass, and the concave and convex points can form a suction port. Therefore, there is no need to separately provide a suction port between the two glass sheets, which saves preparation time and reduces energy consumption; meanwhile, during the blast cleaning process, moisture, organic or inorganic impurities on the glass surface are evaporated, and will not be in the two glass sheets. The formation of bubbles between the two, eliminating the carbonization of the vacuum glass.
  • the glass piece coated with the low melting point sealing glass powder can also be heated to 420 ⁇ 480 ° C, and heated for 20 ⁇ 30min, until the low melting point sealing glass powder is gelatinous, and the temperature is lowered to normal temperature, so that the low melting point sealing glass powder Cured on a glass slide.
  • After heating when applying low-melting sealing glass powder to the four edges of the glass, apply the low-melting sealing glass powder along the upper surface of the coated low-melting sealing glass powder, and apply the low melting point sealing glass powder.
  • the height is higher than the upper surface of the low melting point sealing glass powder, the low melting point sealing glass powder is heated to a gel shape, and after cooling to normal temperature, the low melting point sealing glass powder which is applied by the interval is cooled and solidified, and after the glass is laminated by the step 2 Form a suction port.
  • the low temperature heating sheet or the glass filament sheet may be disposed between the adjacent two glass groups disposed in the step 2, and the low temperature heating sheet or the glass filament sheet is directly in contact with the glued glass sheet; or may be placed in the step 2
  • a low temperature heating sheet or a glass filament sheet is disposed under the bottom glass group, and the low temperature heating sheet or the glass filament sheet is directly in contact with the plastic glass sheet.
  • the glass may be pre-heated in the pre-heating box, and the heating temperature of the high-temperature heating sheet is not higher than 300 ° C, and the temperature of the glass sheet is ensured at the same time. Not higher than 200 ° C to prevent the glue from melting in advance.
  • Preheating the glass can preheat the contents of the preheating box, reducing the heating time in the vacuum kiln and improving the utilization rate of the vacuum kiln.
  • the low temperature heating sheet can be heated without electricity, and is directly connected with the high temperature heating sheet.
  • the contactless glue, less glue or glazed glass will transfer the heat transfer to the glued glass piece which is in direct contact with the low temperature heating piece or the glass wire piece. It is found in the production that even if the low temperature heating piece is not energized, it is heated with low temperature. The temperature of the glass piece that is in direct contact with the sheet also reaches about 200 °C.
  • step 2 When placing the glass in step 2, place at least one high temperature heating sheet. At this time, the high temperature heating sheet and several glass groups are placed in the vertical direction in the order.
  • the small-glue glass sheet that is, the four edges of the glass is coated with a small amount of low-melting sealing glass powder, and when the sheet is heated, there is less between the glass sheet and the glass sheet, compared with the glass sheet with the glue and Adhesive glass sheets are easier to bond and have a better bonding effect.
  • the glazed glass sheet i.e., the four edges of the glass, is coated with an aqueous glass glaze, and the aqueous glass glaze is cured at the four edges of the glass.
  • the purpose of curing the water-based glass glaze at the four edges of the glass is to prevent the low-melting sealing glass glue from collapsing to the inside of the glass at a high temperature, thereby ensuring the aesthetic appearance of the vacuum glass; on the other hand, the water-based glass glaze can also be viscous
  • the bonding effect, that is, the adhesion between the water-based glass glaze and the low-melting sealing glass glue is better than that between the glass and the low-melting sealing glass glue.
  • the beneficial effects of the invention are as follows: (1) The heating time of the vacuum kiln is shorter than the existing production process, saving energy, especially after preheating and heating in the vacuum kiln, which greatly reduces Production time, the entire preparation process only takes 1 ⁇ 2 hours, which reduces the production cost; (2) The glass piece is heated by the heating piece, the temperature change of the glass piece is uniform during the heating process, and is not affected by the vacuum environment. The effect can be achieved by contact heating to transfer heat to the glass to reduce heat loss, thereby achieving energy saving effect; (3) There is no need to separately set the suction port, and the purified low melting point sealing glass powder is on the corner of the glass.
  • the glass glue at the edge seals the two glasses under external force and high temperature; (4) pre-applying low melting point under normal temperature and pressure Sealing the glass powder and curing it at the four edges of the glass in advance can improve the bonding strength of the low melting point sealing glass glue to the glass; (4) Applying low melting by pre-application
  • the glass frit is sealed and pre-cured at the four edges of the glass, and the high-temperature heating sheet and the low-temperature heating sheet are placed together to process the multi-layer vacuum glass at the same time, thereby improving the utilization rate of the equipment, reducing the production cost, and energy-saving energy.
  • the low melting point sealing glass glue does not generate bubbles, is not easily carbonized, does not appear black lines, and ensures the quality of the vacuum glass.
  • FIG. 1 is a schematic view showing the arrangement of a glass piece of the present invention in the first embodiment.
  • the method for preparing vacuum glass according to the present invention comprises the following steps: The first step is to heat the glass, and the low melting point sealing glass powder is cured: the low melting point sealing glass powder is applied to the four edges of the glass sheet, and the melting point of the low melting point sealing glass powder is 420 to 440 ° C ; The glass plate with low melting point sealing glass powder is placed in a tempering furnace and heated to 650 ⁇ 750 °C, and then heated for 2 ⁇ 3 minutes, the low melting point sealing glass powder is melted and gelatinized, and then blown and cooled.
  • the low-melting sealing glass powder is solidified on the glass, and during the blast blowing process, the upper surface of the cured low-melting sealing glass glue forms a concave and convex point which can play a supporting role, and the tempered glass becomes Tempered glass.
  • the glass subjected to the above treatment finally forms a rubberized glass sheet.
  • the glass is placed: the glueless glass piece and the glued glass piece processed by the step 1 form a glass group, and the uneven surface of the upper surface of the low-melting sealing glass glue becomes a glued glass piece and no glue.
  • At least one set of glass sets is arranged above and below the high temperature heating sheet, and at least one high temperature heating piece is used, and each set of glass is placed to ensure direct contact between the glueless glass piece and the high temperature heating piece to prevent the glass from being glued. After the sheet is in direct contact with the high temperature heating sheet, the temperature rises too fast, so that the glue on the glass sheet is melted sufficiently to generate bubbles.
  • the glass placed in the first embodiment is shown in Fig. 1.
  • the glass group A is located at the bottom.
  • a low temperature heating sheet is disposed under the glass group A.
  • a high temperature heating sheet I is arranged above the glass group A
  • a glass group B is arranged above the high temperature heating sheet I
  • a glass group C is arranged above the glass group B
  • a low temperature addition is provided between the glass group B and the glass group C.
  • Warm film A high temperature heating sheet II is arranged above the glass group C
  • a glass group D is arranged above the high temperature heating sheet II, that is, a set of glass groups are arranged above and below the high temperature heating sheet in the embodiment, and two adjacent glass sheets are respectively arranged.
  • the glueless glass sheets are in direct contact with the high temperature heating sheets, and the rubber glass sheets are in direct contact with the low temperature heating sheets.
  • the high temperature heating sheet, the glass group and the low temperature heating sheet are placed in the vertical direction in the above-described order, and the number of the sheets can be determined according to the height inside the vacuum kiln and the actual production.
  • the placed glass set and the high temperature warming sheet are placed in the preheating box.
  • the purpose of setting the low temperature heating sheet is to prevent the glass from being worn and to function as a low temperature heating.
  • the third step, preheating the glass is preheated in the preheating box, and the high temperature heating sheet is energized and heated during the preheating process, and the low temperature heating sheet can be electrified or not energized according to the actual working condition.
  • the heating temperature of the high temperature heating sheet is not higher than 300 ° C ; the temperature of the plastic glass sheet is not higher than 200 ° C.
  • the fourth step heating in the kiln: placing the pre-heating box in the vacuum kiln, and quickly pumping the vacuum to a pressure of 10 - 1 ⁇ 10 - 3 pa in the vacuum kiln, heating the high temperature heating sheet, heating the high temperature sheet and
  • the glueless glass piece is in direct contact, and the heat generated by the electricity is transferred to the glueless glass piece, and the glueless glass piece transfers heat to the rubber surface of the glued glass piece by direct contact with the glued glass piece, and the heat is applied. It is transferred to the rubberized glass sheet to heat the rubberized glass sheet, and the low temperature heating sheet which is in direct contact with the plastic glass sheet can also heat the rubberized glass sheet.
  • the low melting point sealing glass powder is gelatinized again after the first step of curing, and the high temperature heating sheet and the low temperature heating sheet stop heating.
  • the glass sheets are simultaneously pressed together, and when the thickness between the two glass sheets is pressed to the thickness standard of the vacuum glass, the high temperature heating sheet and the low temperature heating sheet stop heating.
  • the low-melting sealing glass glue is simultaneously heated during the splicing process of the external pressure until the low-melting sealing glass glue is completely melted, thereby bonding the upper and lower pieces of glass.
  • the entire molten low-melting sealing glass paste is pressed by the external pressure, and the non-gel glass sheet is pressed against the rubber surface of the rubber glass sheet, so that the low melting point sealing glass glue is not in contact with the vacuum when it is in a molten state, so During the melting process, the low melting point sealing glass glue does not generate bubbles or black lines.
  • Step 5 Take out the vacuum glass: Pass the hot gas into the vacuum kiln, destroy the vacuum environment in the vacuum kiln and cancel the pressure of the splicing. Then take out the pre-heating box and take the vacuum glass out of the pre-heating box to complete the vacuum. Production of glass.
  • the low temperature glass sheets between the adjacent two glass groups and under the bottom glass group may be replaced by glass filament sheets, which may function as heat transfer. It is also possible to arrange no glass filaments or low temperature glass sheets between adjacent glass groups and under the bottom glass group, that is, direct contact between adjacent glass groups.
  • the preheating step can be omitted, that is, the glass is placed and placed directly in the vacuum kiln for heating.
  • at least one set of glass groups is placed above and below the high temperature heating sheet.
  • the inside of the vacuum kiln is provided with at least one layer.
  • a plurality of rows of glass placed through the second step can be placed in the vacuum kiln.
  • the low melting point sealing glass powder is cured, and the low melting point sealing glass powder is applied to the four edges of the glass sheet while sealing along the already coated low melting point.
  • the upper surface of the glass powder is further coated with a low melting point sealing glass powder, and the low melting point sealing glass powder which is applied at intervals is higher than the upper surface of the low melting sealing glass powder, and the glass sheet coated with the low melting point sealing glass powder is heated.
  • the low melting point sealing glass powder is solidified on the glass piece.
  • the intermittently applied low melting point sealing glass frit is cooled and solidified into a suction port between the two glass sheets.
  • the glueless glass piece is replaced by a small glass piece, that is, a small amount of glue formed by heating and solidifying a low melting point sealing glass powder to be cooled and solidified at the four edges of the glass, and heat curing
  • a small glass piece that is, a small amount of glue formed by heating and solidifying a low melting point sealing glass powder to be cooled and solidified at the four edges of the glass, and heat curing
  • the way is achieved by the first step in the first example.
  • the adhesion between the less adhesive glass sheet and the rubberized glass sheet is better.
  • the non-glue glass sheet is replaced by a glazed glass sheet, that is, the water-based glass glaze is cured at the four edges of the glass, and the purpose of providing the cured water-based glass glaze is to prevent the molten state from being low during heating.
  • the melting point seals the glass glue to diffuse into the glass, which affects the appearance of the vacuum glass.
  • the water-based glass glaze can also play the role of bonding, that is, the bonding effect between the water-based glass glaze and the low-melting sealing glass glue is better than that of the glass and Bonding effect between low melting point sealing glass glue it is good. .
  • the glueless glass sheet, the glued glass sheet and the glazed glass sheet can be used in combination at the same time.
  • Example 2 Different from Example 1, in the present embodiment, a low melting point sealing glass paste having a melting point of 460 to 500 ° C was used.
  • the production steps of the vacuum glass were as shown in Example 1, and the glass group after the splicing was preheated and then placed in a vacuum kiln for heating.
  • the glass sheet is heated to 300 ⁇ 430 ° C, the low melting point sealing glass powder is gelatinized again after the first step of curing, and the high temperature heating sheet and the low temperature heating sheet stop heating.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Civil Engineering (AREA)
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Abstract

一种真空玻璃的制备方法，包括以下步骤：①加热玻璃，涂胶固化：将低熔点封接玻璃粉涂于玻璃片的四边边缘处，制成带胶玻璃片，同时带胶玻璃片的四边边缘处设有支点；②摆放玻璃：无胶、少胶或带釉玻璃片与经过步骤①处理的带胶玻璃片合片组成一玻璃组，至少一片高温加温片的上方和下方分别设置至少一组玻璃组，摆放好的玻璃组和高温加温片放置在预加温箱内；③窑内加热：将预加温箱放置于真空窑内，迅速抽真空至压强为10 -1～10 -3pa，高温加温片通电加热，在加热过程中同时对玻璃片加压合片；④取出真空玻璃。该方法缩短制备时间，降低能耗，提高密封性。通过该方法制造的真空玻璃承载能力均匀。

Description

真空玻璃的制备方法 技术领域
本发明涉及真空玻璃领域， 具体地说， 涉及一种真空玻璃的制备方法。
背景技术
真空玻璃的真空层可以有效的阻隔室内外热量传导， 显著地减少室内空调电脑机污染物 和温室气体的排放， 具有很好要的隔热保温性能， 能够降低噪声的传递， 真空玻璃因其优越 的性能应用非常的广泛。
申请号为 2013106090473， 公开日为 2014年 3月 19日， 名称为真空玻璃的制备工艺的发 明专利申请， 公开了一种真空玻璃的制备方法， 将无铅玻璃粉置于分散于玻璃表面， 形成具 有设计高度和面积的支点， 送入钢化炉内钢化制备得到钢化玻璃， 将带有抽气孔的平板玻璃 置于钢化玻璃带支点的一侧， 封边后抽真空， 将排气孔封住。 该方法所制备的真空玻璃存在 两方面缺陷： 一是制备时间比较长， 一般需八小时才能得到真空玻璃， 比如支点的设置， 指 点的高度、 面积、 直径都是需要严格控制的， 费时费力； 二是真空玻璃的表面有抽气孔， 真 空玻璃表面承压能力不同， 同时也不美观。
申请号为 2012103740367， 公开日为 2013年 3月 6日， 名称为真空玻璃及其制备方法的 发明专利申请， 所公开的真空玻璃的制备方法是在真空炉内边加热升温边抽真空， 采用该方 法产生真空玻璃， 低熔点封接玻璃粉在高温及高负压下易起泡、 碳化， 同时低熔点封接玻璃 粉中的铅、 锡等溶解度较低， 铅锡容易从低熔点封接玻璃粉中脱离处理， 形成碳化的黑线， 从而影响低熔点封接玻璃粉的胶凝性， 影响真空玻璃的密封性。
发明内容
为解决上述问题， 本发明提供一种制备时间短、 降低能耗、 密封性好、 承载能力均匀的 真空玻璃的制备方法。
本发明是采用以下的技术方案实现的： 一种真空玻璃的制备方法， 包括以下步骤：
①加热玻璃， 涂胶固化： 将低熔点封接玻璃粉涂于玻璃片的四边边缘处， 高温加热至低 熔点封接玻璃粉呈胶状， 恢复室温后低熔点封接玻璃粉固化在玻璃上， 形成带胶玻璃片， 同 时带胶玻璃片的四边边缘处设有支点；
②摆放玻璃： 无胶、 少胶或带釉玻璃片与经过步骤①处理的带胶玻璃片合片组成一玻璃 组， 高温加温片的上方和下方分别设置至少一组玻璃组， 且至少采用一片高温加温片， 各组 玻璃的摆放要保证无胶、 少胶或带釉玻璃片与高温加温片直接接触， 摆放好的玻璃组和高温 加温片放置在预加温箱内； ③窑内加热： 将预加温箱放置于真空窑内， 迅速抽真空至压强为 10―1〜 10— 3pa， 高温加温 片通电加热， 通过高温加温片与无胶、 少胶或带釉玻璃片之间的直接接触， 将热量由无胶、 少胶或带釉玻璃片传递至带胶玻璃片的胶面上， 加热至低熔点封接玻璃粉呈胶状， 在加热过 程中同时对玻璃片加压合片， 两玻璃片之间的厚度达到真空玻璃的厚度标准时， 高温加温片 停止加热；
④取出真空玻璃： 待低熔点封接玻璃胶达到一定固化后， 向真空窑内通入热气， 注入热 气的目的是防止窑内玻璃在高温下不破损， 破坏真空窑内的真空环境并撤销合片压力后， 取 出预加温箱。
本发明中的步骤①中， 将涂有低熔点封接玻璃粉的玻璃片置于钢化炉内加热至 650〜 750 后， 加热 2〜3min， 使低熔点封接玻璃粉呈胶状， 鼓风吹扫降温， 使低熔点封接玻璃粉 固化在玻璃片上， 玻璃经过钢化处理后成为钢化玻璃， 同时使低熔点封接玻璃粉的上表面形 成用于支撑作用的凹凸点， 经步骤②玻璃合片后形成抽气口。 鼓风吹扫使低熔点封接玻璃胶 表面呈凹凸不平， 无胶、 少胶或带釉玻璃片与带胶玻璃片合片摆放呈一组玻璃组后， 凹凸点 即可形成抽气口， 因此在两玻璃片之间无需另外设置抽气口， 节省了制备时间， 降低能耗； 同时鼓风吹扫过程中， 玻璃表面的水分、 有机或无机杂质被蒸发掉， 不会在两玻璃片之间形 成气泡， 杜绝了真空玻璃碳化的情况。
也可以将涂有低熔点封接玻璃粉的玻璃片加热至 420〜480°C， 并加热 20〜30min， 至低 熔点封接玻璃粉呈胶状， 降温至常温， 使低熔点封接玻璃粉固化在玻璃片上。 加热前， 在玻 璃的四边边缘涂低熔点封接玻璃粉时， 沿已经涂好的低熔点封接玻璃粉的上表面再间隔涂抹 低熔点封接玻璃粉， 间隔涂抹的低熔点封接玻璃粉高度高于低熔点封接玻璃粉的上表面， 低 熔点封接玻璃粉加热至呈胶状， 并降温至常温后， 间隔涂抹的低熔点封接玻璃粉冷却固化， 经步骤②玻璃合片后形成抽气口。
步骤②中摆放的相邻两玻璃组之间可以设有低温加温片或玻璃丝片， 并且低温加温片或 玻璃丝片直接与带胶玻璃片接触； 也可以在步骤②中摆放的位于底部的玻璃组下方设置低温 加温片或玻璃丝片， 低温加温片或玻璃丝片直接与带胶玻璃片接触。 通过设置低温加温片可 以提高玻璃片的升温速度， 提高真空窑的生产效率； 玻璃丝片可以起到传递热量的作用； 同 时低温加温片或玻璃丝片还可以防止玻璃表面的磨损， 保证真空玻璃的成品率。
步骤③中， 预加温箱放入真空窑内之前， 玻璃可以先在预加温箱进行预加热， 高温加温 片的加热温度不高于 300°C，同时要保证带胶玻璃片的温度不高于 200°C，以防止胶提前熔化。 对玻璃进行预加热可以提前对预加温箱内的物品进行烘烧， 减少了在真空窑中加热的时间， 提高了真空窑的利用率。 预加热过程中， 低温加温片可以不通电加热， 与高温加温片直接接 触的无胶、 少胶或带釉玻璃会将传热量传递给与低温加温片或玻璃丝片直接接触的带胶玻璃 片，在生产中发现，即使低温加温片不通电，与低温加温片直接接触的玻璃片温度也达到 200°C 左右。
步骤②中摆放玻璃时， 至少摆放一个高温加温片， 此时高温加温片和数个玻璃组按照顺 序沿竖直方向摆放。
本发明中， 所述的少胶玻璃片即玻璃的四边边缘处涂有少量低熔点封接玻璃粉， 在加热 合片时少胶玻璃片和带胶玻璃片之间， 比带胶玻璃片和无胶玻璃片之间黏合更加容易， 黏合 效果更好。 所述的带釉玻璃片即玻璃的四边边缘处涂有水性玻璃釉， 水性玻璃釉固化在玻璃 的四边边缘处。 在玻璃的四边边缘固化水性玻璃釉的目的是一方面可以防止高温下胶状的低 熔点封接玻璃胶向玻璃内部扩散， 保证真空玻璃的美观性； 另一方面水性玻璃釉也可以起到 粘接的作用， 即水性玻璃釉与低熔点封接玻璃胶之间的黏合效果比玻璃与低熔点封接玻璃胶 之间的黏合效果好。
与现有技术相比， 本发明的有益效果是： （1 ) 真空窑加热时间较现有的生产工艺要短， 节约能源， 尤其是经过预加热后再在真空窑内加热， 极大地降低了生产时间， 整个制备工艺 仅需 1〜2个小时， 降低了生产成本； （2)采用加温片对玻璃片进行加热， 在升温过程中玻璃 片各处的温度变化比较均匀， 不受真空环境的影响， 可通过接触式加热将热量传递给玻璃， 减少热损失， 从而达到节能的效果； （3) 不需要单独设置抽气口， 经吹扫后的低熔点封接玻 璃粉在玻璃边角上呈波浪状， 两玻璃合片后自然形成抽气口， 省时省力， 抽真空后， 边缘处 的玻璃胶在外力和高温作用下密封两块玻璃； （4) 在常温常压下预先涂抹低熔点封接玻璃粉 并提前固化在玻璃的四边边缘处， 可以提高低熔点封接玻璃胶与玻璃的黏合强度； （4) 通过 预先涂抹低熔点封接玻璃粉并提前固化在玻璃的四边边缘处， 并利用高温加热片与低温加热 片的配合摆放， 可同时加工多层真空玻璃， 提高了设备的利用率， 降低生产成本， 节能能源； ( 5)在该真空玻璃的生产方法中， 低熔点封接玻璃胶不会产生气泡， 不易被碳化， 不会出现 黑线， 保证了真空玻璃的质量。
附图说明
图 1为实施例 1中本发明玻璃片摆放示意图。
图中： 1真空窑； 2预热箱； 3低温加温片。
具体实施方式
下面结合说明书附图和实施例对本发明做进一步说明。
实施例 1
本发明所述的真空玻璃的制备方法， 包括以下步骤： 第一步， 加热玻璃， 低熔点封接玻璃粉固化： 将低熔点封接玻璃粉涂于玻璃片的四边边 缘处， 该低熔点封接玻璃粉的熔点为 420〜440°C ; 将涂有低熔点封接玻璃粉的带胶玻璃片置 于钢化炉内加热至 650〜750°C后， 持续加热 2〜3min， 使低熔点封接玻璃粉熔化呈胶状， 然 后鼓风吹扫降温， 使低熔点封接玻璃粉固化在玻璃上， 同时鼓风吹扫过程中， 使固化的低熔 封接玻璃胶的上表面形成可以起到支撑作用的凹凸点， 同时经钢化处理后的玻璃成为钢化玻 璃。 经过上述处理的玻璃最终形成带胶玻璃片。
第二步， 摆放玻璃： 无胶玻璃片与经过步骤①处理的带胶玻璃片合片组成一玻璃组， 此 时低熔封接玻璃胶上表面的凹凸面成为带胶玻璃片和无胶玻璃片之间的抽气口。 高温加温片 的上方和下方分别设置至少一组玻璃组， 且至少采用一片高温加温片， 各组玻璃的摆放要保 证无胶玻璃片与高温加温片直接接触，以防止带胶玻璃片与高温加温片直接接触后升温过快， 使得带胶玻璃片上的胶充分熔化而产生气泡。
实施例 1中采用的玻璃摆放方式如图 1所示， 玻璃组 A位于底部， 为了防止玻璃表面磨 损， 玻璃组 A的下方设有低温加温片。 玻璃组 A的上方设有高温加温片 I， 高温加温片 I的 上方设有玻璃组 B，玻璃组 B的上方设有玻璃组 C，玻璃组 B和玻璃组 C之间设有低温加温片。 玻璃组 C的上方设有高温加温片 II， 高温加温片 II的上方设有玻璃组 D， 即本实施例中高温 加温片的上方和下方分别设置一组玻璃组，相邻两玻璃组之间设有低温加温片或高温加温片， 无胶玻璃片与高温加温片直接接触， 带胶玻璃片与低温加温片直接接触。 高温加温片、 玻璃 组和低温加温片照上述顺序沿竖直方向摆放， 其摆放的数量可以根据真空窑内部的高度以及 实际生产情况来决定。 摆放好的玻璃组和高温加温片放置在预加温箱内。 设置低温加温片的 目的除了防止玻璃磨损， 还可以起到低温加温的作用。
第三步， 预加热： 玻璃在预加温箱进行预加热， 预加热过程中高温加温片通电加热， 低 温加温片可以根据实际工作情况选择通电加热或者不通电。 预加热过程中要保证高温加温片 的加热温度不高于 300°C ; 带胶玻璃片的温度不高于 200°C。
第四步， 窑内加热： 将预加温箱放置于真空窑内，迅速抽真空至真空窑内的压强为 10―1〜 10— 3pa， 高温加温片通电加热， 高温加温片与无胶玻璃片直接接触， 将其通电产生的热量传递 给无胶玻璃片， 无胶玻璃片通过与带胶玻璃片的直接接触而将热量传递给带胶玻璃片的胶面 上， 并且将热量传递给带胶玻璃片， 使带胶玻璃片加热， 同时与带胶玻璃片直接接触的低温 加温片也可以对带胶玻璃片加热。 当带胶玻璃片加热至 240〜360°C时， 低熔点封接玻璃粉经 第一步固化后再次呈胶状， 此时高温加温片和低温加温片停止继续升温。 在加热过程中同时 对玻璃片加压合片， 两玻璃片之间的厚度被压至真空玻璃的厚度标准时， 高温加温片和低温 加温片停止加热。 在该步骤中， 在外压力的合片过程中同时对低熔点封接玻璃胶进行加热， 直至低熔点封 接玻璃胶全部熔融， 从而达到胶合上下两片玻璃。 整个熔融的低熔点封接玻璃胶由于受到外 压力的加压， 无胶玻璃片紧压在带胶玻璃片的胶面上， 使低熔点封接玻璃胶在熔融状态时不 与真空接触， 所以在熔融过程中， 低熔点封接玻璃胶不会产生气泡或出现黑线。
第五步， 取出真空玻璃： 向真空窑内通入热气， 破坏真空窑内的真空环境并撤销合片压 力后，取出预加温箱， 将真空玻璃从预加温箱内取出， 从而完成真空玻璃的生产。
本实施例中，相邻两玻璃组之间和底部玻璃组下方的低温玻璃片可以由玻璃丝片来代替， 玻璃丝片可以起到热传递的作用。 相邻两玻璃组之间以及底部玻璃组下方也可以无需设置玻 璃丝片或低温玻璃片， 即相邻两玻璃组之间直接接触。
实际生产过程中， 预加热的步骤可省略， 即玻璃摆放好后直接放入真空窑内加热即可。 本实施例中， 所述高温加温片的上方和下方分别放置至少一组玻璃组。 所述真空窑的内 部至少设有一层。 为了提高真空玻璃的生产效率， 在真空窑内可以放入多排通过步骤二摆放 好的玻璃。
实施例 2
与实施例 1不同的是， 第一步的加热玻璃， 低熔点封接玻璃粉固化中， 将低熔点封接玻 璃粉涂于玻璃片的四边边缘处， 同时沿已经涂好的低熔点封接玻璃粉的上表面再间隔涂抹低 熔点封接玻璃粉， 间隔涂抹的低熔点封接玻璃粉高度高于低熔点封接玻璃粉的上表面， 将涂 有低熔点封接玻璃粉的玻璃片加热至 420〜480°C， 并加热 20-30min， 至低熔点封接玻璃粉呈 胶状， 然后降温至常温， 使低熔点封接玻璃粉固化在玻璃片上。 此时， 间隔涂抹的低熔点封 接玻璃粉冷却固化成两玻璃片之间的抽气口。
其它同实施例 1。
实施例 3
与实施例 1 不同的是， 无胶玻璃片由少胶玻璃片代替， 即玻璃的四边边缘处设有少量的 由低熔点封接玻璃粉加热成胶状后冷却固化形成的胶， 其加热固化方式通过施例 1中的第一 步来实现。 与无胶玻璃片相比， 少胶玻璃片和带胶玻璃片之间的黏合度更好。
其它同实施例 1。
实施例 4
与实施例 1 不同的是， 无胶玻璃片由带釉玻璃片代替， 即玻璃的四边边缘处固化有水性 玻璃釉， 设置固化的水性玻璃釉的目的是一方面防止加热过程中熔融状态的低熔点封接玻璃 胶向玻璃内部扩散， 影响真空玻璃的美观； 另一方面水性玻璃釉也可以起到粘接的作用， 即 水性玻璃釉与低熔点封接玻璃胶之间的黏合效果比玻璃与低熔点封接玻璃胶之间的黏合效果 好。。
同理， 在本发明中， 无胶玻璃片、 带胶玻璃片和带釉玻璃片可以同时混合使用。
其它同实施例 1。
实施例 5
与实施例 1不同的是， 本实施例中采用熔点为 460〜500°C的低熔点封接玻璃胶。 真空玻 璃的生产步骤如实施例 1所示， 合片后的玻璃组经预加热后放入真空窑内加热。 当带胶玻璃 片加热至 300〜430°C时， 低熔点封接玻璃粉经第一步固化后再次呈胶状， 此时高温加温片和 低温加温片停止继续升温。
其它同实施例 1。

Claims

权 利 要 求 书
1、 一种真空玻璃的制备方法， 其特征在于包括以下步骤：
①加热玻璃， 涂胶固化： 将低熔点封接玻璃粉涂于玻璃片的四边边缘处， 高温加热至低 熔点封接玻璃粉呈胶状， 恢复室温后低熔点封接玻璃粉固化在玻璃上， 形成带胶玻璃片， 同 时带胶玻璃片的四边边缘处设有支点；
②摆放玻璃： 无胶、 少胶或带釉玻璃片与经过步骤①处理的带胶玻璃片合片组成一玻璃 组， 高温加温片的上方和下方分别设置至少一组玻璃组， 且至少采用一片高温加温片， 各组 玻璃的摆放要保证无胶、 少胶或带釉玻璃片与高温加温片直接接触， 摆放好的玻璃组和高温 加温片放置在预加温箱内；
③窑内加热： 将预加温箱放置于真空窑内， 迅速抽真空至压强为 10―1〜 10— 3pa， 高温加温 片通电加热， 通过高温加温片与无胶、 少胶或带釉玻璃片之间的直接接触， 将热量由无胶、 少胶或带釉胶玻璃片传递至带胶玻璃片的胶面上， 加热至低熔点封接玻璃粉呈胶状， 在加热 过程中同时对玻璃片加压合片， 两玻璃片之间的厚度达到真空玻璃的厚度标准时， 高温加温 片停止加热；
④取出真空玻璃： 待低熔点封接玻璃胶固化后， 向真空窑内通入热气， 破坏真空窑内的 真空环境并撤销合片压力后，取出预加温箱。
2、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于： 步骤①中， 将涂有低熔点 封接玻璃粉的玻璃片置于钢化炉内加热至 650〜750°C后， 加热 2〜3min， 使低熔点封接玻璃 粉呈胶状， 鼓风吹扫降温， 使低熔点封接玻璃粉固化在玻璃片上， 玻璃片经钢化处理后成为 钢化玻璃， 同时固化后的低熔点封接玻璃粉的上表面形成用于支撑作用的凹凸点， 经步骤② 玻璃合片后形成抽气口。
3、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于： 步骤①中， 将涂有低熔点 封接玻璃粉的玻璃片加热至 420〜480°C， 并加热 20-30min， 至低熔点封接玻璃粉呈胶状， 降 温至常温， 使低熔点封接玻璃粉固化在玻璃片上。
4、 根据权利要求 3所述的真空玻璃的制备方法， 其特征在于： 步骤①中在玻璃的四边边 缘涂低熔点封接玻璃粉时， 沿已经涂好的低熔点封接玻璃粉的上表面再间隔涂抹低熔点封接 玻璃粉， 间隔涂抹的低熔点封接玻璃粉高度高于低熔点封接玻璃粉的上表面， 低熔点封接玻 璃粉加热至呈胶状， 降温至常温， 间隔涂抹的低熔点封接玻璃粉冷却固化， 经步骤②玻璃合 片后形成抽气口。
5、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于： 步骤②中摆放的相邻两玻 璃组之间设有低加温片或玻璃丝片， 低加温片或玻璃丝片直接与带胶玻璃片接触。
6、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于： 步骤②中摆放的位于底部 的玻璃组下方设有低加温片或玻璃丝片， 低加温片或玻璃丝片直接与带胶玻璃片接触。
7、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于： 步骤③中， 预加温箱放入 真空窑内之前， 玻璃在预加温箱进行预加热， 高温加温片的加热温度不高于 300°C。
8、 根据权利要求 1或 7所述的真空玻璃的制备方法， 其特征在于， 步骤③中， 预加温箱 放入真空窑内之前， 玻璃在预加温箱进行预加热， 带胶玻璃片的温度不高于 200°C。
9、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于， 步骤②中摆放玻璃时， 至 少摆放一个高温加温片， 此时高温加温片和数个玻璃组按照顺序沿竖直方向摆放。
10、 根据权利要求 1所述的真空玻璃的制备方法， 其特征在于， 所述带釉玻璃片是四边 边缘处固化有水性玻璃釉的玻璃。
PCT/CN2014/084161 2014-06-26 2014-08-12 真空玻璃的制备方法 WO2015196537A1 (zh)

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