WO2019119611A1 - 一种具有多孔发热膜结构的陶瓷加热体的制备工艺 - Google Patents

一种具有多孔发热膜结构的陶瓷加热体的制备工艺 Download PDF

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WO2019119611A1
WO2019119611A1 PCT/CN2018/074111 CN2018074111W WO2019119611A1 WO 2019119611 A1 WO2019119611 A1 WO 2019119611A1 CN 2018074111 W CN2018074111 W CN 2018074111W WO 2019119611 A1 WO2019119611 A1 WO 2019119611A1
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heating body
ceramic
porous
ceramic heating
sintering
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PCT/CN2018/074111
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English (en)
French (fr)
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丁毅
程宏生
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深圳市卓力能电子有限公司
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Publication of WO2019119611A1 publication Critical patent/WO2019119611A1/zh
Priority to US16/906,518 priority Critical patent/US11498875B2/en

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Definitions

  • the invention relates to the technical field of preparation of a heating body, and more particularly to a preparation process of a ceramic heating body having a porous heating film structure.
  • the silicon nitride heating sheet is a device combining a high-performance silicon nitride ceramic substrate and a long-life and high-power high-temperature metal heating wire, which has the characteristics of small volume, high power and high thermal efficiency, and heat generation through the silicon nitride heating sheet. It has proven to be a safe and reliable method of heating.
  • the conventional silicon nitride ceramic heating sheet is formed by embedding a tungsten wire in a silicon nitride powder and forming a sheet-like body by hot pressing, and the heater produced by the process is difficult to be positioned due to the process limitation. The position is shifted during the process, resulting in uneven heat transfer of the heater. At the same time, due to the obvious interface between the tungsten wire and the silicon nitride powder, it is difficult to become integrated after sintering, and the tungsten wire and the ceramic contact surface form a gap, during heating. Local oxidation is formed to reduce the service life of the heating sheet.
  • reaction sintering results in poor density, poor mechanical properties, and uneven heating of the heating body.
  • the present invention provides a preparation process of a ceramic heating body having a porous heat-generating film structure, wherein the heating body obtained by the preparation process is heated uniformly and has high heating efficiency.
  • the technical solution adopted by the present invention to solve the technical problem thereof is: a preparation process of a ceramic heating body having a porous heat generating film structure, which is improved in that the process comprises the following steps:
  • step B ball milling: adding the grinding ball to the ceramic matrix slurry prepared in step A, and placing it into a ball mill tank for wet ball milling, the time of wet ball milling is 4-24h;
  • Adding a grinding ball to the resistive slurry prepared in the step A, and placing it in a ball mill tank for wet ball milling, and the wet ball milling time is 24-48 h;
  • step B the wet-ball-milled ceramic matrix slurry in step B is defoamed under vacuum;
  • step B The wet-ball milled resistive slurry in step B is defoamed under vacuum;
  • step C molding and drying: the ceramic base slurry prepared in step C is cast into a ceramic substrate of a desired shape by a casting machine, and the ceramic substrate is dried to form an embryo body;
  • step D the green body prepared in step D is placed in a graphite crucible, and the separation powder is buried. Thereafter, the green body buried in the separation powder is sintered in a box furnace under a normal pressure, and the sintering atmosphere is oxygen. The blank body is sintered to obtain a semi-finished product of the porous ceramic heating body base;
  • Wax The paraffin wax is liquefied by a heating cylinder, and the porous ceramic heating body base semi-finished product obtained in the step E is completely immersed in the liquefied paraffin for 1-5 h, and then cooled at room temperature for 4-24 h to obtain a paraffin-containing porous ceramic heating.
  • Body matrix The paraffin wax is liquefied by a heating cylinder, and the porous ceramic heating body base semi-finished product obtained in the step E is completely immersed in the liquefied paraffin for 1-5 h, and then cooled at room temperature for 4-24 h to obtain a paraffin-containing porous ceramic heating.
  • step G machining: the paraffin-containing porous ceramic heating body substrate prepared in step F is machined to remove the paraffin layer on the outer surface of the porous ceramic heating body substrate;
  • the resistive paste prepared in the step C is applied to the outer surface of the porous ceramic heating body substrate prepared in the step G at a desired thickness, and the resistive paste forms a heat generating film on the surface of the ceramic substrate. ;
  • the porous ceramic heating body substrate having the heat generating film structure prepared in the step H is placed in a graphite crucible, and then placed in a sintering furnace for metallization and sintering of the wax discharge and the porous resistance heating film;
  • Electrode The both ends of the heating body body obtained in the step I are subjected to nickel plating on the surface, and then the electrode is brazed and extracted at the portion after the nickel plating treatment to obtain a finished product of the porous ceramic heating body.
  • the ceramic matrix slurry is composed of the following mass percentages of raw materials:
  • the resistive paste is composed of the following mass percentages of raw materials:
  • the ceramic matrix slurry is composed of the following mass percentages of raw materials:
  • the resistive paste is composed of the following mass percentages of raw materials:
  • the ceramic matrix slurry is composed of the following mass percentages of raw materials:
  • the resistive paste is composed of the following mass percentages of raw materials:
  • the sintering temperature of the embryo body is 900-1400 ° C
  • the heating rate is 1-20 ° C / min
  • the holding time is 2-12 h.
  • the temperature rising rate of the metallization sintering is 1-5 ° C / min
  • the metallization sintering temperature is 800-1000 ° C
  • the time is 1-2 h.
  • the invention has the beneficial effects that the present invention provides a preparation process of a ceramic heating body having a porous heat-generating film structure, which is sequentially passed through mixing, ball milling, tray, forming and drying, sintering, waxing, machining, and coating.
  • the coating, metallization and sintering, and the electrode are simple in the whole manufacturing process.
  • the sintered body is sintered in an oxidizing atmosphere and a normal pressure by using a box furnace, and the obtained heating body is uniformly heated and has high heating efficiency.
  • FIG. 1 is a process flow diagram of a process for preparing a ceramic heating body having a porous heat generating film structure according to the present invention.
  • the present invention discloses a process for preparing a ceramic heating body having a porous heat generating film structure. Specifically, the process includes the following steps:
  • A mixing: 21% diatomaceous earth, 16% starch, 1% nano silica solution, 62% deionized water and mixed and stirred according to the mass percentage, to obtain a ceramic matrix slurry;
  • Ball milling adding the grinding ball to the ceramic base slurry prepared in the step A, and placing it in a ball mill tank for wet ball milling, the wet ball milling time is 24 hours; adding the grinding to the resistance slurry prepared in the step A Ball, and placed in a ball mill for wet ball milling, wet ball milling time is 48h;
  • step B defoaming: the wet-ball-milled ceramic matrix slurry in step B is defoamed under vacuum; the wet-ball-milled resistive slurry in step B is defoamed under vacuum;
  • step C molding and drying: the ceramic base slurry prepared in step C is cast into a ceramic substrate of a desired shape by a casting machine, and the ceramic substrate is dried to form an embryo body;
  • step D the green body prepared in step D is placed in a graphite crucible, and the separation powder is buried. Thereafter, the green body buried in the separation powder is sintered in a box furnace under a normal pressure, and the sintering atmosphere is oxygen.
  • the heating rate is 5 ° C / min
  • the sintering temperature is 1200 ° C
  • the holding time is 2 h
  • the green body is sintered to obtain a semi-finished product of the porous ceramic heating body;
  • the paraffin wax is liquefied by a heating cylinder, the porous ceramic heating body substrate semi-finished product obtained in step E is completely immersed in the liquefied paraffin for 5h, and then cooled at room temperature for 24 hours to obtain a paraffin-containing porous ceramic heating body substrate;
  • step G machining: the paraffin-containing porous ceramic heating body substrate prepared in step F is machined to remove the paraffin layer on the outer surface of the porous ceramic heating body substrate;
  • the resistive paste prepared in the step C is applied to the outer surface of the porous ceramic heating body substrate prepared in the step G at a desired thickness, and the resistive paste forms a heat generating film on the surface of the ceramic substrate. ;
  • Metallization Sintering The porous ceramic heating body substrate having the heat generating film structure obtained in the step H is placed in a graphite crucible, and then placed in a sintering furnace for metallization and sintering of the wax discharge and the porous resistance heating film, wherein the temperature is raised.
  • the rate is 2 ° C / min
  • the metallization sintering temperature is 850 ° C
  • the time is 1 h;
  • Electrode The both ends of the heating body body obtained in the step I are subjected to nickel plating on the surface, and then the electrode is brazed and extracted at the portion after the nickel plating treatment to obtain a finished product of the porous ceramic heating body.
  • the present invention discloses a process for preparing a ceramic heating body having a porous heat generating film structure. Specifically, the process includes the following steps:
  • step B ball milling: adding the grinding ball to the ceramic matrix slurry prepared in step A, and placing it into a ball mill tank for wet ball milling, the time of wet ball milling is 14 h;
  • step B defoaming: the wet-ball-milled ceramic matrix slurry in step B is defoamed under vacuum; the wet-ball-milled resistive slurry in step B is defoamed under vacuum;
  • step C molding and drying: the ceramic base slurry prepared in step C is cast into a ceramic substrate of a desired shape by a casting machine, and the ceramic substrate is dried to form an embryo body;
  • step D the green body prepared in step D is placed in a graphite crucible, and the separation powder is buried. Thereafter, the green body buried in the separation powder is sintered in a box furnace under a normal pressure, and the sintering atmosphere is oxygen. The blank body is sintered to obtain a semi-finished product of the porous ceramic heating body; the sintering temperature when the body is sintered is 900 ° C, the heating rate is 1 ° C / min, and the holding time is 2 h;
  • the paraffin wax is liquefied by a heating cylinder, the porous ceramic heating body substrate semi-finished product obtained in step E is completely immersed in the liquefied paraffin for 1 h, and then cooled at room temperature for 4 h to obtain a paraffin-containing porous ceramic heating body substrate;
  • step G machining: the paraffin-containing porous ceramic heating body substrate prepared in step F is machined to remove the paraffin layer on the outer surface of the porous ceramic heating body substrate;
  • the resistive paste prepared in the step C is applied to the outer surface of the porous ceramic heating body substrate prepared in the step G at a desired thickness, and the resistive paste forms a heat generating film on the surface of the ceramic substrate. ;
  • the porous ceramic heating body substrate having the heat generating film structure prepared in the step H is placed in a graphite crucible, and then placed in a sintering furnace for metallization and sintering of the wax discharge and the porous resistance heating film; metallization
  • the heating rate of sintering is 1 ° C / min, the metallization sintering temperature is 800 ° C, the time is 1 h;
  • Electrode The both ends of the heating body body obtained in the step I are subjected to nickel plating on the surface, and then the electrode is brazed and extracted at the portion after the nickel plating treatment to obtain a finished product of the porous ceramic heating body.
  • the present invention discloses a process for preparing a ceramic heating body having a porous heat generating film structure. Specifically, the process includes the following steps:
  • A mixing: 50% diatomaceous earth, 8% starch, 2% nano silica solution, 40% deionized water and mixed and stirred according to the mass percentage, to obtain a ceramic matrix slurry;
  • step B ball milling: adding the grinding ball to the ceramic matrix slurry prepared in step A, and placing it into a ball mill tank for wet ball milling, the time of wet ball milling is 4 h;
  • step B defoaming: the wet-ball-milled ceramic matrix slurry in step B is defoamed under vacuum;
  • step B The wet-ball milled resistive slurry in step B is defoamed under vacuum;
  • step C molding and drying: the ceramic base slurry prepared in step C is cast into a ceramic substrate of a desired shape by a casting machine, and the ceramic substrate is dried to form an embryo body;
  • step D the green body prepared in step D is placed in a graphite crucible, and the separation powder is buried. Thereafter, the green body buried in the separation powder is sintered in a box furnace under a normal pressure, and the sintering atmosphere is oxygen. The blank body is sintered to obtain a semi-finished product of the porous ceramic heating body base; the sintering temperature when the body body is sintered is 1400 ° C, the heating rate is 20 ° C / min, and the holding time is 12 h;
  • the paraffin wax is liquefied by a heating cylinder, the porous ceramic heating body substrate semi-finished product obtained in step E is completely immersed in the liquefied paraffin for 3h, and then cooled at room temperature for 14h to obtain a paraffin-containing porous ceramic heating body substrate;
  • step G machining: the paraffin-containing porous ceramic heating body substrate prepared in step F is machined to remove the paraffin layer on the outer surface of the porous ceramic heating body substrate;
  • the resistive paste prepared in the step C is applied to the outer surface of the porous ceramic heating body substrate prepared in the step G at a desired thickness, and the resistive paste forms a heat generating film on the surface of the ceramic substrate. ;
  • the porous ceramic heating body substrate having the heat generating film structure prepared in the step H is placed in a graphite crucible, and then placed in a sintering furnace for metallization and sintering of the wax discharge and the porous resistance heating film; metallization
  • the heating rate of sintering is 5 ° C / min, the metallization sintering temperature is 1000 ° C, the time is 2 h;
  • Electrode The both ends of the heating body body obtained in the step I are subjected to nickel plating on the surface, and then the electrode is brazed and extracted at the portion after the nickel plating treatment to obtain a finished product of the porous ceramic heating body.
  • the present invention provides a process for preparing a ceramic heating body having a porous heat-generating film structure, which is sequentially passed through mixing, ball milling, tray, molding and drying, sintering, waxing, machining, coating,
  • the ceramic heating body is obtained by metallization sintering and electrode connection, and the whole manufacturing process is simple.
  • the ceramic body is uniformly heated and has high heating efficiency by using a box furnace to sinter the embryo body under an oxidizing atmosphere and a normal pressure.

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Abstract

本发明公开了一种具有多孔发热膜结构的陶瓷加热体的制备工艺，涉及加热体的制备工艺技术领域；该工艺包括混料、球磨、托盘、成型与干燥、烧结、灌蜡、机加工、涂覆、金属化烧结、接电极；本发明的有益效果是：整个制造工艺简单，通过采用箱式炉在氧化气氛和常压下烧结胚体，制得的加热体加热均匀且加热效率高。

Description

一种具有多孔发热膜结构的陶瓷加热体的制备工艺 技术领域
本发明涉及加热体的制备工艺技术领域，更具体的说，本发明涉及一种具有多孔发热膜结构的陶瓷加热体的制备工艺。
背景技术
氮化硅发热片是一种结合高性能氮化硅陶瓷基体和长寿命大功率的高温金属发热丝的器件，其具有体积小，功率大和热效率高等特点，同时通过氮化硅发热片产热也被证明是一种安全可靠的发热方式。
目前，传统的氮化硅陶瓷加热片是将钨丝埋在氮化硅粉末内成型成片状体热压烧结而成，此工艺生产的加热器由于受工艺限制，钨丝很难定位，成型过程中造成位置偏移，造成加热器整体传热不均，同时由于钨丝与氮化硅粉体有明显的界面，烧结后很难成为一体，钨丝与陶瓷接触面形成空隙，加热过程中形成局部氧化，降低发热片的使用寿命。
目前氮化硅陶瓷加热片的烧结也有采用反应烧结，然而反应烧结致密度差，力学性能差，加热体的加热不均匀。
发明内容
为了克服现有技术的不足，本发明提供一种具有多孔发热膜结构的陶瓷加热体的制备工艺，该制备工艺所制得的加热体加热均匀，且加热效率高。
本发明解决其技术问题所采用的技术方案是：一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其改进之处在于：该工艺包括以下的步骤：
A、混料：按质量百分比称取15-55％的硅藻土、5-25％的淀粉、0-2％的纳米二氧化硅溶液、40-70％的去离子水并混合搅拌均匀，制得陶瓷基体浆料；
按质量百分比称取15-40％的电阻浆料、30-60％的淀粉、10-30％的有机溶剂并混和搅拌均匀，制得有造孔剂的电阻浆料；
B、球磨：向步骤A中制得的陶瓷基体浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为4-24h；
向步骤A中制得的电阻浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿 法球磨的时间为24-48h；
C、将步骤B中湿法球磨后的陶瓷基体浆料在真空条件下进行脱泡；
将步骤B中湿法球磨后的电阻浆料在真空条件下进行脱泡；
D、成型与干燥：将步骤C中制得的陶瓷基体浆料用浇注机浇注制成所需形状的陶瓷基体，并将陶瓷基体进行干燥，以形成胚体；
E、烧结：将步骤D制得的坯体置于石墨坩埚中，并埋入隔离粉，此后用箱式炉将埋于隔离粉中的坯体在常压下进行烧结，烧结气氛为氧气，坯体烧结制得多孔陶瓷加热体基体半成品；
F、灌蜡：将石蜡用加热筒液化，将步骤E制得的多孔陶瓷加热体基体半成品完全浸入到液化的石蜡中1-5h，之后在常温下冷却4-24h得到含有石蜡的多孔陶瓷加热体基体；
G、机加工：将步骤F中制得的含有石蜡的多孔陶瓷加热体基体进行机加工，去除多孔陶瓷加热体基体外表面的石蜡层；
H、涂覆：将步骤C中制得的电阻浆料按所需厚度涂覆于在步骤G中制得的多孔陶瓷加热体基体的外表面，电阻浆料在陶瓷基体表面形成一层发热膜；
I、金属化烧结：将步骤H中制得的具有发热膜结构的多孔陶瓷加热体基体置于石墨坩埚中，此后置于烧结炉中进行排蜡和多孔电阻发热膜的金属化烧结；
J、接电极：将步骤I中制得的加热体坯体两端进行表面镀镍处理，再于镀镍处理后的部位进行钎焊引出电极，制得多孔陶瓷加热体成品。
进一步的，所述的步骤A中，陶瓷基体浆料由以下质量百分比的原料组成：
硅藻土 21％
淀粉 16％
纳米二氧化硅溶液 1％
去离子水 62％。
进一步的，所述的步骤A中，电阻浆料由以下质量百分比的原料组成：
电阻浆料 30％
淀粉 45％
有机溶剂 25％。
进一步的，所述的步骤A中，陶瓷基体浆料由以下质量百分比的原料组成：
硅藻土 15％
淀粉 15％
去离子水 70％。
进一步的，所述的步骤A中，电阻浆料由以下质量百分比的原料组成：
电阻浆料 40％
淀粉 30％
有机溶剂 30％。
进一步的，所述的步骤A中，陶瓷基体浆料由以下质量百分比的原料组成：
硅藻土 50％
淀粉 8％
纳米二氧化硅溶液 2％
去离子水 40％。
进一步的，所述的步骤A中，电阻浆料由以下质量百分比的原料组成：
电阻浆料 30％
淀粉 50％
有机溶剂 20％。
进一步的，所述的步骤E中，对胚体进行烧结时的烧结温度为900-1400℃，升温速率为1-20℃/min，保温时间为2-12h。
进一步的，所述的步骤I中，金属化烧结的升温速率为1-5℃/min，金属化烧结温度为800-1000℃，时间为1-2h。
本发明的有益效果是：本发明提供了一种具有多孔发热膜结构的陶瓷加热体的制备工艺，该工艺依次通过混料、球磨、托盘、成型与干燥、烧结、灌蜡、机加工、涂覆、金属化烧结、接电极，整个制造工艺简单，通过采用箱式炉在氧化气氛和常压下烧结胚体，制得的加热体加热均匀且加热效率高。
附图说明
图1为本发明的一种具有多孔发热膜结构的陶瓷加热体的制备工艺的工艺流程图。
具体实施方式
下面结合附图和实施例对本发明进一步说明。
以下将结合实施例和附图对本发明的构思、具体结构及产生的技术效果进行清楚、完整地描述，以充分地理解本发明的目的、特征和效果。显然，所描述的 实施例只是本发明的一部分实施例，而不是全部实施例，基于本发明的实施例，本领域的技术人员在不付出创造性劳动的前提下所获得的其他实施例，均属于本发明保护的范围。另外，专利中涉及到的所有联接/连接关系，并非单指构件直接相接，而是指可根据具体实施情况，通过添加或减少联接辅件，来组成更优的联接结构。本发明创造中的各个技术特征，在不互相矛盾冲突的前提下可以交互组合。
实施例1
参照图1所示，本发明揭示了一种具有多孔发热膜结构的陶瓷加热体的制备工艺，具体的，该工艺包括以下的步骤：
A、混料：按质量百分比称取21％的硅藻土、16％的淀粉、1％的纳米二氧化硅溶液、62％的去离子水并混合搅拌均匀，制得陶瓷基体浆料；
按质量百分比称取30％的电阻浆料、45％的淀粉、25％的有机溶剂并混和搅拌均匀，制得有造孔剂的电阻浆料；
B、球磨：向步骤A中制得的陶瓷基体浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为24h；向步骤A中制得的电阻浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为48h；
C、脱泡：将步骤B中湿法球磨后的陶瓷基体浆料在真空条件下进行脱泡；将步骤B中湿法球磨后的电阻浆料在真空条件下进行脱泡；
D、成型与干燥：将步骤C中制得的陶瓷基体浆料用浇注机浇注制成所需形状的陶瓷基体，并将陶瓷基体进行干燥，以形成胚体；
E、烧结：将步骤D制得的坯体置于石墨坩埚中，并埋入隔离粉，此后用箱式炉将埋于隔离粉中的坯体在常压下进行烧结，烧结气氛为氧气，升温速率为5℃/min，烧结温度为1200℃，保温时间为2h，坯体烧结制得多孔陶瓷加热体基体半成品；
F、灌蜡：将石蜡用加热筒液化，将步骤E制得的多孔陶瓷加热体基体半成品完全浸入到液化的石蜡中5h，之后在常温下冷却24h得到含有石蜡的多孔陶瓷加热体基体；
G、机加工：将步骤F中制得的含有石蜡的多孔陶瓷加热体基体进行机加工，去除多孔陶瓷加热体基体外表面的石蜡层；
H、涂覆：将步骤C中制得的电阻浆料按所需厚度涂覆于在步骤G中制得的 多孔陶瓷加热体基体的外表面，电阻浆料在陶瓷基体表面形成一层发热膜；
I、金属化烧结：将步骤H中制得的具有发热膜结构的多孔陶瓷加热体基体置于石墨坩埚中，此后置于烧结炉中进行排蜡和多孔电阻发热膜的金属化烧结，其中升温速率为2℃/min，金属化烧结温度为850℃，时间为1h；
J、接电极：将步骤I中制得的加热体坯体两端进行表面镀镍处理，再于镀镍处理后的部位进行钎焊引出电极，制得多孔陶瓷加热体成品。
实施例2
参照图1所示，本发明揭示了一种具有多孔发热膜结构的陶瓷加热体的制备工艺，具体的，该工艺包括以下的步骤：
A、混料：按质量百分比称取15％的硅藻土、15％的淀粉、70％的去离子水并混合搅拌均匀，制得陶瓷基体浆料；
按质量百分比称取40％的电阻浆料、30％的淀粉、30％的有机溶剂并混和搅拌均匀，制得有造孔剂的电阻浆料；
B、球磨：向步骤A中制得的陶瓷基体浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为14h；
向步骤A中制得的电阻浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为36h；
C、脱泡：将步骤B中湿法球磨后的陶瓷基体浆料在真空条件下进行脱泡；将步骤B中湿法球磨后的电阻浆料在真空条件下进行脱泡；
D、成型与干燥：将步骤C中制得的陶瓷基体浆料用浇注机浇注制成所需形状的陶瓷基体，并将陶瓷基体进行干燥，以形成胚体；
E、烧结：将步骤D制得的坯体置于石墨坩埚中，并埋入隔离粉，此后用箱式炉将埋于隔离粉中的坯体在常压下进行烧结，烧结气氛为氧气，坯体烧结制得多孔陶瓷加热体基体半成品；对胚体进行烧结时的烧结温度为900℃，升温速率为1℃/min，保温时间为2h；
F、灌蜡：将石蜡用加热筒液化，将步骤E制得的多孔陶瓷加热体基体半成品完全浸入到液化的石蜡中1h，之后在常温下冷却4h得到含有石蜡的多孔陶瓷加热体基体；
G、机加工：将步骤F中制得的含有石蜡的多孔陶瓷加热体基体进行机加工，去除多孔陶瓷加热体基体外表面的石蜡层；
H、涂覆：将步骤C中制得的电阻浆料按所需厚度涂覆于在步骤G中制得的多孔陶瓷加热体基体的外表面，电阻浆料在陶瓷基体表面形成一层发热膜；
I、金属化烧结：将步骤H中制得的具有发热膜结构的多孔陶瓷加热体基体置于石墨坩埚中，此后置于烧结炉中进行排蜡和多孔电阻发热膜的金属化烧结；金属化烧结的升温速率为1℃/min，金属化烧结温度为800℃，时间为1h；
J、接电极：将步骤I中制得的加热体坯体两端进行表面镀镍处理，再于镀镍处理后的部位进行钎焊引出电极，制得多孔陶瓷加热体成品。
实施例3
参照图1所示，本发明揭示了一种具有多孔发热膜结构的陶瓷加热体的制备工艺，具体的，该工艺包括以下的步骤：
A、混料：按质量百分比称取50％的硅藻土、8％的淀粉、2％的纳米二氧化硅溶液、40％的去离子水并混合搅拌均匀，制得陶瓷基体浆料；
按质量百分比称取30％的电阻浆料、50％的淀粉、20％的有机溶剂并混和搅拌均匀，制得有造孔剂的电阻浆料；
B、球磨：向步骤A中制得的陶瓷基体浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为4h；
向步骤A中制得的电阻浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为24h；
C、脱泡：将步骤B中湿法球磨后的陶瓷基体浆料在真空条件下进行脱泡；
将步骤B中湿法球磨后的电阻浆料在真空条件下进行脱泡；
D、成型与干燥：将步骤C中制得的陶瓷基体浆料用浇注机浇注制成所需形状的陶瓷基体，并将陶瓷基体进行干燥，以形成胚体；
E、烧结：将步骤D制得的坯体置于石墨坩埚中，并埋入隔离粉，此后用箱式炉将埋于隔离粉中的坯体在常压下进行烧结，烧结气氛为氧气，坯体烧结制得多孔陶瓷加热体基体半成品；对胚体进行烧结时的烧结温度为1400℃，升温速率为20℃/min，保温时间为12h；
F、灌蜡：将石蜡用加热筒液化，将步骤E制得的多孔陶瓷加热体基体半成品完全浸入到液化的石蜡中3h，之后在常温下冷却14h得到含有石蜡的多孔陶瓷加热体基体；
G、机加工：将步骤F中制得的含有石蜡的多孔陶瓷加热体基体进行机加工， 去除多孔陶瓷加热体基体外表面的石蜡层；
H、涂覆：将步骤C中制得的电阻浆料按所需厚度涂覆于在步骤G中制得的多孔陶瓷加热体基体的外表面，电阻浆料在陶瓷基体表面形成一层发热膜；
I、金属化烧结：将步骤H中制得的具有发热膜结构的多孔陶瓷加热体基体置于石墨坩埚中，此后置于烧结炉中进行排蜡和多孔电阻发热膜的金属化烧结；金属化烧结的升温速率为5℃/min，金属化烧结温度为1000℃，时间为2h；
J、接电极：将步骤I中制得的加热体坯体两端进行表面镀镍处理，再于镀镍处理后的部位进行钎焊引出电极，制得多孔陶瓷加热体成品。
综上所述，本发明提供了一种具有多孔发热膜结构的陶瓷加热体的制备工艺，该工艺依次通过混料、球磨、托盘、成型与干燥、烧结、灌蜡、机加工、涂覆、金属化烧结、接电极制得陶瓷加热体，整个制造工艺简单，通过采用箱式炉在氧化气氛和常压下烧结胚体，制得的陶瓷加热体加热均匀且加热效率高。
以上是对本发明的较佳实施进行了具体说明，但本发明创造并不限于所述实施例，熟悉本领域的技术人员在不违背本发明精神的前提下还可做出种种的等同变形或替换，这些等同的变形或替换均包含在本申请权利要求所限定的范围内。

Claims (9)

  1. 一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：该工艺包括以下的步骤：
    A、混料：按质量百分比称取15-55％的硅藻土、5-25％的淀粉、0-2％的纳米二氧化硅溶液、40-70％的去离子水，混合搅拌均匀，制得陶瓷基体浆料；
    按质量百分比称取15-40％的电阻浆料、30-60％的淀粉、10-30％的有机溶剂并混和搅拌均匀，制得有造孔剂的电阻浆料；
    B、球磨：向步骤A中制得的陶瓷基体浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为4-24h；
    向步骤A中制得的电阻浆料加入研磨球，并放入球磨罐中进行湿法球磨，湿法球磨的时间为24-48h；
    C、脱泡：将步骤B中湿法球磨后的陶瓷基体浆料在真空条件下进行脱泡；
    将步骤B中湿法球磨后的电阻浆料在真空条件下进行脱泡；
    D、成型与干燥：将步骤C中制得的陶瓷基体浆料用浇注机浇注制成所需形状的陶瓷基体，并将陶瓷基体进行干燥，以形成胚体；
    E、烧结：将步骤D制得的坯体置于石墨坩埚中，并埋入隔离粉，此后用箱式炉将埋于隔离粉中的坯体在常压下进行烧结，烧结气氛为氧气，坯体烧结制得多孔陶瓷加热体基体半成品；
    F、灌蜡：将石蜡用加热筒液化，将步骤E制得的多孔陶瓷加热体基体半成品完全浸入到液化的石蜡中1-5h，之后在常温下冷却4-24h得到含有石蜡的多孔陶瓷加热体基体；
    G、机加工：将步骤F中制得的含有石蜡的多孔陶瓷加热体基体进行机加工，去除多孔陶瓷加热体基体外表面的石蜡层；
    H、涂覆：将步骤C中制得的电阻浆料按所需厚度涂覆于在步骤G中制得的多孔陶瓷加热体基体的外表面，电阻浆料在陶瓷基体表面形成一层发热膜；
    I、金属化烧结：将步骤H中制得的具有发热膜结构的多孔陶瓷加热体基体置于石墨坩埚中，此后置于烧结炉中进行排蜡和多孔电阻发热膜的金属化烧结；
    J、接电极：将步骤I中制得的加热体坯体两端进行表面镀镍处理，再于镀镍处理后的部位进行钎焊引出电极，制得多孔陶瓷加热体成品。
  2. 根据权利要求1所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤A中，陶瓷基体浆料由以下质量百分比的原料组成：
    硅藻土 21％
    淀粉 16％
    纳米二氧化硅溶液 1％
    去离子水 62％。
  3. 根据权利要求2所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤A中，电阻浆料由以下质量百分比的原料组成：
    电阻浆料 30％
    淀粉 45％
    有机溶剂 25％。
  4. 根据权利要求1所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤A中，陶瓷基体浆料由以下质量百分比的原料组成：
    硅藻土 15％
    淀粉 15％
    去离子水 70％。
  5. 根据权利要求4所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤A中，电阻浆料由以下质量百分比的原料组成：
    电阻浆料 40％
    淀粉 30％
    有机溶剂 30％。
  6. 根据权利要求1所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤A中，陶瓷基体浆料由以下质量百分比的原料组成：
    硅藻土 50％
    淀粉 8％
    纳米二氧化硅溶液 2％
    去离子水 40％。
  7. 根据权利要求6所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤A中，电阻浆料由以下质量百分比的原料组成：
    电阻浆料 30％
    淀粉 50％
    有机溶剂 20％。
  8. 根据权利要求1所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤E中，对胚体进行烧结时的烧结温度为900-1400℃，升温速率为1-20℃/min，保温时间为2-12h。
  9. 根据权利要求1所述的一种具有多孔发热膜结构的陶瓷加热体的制备工艺，其特征在于：所述的步骤I中，金属化烧结的升温速率为1-5℃/min，金属化烧结温度为800-1000℃，时间为1-2h。
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