阅读说明：本技术 一种应用于低温窑炉的陶瓷测温环 (Ceramic temperature measuring ring applied to low-temperature kiln ) 是由 蔡毅翔 黄满连 蔡艺虹 于 2021-09-10 设计创作，主要内容包括：本发明公开了一种应用于低温窑炉的陶瓷测温环,包括2-10%wt B2O3、10-50%wt玻璃粉、10-30%wtSiO2、10-30%wtAl2O3、1-5%wt TiO2、1-10%wtMgO和1-5%wt BaC03。本发明制造的陶瓷测温环,从500℃开始持续收缩,有效测温范围500-700℃,可以应用于低至500℃的窑炉测温。(The invention discloses a ceramic temperature measuring ring applied to a low-temperature kiln, which comprises 2-10 wt% of B2O3, 10-50 wt% of glass powder, 10-30 wt% of WtSiO2, 10-30 wt% of WtAl2O3, 1-5 wt% of TiO2, 1-10 wt% of WtMgO and 1-5 wt% of BaC 03. The ceramic temperature measuring ring manufactured by the invention continuously shrinks from 500 ℃, the effective temperature measuring range is 500-700 ℃, and the ceramic temperature measuring ring can be applied to the temperature measurement of a kiln at the temperature as low as 500 ℃.)

1. A ceramic temperature measuring ring applied to a low-temperature kiln comprises 2-10 wt% of B2O3, 10-50 wt% of glass powder, 10-30 wt% of WtSiO2, 10-30 wt% of WtAl2O3, 1-5 wt% of TiO2, 1-10 wt% of WtMgO and 1-5 wt% of BaC 03.

2. The ceramic temperature measuring ring applied to the low-temperature kiln as claimed in claim 1, wherein the softening temperature of the glass powder is 500 ℃.

3. The ceramic temperature measuring ring applied to the low-temperature kiln as claimed in claim 2, wherein the glass powder comprises the following components by weight: 10-25 wt% of B2O3, 1-5 wt% of Li2C03, 30-60 wt% of WtSiO2, 5-20 wt% of wtAl2O3, 5-10 wt% of ZnO and 5-15 wt% of CaO.

4. The process flow of the ceramic temperature measuring ring applied to the low-temperature kiln as claimed in claim 1, is characterized by comprising the following steps:

s1: weighing raw materials according to the weight proportion of the formula of the glass powder, wherein the purity of the raw materials is more than or equal to 99.5 percent, uniformly mixing, placing the raw materials in a crucible for melting at the temperature of 1200 ℃ and 1400 ℃ for 1-2 hours, and directly pouring glass liquid into deionized water for quenching to obtain glass;

s2: crushing glass to be less than 2mm, putting the glass into a ball milling barrel for ball milling, and drying to obtain glass powder with the median particle size of 1-2 um;

s3: weighing raw materials according to the weight proportion of the temperature measuring ring formula, adding deionized water as a medium into a ball milling barrel, and ball milling for 6-12 hours, wherein the purity of the raw materials is more than or equal to 99.5%, and the particle size distribution of the slurry is measured by a laser particle sizer after ball milling, wherein the median particle size is 0.5-2 um;

s4: adding 2-5 wt% of polyacrylic acid into the ball-milled slurry, performing spray granulation to obtain powder, sieving the powder, selecting 100-300 mesh powder, and performing dry pressing molding in a designed mold to obtain a ceramic temperature measuring ring blank, wherein the molding pressure is 100-300MPa, and the size of the temperature measuring ring is as follows: the inner diameter is 10mm, the outer diameter is 20.5mm, and the thickness is 7 mm;

s5: sintering the temperature measuring ring: placing 3 temperature measuring rings in a kiln in a delta shape, placing the temperature measuring rings close to a temperature measuring end of a thermocouple, sintering, wherein the sintering procedure is that the temperature rising speed is 300 ℃/h, the holding time of the highest temperature is 1 h, the temperature reducing speed is 300 ℃/h, cooling to the room temperature under the air atmosphere, standing for 1 h, measuring the diameter of the temperature measuring rings by using a spiral micrometer, the sintering temperature is 470 and 730 ℃, taking one temperature point every 5 ℃, and repeatedly sintering for 5 times at each temperature point, so that each temperature point obtains 15 data, averaging and fitting to obtain a temperature-diameter corresponding curve.

Technical Field

The invention relates to the technical field of special ceramics, in particular to the technical field of ceramic temperature measuring rings, and specifically relates to a manufacturing method of a ceramic temperature measuring ring applied to a low-temperature kiln.

Background

In the industries of glass, semiconductor, ceramic, powder metallurgy and the like, products of the glass, the semiconductor, the ceramic, the powder metallurgy and the like need to be subjected to heat treatment in a kiln. In the heat treatment process, the measurement and control of the actual temperature of the kiln have important influence on the quality and the cost of products. The traditional temperature measurement method has certain limitation, such as the thermocouple can only give the temperature of the position point where the thermocouple is located, but not the temperature of the product placing position. The same set temperature cannot ensure that the heat treatment effect received by the product is the same at different placing positions of the kiln. In addition, the total heat applied to the product during the whole heat treatment process cannot be measured by conventional methods such as a thermocouple and an optical thermometer. In view of the above, a ceramic temperature measuring ring product has been developed. The ceramic temperature measuring ring absorbs heat to shrink in the heat treatment process, the higher the actual temperature is, the longer the heat preservation time is, the more the heated total amount is, the larger the temperature measuring ring shrinks, and the smaller the diameter after sintering. The device can visually reflect the whole actual heating effect of different heat treatment conditions, such as different set temperatures, time, radiators, air flow, heat transfer coefficients and the like, at the placement positions. The temperature measuring ring has small volume, can be placed at any position needing temperature measurement in the kiln, and better indicates the accumulated heat of the whole product in the heat treatment process. Due to the consistency and the repeatability, the device can be used for transversely controlling the temperature difference of different positions of the kiln or different kilns, and can also be used for longitudinally controlling the temperature change of a certain position of the kiln in different periods, so that a user can be helped to control the product quality, optimize the production process and eliminate the kiln faults. Has been widely applied to the industries of electronic ceramics, powder metallurgy, special ceramics, magnetic materials, building ceramics, bathroom ceramics, daily ceramics and the like.

At first, the temperature measuring range of the ceramic temperature measuring ring product is 600-1750 ℃, and the ceramic temperature measuring ring product can only be applied to kilns with higher process temperature. For industries such as glass, low-temperature ceramic glaze, annealing furnaces, semiconductors and the like, part of process temperatures are as low as 500 ℃, and the temperature measuring ring products cannot meet application requirements. In 2017, the temperature measuring range of the temperature measuring ring with the model ZTH developed by the company FERRO in USA is 560-.

Disclosure of Invention

Based on the technical problems in the background art, the invention provides a ceramic temperature measuring ring applied to a low-temperature kiln.

The invention provides a ceramic temperature measuring ring applied to a low-temperature kiln, which comprises 2-10 wt% of B2O3, 10-50 wt% of glass powder, 10-30 wt% of WtSiO2, 10-30 wt% of WtAl2O3, 1-5 wt% of TiO2, 1-10 wt% of WtMgO and 1-5 wt% of BaC 03.

Preferably, the softening temperature of the glass powder is 500 ℃, the melting point of B2O3 is 450 ℃, and during sintering, a liquid phase can be formed to promote low-temperature sintering. The glass powder and the B2O3 play a combined sintering assisting role, so that the temperature measuring ring blank begins to shrink before 500 ℃.

Preferably, the glass powder formula comprises the following components: 10-25 wt% of B2O3, 1-5 wt% of Li2C03, 30-60 wt% of WtSiO2, 5-20 wt% of WtAl2O3, 5-10 wt% of ZnO and 5-15 wt% of CaO.

A process flow of a ceramic temperature measuring ring applied to a low-temperature kiln comprises the following steps:

s1: weighing raw materials according to the weight proportion of the formula of the glass powder, wherein the purity of the raw materials is more than or equal to 99.5 percent, uniformly mixing, placing the raw materials in a crucible for melting at the temperature of 1200 ℃ and 1400 ℃ for 1-2 hours, and directly pouring glass liquid into deionized water for quenching to obtain glass;

s2: crushing glass to be less than 2mm, putting the glass into a ball milling barrel for ball milling, and drying to obtain glass powder with the median particle size of 1-2 um;

s3: weighing the raw materials according to the weight proportion of the temperature measuring ring formula, taking deionized water as a medium, and adding the deionized water into a ball milling barrel for ball milling for 6-12 hours. The purity of the raw material is more than or equal to 99.5 percent, and the particle size distribution of the slurry is measured by a laser particle sizer after ball milling, wherein the median particle size is 0.5-2 um;

s4: adding 2-5 wt% of polyacrylic acid into the ball-milled slurry, performing spray granulation to obtain powder, sieving the powder, selecting 100-300 mesh powder, and performing dry pressing molding in a designed mold to obtain a ceramic temperature measuring ring blank, wherein the molding pressure is 100-300MPa, and the size of the temperature measuring ring is as follows: the inner diameter is 10mm, the outer diameter is 20.5mm, and the thickness is 7 mm;

s5: sintering the temperature measuring ring: placing 3 temperature measuring rings in a kiln in a delta shape, placing the temperature measuring rings close to a temperature measuring end of a thermocouple, sintering, wherein the sintering procedure is that the temperature rising speed is 300 ℃/h, the holding time of the highest temperature is 1 h, the temperature reducing speed is 300 ℃/h, cooling to the room temperature under the air atmosphere, standing for 1 h, measuring the diameter of the temperature measuring rings by using a spiral micrometer, the sintering temperature is 470 and 730 ℃, taking one temperature point every 5 ℃, and repeatedly sintering for 5 times at each temperature point, so that each temperature point obtains 15 data, averaging and fitting to obtain a temperature-diameter corresponding curve.

The beneficial effects of the invention are as follows:

the ceramic temperature measuring ring manufactured by the invention continuously shrinks from 500 ℃, the effective temperature measuring range is 500-700 ℃, and the ceramic temperature measuring ring can be applied to the temperature measurement of a kiln at the temperature as low as 500 ℃.

Drawings

FIG. 1 is a temperature-diameter corresponding curve diagram of a temperature measuring ring of a ceramic temperature measuring ring applied to a low-temperature kiln.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

A ceramic temperature measuring ring applied to a low-temperature kiln comprises 2-10 wt% of B2O3, 10-50 wt% of glass powder, 10-30 wt% of WtSiO2, 10-30 wt% of WtAl2O3, 1-5 wt% of TiO2, 1-10 wt% of WtMgO and 1-5 wt% of BaC 03.

In the invention, the softening temperature of the glass powder is 500 ℃, the melting point of B2O3 is 450 ℃, a liquid phase can be formed in the sintering process to promote low-temperature sintering, the glass powder and B2O3 play a role of combined sintering assistance to ensure that a temperature measuring ring blank begins to shrink before 500 ℃, and the formula composition of the glass powder is as follows: 10-25 wt% of B2O3, 1-5 wt% of Li2C03, 30-60 wt% of WtSiO2, 5-20 wt% of WtAl2O3, 5-10 wt% of ZnO and 5-15 wt% of CaO.

A process flow of a ceramic temperature measuring ring applied to a low-temperature kiln comprises the following steps:

s1: weighing raw materials according to the weight proportion of the formula of the glass powder, wherein the purity of the raw materials is more than or equal to 99.5 percent, uniformly mixing, placing the raw materials in a crucible for melting at the temperature of 1200 ℃ and 1400 ℃ for 1-2 hours, and directly pouring glass liquid into deionized water for quenching to obtain glass;

s2: crushing glass to be less than 2mm, putting the glass into a ball milling barrel, and performing ball milling and drying to obtain glass powder with the median particle size of 1-2 um;

s3: weighing the raw materials according to the weight proportion of the temperature measuring ring formula, taking deionized water as a medium, and adding the deionized water into a ball milling barrel for ball milling for 6-12 hours. The purity of the raw material is more than or equal to 99.5 percent, and the particle size distribution of the slurry is measured by a laser particle sizer after ball milling, wherein the median particle size is 0.5-2 um;

s4: adding 2-5 wt% of polyacrylic acid into the ball-milled slurry, performing spray granulation to obtain powder, sieving the powder, selecting 100-300 mesh powder, and performing dry pressing molding in a designed mold to obtain a ceramic temperature measuring ring blank, wherein the molding pressure is 100-300MPa, and the size of the temperature measuring ring is as follows: the inner diameter is 10mm, the outer diameter is 20.5mm, and the thickness is 7 mm;

s5: sintering the temperature measuring ring: placing 3 temperature measuring rings in a kiln in a delta shape, placing the temperature measuring rings close to a temperature measuring end of a thermocouple, sintering, wherein the sintering procedure is that the temperature rising speed is 300 ℃/h, the holding time of the highest temperature is 1 h, the temperature reducing speed is 300 ℃/h, cooling to the room temperature under the air atmosphere, standing for 1 h, measuring the diameter of the temperature measuring rings by using a spiral micrometer, the sintering temperature is 470 and 730 ℃, taking one temperature point every 5 ℃, and repeatedly sintering for 5 times at each temperature point, so that each temperature point obtains 15 data, averaging and fitting to obtain a temperature-diameter corresponding curve.

Weighing 2.1Kg 2.1KgB2O3, 0.2 Kg Li2C03, 4.8 Kg SiO2, 1.5 Kg Al2O3, 0.7 Kg ZnO and 0.7 Kg CaO powder, uniformly mixing, placing in a crucible for melting at 1350 ℃ for 1.5 hours, directly pouring the glass liquid into deionized water, and performing cold quenching to obtain the glass.

And (3) crushing the glass to below 2mm, putting the glass into a ball milling barrel, carrying out ball milling for 6 hours, and drying to obtain glass powder with the median particle size D50 of 1.48 um.

Weighing 0.3Kg of B2O3, 3.5Kg of glass powder, 1.2Kg of SiO2, 2.1Kg of Al2O3, 0.25Kg of TiO2, 0.5Kg of MgO and 0.15Kg of BaC 03. Deionized water is used as a ball milling medium, ball milling is carried out for 8 hours, and the particle size distribution of the slurry is measured by a laser particle sizer, so that the median particle size D50 is 0.82 um.

Adding 3 percent by weight of polyacrylic acid, stirring uniformly, and performing spray granulation, wherein the outlet temperature is 120 ℃.

And sieving the powder obtained by spraying, and selecting the powder of 100-300 meshes.

In a designed die, dry pressing and molding to obtain a ceramic temperature measuring ring blank, wherein the molding pressure is 240MPa, and the size of the temperature measuring ring is as follows: the inner diameter is 10mm, the outer diameter is 20.5mm, and the thickness is 7 mm.

Sintering the temperature measuring ring

And placing the 3 temperature measuring rings in a kiln in a shape like a Chinese character 'pin', and sintering the temperature measuring rings close to the temperature measuring end of the thermocouple. The sintering procedure is temperature rising speed of 300 ℃/h, the holding time of the highest temperature of 1 h, the temperature lowering speed of 300 ℃/h and air atmosphere. The temperature was cooled to room temperature and left to stand for 1 hour, and the diameter of the temperature measuring ring was measured with a micrometer screw.

The maximum temperature setting range in sintering is 470-730 ℃, one temperature point is taken every 5 ℃, and the sintering is repeated for 5 times at each temperature point. Thus, 15 data are obtained at each temperature point, and the average value is taken and fitted to obtain a temperature-diameter corresponding curve. As can be seen from the curve, the temperature measuring ring starts to shrink at 470 ℃, and continues to shrink to the diameter of 730 ℃, and the temperature measuring ring manufactured by the formula can be applied to the temperature measurement of a kiln in the range of 500-700 ℃.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.