WO2022142168A1 - 一种低熔点多孔陶瓷材料及其制备方法 - Google Patents

一种低熔点多孔陶瓷材料及其制备方法 Download PDF

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WO2022142168A1
WO2022142168A1 PCT/CN2021/100348 CN2021100348W WO2022142168A1 WO 2022142168 A1 WO2022142168 A1 WO 2022142168A1 CN 2021100348 W CN2021100348 W CN 2021100348W WO 2022142168 A1 WO2022142168 A1 WO 2022142168A1
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powder
porous ceramic
raw material
ceramic material
low
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PCT/CN2021/100348
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French (fr)
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陆静
王艳辉
马忠强
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华侨大学
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Priority to JP2023535015A priority Critical patent/JP2023553118A/ja
Publication of WO2022142168A1 publication Critical patent/WO2022142168A1/zh
Priority to US18/208,822 priority patent/US20230322626A1/en

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Definitions

  • the invention belongs to the technical field of ceramic materials, in particular to a low melting point porous ceramic material and a preparation method thereof.
  • Porous ceramic materials have the characteristics of large specific surface area, energy absorption, and damping.
  • the specially processed porous ceramics have selective permeability to liquids, gases and other substances, so they are widely used in various fields, such as automotive environmental protection, chemical industry, mechanical and biomedical fields.
  • commercial porous ceramics mainly use Al 2 O 3 , SiC, ZrO 2 and mullite as the main raw materials.
  • these materials have complex production processes, high sintering temperature, high energy consumption, high cost, or due to pore-forming agents.
  • the purpose of the present invention is to overcome the defects of the prior art and provide a low melting point porous ceramic material.
  • Another object of the present invention is to provide a method for preparing the above-mentioned low melting point porous ceramic material.
  • a low melting point porous ceramic material the firing temperature is 680-830 DEG C, the porosity is 24-42%, and the raw material is composed of a binder and raw material powder, wherein the raw material powder is mixed with the following mass percentages of raw material components After vitrification, wet grinding, drying and sieving to make:
  • the binder is dextrin.
  • the borosilicate sand and Na 2 O powder can pass through a 2000-mesh screen.
  • the purple clay powder, quartz powder and LiO 2 powder can pass through a 1000-mesh screen.
  • the mass ratio of the raw material powder to the temporary binder is 80-90:10-20.
  • the mass ratio of the raw material powder to the temporary binder is 85:15.
  • the raw material powder can pass through a 5000 mesh screen.
  • the preparation method of the above-mentioned low melting point porous ceramic material comprises the following steps:
  • the first mixture is obtained by dry grinding and sieving in turn;
  • the temperature of the vitrification treatment is 800-900°C.
  • the heating rate in the step (7) is 4-6° C./min, and the holding time for sintering is 1.5-2.5 h.
  • the beneficial effects of the present invention are: the raw material components in the present invention act synergistically, and the obtained product has the advantages of simple sintering process, good mechanical strength, no need to add pore-forming agent and can generate pores, etc.
  • the problems of mismatched refractoriness, poor heat dissipation, and poor air permeability of the porogen can improve the life and holding force of the porous ceramic material.
  • the sintering temperature is only 680-780 °C. up to 42%, while maintaining good compressive strength, flexural strength and hardness.
  • FIG. 1 is an electron microscope photograph of the porous structure of the low-melting point porous ceramic material of Example 1 of the present invention after firing.
  • the first mixture is obtained by dry grinding and passing through a 2000-mesh sieve in turn;
  • the raw material powder is obtained by successively undergoing vitrification treatment at 800° C., wet grinding, drying and passing through a 5000-mesh sieve;
  • Table 1 shows the ratio of raw material components, firing temperature and technical effect obtained in Examples 1 to 6, wherein the porous structure of the low melting point porous ceramic material obtained in Example 1 after firing is shown in Figure 1 .
  • the firing temperature of porous ceramics will be as high as 1100 °C. If the firing temperature is too high, its application range (such as ceramic abrasives, etc.) will be reduced, and the firing temperature is too high. It will destroy the morphology of abrasive particles (see Sha X, Yue W, Zhang H, et al. Thermal stability of polycrystalline diamond compact sintered with boron-coated diamond particles[J].Diamond and Related Materials.2020,104:107753.).
  • the firing temperature of porous ceramics still needs to be 680 °C, and the firing temperature does not decrease with the increase of boron glass content.
  • the temporary binder used in the ceramic binder prepared by the present invention is dextrin, and the conventional temporary binder on the market, such as water glass, etc., will react with the ceramic binder during mixing or will generate pores after sintering. Destroying the pores of purple sand soil will make the ceramic bond denser.
  • Example 1 After the raw material powder in Example 1 and water glass (as a binder instead of dextrin, the ratio of water to water glass is 13.6:1) solution is mixed uniformly at a mass ratio of 85:15, and then granulated to obtain mixed raw materials; The mixed raw materials were pressed into the required shape, and fully dried for 24 hours to obtain a green body; the green body was heated to 750 °C at a rate of 5 °C/min for 2 hours, and the porous structure as shown in Figure 2 was obtained. Compared with Example 1, the porous structure of the ceramic main body obtained in this comparative example becomes denser, and the advantage of the natural porous structure brought by the purple clay no longer exists, so that its mechanical properties are improved. The strength is 50.25Mpa and the hardness is 40HRB.
  • the invention discloses a low melting point porous ceramic material and a preparation method thereof.
  • the raw material components in the present invention act synergistically, and the obtained product has the advantages of simple sintering process, good mechanical strength, no need to add pore-forming agent and can generate pores, etc. Problems such as poor heat dissipation and poor air permeability can improve the life and holding power of porous ceramic materials. Good compressive strength, flexural strength and hardness, with industrial practicability.

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Abstract

一种低熔点多孔陶瓷材料及其制备方法，其烧成温度为680-830℃，气孔率为24-42％，其原料由临时粘结剂和原料粉末组成。各原料组分协同作用，所获得的产品具有烧结工艺简单、机械强度好、无需添加造孔剂且能产生气孔等优点，有效解决了结合剂与造孔剂耐火度不匹配、散热能力差、透气性差等问题，能提高多孔陶瓷材料的寿命和把持力，其烧成温度只有680～780℃，在未添加造孔剂的条件下气孔率最高可达42％，同时保持了很好的抗压强度、抗折强度和硬度。

Description

一种低熔点多孔陶瓷材料及其制备方法 技术领域
本发明属于陶瓷材料技术领域，具体涉及一种低熔点多孔陶瓷材料及其制备方法。
背景技术
多孔陶瓷材料有着比表面积大，能量吸收，以及阻尼等特性，经过特殊加工的多孔陶瓷对液体，气体等物质有着选择透过性，因此被广泛的应用在各个领域中，如汽车环保、化工、机械及生物医学等领域。目前，商业化的多孔陶瓷主要以Al 2O 3、SiC、ZrO 2和莫来石为主要原料，然而这些材料制作工艺复杂、烧成温度高、能耗大、成本高、或者由于造孔剂与基体耐火度不匹配等问题导致的成孔困难，使现有的多孔陶瓷产品存在机械强度低、抗震性、阻尼性差、不易产生理想的通孔等问题，从而严重限制了多孔陶瓷的推广和应用。因此寻找合适的原材料，有效降低烧结温度，提高多孔陶瓷的气孔率和比表面积对于多孔陶瓷的广泛应用有着积极的促进作用。
发明内容
本发明的目的在于克服现有技术缺陷，提供一种低熔点多孔陶瓷材料。
本发明的另一目的在于提供上述低熔点多孔陶瓷材料的制备方法。
本发明的技术方案如下：
一种低熔点多孔陶瓷材料，其烧成温度为680-830℃，气孔率为24-42％，其原料由粘结剂和原料粉末组成，其中，原料粉末由如下质量百分比的原料组分混合后经玻化处理、湿磨、烘干及过筛而制成：
Figure PCTCN2021100348-appb-000001
在本发明的一个优选实施方案中，所述粘结剂为糊精。
在本发明的一个优选实施方案中，所述硼玻璃砂与Na 2O粉能够通过2000目筛 网。
在本发明的一个优选实施方案中，所述紫砂土粉、石英粉和LiO 2粉能够通过1000目筛网。
在本发明的一个优选实施方案中，所述原料粉末与临时粘结剂的质量比为80-90:10-20。
进一步优选的，所述原料粉末与临时粘结剂的质量比为85:15。
在本发明的一个优选实施方案中，所述原料粉末能够通过5000目筛网。
上述低熔点多孔陶瓷材料的制备方法，包括如下步骤：
(1)按所述质量百分比称取构成原料粉末的原料组分；
(2)将硼玻璃砂和Na 2O粉混合均匀后，依次经干磨和过筛，获得第一混合物；
(3)将紫砂土粉、石英粉和LiO 2粉混合均匀后，依次经干磨和过筛，获得第二混合物；
(4)将上述第一混合物和第二混合物混合均匀后，依次经玻化处理、湿磨、干燥和过筛，获得所述原料粉末；
(5)将上述原料粉末与临时粘结剂混合均匀后，再经造粒，获得混合原料；
(6)将上述混合原料压制成所需要的形状，并充分干燥，获得坯体；
(7)将上述坯体升温至所述烧成温度保温烧成，即成。
在本发明的一个优选实施方案中，所述玻化处理的温度为800-900℃。
在本发明的一个优选实施方案中，所述步骤(7)中的升温速率为4-6℃/min，保温烧成的时间为1.5-2.5h。
本发明的有益效果是：本发明中的各原料组分协同作用，所获得的产品具有烧结工艺简单、机械强度好、无需添加造孔剂且能产生气孔等优点，有效解决了结合剂与造孔剂耐火度不匹配、散热能力差、透气性差等问题，能提高多孔陶瓷材料的寿命和把持力，其烧成温度只有680～780℃，在未添加造孔剂的条件下气孔率最高可达42％，同时保持了很好的抗压强度、抗折强度和硬度。
附图说明
图1为本发明实施例1的低熔点多孔陶瓷材料烧成后的多孔结构的电镜照片。
图2为本发明对比例6的低熔点多孔陶瓷材料烧成后的多孔结构的电镜照片。
具体实施方式
以下通过具体实施方式结合附图对本发明的技术方案进行进一步的说明和描述。
实施例1至6
(1)按质量百分比称取构成原料粉末的原料组分；
(2)将硼玻璃砂和Na 2O粉混合均匀后，依次经干磨和过2000目筛，获得第一混合物；
(3)将紫砂土粉、石英粉和LiO 2粉混合均匀后，依次经干磨和过1000目筛，获得第二混合物；
(4)将上述第一混合物和第二混合物混合均匀后，依次经800℃玻化处理、湿磨、干燥和过5000目筛，获得所述原料粉末；
(5)将上述原料粉末与糊精以85:15的质量比混合均匀后，再经造粒，获得混合原料；
(6)将上述混合原料压制成所需要的形状，并充分干燥24h，获得坯体；
(7)将上述坯体以5℃/min的速率升温至烧成温度保温烧成2h，即成。
实施例1至6的原料组分的配比、烧成温度和所获得的技术效果如表1所示，其中实施例1所得的低熔点多孔陶瓷材料烧成后的多孔结构如图1所示。
对比例1至5
具体制作过程同实施例1至6，原料组分的配比、烧成温度和所获得的技术效果如表1所示。
表1 各实施例和对比例的对比列表
Figure PCTCN2021100348-appb-000002
Figure PCTCN2021100348-appb-000003
由表1可知，当紫砂粉的添加量低于15％的时候会发现多孔陶瓷的气孔由通孔转变为闭孔，使得多孔陶瓷气孔率快速降低，体现不出多孔陶瓷的优势。而当紫砂粉的添加量高于20％的时候会发现多孔陶瓷的气孔快速交叠变大，使得多孔陶瓷气孔率快速升高，并使陶瓷的力学性能快速降低。这样烧结出来的产品强度太低，使其应用范围大幅度减小，应用寿命急剧降低。
当硼玻璃砂的添加量低于20％的时候会使多孔陶瓷的烧成温度高达1100℃，烧成温度过高会缩小其应用范围(如陶瓷磨具等)，且过高的烧成温度会破坏磨粒的形态(参见Sha X,Yue W,Zhang H,et al.Thermal stability of polycrystalline diamond compact sintered with boron-coated diamond particles[J].Diamond and Related Materials.2020,104:107753.)。而当硼玻璃砂的添加量低于55％的时候会发现多孔陶瓷的烧成温度仍然需要680℃，烧成温度并没有随着硼玻璃含量的增加而降低。本发明所制备的陶瓷结合剂使用的临时粘结剂为糊精，市面上常规的临时粘结剂如水玻璃等，会在混料的时候与陶瓷结合剂发生反应或者经过烧结后会产生孔隙，破坏紫砂土自带的孔隙，会是陶瓷结合剂变得致密。
对比例6
以实施例1中的原料粉末与水玻璃(作为粘结剂代替糊精，水与水玻璃比例13.6:1)溶液以85：15的质量比混合均匀后，再经造粒，获得混合原料；将混合原料压制成所需要的形状，并充分干燥24h，获得坯体；将坯体以5℃/min的速率升温至750℃保温烧成2h，得到如图2所示的多孔结构，与实施例1相比，该对比例获得的陶瓷主体的多孔结构变的致密，由紫砂土带来的天然多孔结构的优势不复存在，使其力学性能提高，其抗压强度为55.4Mpa，抗折强度为50.25Mpa,硬度为40HRB。
以上所述，仅为本发明的较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。
工业实用性
本发明公开了一种低熔点多孔陶瓷材料及其制备方法，其烧成温度为680-830℃，气孔率为24-42％，其原料由临时粘结剂和原料粉末组成。本发明中的各原料组分协同作用，所获得的产品具有烧结工艺简单、机械强度好、无需添加造孔剂且能产生气孔等优点，有效解决了结合剂与造孔剂耐火度不匹配、散热能力差、透气性差等问题，能提高多孔陶瓷材料的寿命和把持力，其烧成温度只有680～780℃，在未添加造孔剂的条件下气孔率最高可达42％，同时保持了很好的抗压强度、抗折强度和硬度,具有工业实用性。

Claims (10)

  1. 一种低熔点多孔陶瓷材料，其特征在于：其烧成温度为680-830℃，气孔率为24-42％，其原料由粘结剂和原料粉末组成，其中，原料粉末由如下质量百分比的原料组分混合后经玻化处理、湿磨、烘干及过筛而制成：
    Figure PCTCN2021100348-appb-100001
  2. 如权利要求1所述的一种低熔点多孔陶瓷材料，其特征在于：所述粘结剂为糊精。
  3. 如权利要求1所述的一种低熔点多孔陶瓷材料，其特征在于：所述硼玻璃砂与Na 2O粉能够通过2000目筛网。
  4. 如权利要求1所述的一种低熔点多孔陶瓷材料，其特征在于：所述紫砂土粉、石英粉和LiO 2粉能够通过1000目筛网。
  5. 如权利要求1至4中任一权利要求所述的一种低熔点多孔陶瓷材料，其特征在于：所述原料粉末与粘结剂的质量比为80-90:10-20。
  6. 如权利要求5所述的一种低熔点多孔陶瓷材料，其特征在于：所述原料粉末与粘结剂的质量比为85:15。
  7. 如权利要求1至4中任一权利要求所述的一种低熔点多孔陶瓷材料，其特征在于：所述原料粉末能够通过5000目筛网。
  8. 权利要求1至7中任一权利要求所述的一种低熔点多孔陶瓷材料的制备方法，其特征在于：包括如下步骤：
    (1)按所述质量百分比称取，得到各组分原料粉末；
    (2)将硼玻璃砂和Na 2O粉混合均匀后，依次经干磨和过筛，获得第一混合物；
    (3)将紫砂土粉、石英粉和LiO 2粉混合均匀后，依次经干磨和过筛，获得第二混合物；
    (4)将上述第一混合物和第二混合物混合均匀后，依次经玻化处理、湿磨、干燥和过筛，获得所述原料粉末；
    (5)将上述原料粉末与粘结剂混合均匀后，再经造粒，获得混合原料；
    (6)将上述混合原料压制成所需要的形状，并充分干燥，获得坯体；
    (7)将上述坯体升温至所述烧成温度保温烧成，即成。
  9. 如权利要求8所述的制备方法，其特征在于：所述玻化处理的温度为800-900℃。
  10. 如权利要求8所述的制备方法，其特征在于：所述步骤(7)中的升温速率为4-6℃/min，保温烧成的时间为1.5-2.5h。
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CN107001149A (zh) * 2014-05-15 2017-08-01 博韦尔公开有限公司 无硼铝合金陶瓷泡沫过滤器
CN105906311A (zh) * 2016-04-18 2016-08-31 方堃 一种低温烧结的日用陶瓷
CN112521177A (zh) * 2020-12-28 2021-03-19 华侨大学 一种低熔点多孔陶瓷材料及其制备方法

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CN115028463A (zh) * 2022-05-23 2022-09-09 中钢洛耐(洛阳)新材料有限公司 一种低导热率耐火砖加工工艺
CN115028463B (zh) * 2022-05-23 2023-06-13 中钢洛耐(洛阳)新材料有限公司 一种低导热率耐火砖加工工艺

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