CN105236953A - Process for preparing low-dielectric-loss microwave electronic ceramic material - Google Patents

Process for preparing low-dielectric-loss microwave electronic ceramic material Download PDF

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Publication number
CN105236953A
CN105236953A CN201510527166.3A CN201510527166A CN105236953A CN 105236953 A CN105236953 A CN 105236953A CN 201510527166 A CN201510527166 A CN 201510527166A CN 105236953 A CN105236953 A CN 105236953A
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China
Prior art keywords
low
dielectric
preparation technology
powder
ball milling
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CN201510527166.3A
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Inventor
王永生
胥阳春
刘珍
侯冬梅
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CHENGDU SHUN KANG SANSEN ELECTRONICS Co Ltd
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CHENGDU SHUN KANG SANSEN ELECTRONICS Co Ltd
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Priority to CN201510527166.3A priority Critical patent/CN105236953A/en
Publication of CN105236953A publication Critical patent/CN105236953A/en
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Abstract

The invention discloses a process for preparing a low-dielectric-loss microwave electronic ceramic material. The preparation process is simple, adopts conventional production equipment, is low in production cost and has an excellent industrial application value. The low-dielectric-loss microwave electronic ceramic material prepared by the process has a dielectric constant of 7-10, and has low loss (Qf is more than 100,000GHz) and a near-zero resonance frequency temperature coefficient. By utilizing the low-dielectric-constant microwave dielectric ceramics, a dielectric resonator, a filter and other microwave elements and devices are suitable for applications with high frequency and high power, and the frequency temperature stability of devices can be improved.

Description

A kind of preparation technology of low-dielectric loss microwave electron stupalith
Technical field
The invention belongs to microwave dielectric ceramic materials manufacturing technology field, be specifically related to a kind of preparation technology of low-dielectric loss microwave electron stupalith.
Background technology
Microwave electron pottery is the class new function stupalith grown up nearly decades, being applied in microwave frequency band (mainly 300MHz ~ 30GHz) circuit as dielectric material and completing one or more functions, is the critical material manufacturing the microwave components such as wave filter, resonator, vibrator, transposer.In recent years, along with the develop rapidly of the modern communication technologys such as mobile communication, satellite communications, Global Positioning System (GPS), Bluetooth technology and WLAN (wireless local area network) (WLAN), microwave technology also turns to higher frequency, namely towards the wider millimeter wave of available band and sub-millimeter wave future development.Specific inductivity is low, has high Q × f value and the research of the microwave dielectric ceramic materials of temperature coefficient of resonance frequency nearly zero is subject to extensive concern simultaneously.This type of material has been widely used in the fields such as satellite communication, guided missile remote control and Global Positioning System (GPS) antenna at present, these Application Areass, except requiring that pottery has except lower dielectric loss, low temperature coefficient of resonance frequency, also require that pottery has less specific inductivity in order to reduce the delay of signal.
Although current existing Al 2o 3, MgAlO 4on medium with low dielectric constant pottery, but have that sintering temperature is high, preparation difficulty and the shortcoming such as temperature coefficient of resonance frequency is larger.
Summary of the invention
The object of the invention is to solve the problem, a kind of preparation technology of low-dielectric loss microwave electron stupalith is provided, make the low-dielectric loss microwave electron ceramic dielectric constant made be 7 ~ 10, have low-loss and good temperature stability simultaneously.
For solving the problems of the technologies described above, the preparation technology of low-dielectric loss microwave electron stupalith of the present invention, comprises the following steps:
Step one, take ZnO, SiO by certain mol proportion rate 2, TiO 2, CaCO 3and Al 2o 3as starting material;
Add water in step 2, starting material in step one and zirconia balls carries out ball milling, after ball milling terminates, dry, sieve, obtain powder;
Step 3, by the temperature lower calcination 2 ~ 4h of powder at 1150 ~ 1300 DEG C, obtain calcining powder;
Step 4, in calcining powder, add water and zirconia balls, and then add binding agent, dispersion agent and releasing agent, ball milling 12 ~ 24h, granulation;
Step 5, grain step 4 made are pressed into finished product, and sinter 2 ~ 4h in the temperature range of 1300 ~ 1450 DEG C, obtain low-dielectric loss microwave electron stupalith.
In step 3, calcining temperature is 1200 DEG C, and calcination time is 3h.
In step 4, described binding agent is selected from the mixture of a kind of in polyvinyl alcohol solution, polyvinyl butyral solution, acrylic acid solution or methylcellulose gum or at least two kinds.
In step 5, described pressing pressure is 4Mpa, and the finished diameter suppressed is 12 ~ 14mm, thickness is 5 ~ 8mm, and described finished product sintering temperature is 1400 DEG C, and sintering time is 3h.
The expression formula of the low-dielectric loss microwave electron stupalith that above-mentioned preparation technology makes is aZnO.bSiO 2.cTiO 2.dCaCO 3.eAl 2o 3,
Wherein a, b, c, d and e independently represent molar ratio, and meet:
35mol%≤a≤45mol%,30mol%≤b≤35mol%,0mol%≤c≤10mol%,10mol%≤d≤20mol%,0mol%≤e≤10mol%,a+b+c+d+e=100mol%。
The preferred content of each composition is: a=40mol%, b=32mol%, c=5mol%, d=18mol%, e=5mol%.
Compared with prior art, advantage of the present invention is as follows:
1, preparation technology is simple, and adopt conventional production equipment, production cost is low, has good industrial application value.
2, its specific inductivity of low-dielectric loss microwave electron stupalith made is 7 ~ 10, have low-loss (Qf > 100000GHz) and near-zero resonance frequency temperature coefficient simultaneously, utilize dielectric constant microwave ceramic medium provided by the invention, the microwave device such as dielectric resonator and wave filter can be made to be applicable to higher frequency and more powerful application, to be conducive to the frequency stability of temperature improving device.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment one
A preparation technology for low-dielectric loss microwave electron stupalith, comprises the following steps:
Step one, take ZnO, SiO by 40mol%, 32mol%, 5mol%, 18mol% and 5mol% molar ratio respectively 2, TiO 2, CaCO 3and Al 2o 3as starting material;
Add water in step 2, starting material in step one and zirconia balls carries out ball milling 12h, after ball milling terminates, dry, sieve, obtain powder;
Step 3, by the temperature lower calcination 4h of powder at 1150 DEG C, obtain calcining powder;
Step 4, in calcining powder, add water and zirconia balls, and then add polyvinyl alcohol solution, dispersion agent and the releasing agent of 5%, ball milling 12h, granulation;
Step 5, grain step 4 made are pressed into finished product, and pressing pressure is 4Mpa, and the finished diameter suppressed is 12mm, thickness is 8mm, and sinter 4h in the temperature range of 1300 DEG C, obtain low-dielectric loss microwave electron stupalith.
Embodiment two
A preparation technology for low-dielectric loss microwave electron stupalith, comprises the following steps:
Step one, take ZnO, SiO by 45mol%, 30mol%, 7mol%, 10mol% and 8mol% molar ratio respectively 2, TiO 2, CaCO 3and Al 2o 3as starting material;
Add water in step 2, starting material in step one and zirconia balls carries out ball milling 12h, after ball milling terminates, dry, sieve, obtain powder;
Step 3, by the temperature lower calcination 2h of powder at 1300 DEG C, obtain calcining powder;
Step 4, in calcining powder, add water and zirconia balls, and then add polyvinyl butyral solution, dispersion agent and releasing agent, ball milling 24h, granulation;
Step 5, grain step 4 made are pressed into finished product, and pressing pressure is 4Mpa, and the finished diameter suppressed is 14mm, thickness is 5mm, and sinter 2h in the temperature range of 1450 DEG C, obtain low-dielectric loss microwave electron stupalith.
Embodiment three
A preparation technology for low-dielectric loss microwave electron stupalith, comprises the following steps:
Step one, take ZnO, SiO by 40mol%, 32mol%, 5mol%, 18mol% and 5mol% molar ratio respectively 2, TiO 2, CaCO 3and Al 2o 3as starting material;
Add water in step 2, starting material in step one and zirconia balls carries out ball milling 12h, after ball milling terminates, dry, sieve, obtain powder;
Step 3, by the temperature lower calcination 3h of powder at 1200 DEG C, obtain calcining powder;
Step 4, in calcining powder, add water and zirconia balls, and then add polyvinyl alcohol solution, acrylic acid solution, dispersion agent and releasing agent, ball milling 12 ~ 24h, granulation;
Step 5, grain step 4 made are pressed into finished product, and pressing pressure is 4Mpa, and the finished diameter suppressed is 13mm, thickness is 7mm, and sinter 3h in the temperature range of 1400 DEG C, obtain low-dielectric loss microwave electron stupalith.
Those of ordinary skill in the art will appreciate that, embodiment described here is to help reader understanding's principle of the present invention, should be understood to that protection scope of the present invention is not limited to so special statement and embodiment.Those of ordinary skill in the art can make various other various concrete distortion and combination of not departing from essence of the present invention according to these technology enlightenment disclosed by the invention, and these distortion and combination are still in protection scope of the present invention.

Claims (5)

1. a preparation technology for low-dielectric loss microwave electron stupalith, is characterized in that, comprises the following steps:
Step one, take ZnO, SiO by certain mol proportion rate 2, TiO 2, CaCO 3and Al 2o 3as starting material;
Add water in step 2, starting material in step one and zirconia balls carries out ball milling, after ball milling terminates, dry, sieve, obtain powder;
Step 3, by the temperature lower calcination 2 ~ 4h of powder at 1150 ~ 1300 DEG C, obtain calcining powder;
Step 4, in calcining powder, add water and zirconia balls, and then add binding agent, dispersion agent and releasing agent, ball milling 12 ~ 24h, granulation;
Step 5, grain step 4 made are pressed into finished product, and sinter 2 ~ 4h in the temperature range of 1300 ~ 1450 DEG C, obtain low-dielectric loss microwave electron stupalith.
2. preparation technology according to claim 1, is characterized in that: in step 3, and calcining temperature is 1200 DEG C, and calcination time is 3h.
3. preparation technology according to claim 1, is characterized in that: in step 4, and described binding agent is selected from the mixture of a kind of in polyvinyl alcohol solution, polyvinyl butyral solution, acrylic acid solution or methylcellulose gum or at least two kinds.
4. preparation technology according to claim 1, is characterized in that: in step 5, described pressing pressure is 4Mpa, and the finished diameter suppressed is 12 ~ 14mm, thickness is 5 ~ 8mm.
5. preparation technology according to claim 1, is characterized in that: in step 5, and described finished product sintering temperature is 1400 DEG C, and sintering time is 3h.
CN201510527166.3A 2015-08-25 2015-08-25 Process for preparing low-dielectric-loss microwave electronic ceramic material Pending CN105236953A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106431388A (en) * 2016-09-22 2017-02-22 深圳方泰新材料技术有限公司 Microwave ceramic dielectric resonator and preparation method and application thereof
CN108341662A (en) * 2018-04-17 2018-07-31 南京大学 A kind of preparation method of low dielectric constant and low loss high-frequency ceramic baseplate material
CN113943147A (en) * 2021-12-07 2022-01-18 无锡市惠丰电子有限公司 Preparation method of dielectric ceramic material

Citations (4)

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Publication number Priority date Publication date Assignee Title
US20020142187A1 (en) * 2000-12-19 2002-10-03 Murata Manufacturing Co., Ltd. Composite multilayer ceramic electronic parts and method of manufacturing the same
CN103613369A (en) * 2013-10-22 2014-03-05 山东科技大学 Silicate low-temperature co-fired ceramic substrate material and preparation method thereof
CN103864406A (en) * 2014-02-12 2014-06-18 同济大学 Low dielectric constant microwave dielectric ceramic and preparation method thereof
CN104496442A (en) * 2014-11-27 2015-04-08 中国计量学院 Microwave dielectric ceramic powder with low dielectric constant, and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020142187A1 (en) * 2000-12-19 2002-10-03 Murata Manufacturing Co., Ltd. Composite multilayer ceramic electronic parts and method of manufacturing the same
CN103613369A (en) * 2013-10-22 2014-03-05 山东科技大学 Silicate low-temperature co-fired ceramic substrate material and preparation method thereof
CN103864406A (en) * 2014-02-12 2014-06-18 同济大学 Low dielectric constant microwave dielectric ceramic and preparation method thereof
CN104496442A (en) * 2014-11-27 2015-04-08 中国计量学院 Microwave dielectric ceramic powder with low dielectric constant, and preparation method thereof

Non-Patent Citations (1)

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Title
邹佳丽: "新型ZnO-SiO2低介高频微波介质陶瓷研究", 《浙江大学博士学位论文》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106431388A (en) * 2016-09-22 2017-02-22 深圳方泰新材料技术有限公司 Microwave ceramic dielectric resonator and preparation method and application thereof
CN108341662A (en) * 2018-04-17 2018-07-31 南京大学 A kind of preparation method of low dielectric constant and low loss high-frequency ceramic baseplate material
CN113943147A (en) * 2021-12-07 2022-01-18 无锡市惠丰电子有限公司 Preparation method of dielectric ceramic material

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Application publication date: 20160113