CN103553610A - Low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device - Google Patents
Low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device Download PDFInfo
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- CN103553610A CN103553610A CN201310528598.7A CN201310528598A CN103553610A CN 103553610 A CN103553610 A CN 103553610A CN 201310528598 A CN201310528598 A CN 201310528598A CN 103553610 A CN103553610 A CN 103553610A
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Abstract
The invention discloses a low-temperature sintered microwave dielectric ceramic material, a preparation method and a microwave device. The material comprises (Ba (1-a)Sra)5 (Nb (1-b) Sbb) 4O15 and zinc borosilicate glass, wherein a is not larger than 0.05 and b is not larger than 0.1. The material disclosed by the invention overcomes the problem in the prior art that a copper element is introduced to increase the dielectric loss, the material is insoluble in such solvents as water, ethanol and the like, generates no gelation reaction with such adhesives as PVA (Polyvinyl Alcohol), PVB (Polyvinyl Butyral) and the like and meets the LTCC (Low Temperature Co-Fired Ceramic) process requirements, and the material disclosed by the invention is high in quality factor, adjustable in frequency resonance temperature coefficient, capable of being prepared to a microwave device with a multilayer or single-layer dielectric layer structure and is more suitable for application in the field of high-frequency and high-temperature microwave communication; the related raw materials are wide in source, low in cost, simple in process, low in production cost and suitable for industrial production of microwave dielectric ceramic devices; and the microwave dielectric material is low in dielectric loss, high in quality factor, adjustable in frequency resonance temperature coefficient and capable of meeting the requirements of the application field of high frequency, variable temperature and high reliability.
Description
Technical field
The microwave-medium ceramics technical field that the present invention relates to the microwave device such as dielectric resonator, vibrator for micro-wave communication, is specifically related to a kind of low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device.
Background technology
Along with modern communication technology is to miniaturization, integrated, modularization and the active demand of components and parts cheaply, LTCC (Low Temperature Co-fired Ceramics, the LTCC) technology with excellent electricity, machinery, thermal characteristics and high reliability has become the general choice technology that components and parts are manufactured for communication.LTCC technology maximum is characterised in that and adopts metal (as Ag) as multilayer wiring conductor material, improves signal transmission rate and reliability, and a plurality of microwave electron components and parts can be embedded in to sintering in substrate and improve packing density at double.The components and parts that adopt this technology to prepare have that dielectric loss is low, reliability is high, low cost and other advantages, have a wide range of applications.
Because the fusing point of metal A g electrode is at 960 ℃, in order to realize with ceramic co-fired, the sintering temperature of LTCC technical requirements pottery is lower than 900 ℃.Most has the microwave-medium ceramics sintering temperature of excellent properties higher than 1200 ℃, has the Ba of excellent microwave dielectric property
5nb
4o
15pottery is also like this.It is reported, Ba
5nb
4o
15the specific inductivity of microwave-medium ceramics is ε
r=39, quality factor q * f=23700GHz, temperature coefficient of resonance frequency τ
f=78ppm/ ℃, but sintering temperature is higher than 1380 ℃ of (S.Kamba etc.Highfrequency dielectric properties of A
5b
4o
15microwave ceramics, Journal of Applied Physics, 200189 (7) 3900-3906).In order to realize low temperature co-fired with Ag electrode, the people such as Kin.J.R are at < < Journal of the American Society > > 85 volumes " Microwave Dielectric Properties of Low-Fired Ba in 2002
5nb
4o
15" one the article pointed out at pottery and add low melting point oxide B
2o
3sintering temperature can be down to 900 ℃, quality factor q * f=18700GHz, also can make temperature coefficient of resonance frequency approach zero simultaneously.But adopt such scheme to prepare LTCC and still have more deficiency, be in particular in B
2o
3soluble in water, ethanol equal solvent, and with the most frequently used binding agent generation gelling reactions such as PVA, PVB, make ceramic powder can not obtain highdensity ceramic diaphragm after curtain coating.Chinese patent application 201210478550 discloses employing CuO and B
2o
3pre-burning mixture reduces sintering temperature, has realized good result, but in this material due to the existence of copper, loss is increased, quality factor reduce.
Therefore, need a kind of low-temperature sintered microwave dielectric ceramic material, do not contain copper, and can further improve with Ba
5nb
4o
15the microwave material dielectric properties of ceramic main, water insoluble, the ethanol equal solvent of this material simultaneously, and not with binding agent generation gelling reactions such as PVA, PVB, meet LTCC processing requirement, can obtain highdensity ceramic diaphragm, and wide material sources, cost is low, and the industrialization that is applicable to microwave-medium ceramics device is produced.
Summary of the invention
In view of this, the object of the invention is to provide a kind of low-temperature sintered microwave dielectric ceramic material, preparation method and microwave device, does not contain copper, and can further improve with Ba
5nb
4o
15the microwave material dielectric properties of ceramic main, water insoluble, the ethanol equal solvent of this material simultaneously, and not with binding agent generation gelling reactions such as PVA, PVB, meet LTCC processing requirement, can obtain highdensity ceramic diaphragm, and wide material sources, cost is low, and the industrialization that is applicable to microwave-medium ceramics device is produced.
Low-temperature sintered microwave dielectric ceramic material disclosed by the invention, comprises (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15with zinc boron glass, a≤0.05 wherein, b≤0.1.
Further, also comprise BaNb
2o
6;
Further,
This stupalith is ywt%[(1-x) (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15-xBaNb
2o
6]+zwt% zinc boron glass, x≤0.3 wherein, 0<z≤20, y+z=100.
Further, in described zinc boron glass, the molar percentage of zinc is 25%～50%;
Further, x=0.05～0.3;
Further, x=0.05～0.2.
The preparation method who the invention also discloses a kind of low-temperature sintered microwave dielectric ceramic material, comprises the following steps:
A. prepare (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
B. prepare BaNb
2o
6ceramic powder;
C. prepare zinc boron glass powder;
D. take (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, BaNb
2o
6ceramic powder and zinc boron glass also form mixed powder.
Further, in step a, by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, add in ball grinder and adopt wet ball-milling method mixing and ball milling containing niobium compound, antimony containing compounds, after drying, 900 ℃～1200 ℃ insulations, within 1～6 hour, obtain (Ba in baking oven
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
In step b, press BaNb
2o
6stoichiometric ratio take containing barium compound, containing niobium compound, add in ball grinder and adopt wet ball-milling method mixing and ball milling, after drying, 900 ℃～1200 ℃ insulations, within 1～6 hour, obtain BaNb in baking oven
2o
6ceramic powder;
In step c, by the molar percentage of zinc in zinc boron glass, be 25%～50% to take zinc compound and boron-containing compound, the raw material taking is added and in ball grinder, adopts wet ball-milling method mixing and ball milling, after drying, at 1100 ℃～1500 ℃, be melt into liquid glass in baking oven, and obtain low melting glass powder through shrend and pulverizing;
Further, described containing barium compound is barium carbonate or nitrate of baryta, containing strontium compound, be Strontium carbonate powder or strontium nitrate, containing niobium compound, be Niobium Pentxoxide or nitric acid niobium, antimony containing compounds is antimonous oxide or antimony peroxide, zinc compound is zinc oxide or zinc acetate, and boron-containing compound is that boron-containing compound is boric acid or boron liver.
The invention also discloses a kind of microwave device, the multilayer of being made by described low-temperature sintered microwave dielectric ceramic material or single-layer medium layer structure.
The invention has the beneficial effects as follows: adopt the divalent strontium element of minor radius and the collaborative doping of 5 valency antimony elements to improve Ba
5nb
4o
15pottery prime factor, the zinc boron low melting glass cooling-down effect simultaneously adopting is obvious, overcome copper of the prior art and introduced increase dielectric loss, and this material is water insoluble, ethanol equal solvent, and not with the binding agent generation gelling reactions such as PVA, PVB, meet LTCC processing requirement, and quality factor of the present invention are high, frequency resonance temperature factor is adjustable, can make the microwave device of multilayer or single-layer medium layer structure, is more suitable for the micro-wave communication field application of high frequency and alternating temperature; The raw material sources that relate to are extensive, and price is suitable, and technique is simple, have lower production cost, and the industrialization that is applicable to microwave-medium ceramics device is produced; The dielectric loss of microwave dielectric material is low, quality factor are high, and temperature coefficient of resonance frequency is adjustable, meets the highly reliable Application Areas requirement of high frequency, alternating temperature.
Embodiment
Low-temperature sintered microwave dielectric ceramic material disclosed by the invention, comprises (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15with zinc boron glass, a≤0.05 wherein, b≤0.1; Zinc boron low melting glass can significantly reduce (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15the sintering temperature of pottery, can burn altogether at low temperatures pottery, and can too much not reduce dielectric material performance with Ag electrode.
In the present embodiment, also comprise BaNb
2o
6; Adopt BaNb
2o
6the characteristic of negative frequency-temperature coefficient, the frequency resonance temperature factor of regulation system, the temperature reliability of raising device, makes device be applicable to alternating temperature application scenario.
In the present embodiment,
This stupalith is ywt%[(1-x) (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15-xBaNb
2o
6]+zwt% zinc boron glass, x≤0.3 wherein, 0<z≤20, y+z=100.
Further, in described zinc boron glass, the molar percentage of zinc is 25%～50%;
Further, x=0.05～0.3;
Further, x=0.05～0.2.
The preparation method who the invention also discloses a kind of low-temperature sintered microwave dielectric ceramic material, comprises the following steps:
A. prepare (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
B. prepare BaNb
2o
6ceramic powder;
C. prepare zinc boron glass powder;
D. take (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, BaNb
2o
6ceramic powder and zinc boron glass also form mixed powder.
Further, in step a, by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, add in ball grinder and adopt wet ball-milling method mixing and ball milling containing niobium compound, antimony containing compounds, after drying, 900 ℃～1200 ℃ insulations, within 1～6 hour, obtain (Ba in baking oven
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
In step b, press BaNb
2o
6stoichiometric ratio take containing barium compound, containing niobium compound, add in ball grinder and adopt wet ball-milling method mixing and ball milling, after drying, 900 ℃～1200 ℃ insulations, within 1～6 hour, obtain BaNb in baking oven
2o
6ceramic powder;
In step c, by the molar percentage of zinc in zinc boron glass, be 25%～50% to take zinc compound and boron-containing compound, the raw material taking is added and in ball grinder, adopts wet ball-milling method mixing and ball milling, after drying, at 1100 ℃～1500 ℃, be melt into liquid glass in baking oven, and obtain low melting glass powder through shrend and pulverizing;
In the present embodiment, described containing barium compound is barium carbonate or nitrate of baryta, containing strontium compound, be Strontium carbonate powder or strontium nitrate, containing niobium compound, be Niobium Pentxoxide or nitric acid niobium, antimony containing compounds is antimonous oxide or antimony peroxide, zinc compound is zinc oxide or zinc acetate, and boron-containing compound is that boron-containing compound is boric acid or boron liver.
The invention also discloses a kind of multilayer or single-layer medium layer structure microwave device; The microwave dielectric material obtaining through steps d adds and adds after proper amount of acetone, appropriate ethanol, appropriate triolein, appropriate PVB and appropriate DBP in ball grinder after ball milling 3h, after defoaming machine de-bubble, curtain coating, cutting, printed wiring, lamination, sintering obtain this microwave device, and this microwave device can be the devices such as microwave base plate, multi-layer capacitor, LC wave filter, temperature compensation wave filter.
Following table is specific embodiments of the invention, and parameter is that final microwave device detects gained:
Microwave dielectric ceramic materials in above-described embodiment adopts following three kinds of technological processs to make:
In above-described embodiment, embodiment bis-, four, six, eight, ten, 11,12,14 raw materials adopt nitrate of baryta, Niobium Pentxoxide, zinc acetate, boric acid, strontium nitrate, antimony peroxide, and embodiment mono-, three, five, seven, nine, 11,13 raw materials adopt barium carbonate, nitric acid niobium, zinc oxide, boron liver, Strontium carbonate powder and antimonous oxide; Above-mentioned raw materials is applicable to preparation (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, preparation BaNb
2o
6ceramic powder and prepare zinc boron glass powder; Do not repeat them here
Preparation technology one
Comprise the following steps:
A. prepare (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder: by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, add and adopt deionized water as ball-milling medium mixing and ball milling 20 hours in ball grinder containing niobium compound, antimony containing compounds, after drying, in retort furnace pre-burning, obtain ceramic powder in baking oven, 900 ℃～1200 ℃ of calcined temperature values, are incubated 1～6 hour and obtain (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, according to the height of calcined temperature, suitably adjusts soaking time, for the quality of the finished product and have no significant effect;
B. prepare BaNb
2o
6ceramic powder: press BaNb
2o
6stoichiometric ratio take containing barium compound, containing niobium compound, add and in ball grinder, adopt ethanol as ball-milling medium mixing and ball milling 12 hours, after drying, in retort furnace pre-burning, obtain ceramic powder in baking oven, 900 ℃～1200 ℃ of calcined temperature values, soaking time value obtains BaNb for 1-6 hour
2o
6ceramic powder; According to the height of calcined temperature, suitably adjust soaking time, for the quality of the finished product and have no significant effect;
C. prepare zinc boron glass powder: by the molar percentage of zinc in zinc boron glass, be 25%～50% to take zinc compound and boron-containing compound, the raw material taking is added and in ball grinder, adopts n-propyl alcohol as ball-milling medium mixing and ball milling 20 hours, after drying, at 1100 ℃～1500 ℃, be melt into liquid glass in baking oven, and obtain low melting glass powder through shrend and pulverizing;
D. by x value and z value, take ceramic powder and low melting glass and form mixed powder, then adding massfraction is after 25% acetone, 17% ethanol, 1% triolein, 1%PVB and 1%DBP, to add in ball grinder after ball milling 3h, after defoaming machine de-bubble, after curtain coating, cutting, print copper circuit, lamination, sintering, obtains microwave device.
As can be seen from the above table:
Embodiment mono-to embodiment five (embodiment mono-is the comparative example of not modification) shows to adopt positive divalent strontium element and the collaborative doping of the positive 5 valency antimony elements Ba of minor radius
5nb
4o
15, can effectively regulate the microwave dielectric property of material.Particularly the microwave property of the material of embodiment 3 is better, DIELECTRIC CONSTANT ε
r=37.1, quality factor q * f can reach 42600GHz, simultaneously temperature coefficient of resonance frequency τ
f=51ppm/ ℃.
Embodiment six to embodiment eight shows BaNb
2o
6pottery can significantly regulate the temperature coefficient of resonance frequency of material, makes material be applicable to the occasion of temperature variation.Particularly work as BaNb
2o
6when ceramic content is 0.1mol, embodiment 7, temperature coefficient of resonance frequency τ
f=3ppm/ ℃.
Embodiment nine to embodiment 14 shows that zinc boron glass has good temperature reduction performance, adds a small amount of zinc boron glass and not only makes material burn altogether with Ag electrode at 900 ℃, nor can significantly worsen material property.The temperature coefficient of resonance frequency τ of material
fby just becoming negative.Particularly embodiment 11 has obtained material system and the preparation technology of excellent combination property.
Embodiment 14 has obtained the most excellent low temperature co-fired microwave dielectric material of over-all properties.Be a=0.02, b=0.05, x=0.1, during z=5wt%, DIELECTRIC CONSTANT ε
r=35.5, quality factor q * f can reach 33600GHz, simultaneously temperature coefficient of resonance frequency τ
f=1ppm/ ℃.
According to the parameter comparison of above-described embodiment, it is moderate that microwave dielectric material of the present invention has specific inductivity, and quality factor are high, the advantage that temperature coefficient of resonance frequency is adjustable.Embodiment tri-, seven and nine to 14 obtains good microwave dielectric material, and particularly embodiment 14 over-all propertieies are best, quality factor q * f>30000GHz, temperature coefficient of resonance frequency τ
fnear zero, other embodiment compare slightly inadequate with embodiment 14, but still meet implementing process of the present invention and requirement.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (10)
1. a low-temperature sintered microwave dielectric ceramic material, is characterized in that: comprise (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15with zinc boron glass, a≤0.05 wherein, b≤0.1.
2. low-temperature sintered microwave dielectric ceramic material according to claim 1, is characterized in that: also comprise BaNb
2o
6.
3. low-temperature sintered microwave dielectric ceramic material according to claim 2, is characterized in that: this stupalith is ywt%[(1-x) (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15-xBaNb
2o
6]+zwt% zinc boron glass, x≤0.3 wherein, 0<z≤20, y+z=100.
4. low-temperature sintered microwave dielectric ceramic material according to claim 3, is characterized in that: in described zinc boron glass, the molar percentage of zinc is 25%～50%.
5. low-temperature sintered microwave dielectric ceramic material according to claim 4, is characterized in that: x=0.05～0.3.
6. low-temperature sintered microwave dielectric ceramic material according to claim 5, is characterized in that: x=0.05～0.2.
7. a preparation method for low-temperature sintered microwave dielectric ceramic material, is characterized in that: comprise the following steps:
A. prepare (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
B. prepare BaNb
2o
6ceramic powder;
C. prepare zinc boron glass powder;
D. take (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder, BaNb
2o
6ceramic powder and zinc boron glass also form mixed powder.
8. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 7, is characterized in that: in step a, by (Ba
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15stoichiometric ratio take containing barium compound, containing strontium compound, add in ball grinder and adopt wet ball-milling method mixing and ball milling containing niobium compound, antimony containing compounds, after drying, 900 ℃～1200 ℃ insulations, within 1～6 hour, obtain (Ba in baking oven
(1-a)sr
a)
5(Nb
(1-b)sb
b)
4o
15ceramic powder;
In step b, press BaNb
2o
6stoichiometric ratio take containing barium compound, containing niobium compound, add in ball grinder and adopt wet ball-milling method mixing and ball milling, after drying, 900 ℃～1200 ℃ insulations, within 1～6 hour, obtain BaNb in baking oven
2o
6ceramic powder;
In step c, by the molar percentage of zinc in zinc boron glass, be 25%～50% to take zinc compound and boron-containing compound, the raw material taking is added and in ball grinder, adopts wet ball-milling method mixing and ball milling, after drying, at 1100 ℃～1500 ℃, be melt into liquid glass in baking oven, and obtain low melting glass powder through shrend and pulverizing.
9. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 8, it is characterized in that: described containing barium compound is barium carbonate or nitrate of baryta, containing strontium compound, be Strontium carbonate powder or strontium nitrate, containing niobium compound, be Niobium Pentxoxide or nitric acid niobium, antimony containing compounds is antimonous oxide or antimony peroxide, zinc compound is zinc oxide or zinc acetate, and boron-containing compound is that boron-containing compound is boric acid or boron liver.
10. a microwave device, is characterized in that: the multilayer of being made by the low-temperature sintered microwave dielectric ceramic material described in the arbitrary claim of claim 1-6 or single-layer medium layer structure.
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| CN107244916A (en) * | 2017-05-19 | 2017-10-13 | 电子科技大学 | A kind of niobate low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN110171972A (en) * | 2019-01-04 | 2019-08-27 | 南京汇聚新材料科技有限公司 | A kind of low-temperature sintered ceramics material |
| CN112010649A (en) * | 2020-09-08 | 2020-12-01 | 中物院成都科学技术发展中心 | Low-cost ceramic substrate large-scale preparation method for filter |
| TWI728509B (en) * | 2019-10-16 | 2021-05-21 | 道登電子材料股份有限公司 | Low temperature co-fired ceramic paste and method for preparing high-frequency microwave dielectric unit therefrom |
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| CN101182205A (en) * | 2007-11-16 | 2008-05-21 | 北京交通大学 | Yttrium niobate solid-phase reaction synthetic sintering method capable of being used for microwave dielectric ceramic |
| CN102976751A (en) * | 2012-11-22 | 2013-03-20 | 云南云天化股份有限公司 | Low-temperature sintering microwave dielectric ceramic material and preparation method thereof |
| CN103146345A (en) * | 2013-01-30 | 2013-06-12 | 云南云天化股份有限公司 | Microwave dielectric materials capable of burning with copper electrodes together, preparation method and application thereof |
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| CN101050101A (en) * | 2007-05-18 | 2007-10-10 | 厦门大学 | Microwave medium ceramic material in series of low temperature sintered Ba5(Nb, Sb)4O15, and preparation method |
| CN101182205A (en) * | 2007-11-16 | 2008-05-21 | 北京交通大学 | Yttrium niobate solid-phase reaction synthetic sintering method capable of being used for microwave dielectric ceramic |
| CN102976751A (en) * | 2012-11-22 | 2013-03-20 | 云南云天化股份有限公司 | Low-temperature sintering microwave dielectric ceramic material and preparation method thereof |
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| CN107244916A (en) * | 2017-05-19 | 2017-10-13 | 电子科技大学 | A kind of niobate low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN107244916B (en) * | 2017-05-19 | 2020-05-12 | 电子科技大学 | Niobate-series low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN110171972A (en) * | 2019-01-04 | 2019-08-27 | 南京汇聚新材料科技有限公司 | A kind of low-temperature sintered ceramics material |
| TWI728509B (en) * | 2019-10-16 | 2021-05-21 | 道登電子材料股份有限公司 | Low temperature co-fired ceramic paste and method for preparing high-frequency microwave dielectric unit therefrom |
| CN112010649A (en) * | 2020-09-08 | 2020-12-01 | 中物院成都科学技术发展中心 | Low-cost ceramic substrate large-scale preparation method for filter |
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|---|---|
| CN103553610B (en) | 2015-04-15 |
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Effective date of registration: 20170119 Address after: The 401220 Chongqing economic and Technological Zone Changshou District Qixin Road No. 22 Patentee after: Chongqing Yuntianhua hanen New Material Development Co Ltd Patentee after: Yutianhua Co., Ltd., Yunnan Address before: 650228 Dianchi Road, Yunnan, China, No. 1417, No. Patentee before: Yutianhua Co., Ltd., Yunnan |