CN107746263A - A kind of Compound Ceramic Evaporator and its manufacture method - Google Patents
A kind of Compound Ceramic Evaporator and its manufacture method Download PDFInfo
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Abstract
The invention discloses a kind of Compound Ceramic Evaporator and its manufacture method, comprise the following steps：(1) dispensing batch mixing：Mixed powder：Zirconium silicate powder, boron oxide powder, boron nitride powder, nano carbon black powder, aluminum oxide, yttrium oxide powder, it is added to according to a certain percentage in deionized water, add polyvinyl alcohol to be well mixed as binding agent, strong stirring, obtain the mixed slurry of certain viscosity；(2) drying and screening；(3) it is preforming；(3) high temperature sintering.Between the diphase ceramic material room temperature resistivity manufactured using this method is distributed in 500 2000 μ Ω cm, machinability and antioxygenic property are good, and thermal conductivity is high, can be used in manufacturing vacuum aluminum-coated membrane process conductive evaporation boat, greatly improves its working life.
Description
Technical field
The present invention relates to a kind of Compound Ceramic Evaporator and its manufacture method, can be used in very more particularly to one kind
Sky is aluminized the hot pressed sintering boride ceramics evaporation boat of membrane process, belongs to engineering ceramic material technical field.
Background technology
Vacuum evaporation, which is aluminized, to have a very wide range of applications, such as food fresh keeping packaging, polyester polypropylene film plating aluminum capacitor
Aluminize anti-false trademark, crt screen of device, laser is aluminized with large scale integrated circuit beam evaporation of aluminum etc., and wherein evaporation boat is most important
Attrition component, the production efficiency and cost of the height direct relation enterprise of its service life.It is suitable that evaporation boat requires that material has
Electrical resistivity range and temperature-coefficient of electrical resistance, excellent high temperature resistant and thermal shock characteristic, have good wetting with aluminium liquid under high temperature
Characteristic, and excellent preventing corrosion from molten metals characteristic, high mechanical strength and are easily worked.
The evaporation boat material of early stage is mainly graphite, but is easily corroded by aluminium liquid, and service life is low, is eliminated substantially.Mesh
Preceding evaporation boat main product employed both at home and abroad is BN-TiB2(two components), BN-TiB2- Al (three components) and BN-TiB2-
AlN-Al (four components) titanium boride base complex phase ceramic.Using micron order raw material, hot-pressing sintering technique manufacture.Its primary raw material boronation
Titanium valve body is domestic to be manufactured using carbothermic method, and granularity is thicker, and follow-up powder has to pass through multiple tracks grinding, causes powder purity
Reduce, high impurity causes the resistivity of evaporation boat unstable, poor corrosion resistance.Meanwhile titanium boride ceramicses exceed in temperature
After 1000 DEG C, antioxygenic property is poor, causes that evaporation boat temperature in use is low, and service life is low, has a strong impact on coating quality.Therefore,
The necessary import of the evaporation boat of domestic high quality, greatly limit the development of China's vacuum evaporation industry.
The content of the invention
It is an object of the invention to provide a kind of Compound Ceramic Evaporator and its manufacture method, the present invention uses following technology
Scheme：
A kind of manufacture method of Compound Ceramic Evaporator, comprises the following steps：
(1) dispensing batch mixing：
Mixed powder：Zirconium silicate powder, boron oxide powder, boron nitride powder, nano carbon black powder, aluminum oxide, yittrium oxide
Powder, it is added to according to a certain percentage in deionized water, adds polyvinyl alcohol and be well mixed as binding agent, strong stirring, obtained
To the mixed slurry of certain viscosity；
(2) drying and screening
In an oven 2-4 hours are dried for 80-100 DEG C in mixed slurry, sieving obtains composite granule；
(3) it is preforming
Composite granule is placed in graphite jig, is molded in dry-pressing formed machine precompressed 5-15MPa；
(3) high temperature sintering
Graphite jig after will be preforming is placed in hot-pressed sintering furnace high temperature sintering, maximum sintering temperature 1900-2100
DEG C, pressure 10-30MPa, soaking time is 1-2 hours.
Described manufacture method, in step (1), the weight percent content of zirconium silicate powder is 35-42%, boron oxide powder
The weight percent content of body is 13.5-16%, the weight percent content of boron nitride powder is 11-25%, silicon carbide powder
Weight percent content be 0-4%, the weight percent content of nano carbon black is 18.5-22%, the weight of alumina powder
Degree is 3-5%, and the weight percent content of yttrium oxide powder is 4-8%.
Described manufacture method, in step (1), the granularity of the zirconium silicate powder is 0.5-5.0 μm, boron oxide powder
Granularity is 0.5-10.0 μm, and the granularity of boron nitride powder is 0.5-5.0 μm, and the granularity of silicon carbide powder is 0.5-3.0 μm, nanometer
The granularity of carbon black is 0.02-0.2 μm；Aluminum oxide, the granularity of yttrium oxide powder are 0.05-0.5 μm.
Described manufacture method, in step (1), the weight of alumina powder and yttrium oxide powder ratio in the mixed powder
For 0.6-0.8.
Described manufacture method, in step (3), maximum sintering temperature is 1900-2100 DEG C.
Described manufacture method, maximum sintering temperature are 2060 DEG C.
Described manufacture method, in step (3), highest dwell pressure is 10-30MPa.
Described manufacture method, highest dwell pressure are 25MPa.
It is a kind of according to any of the above-described methods described manufacture Compound Ceramic Evaporator, its composition include zirconium boride, boron nitride,
Carborundum and yttrium-aluminium-garnet；The content of zirconium boride is 35-45%, and the content of boron nitride is in 20-40%, the content of carborundum
10-20%, the content of yttrium-aluminium-garnet is in 12-20%.
The present invention has following clear advantage：
(1) raw material synthesized using zirconium silicate, boron oxide, nano carbon black as zirconium boride powder, raw material sources are compared
Abundant, cost is cheap, and cost of material only has the 1/5 of traditional raw material.
(2) use and boron nitride, carborundum are introduced in material powder, improve mixture homogeneity, after being advantageous to regulation and control sintering
The resistivity and mechanical strength of complex phase ceramic.
(3) manufactured using the technique of in-situ reducing combination hot pressed sintering, eliminate advance carbon thermal reduction system in other techniques
Standby zirconium boride powder, so as to greatly reduce energy consumption, reduces manufacturing cost.
(4) technique for using reaction in-situ combination hot pressed sintering, and aluminum oxide and yittrium oxide reduce as sintering aid
Sintering temperature, improves the consistency of material, and sintering cost reduces.
The second object of the present invention is to provide a kind of evaporation boat diphase ceramic material, has following features：
The content of zirconium boride is 35-45% in the diphase ceramic material, and the content of boron nitride is 20-40%, carborundum
Content is 10-20%, and the content of yttrium-aluminium-garnet is 12-20%.
The diphase ceramic material compares existing boronation titanium base material, has advantage as is evident below：
(1) diphase ceramic material contains four kinds of main components, and uniform microstructure, crystallite dimension is tiny, and purity is high, carries
High Stability of Resistivity.
(2) diphase ceramic material contains 10-20% carborundum, substantially increases the anti-oxidant and mechanicalness of material
Can, temperature in use is up to more than 1800 DEG C.
(3) diphase ceramic material contains 20-40% boron nitride and 10-20% carborundum, the resistivity of material and
Temperature-coefficient of electrical resistance is adjustable, has good preventing corrosion from molten metals.
(4) diphase ceramic material contains 12-16% yttrium-aluminium-garnet, the elevated temperature strength and thermal shock resistance of material
Greatly improve.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The boron oxide powder for being 0.5 μm by zirconium silicate powder that 36.6Kg D50 is 0.5 μm, 14Kg D50,10Kg
D50 is 0.5 μm of boron nitride powder, 0.5Kg D50 is 0.5 μm silicon carbide powder, 19.2Kg granularity are 0.02 μm
Nano carbon black, the alumina powder that 3.0Kg D50 is 0.05 μm, the yttrium oxide powder that 5Kg D50 is 0.05 μm, 2.3Kg
In poly-vinyl alcohol solution and 132Kg deionized water, it is well mixed in machine,massing and obtains mixed slurry.Mixed slurry
Material is dried 4 hours for 80 DEG C in an oven, and sieving obtains composite granule.Composite granule is placed in graphite jig, dry-pressing into
Type machine precompressed 5MPa is molded.After preforming hot-pressed sintering furnace high temperature sintering, highest sintering temperature are placed in together with one piece of graphite jig
Spend for 1900 DEG C, pressure 30MPa, soaking time is 2 hours.The diphase ceramic material zirconium boride obtained by the manufacturing process
Content is 44.2%, carborundum content 16.6%, boron nitride content 23.5%, and yttrium-aluminium-garnet content is 15.7%.Cause
Density is 97.5%, and room temperature resistivity is 600 μ Ω cm, and processability is good.The vacuum manufactured with the diphase ceramic material
Aluminize membrane process conductive evaporation boat, the continuous use life-span up to more than 15 hours, is significantly better than existing product.
Embodiment 2
The boron oxide powder for being 0.5 μm by zirconium silicate powder that 36.6Kg D50 is 0.5 μm, 14Kg D50,24Kg
D50 is 0.5 μm of boron nitride powder, 19.2Kg granularity is 0.02 μm nano carbon black, 4.0Kg D50 are 0.05 μm
Yttrium oxide powder, 10.2Kg poly-vinyl alcohol solution and the 102Kg deionized water that alumina powder, 5Kg D50 are 0.05 μm
In, it is well mixed in machine,massing and obtains mixed slurry.Mixed slurry is dried 2 hours for 100 DEG C in an oven,
Sieving obtains composite granule.Composite granule is placed in graphite jig, is molded in dry-pressing formed machine precompressed 15MPa.Connect after preforming
With graphite jig, one piece is placed in hot-pressed sintering furnace high temperature sintering, and maximum sintering temperature is 2100 DEG C, pressure 10MPa, insulation
Time is 1 hour.The diphase ceramic material boronation zirconium content obtained by the manufacturing process is 36.1%, and carborundum content is
12.5%, boron nitride content 38.3%, yttrium-aluminium-garnet content is 12.8%.Consistency is 98.1%, and room temperature resistivity is
1890 μ Ω cm, processability are good.The vacuum aluminum-coated membrane process conductive evaporation boat manufactured with the diphase ceramic material,
The life-span is used continuously up to more than 15 hours, is significantly better than existing product.
Embodiment 3
The boron oxide powder for being 0.5 μm by zirconium silicate powder that 36.6Kg D50 is 0.5 μm, 14Kg D50,18Kg
D50 is 0.5 μm of boron nitride powder, 2Kg D50 is 1.2 μm silicon carbide powder, 19.2Kg granularity are 0.02 μm and received
Rice carbon black, the alumina powder that 3.5Kg D50 is 0.05 μm, the yttrium oxide powder that 5Kg D50 is 0.05 μm, 6.1Kg it is poly-
In glycohol solution and 120Kg deionized water, it is well mixed in machine,massing and obtains mixed slurry.Mixed slurry
80 DEG C are dried 4 hours in an oven, and sieving obtains composite granule.Composite granule is placed in graphite jig, dry-pressing formed
Machine precompressed 10MPa is molded.After preforming hot-pressed sintering furnace high temperature sintering, maximum sintering temperature are placed in together with one piece of graphite jig
For 2060 DEG C, pressure 25MPa, soaking time is 2 hours.The diphase ceramic material zirconium boride obtained by the manufacturing process contains
Measure as 38.6%, carborundum content 17.1%, boron nitride content 30.7%, yttrium-aluminium-garnet content is 13.7%.It is fine and close
Spend for 99.2%, room temperature resistivity is 1340 μ Ω cm, and processability is good.The vacuum manufactured with the diphase ceramic material
Aluminize membrane process conductive evaporation boat, the continuous use life-span up to more than 15 hours, is significantly better than existing product.
Embodiment 4
The boron oxide powder for being 0.5 μm by zirconium silicate powder that 36.6Kg D50 is 0.5 μm, 14Kg D50,12Kg
D50 is 0.5 μm of boron nitride powder, 0.5Kg D50 is 0.6 μm silicon carbide powder, 19.2Kg granularity are 0.02 μm
Nano carbon black, the alumina powder that 3.6Kg D50 is 0.05 μm, the yttrium oxide powder that 6Kg D50 is 0.05 μm, 2.3Kg
In poly-vinyl alcohol solution and 138Kg deionized water, it is well mixed in machine,massing and obtains mixed slurry.Mixed slurry
Material is dried 2 hours for 100 DEG C in an oven, and sieving obtains composite granule.Composite granule is placed in graphite jig, dry-pressing into
Type machine precompressed 5MPa is molded.After preforming hot-pressed sintering furnace high temperature sintering, highest sintering temperature are placed in together with one piece of graphite jig
Spend for 1950 DEG C, pressure 25MPa, soaking time is 2 hours.The diphase ceramic material zirconium boride obtained by the manufacturing process
Content is 42.9%, carborundum content 16.1%, boron nitride content 22.8%, and yttrium-aluminium-garnet content is 18.2%.Cause
Density is 97.2%, and room temperature resistivity is 550 μ Ω cm, and processability is good.The vacuum manufactured with the diphase ceramic material
Aluminize membrane process conductive evaporation boat, the continuous use life-span up to more than 15 hours, is significantly better than existing product.
Embodiment 5
The boron oxide powder for being 0.5 μm by zirconium silicate powder that 36.6Kg D50 is 0.5 μm, 14Kg D50,22Kg
D50 is 0.5 μm of boron nitride powder, 0.5Kg D50 is 0.6 μm silicon carbide powder, 19.2Kg granularity are 0.02 μm
Nano carbon black, the alumina powder that 4.8Kg D50 is 0.05 μm, the yttrium oxide powder that 6Kg D50 is 0.05 μm, 2.6Kg
In poly-vinyl alcohol solution and 154Kg deionized water, it is well mixed in machine,massing and obtains mixed slurry.Mixed slurry
Material is dried 4 hours for 80 DEG C in an oven, and sieving obtains composite granule.Composite granule is placed in graphite jig, dry-pressing into
Type machine precompressed 15MPa is molded.After preforming hot-pressed sintering furnace high temperature sintering, highest sintering temperature are placed in together with one piece of graphite jig
Spend for 2000 DEG C, pressure 25MPa, soaking time is 2 hours.The diphase ceramic material zirconium boride obtained by the manufacturing process
Content is 35.6%, carborundum content 12.6%, boron nitride content 34.7%, and yttrium-aluminium-garnet content is 17%.It is fine and close
Spend for 97.9%, room temperature resistivity is 1650 μ Ω cm, and processability is good.The vacuum manufactured with the diphase ceramic material
Aluminize membrane process conductive evaporation boat, the continuous use life-span up to more than 15 hours, is significantly better than existing product.
Embodiment 6
The boron oxide powder for being 0.5 μm by zirconium silicate powder that 36.6Kg D50 is 0.5 μm, 14Kg D50,14Kg
D50 is 0.5 μm of boron nitride powder, 1.5Kg D50 is 1.2 μm silicon carbide powder, 19.2Kg granularity are 0.02 μm
Nano carbon black, the alumina powder that 4.2Kg D50 is 0.05 μm, the yttrium oxide powder that 6Kg D50 is 0.05 μm, 2.5Kg
In poly-vinyl alcohol solution and 146Kg deionized water, it is well mixed in machine,massing and obtains mixed slurry.Mixed slurry
Material is dried 2 hours for 100 DEG C in an oven, and sieving obtains composite granule.Composite granule is placed in graphite jig, dry-pressing into
Type machine precompressed 10MPa is molded.After preforming hot-pressed sintering furnace high temperature sintering, highest sintering temperature are placed in together with one piece of graphite jig
Spend for 2050 DEG C, pressure 25MPa, soaking time is 2 hours.The diphase ceramic material zirconium boride obtained by the manufacturing process
Content is 38.8%, carborundum content 16.3%, boron nitride content 27.4%, and yttrium-aluminium-garnet content is 17.5%.Cause
Density is 97.9%, and room temperature resistivity is 1250 μ Ω cm, and processability is good.Manufactured with the diphase ceramic material true
Sky is aluminized membrane process conductive evaporation boat, and the continuous use life-span up to more than 15 hours, is significantly better than existing product.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (9)
1. a kind of manufacture method of Compound Ceramic Evaporator, it is characterised in that comprise the following steps：
(1) dispensing batch mixing：
Mixed powder：Zirconium silicate powder, boron oxide powder, boron nitride powder, nano carbon black powder, aluminum oxide, yttrium oxide powder,
It is added to according to a certain percentage in deionized water, adds polyvinyl alcohol and be well mixed as binding agent, strong stirring, obtains certain
The mixed slurry of viscosity；
(2) drying and screening
In an oven 2-4 hours are dried for 80-100 DEG C in mixed slurry, sieving obtains composite granule；
(3) it is preforming
Composite granule is placed in graphite jig, is molded in dry-pressing formed machine precompressed 5-15MPa；
(3) high temperature sintering
Graphite jig after will be preforming is placed in hot-pressed sintering furnace high temperature sintering, and maximum sintering temperature is 1900-2100 DEG C, pressure
Power is 10-30MPa, and soaking time is 1-2 hours.
2. manufacture method according to claim 1, it is characterised in that in step (1), the percentage by weight of zirconium silicate powder
Content is 35-42%, the weight percent content of boron oxide powder is 13.5-16%, the percentage by weight of boron nitride powder contains
The weight percent content measured as 11-25%, silicon carbide powder is 0-4%, the weight percent content of nano carbon black is 18.5-
22%th, the weight percent content of alumina powder is 3-5%, and the weight percent content of yttrium oxide powder is 4-8%.
3. manufacture method according to claim 1, it is characterised in that in step (1), the granularity of the zirconium silicate powder is
0.5-5.0 μm, the granularity of boron oxide powder is 0.5-10.0 μm, and the granularity of boron nitride powder is 0.5-5.0 μm, silicon carbide powder
Granularity be 0.5-3.0 μm, the granularity of nano carbon black is 0.02-0.2 μm；Aluminum oxide, the granularity of yttrium oxide powder are 0.05-
0.5μm。
4. manufacture method according to claim 1, it is characterised in that in step (1), alumina powder in the mixed powder
The weight of body and yttrium oxide powder ratio is 0.6-0.8.
5. manufacture method according to claim 1, it is characterised in that in step (3), maximum sintering temperature 1900-
2100℃。
6. manufacture method according to claim 5, it is characterised in that maximum sintering temperature is 2060 DEG C.
7. manufacture method according to claim 1, it is characterised in that in step (3), highest dwell pressure is 10-
30MPa。
8. manufacture method according to claim 7, it is characterised in that highest dwell pressure is 25MPa.
9. a kind of Compound Ceramic Evaporator manufactured according to any methods describeds of above-mentioned 1-8, it is characterised in that its composition includes boron
Change zirconium, boron nitride, carborundum and yttrium-aluminium-garnet；The content of zirconium boride is 35-45%, and the content of boron nitride is in 20-40%, carbon
The content of SiClx is 10-20%, and the content of yttrium-aluminium-garnet is in 12-20%.
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Cited By (1)
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| CN113474313A (en) * | 2018-12-27 | 2021-10-01 | 迈图高新材料石英股份有限公司 | Ceramic composite heater including boron nitride and titanium diboride |
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