CN107841671A - A kind of preparation method of beryllium oxide based ceramic metal - Google Patents
A kind of preparation method of beryllium oxide based ceramic metal Download PDFInfo
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- CN107841671A CN107841671A CN201711269067.5A CN201711269067A CN107841671A CN 107841671 A CN107841671 A CN 107841671A CN 201711269067 A CN201711269067 A CN 201711269067A CN 107841671 A CN107841671 A CN 107841671A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention discloses a kind of preparation method of beryllium oxide based ceramic metal, comprise the following steps：Step 1, nickel metal powder and beryllium oxide based ceramic powder end be mixed to get primary batch mixing；Step 2, it is pressed, obtains pressed compact part；Step 3, drying insulation；Step 4, vacuum-sintering is carried out, obtain semi-finished product；Step 5, obtained semi-finished product are polished, finishing and are produced after drying.The preparation method of beryllium oxide base metal-ceramic material provided by the invention, mainly solve the problems, such as that conventional cermets heat exchanger tube service life is short, heat exchange efficiency is low, the thermal conductivity factor of obtained beryllium oxide base metal-ceramic material is set to reach 270.3 W/mK, elongation reaches 3.0%, and then the thermal conductivity factor of heat exchanger tube and elongation is effectively improved, solve the problems of current traditional heat exchanger tube.
Description
Technical field
The present invention relates to high temperature preheating stove manufacturing technology field, more particularly to a kind of oxygen for being used to manufacture preheating furnace heat exchanger tube
Change the preparation method of beryllium base metal-ceramic material.
Background technology
The preparation method of Nano titanium dioxide mainly includes Physical and chemical method, Physical mainly include sputtering method,
Thermal evaporation and laser evaporization method, chemical method mainly include liquid phase method and vapor phase method, liquid phase method mainly include sluggish precipitation and
Sol-gel process, vapor phase method mainly include TiCl4Vapour phase oxidation process, typically use TiCl at present4Vapour phase oxidation process is received to prepare
Rice titanium dioxide.TiCl4Vapour phase oxidation process is usually with nitrogen as TiCl4Carrier gas, using oxygen as oxidant, in high temperature
Oxidation reaction is carried out in tubular reactor, through gas solid separation, obtains nanometer level titanium dioxide powder.In actual production, oxygen
Needing to be pre-heated to more than 800 DEG C could be with the TiCl of gas phase4Hybrid reaction, then need to use gas phase preheating furnace, and it is traditional
Gas phase preheating furnace many defects be present, for example, the heat exchanger tube used in preheating furnace is using resistant to elevated temperatures aluminum oxide or oxidation
Silicon based metal ceramic material, and aluminum oxide or silica base metal-ceramic material thermal conductivity factor are relatively low, it is necessary in the timing of heating one
Between after could be exchanged heat, its heat exchange efficiency is poor, and rapidly heat up under be also easy to produce hot tearing, thus cause traditional heat exchanger tube
Service life it is shorter, it is necessary to change often.
The content of the invention
The goal of the invention of the present invention is：For above-mentioned problem, there is provided one kind is used to manufacture preheating furnace heat exchanger tube
Beryllium oxide base metal-ceramic material preparation method, mainly solve conventional cermets heat exchanger tube service life it is short, heat exchange effect
The problem of rate is low, by compounding a kind of beryllium oxide base metal-ceramic material with thermal conductive resin and elongation, improves and prepare
Technique, the thermal conductivity factor and elongation for making obtained beryllium oxide based ceramic metal heat exchanger tube effectively improve, and then solve to pass
The problems of system heat exchanger tube.
The technical solution adopted by the present invention is as follows：A kind of preparation method of beryllium oxide based ceramic metal, it is characterised in that bag
Include following steps：
Step 1, the nickel metal powder for taking design flow and beryllium oxide based ceramic powder end are placed in high speed ball mill and carry out mixed grinding
2-4h, high speed ball mill rotating speed are 400rad/min, are subsequently placed in high-speed mixer and are well mixed, obtain primary batch mixing；
Step 2, design compacting tool set, the inner chamber of compacting tool set is lubricated with zinc stearate alcoholic solution, then pours into compound
In designed mould, mould is put into powder compressing machine and is pressed, obtain pressed compact part；
Step 3, by obtained pressed compact part be placed in drying oven carry out 80 DEG C insulation drying 3-4h；
Step 4, the pressed compact part after drying is put into vacuum sintering furnace carries out vacuum-sintering, vacuum sintering furnace is first warming up to 300
DEG C, 2h is sintered, then heats to 900 DEG C, is incubated 1h, then 1220 DEG C are warming up to, 1h is incubated, is then cooled to 450 DEG C again, insulation
1h, finally cool to room temperature with the furnace, obtain semi-finished product；
Step 5, obtained semi-finished product are polished and finishing, be cleaned by ultrasonic in deionized water, produced after drying.
Beryllium oxide base metal-ceramic material is manufactured by powder metallurgic method, the machine for meeting design requirement can be obtained
Tool intensity and physicochemical property, industrial production can be applied to, moreover, by overcoming conventional oxidation beryllium to the accurate control of parameter
The defects of thermal conductivity factor present in based ceramic metal is poor, heat endurance difference, thus solves existing deficiency.
Further, in step 2, pressing pressure 220-240MPa, pressing speed 1.5mm/min, dwell time be
10min.Pressing pressure need to select appropriately, if pressure is too small, the density of pressed compact part is relatively low so that ferromagnetic material in pressed compact part
（Such as cobalt）Magnetic induction line weaken, can not be combined well between metallic particles and ceramic particle so that the hole of final cermet
Porosity is larger, and intensity is poor, and thermal conductivity is poor, and in the present invention, pressing pressure is in 220-240MPa, and pressing speed is in 1.5mm/
It is more suitable during min.
Further, in step 4, when being first warming up to 300 DEG C, initial heating rate is 130 DEG C/h, then heats to 900
DEG C when, heating rate is 1200 DEG C/h, then when being warming up to 1220 DEG C, heating rate is 1000 DEG C/h.Heating rate needs strict
Control, heating rate is too high, then can cause in pressed compact part it is gas generated increased dramatically, pressed compact part internal/external heating is uneven, interior
Thermal expansion deformation difference increase, causes pressed compact part to produce larger internal stress in the process and constantly saves bit by bit, burnt in the later stage
During system, this internal stress can largely discharge and sintering crack occurs, have a strong impact on sintering quality, and heating rate is too small
Manufacturing cycle can then be extended, increase production cost, be unfavorable for inexpensive production, therefore, must be strict in sintering procedure
Operated according to above-mentioned parameter.
In the preparation method of the beryllium oxide base metal-ceramic material of the present invention, the preparation method at beryllium oxide based ceramic powder end
Comprise the following steps：
Step 4-1, blank is prepared using existing process, then in the uniform application of glaze in the surface of blank, then will at 1250 DEG C
It is fired into fired body；
Step 4-2, powder of the precast body formed with zinc oxide together attrition grinding into average grain diameter less than 50 μm will be fired, i.e.,
Ceramic powders are obtained, wherein, 2.5 % of low quality in fired body mass fraction of the zinc oxide of addition.
The present invention beryllium oxide base metal-ceramic material preparation method in, in the raw material of beryllium oxide based blank contain with
The component of lower mass percentage content：The Ti content that is carbonized is 4-7%, the oxide content of alkali metal is 4-7%, the oxide of zirconium contains
The oxide content measured as 1.5-2.0%, vanadium is 0.2-0.3%, the oxide content of gallium is 0.05-0.1% and the oxygen of rare earth element
Compound content is not more than 1.0%；Contain the component of following mass percentage content in the raw material of glaze：The oxide content of iron is
1-3%, the oxide content of cobalt are 2-4%, the oxide content of alkali metal is 2-6%, the oxide content of copper be 1.0-1.3%,
The oxide content of gallium be 0.05-0.1%, indium oxide content no more than 0.05% and rare earth element oxide content it is little
In 1.0%.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：A kind of use provided by the invention
In the preparation method of the beryllium oxide base metal-ceramic material of manufacture preheating furnace heat exchanger tube, mainly solves conventional cermets heat exchanger tube
The problem of service life is short, heat exchange efficiency is low, by compounding a kind of beryllium oxide Base Metal with thermal conductive resin and elongation
Ceramic material, preparation technology is improved, the thermal conductivity factor of obtained beryllium oxide base metal-ceramic material is reached 270.3 W/mK,
Elongation reaches 3.0%, and then the thermal conductivity factor of heat exchanger tube and elongation is effectively improved, and solves tradition heat exchange at present
The problems of pipe.
Embodiment
With reference to embodiment, the present invention is described in detail.
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
A kind of beryllium oxide base metal-ceramic material, it is mainly by beryllium oxide based ceramic powder end and nickel metal powder according to quality
Than for（75-78）：（22-25）It is combined, wherein, beryllium oxide based ceramic powder end includes blank and glaze, the blank and glaze
The mass ratio of material is（95-97）：（3-5）.
In above-mentioned, the metal ingredient accounting in beryllium oxide base metal-ceramic material reaches 22-25%, and this causes cermet
The property of more metals is provided with, cermet is provided with good thermal conductivity and elongation, thermal conductivity and elongation
Improve and the pyroconductivity of its manufactured heat exchanger tube is effectively improved, when expanding with heat and contract with cold, due to containing higher metal
Composition, the change amplitude of its elongation is wider, and cermet can preferably buffer and discharge this stress deformation, make its surface
Crackle is not likely to produce, thus extends the service life of cermet heat exchanger tube.
Further, in order that the beryllium oxide base metal-ceramic material of the present invention preferably has above-mentioned performance, the base
Contain the component of following mass percentage content in the raw material of material：Carbonization Ti content is 4-7%, the oxide content of alkali metal is
4-7%, the oxide content of zirconium are 1.5-2.0%, the oxide content of vanadium is 0.2-0.3%, the oxide content of gallium is 0.05-
0.1% and rare earth element oxide content be not more than 1.0%.
Further, in order that the beryllium oxide base metal-ceramic material of the present invention preferably has above-mentioned performance, the glaze
Contain the component of following mass percentage content in the raw material of material：The oxide content of iron is 1-3%, the oxide content of cobalt is
2-4%, the oxide content of alkali metal is 2-6%, the oxide content of copper is 1.0-1.3%, the oxide content of gallium is 0.05-
0.1%th, the oxide content of indium no more than 0.05% and rare earth element oxide content be not more than 1.0%.
Further, the rare earth element is selected from the one or more of lanthanum, neodymium, yttrium, samarium, scandium and cerium；The alkali metal
One or more of the oxide in potassium oxide, sodium oxide molybdena and lithia.
Further, in the present invention, the preparation method at beryllium oxide based ceramic powder end comprises the following steps：
Step 1, blank is prepared using existing process, then in the uniform application of glaze in the surface of blank, then will be burnt at 1250 DEG C
Fired body is made；
Step 2, powder of the precast body formed with zinc oxide together attrition grinding into average grain diameter less than 50 μm will be fired, produced
To ceramic powders, wherein, 2.5 % of low quality in fired body mass fraction of the zinc oxide of addition.
Present invention additionally comprises a kind of preparation method of beryllium oxide base metal-ceramic material, comprise the following steps：
Step 1, the beryllium oxide based metal powder for taking design flow and ceramic powders, which are placed in high speed ball mill, carries out mixed grinding 2-
4h, high speed ball mill rotating speed are 400rad/min, are subsequently placed in high-speed mixer and are well mixed, obtain primary batch mixing；
Step 2, design compacting tool set, the inner chamber of compacting tool set is lubricated with zinc stearate alcoholic solution, then pours into compound
In designed mould, upper trimming die is installed, makes the upper surface keep level of punch die, after installation, mould is put into powder
It is pressed in tablet press machine, pressing pressure 220-240MPa, pressing speed 1.5mm/min, dwell time 10min,
Obtain pressed compact part；
Step 3, by obtained pressed compact part be placed in drying oven carry out 80 DEG C insulation drying 3-4h；
Step 4, the pressed compact part after drying is put into vacuum sintering furnace carries out vacuum-sintering, vacuum sintering furnace is first warming up to 300
DEG C, initial heating rate is 130 DEG C/h, sinters 2h, then heats to 900 DEG C, and heating rate is 1200 DEG C/h, is incubated 1h, then
1220 DEG C are warming up to, heating rate is 1000 DEG C/h, is incubated 1h, is then cooled to 450 DEG C again, is incubated 1h, last furnace cooling
To room temperature, semi-finished product are obtained；
Step 5, obtained semi-finished product are polished and finishing, be cleaned by ultrasonic in deionized water, produced after drying.
In above-mentioned preparation method, can the cermet finished product that sinter out reach design requirement, and step 4 is closed the most
Key, in step 4, each parameter value are not random setting, but test what is obtained by numerous experiments, such as：It is initial to rise
300 DEG C of temperature, heating rate is 130 DEG C/h, sinters 2h, and this three kinds of parameters are required to simultaneously meet, in the process, if rising
Warm speed is higher than 130 DEG C/h（Such as reach 135 DEG C）, reaching 135 DEG C/h in heating rate makes, then can cause the gas in pressed compact part
Body yield increased dramatically, and pressed compact part internal/external heating is uneven, inside and outside thermal expansion deformation difference increase, cause pressed compact part in this process
It is middle to produce larger internal stress and simultaneously constantly save bit by bit, in more than 1000 DEG C of sintering process of later stage, the internal stress meeting saved bit by bit before
Discharge suddenly and cause occur sintering crack inside and outside pressed compact part, thus produce the phenomenon of " collapsing flower ", cause sintering to fail.Therefore,
Want to obtain the beryllium oxide base metal-ceramic material for meeting design requirement, then have to the parameters of strict implement step 4.
In order to which the beryllium oxide base metal-ceramic material that the present invention is better described has good thermal conductivity and elongation etc.
Performance, table 1 give the formula of section Example.（% represents mass percent）
The embodiment 1-4 of table 1 formula
Performance test
Determination of conductive coefficients：According to ASTM E1461 flicker method Determination of conductive coefficients；
Test of elongation rate：Tested with universal testing machine according to ASTM E8/E8M.
Test result is as shown in table 2：
It can be obtained by Tables 1 and 2, when gallium oxide containing more amount in beryllium oxide based ceramic metal heat exchanger tube, metal pottery
The thermal conductivity factor and elongation of porcelain heat exchanger tube effectively improve, and reason may is that, can be in gold in the gallium oxide of Dispersed precipitate
Build the netted conductive structure of three-dimensional in category ceramics jointly with other materials, thus make obtained beryllium oxide based ceramic metal
Thermal conductivity factor and elongation significantly improve, and thermal conductivity factor reaches 213.3 W/mK, and elongation reaches 4.0%, therefore, the present invention
Preparation method can make beryllium oxide base metal-ceramic material that there is excellent thermal conductivity factor and elongation, solve conventional oxidation
The problem of beryllium based ceramic metal heat exchanger tube service life is short, heat exchange efficiency is low, the pre- thermal efficiency of preheating furnace is improved indirectly.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (5)
1. a kind of preparation method of beryllium oxide based ceramic metal, it is characterised in that comprise the following steps：
Step 1, the nickel metal powder for taking design flow and beryllium oxide based ceramic powder end are placed in high speed ball mill and carry out mixed grinding
2-4h, high speed ball mill rotating speed are 400rad/min, are subsequently placed in high-speed mixer and are well mixed, obtain primary batch mixing；
Step 2, design compacting tool set, the inner chamber of compacting tool set is lubricated with zinc stearate alcoholic solution, then pours into compound
In designed mould, upper trimming die is installed, makes the upper surface keep level of punch die, after installation, mould is put into powder
It is pressed in tablet press machine, obtains pressed compact part；
Step 3, by obtained pressed compact part be placed in drying oven carry out 80 DEG C insulation drying 3-4h；
Step 4, the pressed compact part after drying is put into vacuum sintering furnace carries out vacuum-sintering, vacuum sintering furnace is first warming up to 300
DEG C, 2h is sintered, then heats to 900 DEG C, is incubated 1h, then 1220 DEG C are warming up to, 1h is incubated, is then cooled to 450 DEG C again, insulation
1h, finally cool to room temperature with the furnace, obtain semi-finished product；
Step 5, obtained semi-finished product are polished and finishing, be cleaned by ultrasonic in deionized water, produced after drying.
2. the preparation method of beryllium oxide based ceramic metal as claimed in claim 1, it is characterised in that in step 2, compacting pressure
Power is 220-240MPa, pressing speed 1.5mm/min, dwell time 10min.
3. the preparation method of beryllium oxide based ceramic metal as claimed in claim 1, it is characterised in that in step 4, first heat up
During to 300 DEG C, initial heating rate is 130 DEG C/h, and when then heating to 900 DEG C, heating rate is 1200 DEG C/h, then is warming up to
At 1220 DEG C, heating rate is 1000 DEG C/h.
4. the preparation method of beryllium oxide based ceramic metal as claimed in claim 1, it is characterised in that beryllium oxide based ceramic powder end
Preparation method comprise the following steps：
Step 4-1, blank is prepared using existing process, then in the uniform application of glaze in the surface of blank, then will at 1250 DEG C
It is fired into fired body；
Step 4-2, powder of the precast body formed with zinc oxide together attrition grinding into average grain diameter less than 50 μm will be fired, i.e.,
Ceramic powders are obtained, wherein, 2.5 % of low quality in fired body mass fraction of the zinc oxide of addition.
5. the preparation method of beryllium oxide based ceramic metal as claimed in claim 4, it is characterised in that the original of beryllium oxide based blank
Contain the component of following mass percentage content in material：The Ti content that is carbonized is 4-7%, the oxide content of alkali metal is 4-7%, zirconium
Oxide content be 1.5-2.0%, the oxide content of vanadium is 0.2-0.3%, the oxide content of gallium is 0.05-0.1% and dilute
The oxide content of earth elements is not more than 1.0%；Contain the component of following mass percentage content in the raw material of glaze：The oxygen of iron
Compound content is 1-3%, the oxide content of cobalt is 2-4%, and the oxide content of alkali metal is 2-6%, the oxide content of copper is
1.0-1.3%, gallium oxide content for 0.05-0.1%, indium oxide content no more than 0.05% and rare earth element oxidation
Thing content is not more than 1.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116514575A (en) * | 2023-05-05 | 2023-08-01 | 郑州大学 | Beryllium oxide electrode material, beryllium-beryllium oxide cermet and preparation method thereof |
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| CN87101815A (en) * | 1986-03-12 | 1987-09-23 | 奥林公司 | With glass is the sintering metal substrate of adhesion component |
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| CN106017196A (en) * | 2016-06-02 | 2016-10-12 | 成都爻能节能科技有限公司 | Heat exchange device and energy-saving net used in heat exchange device |
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| CN116514575A (en) * | 2023-05-05 | 2023-08-01 | 郑州大学 | Beryllium oxide electrode material, beryllium-beryllium oxide cermet and preparation method thereof |
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