CN107739953A - A kind of beryllium oxide base metal-ceramic material and preparation method thereof - Google Patents
A kind of beryllium oxide base metal-ceramic material and preparation method thereof Download PDFInfo
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- CN107739953A CN107739953A CN201711267301.0A CN201711267301A CN107739953A CN 107739953 A CN107739953 A CN 107739953A CN 201711267301 A CN201711267301 A CN 201711267301A CN 107739953 A CN107739953 A CN 107739953A
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- oxide
- beryllium oxide
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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
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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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
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of beryllium oxide base metal-ceramic material, and it is mainly according to mass ratio with nickel metal powder by beryllium oxide based ceramic powder end（75‑78）：（22‑25）It is combined, wherein, beryllium oxide based ceramic powder end includes blank and glaze, and the mass ratio of the blank and glaze is（95‑97）：（3‑5）.It is provided by the invention a kind of for manufacturing beryllium oxide base metal-ceramic material of preheating furnace heat exchanger tube and preparation method thereof, mainly solve the problems, such as that conventional cermets heat exchanger tube service life is short, heat exchange efficiency is low, by compounding a kind of beryllium oxide base metal-ceramic material with thermal conductive resin and elongation, the thermal conductivity factor of 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 beryllium base metal-ceramic material and preparation method thereof.
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 and preparation method thereof, mainly solve that conventional cermets heat exchanger tube service life is short, heat exchange
The problem of efficiency is low, by compounding a kind of beryllium oxide base metal-ceramic material with thermal conductive resin and elongation, make heat exchange
The thermal conductivity factor and elongation of pipe effectively improve, and then solve the problems of traditional heat exchanger tube.
The technical solution adopted by the present invention is as follows：A kind of beryllium oxide base metal-ceramic material, it is characterised in that it mainly by
Beryllium oxide based ceramic powder end is according to mass ratio with nickel metal powder（75-78）：（22-25）It is combined, wherein, beryllium oxide base
Ceramic powders include blank and glaze, and the mass ratio of the blank and glaze is（95-97）：（3-5）.
Further, the component of following mass percentage content is contained in the raw material of the blank：Carbonization Ti content be 4-7%,
The oxide content of alkali metal is 4-7%, the oxide content of zirconium is 1.5-2.0%, the oxide content of vanadium is 0.2-0.3%, gallium
Oxide content be not more than 1.0% for the oxide content of 0.05-0.1% and rare earth element.
Further, the component of following mass percentage content is contained in the raw material of the 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%.
Further, the rare earth element is selected from the one or more of lanthanum, neodymium, yttrium, samarium, scandium and cerium；The oxygen of the alkali metal
One or more of the compound in potassium oxide, sodium oxide molybdena and lithia.
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 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, 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 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 beryllium oxide base metal-ceramic material of manufacture preheating furnace heat exchanger tube and preparation method thereof, mainly solves conventional cermets heat exchange
The problem of pipe service life is short, heat exchange efficiency is low, by compounding a kind of beryllium oxide fund with thermal conductive resin and elongation
Belong to ceramic material, the thermal conductivity factor of beryllium oxide base metal-ceramic material is reached 270.3 W/mK, elongation reaches 3.0%, enters
And the thermal conductivity factor of heat exchanger tube and elongation is effectively improved, solve the problems of current traditional heat exchanger tube.
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 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, 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
Heating rate 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 in pressed compact part
Gas generated to increased dramatically, pressed compact part internal/external heating is uneven, inside and outside thermal expansion deformation difference increase, causes pressed compact part mistake herein
Larger internal stress is produced in journey and is constantly saved bit by bit, in more than 1000 DEG C of sintering process of later stage, the internal stress saved bit by bit before
It can suddenly discharge and cause to occur inside and outside pressed compact part sintering crack, thus produce the phenomenon of " collapsing flower ", cause sintering to fail.Cause
This, it is desirable to the beryllium oxide base metal-ceramic material for meeting design requirement is obtained, then has to every ginseng of strict implement step 4
Number.
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 thermal conductivity factor and the elongation of cermet
Rate significantly improves, and thermal conductivity factor reaches 213.3 W/mK, and elongation reaches 4.0%, therefore, beryllium oxide Base Metal of the invention
Ceramic material has excellent thermal conductivity factor and elongation, solves conventional oxidation beryllium based ceramic metal heat exchanger tube service life
Short, the problem of 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 (6)
1. a kind of beryllium oxide base metal-ceramic material, it is characterised in that it is mainly by beryllium oxide based ceramic powder end and nickel metal powder
End is according to mass ratio（75-78）：（22-25）It is combined, wherein, beryllium oxide based ceramic powder end includes blank and glaze, institute
The mass ratio for stating blank and glaze is（95-97）：（3-5）.
2. beryllium oxide base metal-ceramic material as claimed in claim 1, it is characterised in that in the raw material of the 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%.
3. beryllium oxide base metal-ceramic material as claimed in claim 1, it is characterised in that in the raw material of the glaze contain with
The component of lower mass percentage content：The oxide content of iron is 1-3%, the oxide content of cobalt is 2-4%, the oxidation of alkali metal
Thing content is 2-6%, the oxide content of copper is 1.0-1.3%, the oxide content of gallium is 0.05-0.1%, the oxide of indium contains
The oxide content for being not more than 0.05% and rare earth element is measured no more than 1.0%.
4. beryllium oxide base metal-ceramic material as claimed in claim 2 or claim 3, it is characterised in that the rare earth element be selected from lanthanum,
Neodymium, yttrium, samarium, the one or more of scandium and cerium；The oxide of the alkali metal in potassium oxide, sodium oxide molybdena and lithia one
Kind is several.
5. beryllium oxide base metal-ceramic material as claimed in claim 1, it is characterised in that the preparation at beryllium oxide based ceramic powder end
Method 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.
6. beryllium oxide base metal-ceramic material as claimed in claim 1, it is characterised in that beryllium oxide base metal-ceramic material
Preparation method comprises 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, 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.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358611A (en) * | 2018-03-06 | 2018-08-03 | 济南大学 | Preparation of BeO composite ceramic powder for three-dimensional printing forming process |
| 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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| CN87102385A (en) * | 1986-03-31 | 1987-10-14 | 陶氏化学公司 | The composition of new pottery, sintering metal or metal-powder and production method thereof |
| CN1088556A (en) * | 1992-12-12 | 1994-06-29 | 天津市硅酸盐研究所 | The preparation technology and the goods of far infrared electrothermal dark-red pottery powder raw material |
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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 |
| CN87102385A (en) * | 1986-03-31 | 1987-10-14 | 陶氏化学公司 | The composition of new pottery, sintering metal or metal-powder and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358611A (en) * | 2018-03-06 | 2018-08-03 | 济南大学 | Preparation of BeO composite ceramic powder for three-dimensional printing forming process |
| 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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