CN109266943A - The preparation method of low thermal expansion composite material - Google Patents

The preparation method of low thermal expansion composite material Download PDF

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Publication number
CN109266943A
CN109266943A CN201810934001.1A CN201810934001A CN109266943A CN 109266943 A CN109266943 A CN 109266943A CN 201810934001 A CN201810934001 A CN 201810934001A CN 109266943 A CN109266943 A CN 109266943A
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preparation
condition
temperature
low thermal
thermal expansion
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赵浩峰
于鹏
夏俊
郑建华
张椿英
李子嫣
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Anhui Institute of Information Engineering
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Anhui Institute of Information Engineering
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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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention discloses a kind of preparation method of low thermal expansion composite material, the preparation method includes: that C, Sn, Eu, S, Cr, Cd and Fe are carried out mix, and melting obtains alloy liquid, obtains materials A through atomization process；By C, Fe, Eu, Cd, Si, Pb, Cu and Sn into ingredient, melting obtains alloy liquid, obtains material B through atomization process；By CdO, PbO2、K2O、Eu2O3And Al2O3Ingredient is carried out, obtains material C after processing；By PbO2、ZnO、Cr2O3、Mn2O3、CdO、Eu2O3And Fe2O3Mix is carried out, material D is obtained after processing；Materials A, material B and material C are mixed, sintering obtains ABC mixture after grinding；It by ABC mixture and material D and mixes, and is compacted form blank N, blank N is sintered respectively and handles to obtain low thermal expansion composite material with double tempering.It solves the problems, such as traditional low thermal expansion composite material there are magnetic properties and is lower.

Description

The preparation method of low thermal expansion composite material
Technical field
The present invention relates to electronic technology fields, and in particular, to a kind of preparation method of low thermal expansion composite material.
Background technique
Low thermal expansion composite material be widely used in electronic transformer, filter, the magnetic core of inductor, power adapter, The fields such as computer, audio-visual equipment and mobile communication；The Chinese patent of Patent No. CN201510839760.6 discloses one kind The preparation method of low thermal coefficient of expansion Ni-Zn soft magnetic ferrite core material, the low thermal coefficient of expansion Ni-Zn soft magnetic ferrite magnetic core Material is by Fe2O3、NiO、ZnO、Cr2O3、MoO3、Dy2O3、CdO、AlN、B4C、Bi2O3、Co2O3、MnO2、WO3、V2S3、TiC、 CaZrO3Equal raw materials composition；Material of the present invention by Primary batching system, a ball milling, once sintered, second batch, secondary ball milling, Compression moulding, double sintering and etc. be made.Ni-Zn soft magnetic ferrite core material excellent combination property produced by the present invention, no Only there is lower thermal expansion coefficient, magnetic conductivity also with higher and saturation flux density, magnetic conductivity and Curie temperature.But Its magnetic property is also relatively low.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of low thermal expansion composite material, solve traditional low thermal expansion Composite material has that magnetic property is lower.
To achieve the goals above, the present invention provides a kind of preparation method of low thermal expansion composite material, the preparations Method includes:
(1) preparation of materials A: C, Sn, Eu, S, Cr, Cd and Fe are subjected to mix, closed its melting after mixing Alloy liquid is obtained materials A through atomization process by golden liquid；
(2) preparation of material B: by C, Fe, Eu, Cd, Si, Pb, Cu and Sn into mix, its melting is obtained after mixing Alloy liquid is obtained material B through atomization process by alloy liquid；
(3) preparation of material C: by CdO, PbO2、K2O、Eu2O3And Al2O3Carry out mix, after through broken, drying With material C is obtained after sieving；
(4) preparation of material D: by PbO2、ZnO、Cr2O3、Mn2O3、CdO、Eu2O3And Fe2O3Mix is carried out, later Material D is obtained after drying, sieving and sintering；
(5) materials A, material B and material C are mixed according to 0.3-0.8:0.1-0.5:10, then in 1210-1270 It is sintered at DEG C, ABC mixture is obtained after grinding；
(6) it by ABC mixture and material D and mixes, and is compacted form blank N, blank N is sintered place respectively Reason and double tempering handle to obtain low thermal expansion composite material.
Through the above technical solutions, the present invention provides a kind of preparation methods of low thermal expansion composite material, obtained In low thermal expansion composite material, materials A is alloy material, and the gap of ferrite base-material can be filled, and close material matrix rises simultaneously The effect of toughening material；The crystal grain of C, Sn, Cr, Cd refining alloy therein itself, Eu and S can reinforced alloys soft magnetism, be The magnetic enhancement of ferrite matrix plays relay supplementary function；Materials A, material B, material C form sinter mixture, are in iron oxygen The boundary of body crystal grain not only improves the resistivity of grain boundaries, promotes lower power consumption；And enhance crystal boundary density and Soft magnetism；Material expansion is reduced simultaneously to the sensibility of heat, material B is low melting material, ferrite crystal grains can be effectively wrapped up, Play the role of liquid-phase sintering, grain growth can be effectively facilitated and inhibit the annexation of crystal grain, so that crystal grain homoepitaxial, stomata subtract Few, the porosity in crystal boundary and crystal grain reduces, and improves ferritic microstructure, and domain wall displacement and domain rotation resistance reduce, Therefore magnetic hystersis loss reduces；Low-melting alloy can play toughening ferrite base-material grain boundary simultaneously.Cd, Pb, Eu can be thin Change the crystal grain of low melting point alloy, Sb, Si, Cu, C, Fe can be improved the intensity and hardness of low-melting alloy, can effectively strengthen iron The crystal boundary of oxysome reduces the brittleness of inorganic composite material；Material D is ferrite base-material, PbO2、ZnO、Mn2O3And Fe2O3It is formed Spinel structure constitutes ferritic matrix；CdO promotes crystal growth, reduces stomata；Rare earth oxide Cr2O3、Eu2O3In material Promote crystal grain homoepitaxial in material, inhibits abnormal grain growth；Eu2O3Improve the resistivity of material, promotes lower power consumption. Low thermal expansion composite material provided by the invention has good magnetic property, while with good stability and practicability, can It is widely used in field of electronic devices etc..
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the organization chart of low thermal expansion composite material provided by the invention.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of preparation method of low thermal expansion composite material, the preparation method includes:
(1) preparation of materials A: C, Sn, Eu, S, Cr, Cd and Fe are subjected to mix, closed its melting after mixing Alloy liquid is obtained materials A through atomization process by golden liquid；
(2) preparation of material B: by C, Fe, Eu, Cd, Si, Pb, Cu and Sn into mix, its melting is obtained after mixing Alloy liquid is obtained material B through atomization process by alloy liquid；
(3) preparation of material C: by CdO, PbO2、K2O、Eu2O3And Al2O3Carry out mix, after through broken, drying With material C is obtained after sieving；
(4) preparation of material D: by PbO2、ZnO、Cr2O3、Mn2O3、CdO、Eu2O3And Fe2O3Mix is carried out, later Material D is obtained after drying, sieving and sintering；
(5) materials A, material B and material C are mixed according to 0.3-0.8:0.1-0.5:10, then in 1210-1270 It is sintered at DEG C, ABC mixture is obtained after grinding；
(6) it by ABC mixture and material D and mixes, and is compacted form blank N, blank N is sintered place respectively Reason and double tempering handle to obtain low thermal expansion composite material.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, materials A includes the material composition of following parts by weight: C 0.5-0.9%, Sn 0.5-0.9%, Eu 0.35-0.48%, S 3- 8%, Cr 21-25%, Cd 0.01-0.05% and surplus Fe.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, in step (1), the condition of melting includes: that temperature is 1480-1520 DEG C, soaking time 10-30min；And/or
The condition of atomization process includes: that atomization pressure is 6-8MPa, and the flow of alloy liquid is 3-4kg/min, is closed The injection temperature of golden liquid is 1490-1540 DEG C, and atomization angle is 35 degree.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, material B includes the material composition of following parts by weight: C 0.05-0.09%, Fe 5-9%, Eu0.65-0.95%, Cd 0.01-0.05%, Si 0.02-0.07%, Pb 9-11%, Cu 4-8% and surplus Sn.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, in step (2), the condition of melting includes: that temperature is 730-760 DEG C, soaking time 20-30min；And/or
The condition of atomization process includes: that atomization pressure is 4-5MPa, and the flow of alloy liquid is 2-3kg/min, is closed The injection temperature of golden liquid is 680-710 DEG C, and atomization angle is 31 degree.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, material C includes the material composition of following parts by weight: CdO 0.1-0.4%, PbO20.1-0.4%, K2O 8-12%, Eu2O3 0.2-0.5% and surplus Al2O3。
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, in step (3), the condition of drying includes: that temperature is 780-930 DEG C；And/or
The condition of sieving includes: that the sieve of selection is 180-220 mesh.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, material D includes the material composition of following parts by weight: PbO20.1-0.4%, ZnO 13-18%, Cr2O30.3-0.8%, Mn2O312-19%, CdO 0.1-0.4%, Eu2O30.1-0.4% and surplus Fe2O3。
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, in step (4), the condition of drying includes: that temperature is 310-350 DEG C；And/or
The condition of sieving includes: that the sieve of selection is 180-220 mesh；
The condition of sintering includes: that the temperature of sintering is 1310-1360 DEG C.
In a preferred embodiment of the invention, in order to further increase the magnetism of low thermal expansion composite material Can, in step (6), ABC mixture and material D are mixed according to the ratio that mass ratio is 1:25-30；And/or
The condition of sintering processes includes: that blank N is first warming up to 700-740 DEG C, keeps the temperature 3-4h, then heats to 1350- 1380 DEG C, keep the temperature 2-4h；And/or
The condition of double tempering processing include: respectively in 990-1110 DEG C and 840-870 DEG C of each tempering heat treatment 1-2h, it By 210-250 DEG C of ageing treatment.
The present invention will be described in detail by way of examples below.In following embodiment, high low thermal expansion composite material It is specific the preparation method is as follows:
The preparation of materials A: C, Sn, Eu, S, Cr, Cd and Fe are subjected to mix；C, Sn, Eu, Cr, Cd, Fe are pure object Matter (constituent content is greater than 99.9%)；S is added in the form of sulphur iron intermediate alloy, and the amount containing S of sulphur iron intermediate alloy is 50%, remaining For iron；In first raw material is put into induction furnace, heat up melting, keeps the temperature 20 minutes after reaching 1500 DEG C of smelting temperature；It will so close Golden liquid injection is located in the tundish on atomizer.Aluminium alloy by tundish bottom leakage eye outflow, when passing through nozzle with High-speed flow, which meets, to be atomized as fine drop, and atomized drop is rapidly solidificated into alloy powder in closed atomizing cup.Alloy Powder mean particle sizes are 11 μm；Atomization pressure is 7MPa, and liquid metal fluid flow is 3.5kg/min, alloy liquid Injecting temperature is 1515 DEG C, and atomizing angle is 35 degree；
The preparation of material B: C, Fe, Eu, Cd, Si, Pb, Cu and Sn are subjected to mix；Each material purity is all larger than 99.9%, first raw material is put into induction furnace in, heat up melting, keeps the temperature 25 minutes after reaching 745 DEG C of smelting temperature；Then will Alloy liquid injection is located in the tundish on atomizer, and aluminium alloy is flowed out by tundish bottom leakage eye, when passing through nozzle It meets and is atomized as fine drop with high-speed flow, atomized drop is rapidly solidificated into alloy powder in closed atomizing cup, closes Golden powder mean particle sizes are 13 μm, atomization pressure 4.5MPa, and state metal fluid flow is 2.5kg/min, aluminium alloy It is 695 DEG C that body, which injects temperature, and atomizing angle is 31 degree；
The preparation of material C: by CdO, PbO2、K2O、Eu2O3And Al2O3；Each material purity is all larger than 99.9%；By each raw material Mixing and breaking up is carried out in sand mill, is then dried powder at 855 DEG C, re-sieving after drying, and sieve is 200 mesh；
The preparation of material D: by PbO2、ZnO、Cr2O3、Mn2O3、CdO、Eu2O3And Fe2O3Mix is carried out, each raw material is pure Degree is all larger than 99.9%；Each raw material is subjected to mixing and breaking up in sand mill, then dries powder at 330 DEG C, is dried Re-sieving afterwards, sieve are 200 mesh, are then placed in sintering furnace and are sintered；Sintering temperature is 1335 DEG C, and finally sintered product exists Diameter of particle is set to reach 12 microns in grinder；
Materials A, material B and material C are mixed, sintering furnace is then placed in and is sintered, sintering temperature is 1240 DEG C, Sinter mixture ABC is finally obtained, so that diameter of particle is reached 12 microns in grinder sintered product；
Sinter mixture ABC and material D are mixed, is added in three-dimensional mixer and is uniformly mixed, obtain mixed powder； Then mixed powder is orientated in Magnetic field press, using etc. static pressure mode form, molded blank is put under protection of argon gas Sintering furnace is sintered, and is first warming up to 720 DEG C, is kept the temperature 3.5h, is then heated to 1365 DEG C of sintering 3h, after being cooled to room temperature, into The processing of row double tempering, i.e., respectively in 1050 DEG C and 855 DEG C of tempering heat treatment 1.5h, most produced through 230 DEG C of ageing treatments afterwards Product.
Embodiment 1
It is carried out according to above-mentioned preparation method, wherein materials A includes the material composition of following parts by weight: C 0.5%, Sn 0.5%, Eu 0.35%, S 3%, Cr 21%, Cd 0.01% and surplus Fe；Material B include following parts by weight raw material at Point: C 0.05%, Fe 5%, Eu 0.65%, Cd 0.01%, Si 0.02%, Pb 9%, Cu 4% and surplus Sn；Material C Material composition including following parts by weight: CdO 0.1%, PbO20.1%, K2O 8%, Eu2O30.2% and surplus Al2O3；Material Material D includes the material composition of following parts by weight: PbO20.1%, ZnO 13%, Cr2O30.3%, Mn2O312%, CdO 0.1%, Eu2O30.1% and surplus Fe2O3；The weight ratio of materials A, material B and material C is 0.3:0.1:10；Materials A, material B Weight ratio with the mixture and material D that are formed after material C mixing is 1:25.
Embodiment 2
It is carried out according to above-mentioned preparation method, wherein materials A includes the material composition of following parts by weight: C 0.7%, Sn 0.7%, Eu 0.4%, S 5%, Cr 23%, Cd 0.03% and surplus Fe；Material B includes the material composition of following parts by weight: C 0.07%, Fe 7%, Eu 0.8%, Cd 0.03%, Si 0.05%, Pb 10%, Cu 6% and surplus Sn；Material C includes The material composition of following parts by weight: CdO 0.3%, PbO20.3%, K2O 10%, Eu2O30.4% and surplus Al2O3；Material D Material composition including following parts by weight: PbO20.3%, ZnO 15%, Cr2O30.6%, Mn2O316%, CdO 0.2%, Eu2O30.3% and surplus Fe2O3；The weight ratio of materials A, material B and material C is 0.5:0.3:10；Materials A, material B and material The weight ratio of the mixture and material D that are formed after C mixing is 1:28.
Embodiment 3
It is carried out according to above-mentioned preparation method, wherein materials A includes the material composition of following parts by weight: C 0.9%, Sn 0.9%, Eu 0.48%, S 8%, Cr 25%, Cd 0.05% and surplus Fe；Material B include following parts by weight raw material at Point: C 0.09%, Fe 9%, Eu 0.95%, Cd 0.05%, Si 0.07%, Pb 11%, Cu 8% and surplus Sn；Material C Material composition including following parts by weight: CdO 0.4%, PbO20.4%, K2O 12%, Eu2O30.5% and surplus Al2O3； Material D includes the material composition of following parts by weight: PbO20.4%, ZnO 18%, Cr2O30.8%, Mn2O319%, CdO 0.4%, Eu2O30.4% and surplus Fe2O3；The weight ratio of materials A, material B and material C is 0.8:0.5:10；Materials A, material B Weight ratio with the mixture and material D that are formed after material C mixing is 1:30.
Embodiment 4
It is carried out according to above-mentioned preparation method, wherein materials A includes the material composition of following parts by weight: C 0.4%, Sn 0.3%, Eu 0.3%, S 2%, Cr 19%, Cd 0.005% and surplus Fe；Material B include following parts by weight raw material at Point: C 0.03%, Fe 4%, Eu 0.5%, Cd 0.005%, Si 0.01%, Pb 8%, Cu 3% and surplus Sn；Material C Material composition including following parts by weight: CdO 0.08%, PbO20.07%, K2O 7%, Eu2O30.1% and surplus Al2O3； Material D includes the material composition of following parts by weight: PbO20.09%, ZnO 11%, Cr2O30.2%, Mn2O311%, CdO 0.06%, Eu2O30.08% and surplus Fe2O3；The weight ratio of materials A, material B and material C is 0.2:0.05:10；Materials A, The weight ratio of mixture and material D that material B and material C are formed after mixing is 1:31.
Embodiment 5
It is carried out according to above-mentioned preparation method, wherein materials A includes the material composition of following parts by weight: C 1.1%, Sn 1.1%, Eu 0.6%, S 9%, Cr 26%, Cd 0.06% and surplus Fe；Material B includes the material composition of following parts by weight: C 0.12%, Fe 11%, Eu 1%, Cd 0.07%, Si 0.08%, Pb 12%, Cu 9% and surplus Sn；Material C includes The material composition of following parts by weight: CdO 0.5%, PbO20.5%, K2O 13%, Eu2O30.6% and surplus Al2O3；Material D Material composition including following parts by weight: PbO20.5%, ZnO 19%, Cr2O30.9%, Mn2O321%, CdO 0.6%, Eu2O30.6% and surplus Fe2O3；The weight ratio of materials A, material B and material C is 0.9:0.6:10；Materials A, material B and material The weight ratio of the mixture and material D that are formed after C mixing is 1:24.
Comparative example 1
The property of low thermal coefficient of expansion Ni-Zn soft magnetic ferrite core material disclosed in Patent No. CN201510839760.6 It can parameter.
Table 1
Fig. 1 is the organization chart of low thermal expansion composite material provided by the invention, and even tissue is fine and close.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (10)

1. a kind of preparation method of low thermal expansion composite material, which is characterized in that the preparation method includes:
(1) preparation of materials A: C, Sn, Eu, S, Cr, Cd and Fe are subjected to mix, its melting is obtained into aluminium alloy after mixing Alloy liquid is obtained materials A through atomization process by body；
(2) by C, Fe, Eu, Cd, Si, Pb, Cu and Sn into mix, its melting the preparation of material B: is obtained into alloy after mixing Alloy liquid is obtained material B through atomization process by liquid；
(3) preparation of material C: by CdO, PbO2、K2O、Eu2O3And Al2O3Carry out mix, after through broken, drying and mistake Material C is obtained after sieve；
(4) preparation of material D: by PbO2、ZnO、Cr2O3、Mn2O3、CdO、Eu2O3And Fe2O3Carry out mix, after through drying Material D is obtained after dry, sieving and sintering；
(5) materials A, material B and material C are mixed according to 0.3-0.8:0.1-0.5:10, then at 1210-1270 DEG C Sintering, obtains ABC mixture after grinding；
(6) by ABC mixture and material D and mix, and be compacted form blank N, blank N is sintered respectively and Double tempering handles to obtain low thermal expansion composite material.
2. preparation method according to claim 1, wherein materials A includes the material composition of following parts by weight: C 0.5- 0.9%, Sn 0.5-0.9%, Eu 0.35-0.48%, S 3-8%, Cr 21-25%, Cd 0.01-0.05% and surplus Fe.
3. preparation method according to claim 1, wherein in step (1), the condition of melting includes: that temperature is 1480- 1520 DEG C, soaking time 10-30min；And/or
The condition of atomization process includes: that atomization pressure is 6-8MPa, and the flow of alloy liquid is 3-4kg/min, aluminium alloy The injection temperature of body is 1490-1540 DEG C, and atomization angle is 35 degree.
4. preparation method according to claim 1, wherein material B includes the material composition of following parts by weight: C 0.05- 0.09%, Fe 5-9%, Eu 0.65-0.95%, Cd 0.01-0.05%, Si 0.02-0.07%, Pb 9-11%, Cu 4- 8% and surplus Sn.
5. preparation method according to claim 1, wherein in step (2), the condition of melting includes: that temperature is 730- 760 DEG C, soaking time 20-30min；And/or
The condition of atomization process includes: that atomization pressure is 4-5MPa, and the flow of alloy liquid is 2-3kg/min, aluminium alloy The injection temperature of body is 680-710 DEG C, and atomization angle is 31 degree.
6. preparation method according to claim 1, wherein material C includes the material composition of following parts by weight: CdO 0.1- 0.4%, PbO20.1-0.4%, K2O 8-12%, Eu2O30.2-0.5% and surplus Al2O3。
7. preparation method according to claim 1, wherein in step (3), the condition of drying includes: that temperature is 780- 930℃；And/or
The condition of sieving includes: that the sieve of selection is 180-220 mesh.
8. preparation method according to claim 1, wherein material D includes the material composition of following parts by weight: PbO2 0.1- 0.4%, ZnO 13-18%, Cr2O30.3-0.8%, Mn2O312-19%, CdO 0.1-0.4%, Eu2O30.1-0.4% and Surplus Fe2O3。
9. preparation method according to claim 1, wherein in step (4), the condition of drying includes: that temperature is 310- 350℃；And/or
The condition of sieving includes: that the sieve of selection is 180-220 mesh；
The condition of sintering includes: that the temperature of sintering is 1310-1360 DEG C.
10. preparation method according to claim 1, wherein in step (6), ABC mixture and material D are according to quality Than being mixed for the ratio of 1:25-30；And/or
The condition of sintering processes includes: that blank N is first warming up to 700-740 DEG C, keeps the temperature 3-4h, then heats to 1350-1380 DEG C, keep the temperature 2-4h；And/or
The condition of double tempering processing include: respectively in 990-1110 DEG C and 840-870 DEG C of each tempering heat treatment 1-2h, after pass through 210-250 DEG C of ageing treatment.
CN201810934001.1A 2018-08-16 2018-08-16 The preparation method of low thermal expansion composite material Pending CN109266943A (en)

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