CN104294133A - ZrO2 ceramic particle reinforced molybdenum-based composite material and preparation method thereof - Google Patents

ZrO2 ceramic particle reinforced molybdenum-based composite material and preparation method thereof Download PDF

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CN104294133A
CN104294133A CN201410027279.2A CN201410027279A CN104294133A CN 104294133 A CN104294133 A CN 104294133A CN 201410027279 A CN201410027279 A CN 201410027279A CN 104294133 A CN104294133 A CN 104294133A
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composite material
molybdenum
ceramic particle
base composite
preparation
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CN104294133B (en
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张国赏
魏世忠
崔超鹏
郭松亮
徐流杰
李继文
刘伟
徐锐
周玉成
朱向炜
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Henan University of Science and Technology
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Abstract

The invention discloses ZrO2 ceramic particle reinforced molybdenum-based composite material and a preparation method thereof. The ZrO2 ceramic particle reinforced molybdenum-based composite material is mainly prepared from the following raw materials by weight: 1-14 parts of zirconium nitrate, 80-92 parts of ammonium dimolybdate and 120-138 parts of citric acid. The ZrO2 ceramic particle reinforced molybdenum-based composite material takes zirconium nitrate, ammonium dimolybdate and citric acid as raw materials; in the obtained molybdenum-based composite material, the particle size of the reinforcement phase ZrO2 ceramic particles is small, the particle size is on a nano or submircro level; the distribution of the ceramic particles is uniform; and the content of impurities is low. The ZrO2 ceramic particle reinforced molybdenum-based composite material has good high-temperature mechanical properties, processability and high usage temperature.

Description

A kind of ZrO 2ceramic particle strengthens molybdenum-base composite material and preparation method thereof
Technical field
The invention belongs to molybdenum-base composite material technical field, be specifically related to a kind of ZrO 2ceramic particle strengthens molybdenum-base composite material, also relates to a kind of ZrO simultaneously 2ceramic particle strengthens the preparation method of molybdenum-base composite material.
Background technology
Metal Mo and Mo alloys has that fusing point is high, high temperature creep rate is low, the coefficient of expansion is little, heat-conductivity conducting and thermal shock resistance excellent, resistance to wear and the characteristic such as corrosion resistance is strong, be widely used in the numerous areas such as metallurgy, machinery, oil, chemical industry, national defence, Aeronautics and Astronautics, electronics, nuclear industry as high performance material.But metal molybdenum at high temperature intensity, toughness, hardness is poor, and recrystallization temperature is low, easy brittle failure after recrystallize, these disadvantages affect processing characteristics of Mo and Mo alloys, limits its range of application, can't meet the requirement that people use.
Summary of the invention
The object of this invention is to provide a kind of ZrO 2ceramic particle strengthens molybdenum-base composite material, and the high-temperature behavior solving existing metal molybdenum and molybdenum alloy can not meet the problem of people's service requirements.
Second object of the present invention is to provide a kind of ZrO 2ceramic particle strengthens the preparation method of molybdenum-base composite material.
In order to realize above object, the technical solution adopted in the present invention is: a kind of ZrO 2ceramic particle strengthens molybdenum-base composite material, and the raw material primarily of following parts by weight is made: zirconium nitrate 1 ~ 14 part, ammonium dimolybdate 80 ~ 92 parts, citric acid 120 ~ 138 parts.
A kind of above-mentioned ZrO 2ceramic particle strengthens the preparation method of molybdenum-base composite material, comprises the following steps:
1) ammonium dimolybdate, citric acid and zirconium nitrate is got, be made into the corresponding aqueous solution respectively, the zirconium nitrate aqueous solution is added in the ammonium dimolybdate aqueous solution, then add aqueous citric acid solution and obtain mixing solutions, regulate the pH value <2 of mixing solutions, after water-bath, obtain colloidal sol;
2) step 1) gained colloidal sol is carried out roasting after vacuum-drying, obtain mixed powder A;
3) by step 2) gained mixed powder A hydrogen carries out two sections of heat reductions, obtains mixed powder B;
4) by after step 3) gained mixed powder B cold-press moulding, sinter molding under an argon atmosphere, to obtain final product.
Step 1) can also replace in order to lower operation steps:
Get ammonium dimolybdate, zirconium nitrate and citric acid, be made into the corresponding aqueous solution respectively, the pH value regulating the ammonium dimolybdate aqueous solution is 1 ~ 2, then adds the zirconium nitrate aqueous solution and aqueous citric acid solution obtains mixing solutions, after mixing solutions water-bath colloidal sol.
The mass concentration of the described zirconium nitrate aqueous solution is 25% ~ 35%; The mass concentration of the described ammonium dimolybdate aqueous solution is 25% ~ 35%; The mass concentration of described aqueous citric acid solution is 25% ~ 35%.
Also Yttrium trinitrate is added in described mixing solutions; The mol ratio of described Yttrium trinitrate and zirconium nitrate is 6:97.
The method of adjust ph is for adding nitric acid or ammoniacal liquor.
The temperature of described water-bath is 70 ~ 90 DEG C, and the time is 7 ~ 9h.
Step 2) in, described vacuum drying temperature is 100 ~ 120 DEG C, and the time is 6 ~ 8h; The temperature of described roasting is 530 ~ 560 DEG C, and the time is 6 ~ 8h.
In two sections of heat reduction processes described in step 3), the temperature of first paragraph is 530 ~ 560 DEG C, by MoO 3be reduced to MoO 2, the recovery time is 4 ~ 6h; The temperature of second segment is 930 ~ 960 DEG C, by MoO 2be reduced to Mo, the recovery time is 4 ~ 6h.
In step 4), the pressure of described cold-press moulding is 300 ~ 350MPa; The temperature of described sinter molding is 1800 ~ 1860 DEG C, and the time is 12 ~ 16h.
ZrO of the present invention 2ceramic particle strengthens molybdenum-base composite material, with zirconium nitrate, ammonium dimolybdate, citric acid for raw material, in gained molybdenum-base composite material, and wild phase ZrO 2the granularity of ceramic particle is less, is nanometer or submicron order; Being more evenly distributed of ceramic particle, foreign matter content is few, has the use temperature of better mechanical behavior under high temperature, workability and Geng Gao.
ZrO of the present invention 2ceramic particle strengthens the preparation method of molybdenum-base composite material, adopt the technique of sol-gel, prepare the mixed powder of the less nanometer of granularity or submicron order, not only increase the distributing homogeneity of metal and ceramic phase, also avoid the introducing of other impurity, the metallographic phase problem pockety that uneven, the easy introducing impurity of batch mixing solving the existence of general milling batch mixing causes; Gained molybdenum-base composite material has better over-all properties and mechanical behavior under high temperature; Preparation method of the present invention, technique is simple, easy to operate, is easy to Automated condtrol, is applicable to large-scale industrial production.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
The ZrO of the present embodiment 2ceramic particle strengthens molybdenum-base composite material, is made up: five water zirconium nitrate 1.74g, ammonium dimolybdate 91.04g, citric acid 136.56g of the raw material of following weight.
The ZrO of the present embodiment 2ceramic particle strengthens the preparation method of molybdenum-base composite material, comprises the following steps:
1) ammonium dimolybdate getting 91.04g is mixed with the aqueous solution that mass concentration is 25%, the citric acid getting 136.56g is mixed with the aqueous solution that mass concentration is 30%, the five water zirconium nitrates getting 1.74g are mixed with the aqueous solution that zirconium nitrate mass concentration is 35%, the zirconium nitrate aqueous solution is added in the ammonium dimolybdate aqueous solution, produce white precipitate, add aqueous citric acid solution again, the mixing solutions that white precipitate disappears transparent, be 1 to mixed solution and dripping nitric acid or ammoniacal liquor to its pH value, after 80 DEG C of water-baths colloidal sol;
2) step 1) gained colloidal sol is put into vacuum drying oven and carry out vacuum-drying, drying temperature is 100 DEG C, time of drying 8h, after in retort furnace roasting 8h, maturing temperature is 540 DEG C, obtains the oxide compound of molybdenum and zirconic mixed powder A;
3) by step 2) gained mixed powder A is placed in push rod reduction furnace, carries out two sections of heat reductions with hydrogen, first paragraph under temperature 540 DEG C of conditions by MoO 3be reduced to MoO 2, the recovery time is 6h; Second segment under temperature 940 DEG C of conditions by MoO 2be reduced to Mo, the recovery time is 6h, obtains metal molybdenum and zirconic mixed powder B;
4) step 3) gained mixed powder B after cold-press moulding, is carried out sinter molding under 300MPa condition in argon shield stove, sintering temperature is 1800 DEG C, and sintering time is 12h, obtains containing ZrO 2massfraction is the molybdenum-base composite material of 1%.
Embodiment 2
The ZrO of the present embodiment 2ceramic particle strengthens molybdenum-base composite material, is made up: five water zirconium nitrate 8.72g, ammonium dimolybdate 87.36g, citric acid 131.05g of the raw material of following weight.
The ZrO of the present embodiment 2ceramic particle strengthens the preparation method of molybdenum-base composite material, comprises the following steps:
1) ammonium dimolybdate getting 91.04g is mixed with the aqueous solution that mass concentration is 30%, the citric acid getting 136.56g is mixed with the aqueous solution that mass concentration is 35%, the five water zirconium nitrates getting 8.72g are mixed with the aqueous solution that zirconium nitrate mass concentration is 25%, the zirconium nitrate aqueous solution is added in the ammonium dimolybdate aqueous solution, produce white precipitate, add aqueous citric acid solution again, the mixing solutions that white precipitate disappears transparent, be 1.5 to mixed solution and dripping nitric acid or ammoniacal liquor to its pH value, after 85 DEG C of water-baths colloidal sol;
2) step 1) gained colloidal sol is put into vacuum drying oven and carry out vacuum-drying, drying temperature is 110 DEG C, time of drying 7h, after in retort furnace roasting 7h, maturing temperature is 550 DEG C, obtains the oxide compound of molybdenum and zirconic mixed powder A;
3) by step 2) gained mixed powder A is placed in push rod reduction furnace, carries out two sections of heat reductions with hydrogen, first paragraph under temperature 550 DEG C of conditions by MoO 3be reduced to MoO 2, the recovery time is 5h; Second segment under temperature 950 DEG C of conditions by MoO 2be reduced to Mo, the recovery time is 5h, obtains metal molybdenum and zirconic mixed powder B;
4) step 3) gained mixed powder B after cold-press moulding, is carried out sinter molding under 300MPa condition in argon shield stove, sintering temperature is 1800 DEG C, and sintering time is 14h, obtains containing ZrO 2massfraction is the molybdenum-base composite material of 5%.
Embodiment 3
The ZrO of the present embodiment 2ceramic particle strengthens molybdenum-base composite material, is made up: five water zirconium nitrate 17.44g, ammonium dimolybdate 82.76g, citric acid 124.15g of the raw material of following weight.
The ZrO of the present embodiment 2ceramic particle strengthens the preparation method of molybdenum-base composite material, comprises the following steps:
1) ammonium dimolybdate getting 82.76g is mixed with the aqueous solution that mass concentration is 35%, the citric acid getting 124.15g is mixed with the aqueous solution that mass concentration is 25%, the five water zirconium nitrates getting 17.44g are mixed with the aqueous solution that zirconium nitrate mass concentration is 30%, nitric acid is dripped or ammoniacal liquor regulates its pH value to be 1 in the ammonium dimolybdate aqueous solution, the zirconium nitrate aqueous solution is added in the ammonium dimolybdate aqueous solution, produce white precipitate, add aqueous citric acid solution again, the mixing solutions that white precipitate disappears transparent, obtains colloidal sol after 90 DEG C of water-baths;
2) step 1) gained colloidal sol is put into vacuum drying oven and carry out vacuum-drying, drying temperature is 120 DEG C, time of drying 6h, after in retort furnace roasting 6h, maturing temperature is 560 DEG C, obtains the oxide compound of molybdenum and zirconic mixed powder A;
3) by step 2) gained mixed powder A is placed in push rod reduction furnace, carries out two sections of heat reductions with hydrogen, first paragraph under temperature 560 DEG C of conditions by MoO 3be reduced to MoO 2, the recovery time is 4h; Second segment under temperature 960 DEG C of conditions by MoO 2be reduced to Mo, the recovery time is 4h, obtains metal molybdenum and zirconic mixed powder B;
4) step 3) gained mixed powder B after cold-press moulding, is carried out sinter molding under 350MPa condition in argon shield stove, sintering temperature is 1860 DEG C, and sintering time is 16h, obtains containing ZrO 2massfraction is the molybdenum-base composite material of 10%.
Embodiment 4
The ZrO of the present embodiment 2ceramic particle strengthens molybdenum-base composite material, and the raw material primarily of following weight is made: five water zirconium nitrate 1.74g, ammonium dimolybdate 91.04g, citric acid 136.56g.
The ZrO of the present embodiment 2ceramic particle strengthens the preparation method of molybdenum-base composite material, comprises the following steps:
1) ammonium dimolybdate getting 91.04g is mixed with the aqueous solution that mass concentration is 25%, the citric acid getting 136.56g is mixed with the aqueous solution that mass concentration is 30%, the five water zirconium nitrates getting 1.74g are mixed with the aqueous solution that zirconium nitrate mass concentration is 35%, the zirconium nitrate aqueous solution is added in the ammonium dimolybdate aqueous solution, produce white precipitate, add aqueous citric acid solution again, the mixing solutions that white precipitate disappears transparent, also Yttrium trinitrate is added in described mixing solutions, the mol ratio of Yttrium trinitrate and zirconium nitrate is 6:97, be 1 to mixed solution and dripping nitric acid or ammoniacal liquor to its pH value, colloidal sol is obtained after 80 DEG C of water-baths,
2) step 1) gained colloidal sol is put into vacuum drying oven and carry out vacuum-drying, drying temperature is 100 DEG C, time of drying 8h, after in retort furnace roasting 8h, maturing temperature is 540 DEG C, obtains mixed powder A;
3) by step 2) gained mixed powder A is placed in push rod reduction furnace, carries out two sections of heat reductions with hydrogen, first paragraph under temperature 540 DEG C of conditions by MoO 3be reduced to MoO 2, the recovery time is 6h; Second segment under temperature 940 DEG C of conditions by MoO 2be reduced to Mo, the recovery time is 6h, obtains mixed powder B;
4) step 3) gained mixed powder B after cold-press moulding, is carried out sinter molding under 300MPa condition in argon shield stove, sintering temperature is 1800 DEG C, and sintering time is 12h, obtains containing ZrO 2the molybdenum-base composite material of stable crystal form.
The present embodiment gained molybdenum-base composite material, at zirconium nitrate, ammonium dimolybdate, citric acid be raw material basis on add stablizer Yttrium trinitrate, thus obtain the m-ZrO of stable crystal form 2, solve molybdenum-base composite material in use due to ZrO 2crystal formation change the problem of volumetric expansion and contraction of causing, improve work-ing life.
Experimental example
The performance of this experimental example to embodiment 1-4 gained molybdenum-base composite material detects, and compares with pure molybdenum, and result is as shown in table 1.
Table 1 embodiment 1-4 gained molybdenum-base composite material performance test results

Claims (10)

1. a ZrO 2ceramic particle strengthens molybdenum-base composite material, it is characterized in that: the raw material primarily of following parts by weight is made: zirconium nitrate 1 ~ 14 part, ammonium dimolybdate 80 ~ 92 parts, citric acid 120 ~ 138 parts.
2. a ZrO as claimed in claim 1 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: comprise the following steps:
1) get ammonium dimolybdate, zirconium nitrate and citric acid, be made into the corresponding aqueous solution respectively, gained ammonium dimolybdate, zirconium nitrate, aqueous citric acid solution are mixed and made into mixing solutions, regulate the pH value <2 of mixing solutions, after water-bath, obtain colloidal sol;
2) step 1) gained colloidal sol is carried out roasting after vacuum-drying, obtain mixed powder A;
3) by step 2) gained mixed powder A hydrogen carries out two sections of heat reductions, obtains mixed powder B;
4) by after step 3) gained mixed powder B cold-press moulding, sinter molding under protection of inert gas, to obtain final product.
3. ZrO according to claim 2 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: step 1) can also replace in order to lower operation steps:
Get ammonium dimolybdate, zirconium nitrate and citric acid, be made into the corresponding aqueous solution respectively, the pH value regulating the ammonium dimolybdate aqueous solution is 1 ~ 2, then adds the zirconium nitrate aqueous solution and aqueous citric acid solution obtains mixing solutions, after mixing solutions water-bath colloidal sol.
4. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: the mass concentration of the described zirconium nitrate aqueous solution is 25% ~ 35%; The mass concentration of the described ammonium dimolybdate aqueous solution is 25% ~ 35%; The mass concentration of described aqueous citric acid solution is 25% ~ 35%.
5. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: also add Yttrium trinitrate in described mixing solutions; The mol ratio of described Yttrium trinitrate and zirconium nitrate is 6:97.
6. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: the method for adjust ph is for adding nitric acid or ammoniacal liquor.
7. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: the temperature of described water-bath is 70 ~ 90 DEG C, and the time is 7 ~ 9h.
8. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, it is characterized in that: step 2) in, described vacuum drying temperature is 100 ~ 120 DEG C, and the time is 6 ~ 8h; The temperature of described roasting is 530 ~ 560 DEG C, and the time is 6 ~ 8h.
9. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, and it is characterized in that: in two sections of heat reduction processes described in step 3), the temperature of first paragraph is 530 ~ 560 DEG C, by MoO 3be reduced to MoO 2, the recovery time is 4 ~ 6h; The temperature of second segment is 930 ~ 960 DEG C, by MoO 2be reduced to Mo, the recovery time is 4 ~ 6h.
10. the ZrO according to Claims 2 or 3 2ceramic particle strengthens the preparation method of molybdenum-base composite material, and it is characterized in that: in step 4), the pressure of described cold-press moulding is 300 ~ 350MPa; The temperature of described sinter molding is 1800 ~ 1860 DEG C, and the time is 12 ~ 16h.
CN201410027279.2A 2014-01-21 2014-01-21 A kind of ZrO2ceramic particle strengthens molybdenum-base composite material and preparation method thereof Expired - Fee Related CN104294133B (en)

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Cited By (5)

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CN105081339A (en) * 2015-09-29 2015-11-25 河南科技大学 Preparing method of tungsten-zirconium-yttrium ternary alloy powder
CN107245621A (en) * 2017-06-12 2017-10-13 河南科技大学 A kind of wear-and corrosion-resistant molybdenum alloy and preparation method thereof
CN107686931A (en) * 2017-08-29 2018-02-13 东莞市联洲知识产权运营管理有限公司 Zirconium boride niobium molybdenum-base composite material that a kind of yttrium ceramic whisker surface is modified and preparation method thereof
CN108149042A (en) * 2017-12-22 2018-06-12 北京工业大学 A kind of cryogenic activating sintering preparation method of high-compactness molybdenum material
CN110066952A (en) * 2019-06-06 2019-07-30 淮北师范大学 A kind of preparation method of zirconium oxide enhancing molybdenum alloy bar material

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CN102896317A (en) * 2012-10-23 2013-01-30 上海大学 Method for preparing Mo-ZrO2 metal ceramic electrode by utilizing sol-gel method

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Publication number Priority date Publication date Assignee Title
CN105081339A (en) * 2015-09-29 2015-11-25 河南科技大学 Preparing method of tungsten-zirconium-yttrium ternary alloy powder
CN107245621A (en) * 2017-06-12 2017-10-13 河南科技大学 A kind of wear-and corrosion-resistant molybdenum alloy and preparation method thereof
CN107245621B (en) * 2017-06-12 2019-02-05 河南科技大学 A kind of wear-and corrosion-resistant molybdenum alloy and preparation method thereof
CN107686931A (en) * 2017-08-29 2018-02-13 东莞市联洲知识产权运营管理有限公司 Zirconium boride niobium molybdenum-base composite material that a kind of yttrium ceramic whisker surface is modified and preparation method thereof
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CN108149042A (en) * 2017-12-22 2018-06-12 北京工业大学 A kind of cryogenic activating sintering preparation method of high-compactness molybdenum material
CN108149042B (en) * 2017-12-22 2020-04-14 北京工业大学 Low-temperature activation sintering preparation method of high-density molybdenum material
CN110066952A (en) * 2019-06-06 2019-07-30 淮北师范大学 A kind of preparation method of zirconium oxide enhancing molybdenum alloy bar material
CN110066952B (en) * 2019-06-06 2020-08-14 淮北师范大学 Preparation method of zirconium oxide reinforced molybdenum alloy bar

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