CN104108694B - A kind of negative thermal expansion material HfMnMo 2pO 12and preparation method thereof - Google Patents
A kind of negative thermal expansion material HfMnMo 2pO 12and preparation method thereof Download PDFInfo
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- CN104108694B CN104108694B CN201410330921.4A CN201410330921A CN104108694B CN 104108694 B CN104108694 B CN 104108694B CN 201410330921 A CN201410330921 A CN 201410330921A CN 104108694 B CN104108694 B CN 104108694B
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- hfmnmo
- thermal expansion
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- expansion material
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Abstract
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to a kind of negative thermal expansion material HfMnMo
2pO
12and preparation method thereof.This material is by HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4hot pressed sintering is made.Preparation method comprises the steps such as grinding, embryo processed, sintering.Negative thermal expansion material HfMnMo provided by the present invention
2pO
12, have that negative expansion coefficient is large, the advantage of wide temperature region, be thus with a wide range of applications; Negative thermal expansion material HfMnMo
2pO
12raw materials source wide, cost is low; Preparation method is simple, the cycle is short, and pollution-free, is thus suitable for suitability for industrialized production, has better application value.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to a kind of negative thermal expansion material HfMnMo
2pO
12and preparation method thereof.
Background technology
The most material of occurring in nature has the character of expanding with heat and contract with cold, and the thermal expansivity between the expanding with heat and contract with cold of material, material does not mate often can cause that device is tired, degradation or even temporarily or eventual failure.Along with the development of the high-quality precision and sophisticated technology such as space flight, electronics, expanding with heat and contract with cold of material more and more becomes the focal issue of engineering field people care.
The appearance of negative thermal expansion material, provides opportunity and possibility for addressing this problem, and design and modulation controllable expansion, Zero-expansion material have important application prospect at high-tech engineering fields such as aerospace, precision instruments, photoelectrons.But the research of negative thermal expansion material is current is still in the exploratory stage, considers the factor such as preparation condition and environmental protection, be easy to suitability for industrialized production and to drop into the negative thermal expansion material of widespread use also less.Therefore, develop that a kind of negative expansion performance is good, preparation technology is simple, cost is lower, can be of great significance for the novel negative thermal expansion material tool of widespread use.
Summary of the invention
The object of the present invention is to provide a kind of material HfMnMo of negative expansion better performances
2pO
12and preparation method thereof.
For achieving the above object, the technical scheme taked of the present invention is as follows.
A kind of negative thermal expansion material HfMnMo
2pO
12, by HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4hot pressed sintering is made.
Described negative thermal expansion material HfMnMo
2pO
12preparation method, comprise the following steps:
(1) by raw material HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4mix, grinding;
(2) by after step (1) Raw drying, compressing tablet embryo;
(3) by step (2) idiosome under 700 ~ 1000 DEG C of conditions, sintering 5 ~ 10h; Namely negative thermal expansion material HfMnMo is obtained after sintered product naturally cooling
2pO
12.
Step (1) Raw with molar ratio computing, HfO
2︰ Mn
2o
3︰ MoO
3︰ NH
4h
2pO
4=2 ︰ 1 ︰ 4 ︰ 2.
For making raw material mix in step (1), add dehydrated alcohol, grinding 2h.
The described compressing tablet of step (2) adopts single shaft dry powder sheeting machine to suppress under 200MPa pressure.
In step (3), sintering sinters in box-type furnace, and temperature rise rate is 5 DEG C/min.
Negative thermal expansion material HfMnMo provided by the present invention
2pO
12, have that negative expansion coefficient is large, the advantage of wide temperature region, be thus with a wide range of applications; Negative thermal expansion material HfMnMo
2pO
12raw materials source wide, cost is low; Preparation method is simple, the cycle is short, and pollution-free, is thus suitable for suitability for industrialized production, has better application value.
Accompanying drawing explanation
Fig. 1 is novel negative thermal expansion material HfMnMo prepared by embodiment 1
2pO
12xRD figure spectrum;
Fig. 2 is novel negative thermal expansion material HfMnMo prepared by embodiment 2
2pO
12xRD figure spectrum;
Fig. 3 is novel negative thermal expansion material HfMnMo prepared by embodiment 3
2pO
12xRD figure spectrum;
Fig. 4 is novel negative thermal expansion material HfMnMo prepared by embodiment 4
2pO
12xRD figure spectrum;
Fig. 5 is novel negative thermal expansion material HfMnMo prepared by embodiment 1
2pO
12relative length with the change curve of probe temperature;
Fig. 6 is novel negative thermal expansion material HfMnMo prepared by embodiment 2
2pO
12relative length with the change curve of probe temperature;
Fig. 7 is novel negative thermal expansion material HfMnMo prepared by embodiment 3
2pO
12relative length with the change curve of probe temperature;
Fig. 8 is novel negative thermal expansion material HfMnMo prepared by embodiment 4
2pO
12relative length with the change curve of probe temperature;
Fig. 9 is novel negative thermal expansion material HfMnMo prepared by embodiment 1-4
2pO
12the coefficient of linear expansion of different warm area matchings;
Figure 10 is novel negative thermal expansion material HfMnMo prepared by embodiment 1
2pO
12surface scan electromicroscopic photograph.
Embodiment
Below in conjunction with embodiment the present invention will be further explained explanation.
embodiment 1
Negative thermal expansion material HfMnMo prepared by the present embodiment
2pO
12, by HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4hot pressed sintering is made, and specifically comprises the following steps:
(1) with molar ratio computing, raw material is pressed HfO
2︰ Mn
2o
3︰ MoO
3︰ NH
4h
2pO
4the amount of=2 ︰ 1 ︰ 4 ︰ 2 takes, and mixes, grinding 2h; For making raw material mix, during raw material mixing or grinding, add appropriate dehydrated alcohol;
(2) by after step (1) Raw drying, compressing tablet embryo;
Drying is dry half an hour under 80 DEG C of conditions;
Compressing tablet is adopt single shaft dry powder sheeting machine under the pressure of 200MPa, powder to be made diameter 10 millimeters, the green body cylinders of high 5 millimeter;
(3) step (2) idiosome is placed in box-type furnace, temperature rise rate is 5/min, reaches 700 DEG C, insulation 10h; Namely negative thermal expansion material HfMnMo is obtained after the cooling of sintered product naturally cooling
2pO
12.
Negative thermal expansion material HfMnMo prepared by the present embodiment
2pO
12corresponding XRD figure spectrum material phase analysis is shown in Fig. 1, and know that resultant is mainly orthohormbic structure mutually by analysis, its main diffraction peak is consistent with PDF card number 00-051-0581, illustrates that the sample of preparation is the material of pure phase.
embodiment 2
The preparation of the present embodiment is identical with embodiment 1, and only adjusting sintering temperature is 800 DEG C, and soaking time is 8h.
Negative thermal expansion material HfMnMo prepared by the present embodiment
2pO
12corresponding XRD figure spectrum material phase analysis is shown in Fig. 2, and know that resultant is mainly orthohormbic structure mutually by analysis, its main diffraction peak is consistent with PDF card number 00-051-0581, illustrates that the sample of preparation is the material of pure phase.
embodiment 3
The preparation of the present embodiment is identical with embodiment 1, and only adjusting sintering temperature is 900 DEG C, and soaking time is 6h.
Negative thermal expansion material HfMnMo prepared by the present embodiment
2pO
12corresponding XRD figure spectrum material phase analysis is shown in Fig. 3, and know that resultant is mainly orthohormbic structure mutually by analysis, its main diffraction peak is consistent with PDF card number 00-051-0581, illustrates that the sample of preparation is the material of pure phase.
embodiment 4
The preparation of the present embodiment is identical with embodiment 1, and only adjusting sintering temperature is 1000 DEG C, and soaking time is 5h.
Negative thermal expansion material HfMnMo prepared by the present embodiment
2pO
12corresponding XRD figure spectrum material phase analysis is shown in Fig. 4, and know that resultant is mainly orthohormbic structure mutually by analysis, its main diffraction peak is consistent with PDF card number 00-051-0581, illustrates that the sample of preparation is the material of pure phase.
For the negative thermal expansion material HfMnMo prepared by inspection above-described embodiment
2pO
12properties, done coefficient of expansion test and electron-microscope scanning further, coefficient of expansion test adopts Lin Saisi L76, and electron-microscope scanning adopts FE-SEM(ModelJSM-6700F), concrete outcome is described below.
the coefficient of expansion is tested
Fig. 5 is the HfMnMo prepared by embodiment 1
2pO
12the relative length variation with temperature curve of sample.As can be seen from the figure, the length of sample reduces with the increase of temperature to 170 DEG C at 30 DEG C, shows that prepared material is for having negative heat expansion characteristics; The thermal expansivity of linear fit is-3.34 × 10
-6dEG C
-1(30 ~ 170 DEG C).
Fig. 6 is the HfMnMo prepared by embodiment 2
2pO
12the relative length variation with temperature curve of sample.As can be seen from the figure, the length of sample reduces with the increase of temperature to 160 DEG C at 25 DEG C, shows that prepared material is for having negative heat expansion characteristics; The thermal expansivity of linear fit is-3.20 × 10
-6dEG C
-1(25 ~ 160 DEG C).
Fig. 7 is the HfMnMo prepared by embodiment 3
2pO
12the relative length variation with temperature curve of sample.As can be seen from the figure, the length of sample reduces with the increase of temperature to 150 DEG C at 25 DEG C, shows that prepared material is for having negative heat expansion characteristics; The thermal expansivity of linear fit is-4.01 × 10
-6dEG C
-1(25 ~ 150 DEG C).
Fig. 8 is the HfMnMo prepared by embodiment 4
2pO
12the relative length variation with temperature curve of sample.As can be seen from the figure, the length of sample reduces with the increase of temperature at 20 to 170 DEG C, shows that prepared material is for having negative heat expansion characteristics; The thermal expansivity of linear fit is-3.88 × 10
-6dEG C
-1(20 ~ 170 DEG C).
Fig. 9 is the coefficient of linear expansion of embodiment 1-4 in different warm area matching, show the negative thermal expansion material (30 ~ 150 DEG C) that can obtain negative expansion stable performance at 700 ~ 1000 DEG C of sintering, and positive thermal expansion warm area (150 ~ 400 DEG C) coefficient of expansion (the embodiment 1-4 average linear coefficient of expansion is 0.87 × 10 close to zero
-6dEG C
-1).
electronic scanning Electronic Speculum is tested
Figure 10 is novel negative thermal expansion material HfMnMo prepared by embodiment 1
2pO
12surface scan electromicroscopic photograph, wherein (a) and (b) magnification is respectively 2000,4000 times, and granular size is about tens microns.
Claims (4)
1. a negative thermal expansion material HfMnMo
2pO
12, it is characterized in that, this material is by HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4hot pressed sintering is made as follows,
(1) by raw material HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4mix, grinding;
(2) by after the drying of step (1) gained mixture, adopt single shaft dry powder sheeting machine at 200MPa pressure lower sheeting embryo;
(3) by step (2) gained idiosome under 700 ~ 1000 DEG C of conditions, sintering 5 ~ 10h; Namely negative thermal expansion material HfMnMo is obtained after sintered product naturally cooling
2pO
12;
In step (1), raw material with molar ratio computing, HfO
2: Mn
2o
3: MoO
3: NH
4h
2pO
4=2:1:4:2.
2. a negative thermal expansion material HfMnMo
2pO
12preparation method, it is characterized in that, preparation method comprises the following steps:
(1) by raw material HfO
2, Mn
2o
3, MoO
3, NH
4h
2pO
4mix, grinding;
(2) by after the drying of step (1) gained mixture, compressing tablet embryo;
(3) by step (2) gained idiosome under 700 ~ 1000 DEG C of conditions, sintering 5 ~ 10h; Namely negative thermal expansion material HfMnMo is obtained after sintered product naturally cooling
2pO
12;
Step (1) Raw with molar ratio computing, HfO
2: Mn
2o
3: MoO
3: NH
4h
2pO
4=2:1:4:2;
The described compressing tablet of step (2) adopts single shaft dry powder sheeting machine to suppress under 200MPa pressure.
3. negative thermal expansion material HfMnMo as claimed in claim 2
2pO
12preparation method, it is characterized in that, in step (1), add dehydrated alcohol during raw material mixing or grinding, and grind 2h.
4. negative thermal expansion material HfMnMo as claimed in claim 2
2pO
12preparation method, it is characterized in that, sintering sinters in box-type furnace in step (3), and temperature rise rate is 5 DEG C/min.
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|---|---|---|---|
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|---|---|---|---|
| CN201410330921.4A CN104108694B (en) | 2014-07-11 | 2014-07-11 | A kind of negative thermal expansion material HfMnMo 2pO 12and preparation method thereof |
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| CN104108694B true CN104108694B (en) | 2016-04-13 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844205A (en) * | 2015-04-23 | 2015-08-19 | 郑州大学 | Novel negative thermal expansion luminescence material HfScW2PO12 and solid phase sintering synthesis method thereof |
| CN104876579A (en) * | 2015-05-13 | 2015-09-02 | 郑州大学 | Novel negative thermal expansion light-emitting ceramic material HfScMo2VO12 and synthesis method thereof by solid-phase sintering |
| CN106145942B (en) * | 2016-07-11 | 2018-12-28 | 郑州大学 | A kind of negative thermal expansion material ZrMoV2O10And preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4587067A (en) * | 1984-07-20 | 1986-05-06 | The Perkin-Elmer Corporation | Method of manufacturing low thermal expansion modified cordierite ceramics |
| CN101024580A (en) * | 2006-12-30 | 2007-08-29 | 郑州大学 | Negative heat expansion coefficient material quick sintering synthesizing method |
| CN102390866A (en) * | 2011-08-03 | 2012-03-28 | 北京师范大学 | Modified hafnium tungstate and preparation method thereof |
-
2014
- 2014-07-11 CN CN201410330921.4A patent/CN104108694B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4587067A (en) * | 1984-07-20 | 1986-05-06 | The Perkin-Elmer Corporation | Method of manufacturing low thermal expansion modified cordierite ceramics |
| CN101024580A (en) * | 2006-12-30 | 2007-08-29 | 郑州大学 | Negative heat expansion coefficient material quick sintering synthesizing method |
| CN102390866A (en) * | 2011-08-03 | 2012-03-28 | 北京师范大学 | Modified hafnium tungstate and preparation method thereof |
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