CN102285798A - Sintering synthesis method of ZrO2/ZrW2O8 composite material with controlled thermal expansion - Google Patents

Sintering synthesis method of ZrO2/ZrW2O8 composite material with controlled thermal expansion Download PDF

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CN102285798A
CN102285798A CN2011101589950A CN201110158995A CN102285798A CN 102285798 A CN102285798 A CN 102285798A CN 2011101589950 A CN2011101589950 A CN 2011101589950A CN 201110158995 A CN201110158995 A CN 201110158995A CN 102285798 A CN102285798 A CN 102285798A
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zro
zrw
sintering
composite
zro2
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梁二军
郭向阳
程春晓
梁源
晁明举
刘晓旻
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Zhengzhou University
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Abstract

The invention belongs to the field of inorganic nonmetallic materials, and discloses a sintering synthesis method of a ZrO2/ZrW2O8 composite material with controlled thermal expansion. The sintering synthesis method comprises the steps of weighing ZrO2 and WO3 used as raw materials according to the chemical mass ratio requirements of ZrO2 and ZrW2O8 in the target product ZrO2/ZrW2O8 composite material, uniformly grinding and mixing, directly carrying out one-time sintering or carrying out one-time sintering after tabletting to synthesize a product, and cooling the obtained product with water to obtain the target product. In the sintering synthesis method disclosed by the invention, the ZrO2/ZrW2O8 composite material with controlled thermal expansion is prepared by using a high-temperature rapid sintering technology, simultaneously ZrO2, WO3 and Y2O3 are selected as the raw materials, and second phase ZrW2O8 granules are introduced into a ceramic base body ZrO2 by an in-situ synthesis method and are uniformly dispersed and distributed, thereby obtaining a composite ceramic with low expansion performance and avoiding interface contamination between ZrO2 and ZrW2O8; and at the same time, the sintering synthesis method can be completed by one-time sintering, the raw materials are sufficiently reacted at a high temperature, the preparation process is simple, the sintering rate is high, the sintering time is short and the second phase is easy to disperse.

Description

A kind of controlled thermal expansion ZrO＜sub〉2＜/sub 〉/ZrW＜sub〉2＜/sub〉O＜sub〉8＜/sub〉sintering and synthesizing method of matrix material
Technical field
The invention belongs to field of inorganic nonmetallic material, particularly a kind of controlled thermal expansion ZrO 2/ ZrW 2O 8The sintering and synthesizing method of composite.
Background technology
Most materials all have the character of expanding with heat and contract with cold.The stress that material produces owing to expanding with heat and contract with cold often causes device fatigue, hydraulic performance decline, inefficacy even fracture and comes off.The negative expansion material is meant the class material that average coefficient of linear expansion in certain temperature range or volume coefficient are negative value (NTE), has the characteristic of " pyrocondensation cold expanding ".1996, American scholar Mary TA etc. delivered " Negative thermal expansion from 0.3 to 1050 Kelvin in ZrW at " science " 2O 8" report ZrW 2O 8Has the big negative expansion coefficient of isotropism, ZrW 2O 8Cause scientist's extensive concern and further investigation with its superior hot expansibility.ZrW 2O 8With the compound materials and devices that can Design and manufacture has zero thermal expansion and controllable expansion coefficient of other materials, can effectively reduce like this micro-crack that in material, forms owing to thermal cycling stresses, prolong the service life of material, thereby have potential important use at numerous areas such as optics, electronics, medical science, machinery, aviations.For example, the Fiber Bragg Grating FBG of optical communication or optically filtering sheet exists the influence of serious temperature to the filter light wavelength, and temperature has caused the grating index variation to cause reflection wavelength to change.If can develop the ZrO of the controllable expansion coefficient of excellent performance 2/ ZrW 2O 8Composite addresses this problem perfection.ZrO 2Chemical stability is good, is a kind of important 26S Proteasome Structure and Function material, has obtained to use widely in refractory materials, pottery, machinery, electronics, optics, aerospace or the like every field.ZrO 2Based composites has high-strength and high ductility (being the highest class of toughness in the present stupalith), wear-and corrosion-resistant, high temperature resistant and good characteristic such as at high temperature can conduct electricity, and has a good application prospect.At present, ZrO 2/ ZrW 2O 8The synthetic method that matrix material is commonly used mainly contains high-temperature solid phase reaction method [US6258743B1; US6403511B2] and spraying drying sintering process [P. Lommens et al. Journal of the European Ceramic Society 25 (2005) 3605 – 3610].Although these methods can be prepared ZrO 2/ ZrW 2O 8Composite, but exist preparation process longer, step is many, length consuming time, and power consumption is high, the deficiencies such as the easy pollution of the sample of preparing.If particularly prepare earlier ZrW 2O 8Powder is then with the ZrO of different quality mark 2Preparation ZrO after mixing 2/ ZrW 2O 8Composite, will be repeatedly during preparation long-time sintering generally needed tens hours just can prepare ZrO 2/ ZrW 2O 8Composite.
Therefore, research and develop a kind of pollution less, preparation fast, cost is low, the ZrO that is fit to large-scale production 2/ ZrW 2O 8The composite manufacture method is significant.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, pollute less, sintering velocity is fast and the controlled thermal expansion ZrO of suitable large-scale production 2/ ZrW 2O 8The sintering and synthesizing method of composite.
For achieving the above object, the technical scheme taked of the present invention is as follows:
A kind of controlled thermal expansion ZrO 2/ ZrW 2O 8The sintering and synthesizing method of composite: with zirconium dioxide ZrO 2, tungstic acid WO 3Be raw material, according to target product ZrO 2/ ZrW 2O 8ZrO in (zirconium dioxide/wolframic acid zirconium) composite 2And ZrW 2O 8Chemical quality take by weighing material raw material ZrO than demand 2And WO 3(1mol ZrW 2O 8Need 1mol ZrO 2With 2mol WO 3), ground and mixed is even, and is once sintered synthetic and products therefrom is carried out water-cooled get target product directly or behind the compressing tablet; Wherein, sintering parameter is: 1250 ~ 1300 ℃ of temperature, time 1 ~ 3h.Among the present invention, ZrO 2, WO 3Under hot conditions, pass through chemical reaction, at ZrO 2Original position generates ZrW in the matrix 2O 8Thereby, reach compound purpose; Compressing tablet can not synthesize (being that direct sintering is synthetic) by sintering yet, but the contact of compressing tablet feed particles is not tight, and reaction is difficult to abundant; The benefit of compressing tablet is the shape that can directly burn till rule, in addition, reacts easier and fully carries out.
Preferably, because ZrO 2Crystal conversion taking place when sintering and can make sintering densification that difficulty takes place with the comparatively large vol effect, and cause the sample cracking for preparing easily, is to improve sintering velocity and improve the matrix material density, and the present invention introduces electricity price and compares Zr 4+Low Y 3+Oxide compound Y 2O 3(yttrium oxide) suppressed this as additive, Y 2O 3Add-on accounts for ZrO 2With WO 30.1 ~ 1% of gross weight.
Beneficial effect of the present invention is:
1, the present invention adopts high temperature Fast Sintering technology to prepare controlled thermal expansion ZrO 2/ ZrW 2O 8Composite is selected ZrO simultaneously 2, WO 3And Y 2O 3Be raw material, by in-situ synthesis with second-phase ZrW 2O 8Particle is incorporated in the ceramic matrix, makes it be the complex phase ceramic that even dispersion distributes and reaches the low bulk performance, has avoided ZrO 2And ZrW 2O 8Interface pollution, simultaneously the present invention can once sinteredly finish, and at high temperature raw material reaction is very abundant, and preparation process is simple, and sintering velocity is fast, and the time is short, and second-phase disperses easily.
2, Y 2O 3Form solid solution with sinter, increased the vacancy concentration in the crystal, change significantly sintering velocity, the relative density of composite can reach 98% of solid density.
3, the matrix of composite is positive expanding material ZrO 2, second-phase is negative expansion material ZrW 2O 8, can be by regulating ZrO 2Mass fraction in composite is accurately controlled the coefficient of volume expansion of material, from negative, zero on the occasion of continuous variation.
Description of drawings
Fig. 1 is the ZrO that embodiment 1 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 2 is the ZrO that embodiment 2 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 3 is the ZrO that embodiment 3 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 4 is the ZrO that embodiment 4 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 5 is the ZrO that embodiment 5 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 6 is the ZrO that embodiment 6 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 7 is the ZrO that embodiment 7 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 8 is the ZrO that embodiment 8 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Fig. 9 is the ZrO that embodiment 9 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Figure 10 is the ZrO that embodiment 10 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Figure 11 is the ZrO that embodiment 11 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Figure 12 is the ZrO that embodiment 12 synthesizes 2/ ZrW 2O 8The XRD figure of composite.
Figure 13 is the ZrO that embodiment 9 synthesizes 2/ ZrW 2O 8The SEM collection of illustrative plates of composite.
Figure 14 is ZrO 2/ ZrW 2O 8The thermal expansion curve map of composite: No.1--embodiment 1, No.2--embodiment 2, No.3--embodiment 3.
Figure 15 is ZrO 2/ ZrW 2O 8The thermal expansion curve map of composite: No.1--embodiment 8, No.2--embodiment 9, No.3--embodiment 10, No.4--embodiment 11, No.5--embodiment 12.
Embodiment
Embodiment 1
High temperature process furnances is set makes it be warming up to 1300 ℃ of sintering temperatures.
Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:2 2O 85.8690g, ZrO 211.7381g) take by weighing raw material ZrO 212.9703g and WO 34.6368g, in agate mortar, grind 2h, raw material is mixed; Material powder is pressed into the uniform raw material of ground and mixed cylindric with the pressure of 12MPa with hydraulic press, size is diameter 1.2cm, thick 2mm is placed on sintering 2h in the high temperature process furnances that has been warming up to 1300 ℃ behind the compressing tablet, place fast the room temperature water cooling to get final product after sintering is finished.
The X-ray diffraction material phase analysis that product is corresponding is seen Fig. 1, and the XRD result of Fig. 1 shows and synthesized highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 2
Be with the difference of embodiment 1: high temperature process furnances is set makes it be warming up to 1300 ℃ of sintering temperatures, sintering time is 1h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:1 2O 85.8690g, ZrO 25.8690g) take by weighing raw material ZrO 27.1013g and WO 34.6368g; The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 2, and the XRD result of Fig. 2 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 3
Be with the difference of embodiment 1: high temperature process furnances is set makes it be warming up to 1300 ℃ of sintering temperatures, sintering time is 1h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=2:1 2O 85.8690g, ZrO 22.9345g) take by weighing raw material ZrO 24.1668g and WO 34.6368g; The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 3, and the XRD result of Fig. 3 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 4
Be with the difference of embodiment 1: high temperature process furnances is set makes it be warming up to 1250 ℃ of sintering temperatures, sintering time is 3h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:2 2O 85.8690g, ZrO 211.7381g) take by weighing raw material ZrO 212.9703g and WO 34.6368g; The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 4, and the XRD result of Fig. 4 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 5
Be with the difference of embodiment 1: material powder is synthetic without the compressing tablet direct sintering; The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 5, and the XRD result of Fig. 5 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 6
Be with the difference of embodiment 4: high temperature process furnances is set makes it be warming up to 1250 ℃ of sintering temperatures, sintering time is 2h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:2 2O 85.8690g, ZrO 211.7381g) take by weighing raw material ZrO 212.9703g and WO 34.6368g, and add the Y of 0.1wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 6, and the XRD result of Fig. 6 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 7
Be with the difference of embodiment 4: high temperature process furnances is set makes it be warming up to 1250 ℃ of sintering temperatures, sintering time is 2h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:2 2O 85.8690g, ZrO 211.7381g) take by weighing raw material ZrO 212.9703g and WO 34.6368g, and add the Y of 0.5wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 7, and the XRD result of Fig. 7 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 8
Be with the difference of embodiment 1: high temperature process furnances is set makes it be warming up to 1250 ℃ of sintering temperatures, sintering time is 1h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:2 2O 85.8690g, ZrO 211.7381g) take by weighing raw material ZrO 212.9703g and WO 34.6368g, and add the Y of 1wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 8, and the XRD result of Fig. 8 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 9
Be with the difference of embodiment 1: high temperature process furnances is set makes it be warming up to 1250 ℃ of sintering temperatures, sintering time is 3h; Can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1:1 2O 85.8690g, ZrO 25.8690g) take by weighing raw material ZrO 27.1013g and WO 34.6368g, and add the Y of 1wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Fig. 9, and the XRD result of Fig. 9 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 10
Be with the difference of embodiment 8: can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1.3:1 2O 85.8690g, ZrO 24.5147g) take by weighing raw material ZrO 25.7469g and WO 34.6368g, and add the Y of 1wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Figure 10, and the XRD result of Figure 10 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 11
Be with the difference of embodiment 8: can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=1.5:1 2O 85.8690g, ZrO 23.9127g) take by weighing raw material ZrO 25.1449g and WO 34.6368g, and add the Y of 1wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Figure 11, and the XRD result of Figure 11 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Embodiment 12
Be with the difference of embodiment 8: can generate ZrO 2/ ZrW 2O 8The raw material ZrO of composite 2And WO 3Press ZrO 2And WO 3Target product ZrW 2O 8: ZrO 2Mass ratio (the ZrW of=2:1 2O 85.8690g, ZrO 22.9345g) take by weighing raw material ZrO 24.1668g and WO 34.6368g, and add the Y of 1wt.% 2O 3As additive.The ZrO that forms 2/ ZrW 2O 8The X-ray diffraction material phase analysis that composite is corresponding is seen Figure 12, and the XRD result of Figure 12 shows and formed highly purified ZrO 2/ ZrW 2O 8Composite, its constituent element are α-ZrW 2O 8With m-ZrO 2Phase.
Figure 13 is ZrW 2O 8: ZrO 2The mass ratio of=1:1, and add the Y of 1wt.% 2O 3The composite of additive (embodiment 9) SEM collection of illustrative plates, as seen from Figure 13 ZrO 2And ZrW 2O 8Bi-material evenly distributes in composite.
The thermal expansion curve of the composite of embodiment 1 ~ 3 correspondence is seen Figure 14, and the thermal expansion curve of the composite of embodiment 8 ~ 12 correspondences is seen Figure 15, no matter is not add Y by comparative analysis 2O 3Series is still added Y 2O 3The thermal expansion curve of the different proportion composite that series is prepared can be found out: along with ZrO 2The change ZrO of quality 2/ ZrW 2O 8The thermal expansion of composite can regulation and control.
Table 1 is the performance test data of the composite of corresponding embodiment preparation, as seen from Table 1 along with adding Y 2O 3The increase ZrO of quality 2/ ZrW 2O 8The bulk density of composite significantly increases.
Employed high temperature process furnances is the AY-TF-80-175 type tube furnace that Henan peace enlightening heat product company limited produces among the above embodiment.The material phase analysis that X ' the Pert PRO X-ray diffractometer that adopts Holland to produce carries out composite shows that prepared composite phase is by m-ZrO 2And α-ZrW 2O 8Form, and do not contain other impurity peaks.The JSM-6700F SEM (SEM) that adopts Japan to produce is observed the cross-section morphology of composite.The Lin Saisi thermal dilatometer LINSEIS DIL L76 that adopts Germany to produce has provided the thermal expansion curve of matrix material.Based on Archimedes' principle, the model of Nereid section balance production is the upper utensil type electronic balance of FA1104 in the employing, measures volume density, water-intake rate and void content.

Claims (2)

1. controlled thermal expansion ZrO 2/ ZrW 2O 8The sintering and synthesizing method of composite is characterized in that: with ZrO 2, WO 3Be raw material, according to target product ZrO 2/ ZrW 2O 8ZrO in the composite 2With ZrW 2O 8Chemical quality take by weighing raw material than demand, ground and mixed is even, and is once sintered synthetic and products therefrom is carried out water-cooled get target product directly or behind the compressing tablet; Wherein, sintering parameter is: 1250 ~ 1300 ℃ of temperature, time 1 ~ 3h.
2. controlled thermal expansion ZrO as claimed in claim 1 2/ ZrW 2O 8The sintering and synthesizing method of composite is characterized in that: adding accounts for ZrO in the raw material 2With WO 3The Y of gross weight 0.1 ~ 1% 2O 3
CN2011101589950A 2011-06-14 2011-06-14 Sintering synthesis method of ZrO2/ZrW2O8 composite material with controlled thermal expansion Pending CN102285798A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104557037A (en) * 2014-12-30 2015-04-29 郑州大学 Novel near-zero expansion ceramic and solid-phase sintering synthesis method thereof
CN104844201A (en) * 2015-06-09 2015-08-19 哈尔滨工业大学 Method for preparing zirconium oxide/zirconium tungstate composite material by utilizing crystal form stabilized zirconium oxide as raw material
CN115338414A (en) * 2022-08-22 2022-11-15 西安交通大学 Light Al-ZrW with adjustable thermal expansion coefficient 2 O 8 Method for producing a material

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JP2007091577A (en) * 2005-09-05 2007-04-12 Ohara Inc Inorganic substance powder and composite material using the same

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JP2007091577A (en) * 2005-09-05 2007-04-12 Ohara Inc Inorganic substance powder and composite material using the same
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Title
KLAARTJE DE BUYSSER等: "ZrO2-ZrW2O8 COMPOSITES WITH TAILOR-MADE THERMAL EXPANSION", 《ZRO2-ZRW2O8 COMPOSITES WITH TAILOR-MADE THERMAL EXPANSION》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104557037A (en) * 2014-12-30 2015-04-29 郑州大学 Novel near-zero expansion ceramic and solid-phase sintering synthesis method thereof
CN104844201A (en) * 2015-06-09 2015-08-19 哈尔滨工业大学 Method for preparing zirconium oxide/zirconium tungstate composite material by utilizing crystal form stabilized zirconium oxide as raw material
CN115338414A (en) * 2022-08-22 2022-11-15 西安交通大学 Light Al-ZrW with adjustable thermal expansion coefficient 2 O 8 Method for producing a material
CN115338414B (en) * 2022-08-22 2023-12-19 西安交通大学 Light Al-ZrW with adjustable thermal expansion coefficient 2 O 8 Method for producing materials

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Application publication date: 20111221