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 PDFInfo
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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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- thermal expansion
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- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 238000005245 sintering Methods 0.000 title claims abstract description 41
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title abstract description 8
- 238000001308 synthesis method Methods 0.000 title abstract 2
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 13
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000919 ceramic Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 30
- 239000012071 phase Substances 0.000 description 30
- 239000000047 product Substances 0.000 description 16
- 238000004458 analytical method Methods 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 239000000470 constituent Substances 0.000 description 12
- 239000000654 additive Substances 0.000 description 9
- 230000000996 additive effect Effects 0.000 description 9
- 238000010792 warming Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 108010022579 ATP dependent 26S protease Proteins 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明属于无机非金属材料领域，公开了一种可控热膨胀ZrO2/ZrW2O8复合材料的烧结合成方法。以ZrO2、WO3为原料，按目标产物ZrO2/ZrW2O8复合材料中ZrO2与ZrW2O8的化学质量比需求称取原料，研磨混合均匀，直接或压片后一次烧结合成并将所得产物进行水冷得目标产物。本发明采用高温快速烧结技术来制备可控热膨胀ZrO2/ZrW2O8复合材料，同时选用ZrO2、WO3和Y2O3为原料，通过原位合成法将第二相ZrW2O8颗粒引入到陶瓷基体ZrO2中，使其呈均匀弥散分布并达到低膨胀性能的复相陶瓷，避免了ZrO2和ZrW2O8界面污染，同时本发明可一次烧结完成，在高温下原料反应非常充分，制备过程简单，烧结速度快，时间短，第二相分散容易。The invention belongs to the field of inorganic non-metallic materials and discloses a sintering synthesis method of a ZrO 2 /ZrW 2 O 8 composite material with controllable thermal expansion. Using ZrO 2 and WO 3 as raw materials, weigh the raw materials according to the chemical mass ratio requirements of ZrO 2 and ZrW 2 O 8 in the target product ZrO 2 /ZrW 2 O 8 composite material, grind and mix them evenly, and sinter together directly or after tableting And the resulting product is water-cooled to obtain the target product. The present invention adopts high-temperature rapid sintering technology to prepare ZrO 2 /ZrW 2 O 8 composite material with controllable thermal expansion . Particles are introduced into the ceramic matrix ZrO2 to make it uniformly dispersed and low-expansion multiphase ceramics, avoiding ZrO2 and ZrW2O8 interface pollution, and the invention can be sintered once, and the raw materials react at high temperature It is very full, the preparation process is simple, the sintering speed is fast, the time is short, and the second phase is easily dispersed.
Description
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
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Cited By (3)
| 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 | A preparation method of light-weight Al-ZrW2O8 material with adjustable thermal expansion coefficient |
Citations (2)
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|---|---|---|---|---|
| CN1911860A (en) * | 2006-09-05 | 2007-02-14 | 电子科技大学 | Preparation method of low temperature sintered electron ceramic material |
| JP2007091577A (en) * | 2005-09-05 | 2007-04-12 | Ohara Inc | Inorganic substance powder and composite material using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007091577A (en) * | 2005-09-05 | 2007-04-12 | Ohara Inc | Inorganic substance powder and composite material using the same |
| CN1911860A (en) * | 2006-09-05 | 2007-02-14 | 电子科技大学 | Preparation method of low temperature sintered electron ceramic material |
Non-Patent Citations (1)
| Title |
|---|
| KLAARTJE DE BUYSSER等: "ZrO2-ZrW2O8 COMPOSITES WITH TAILOR-MADE THERMAL EXPANSION", 《ZRO2-ZRW2O8 COMPOSITES WITH TAILOR-MADE THERMAL EXPANSION》 * |
Cited By (4)
| 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 | A preparation method of light-weight Al-ZrW2O8 material with adjustable thermal expansion coefficient |
| 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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