CN109437898A - A kind of preparation process of negative thermal expansion material tungsten wire array - Google Patents

A kind of preparation process of negative thermal expansion material tungsten wire array Download PDF

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Publication number
CN109437898A
CN109437898A CN201811544350.9A CN201811544350A CN109437898A CN 109437898 A CN109437898 A CN 109437898A CN 201811544350 A CN201811544350 A CN 201811544350A CN 109437898 A CN109437898 A CN 109437898A
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tungsten wire
wire array
briquet
sintered
thermal expansion
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罗秋玲
刘国强
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ANHUI SHENGHONG ELECTRONIC Co Ltd
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ANHUI SHENGHONG ELECTRONIC Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3258—Tungsten oxides, tungstates, or oxide-forming salts thereof
    • C04B2235/326—Tungstates, e.g. scheelite

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  • Chemical & Material Sciences (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention provides a kind of preparation process of negative thermal expansion material tungsten wire array, is related to field of material synthesis technology, comprising the following steps: 1) weigh ZrO in molar ratio2Powder and WO3Powder mixes the two, and mixed material and distilled water are added in ball mill and carry out wet ball grinding；2) mixture paste is taken out, dries, is sintered 2h under the conditions of 600-800 DEG C；3) sintered material is cooling, and grinding is pressed into briquet；4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1150-1200 DEG C, sintering time 2h；5) quenching device will be quickly put by the sintered saggar of step 4), quenching device is cooled down quenching using the mode of spray liquid nitrogen；6) briquet after quenching is cooled to room temperature, obtains product tungsten wire array briquet；7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder, which simplifies the conventional solid synthesis technology being repeatedly sintered repeatedly, the tungsten wire array purity is high of synthesis.

Description

A kind of preparation process of negative thermal expansion material tungsten wire array
Technical field
The present invention relates to field of material synthesis technology, and in particular to a kind of preparation process of negative thermal expansion material tungsten wire array.
Background technique
In recent years, it in some high-technology fields, needs to use minus thermal-expansion coefficient.Minus thermal-expansion coefficient Thermal expansion coefficient is negative value, that is, has the raising with temperature and the characteristic shunk, wolframic acid zirconia material be not only to have it is corrosion-resistant, it is resistance to High temperature, the properties such as heat transfer, while it is also a kind of negative thermal expansion coefficient material, and in 0.3-1050K temperature range, tungsten wire array tool There is very strong isotropic negative expansion effect, do not absorb water without phase-change, negative expansion coefficient is α=- 9 × 10-6/K.Tungsten Sour zirconium price is relatively cheap, has a extensive future, and is the hot spot of research.
But the preparation of tungsten wire array always exists some difficulties, is primarily due in its preparation process, only at 1105-1231 DEG C Thermodynamically stable within the scope of very narrow temperature, temperature is excessively high, will form ZrO2-WO3Amorphous glass state, in temperature-fall period, Between 780-1105 DEG C, tungsten wire array can resolve into ZrO2And WO3.Therefore, in order to keep tungsten wire array stable crystal form, it is necessary to quickly Resolver is skipped, by product quenching, thus the preparation process of caused tungsten wire array is extremely complex.
The preparation method of tungsten wire array has: solid phase method, coprecipitation, sol-gal process, hydro-thermal method, combustion method, microwave synthesis Method and spray drying process.For industrial angle, solid phase method is most simple, inexpensive, of low pollution conventional method, but It is the synthesis temperature narrow range due to tungsten wire array, the features such as the vaporization at high temperature of low-temperature decomposition and tungsten oxide, causes conventional solid When method synthesizes tungsten wire array, obtained product purity is lower.And other several preparation methods can also have preparation condition harshness, preparation It is at high cost, have the shortcomings that waste gas and waste liquid discharge.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of preparation processes of negative thermal expansion material tungsten wire array, solve Conventional solid-state method there are the problem of, preparation process is more simple and environmentally-friendly, save the cost, and the tungsten wire array product purity being prepared is more It is high.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of preparation process of negative thermal expansion material tungsten wire array, comprising the following steps:
1) ZrO is weighed respectively for 1:1.8-2.4 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, Mixed material and distilled water are added in ball mill and carry out wet ball grinding, obtains mixture paste；
2) mixture paste is taken out, dries, material after drying is sintered 2h under the conditions of 600-800 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1150-1200 DEG C, and sintering time is 2h opens rapidly fire door and releases saggar after the completion of sintering；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device uses the mode for spraying liquid nitrogen Cool down quenching；
6) it is cooled to room temperature after the briquet after step 5) quenching being skipped decomposition temperature section, obtains product tungsten wire array Briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
Preferred: mixed material and distilled water mass ratio are 1:1-2.5 in step 1), and the wet ball grinding time is 3-6h.
Preferred: drying temperature is 90-110 DEG C in step 2), drying time 10-12h.
Preferred: sintering temperature is 680-740 DEG C in step 2), and sintering temperature is 1170-1190 DEG C in step 4).
It is preferred: when saggar being released pushed bat kiln in step 4), point of the intracorporal temperature of ejection plate kiln not less than tungsten wire array Solve temperature.
It is preferred: using the natural type of cooling to room temperature in step 6).
(3) beneficial effect
The present invention provides a kind of preparation process of negative thermal expansion material tungsten wire array, the tradition being repeatedly sintered repeatedly is simplified Process for solid phase synthesis only needs two-step sintering, opens fire door after the completion of sintering rapidly and releases saggar, quick joining quenching device, contracting Short During Quenching can more rapidly cool down compared to quenchings mode, liquid nitrogen such as water, ice, and environment friendly and pollution-free, skip tungsten rapidly Sour zirconium decomposition temperature section, stable crystal form, the tungsten wire array purity is high of synthesis.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention, Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of preparation process of negative thermal expansion material tungsten wire array, comprising the following steps:
1) ZrO is weighed respectively for 1:1.8 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, will mix It closes material and distilled water 1:1 in mass ratio is added to progress wet ball grinding 4h in ball mill, obtain mixture paste；
2) mixture paste is taken out, dries, drying temperature is 110 DEG C, and drying time 11h exists material after drying 2h is sintered under the conditions of 600 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1150 DEG C, sintering time 2h, is burnt Fire door is opened after the completion of knot rapidly and releases saggar, when saggar is released pushed bat kiln, the intracorporal temperature of ejection plate kiln is not less than wolframic acid The decomposition temperature of zirconium；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device uses the mode for spraying liquid nitrogen Cool down quenching；
6) it keeps stable crystal form water cooling to room temperature after the briquet after step 5) quenching being skipped decomposition temperature section, obtains To product tungsten wire array briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
Embodiment 2:
A kind of preparation process of negative thermal expansion material tungsten wire array, comprising the following steps:
1) ZrO is weighed respectively for 1:2.2 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, will mix It closes material and distilled water 1:2 in mass ratio is added to progress wet ball grinding 5h in ball mill, obtain mixture paste；
2) mixture paste is taken out, dries, drying temperature is 95 DEG C, and drying time 12h exists material after drying 2h is sintered under the conditions of 680 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1200 DEG C, sintering time 2h, is burnt Fire door is opened after the completion of knot rapidly and releases saggar, when saggar is released pushed bat kiln, the intracorporal temperature of ejection plate kiln is not less than wolframic acid The decomposition temperature of zirconium；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device uses the mode for spraying liquid nitrogen Cool down quenching；
6) stable crystal form is kept to naturally cool to room after the briquet after step 5) quenching being skipped decomposition temperature section Temperature obtains product tungsten wire array briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
Embodiment 3:
A kind of preparation process of negative thermal expansion material tungsten wire array, comprising the following steps:
1) ZrO is weighed respectively for 1:2 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, will mix Material and distilled water 1:1.5 in mass ratio are added to progress wet ball grinding 3h in ball mill, obtain mixture paste；
2) mixture paste is taken out, dries, drying temperature is 100 DEG C, and drying time 10h exists material after drying 2h is sintered under the conditions of 800 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1180 DEG C, sintering time 2h, is burnt Fire door is opened after the completion of knot rapidly and releases saggar, when saggar is released pushed bat kiln, the intracorporal temperature of ejection plate kiln is not less than wolframic acid The decomposition temperature of zirconium；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device uses the mode for spraying liquid nitrogen Cool down quenching；
6) it keeps stable crystal form air-cooled to room temperature after the briquet after step 5) quenching being skipped decomposition temperature section, obtains To product tungsten wire array briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
Embodiment 4:
A kind of preparation process of negative thermal expansion material tungsten wire array, comprising the following steps:
1) ZrO is weighed respectively for 1.:2.4 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, will mix It closes material and distilled water 1:2.5 in mass ratio is added to progress wet ball grinding 6h in ball mill, obtain mixture paste；
2) mixture paste is taken out, dries, drying temperature is 90 DEG C, and drying time 11h exists material after drying 2h is sintered under the conditions of 700 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1170 DEG C, sintering time 2h, is burnt Fire door is opened after the completion of knot rapidly and releases saggar, when saggar is released pushed bat kiln, the intracorporal temperature of ejection plate kiln is not less than wolframic acid The decomposition temperature of zirconium；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device uses the mode for spraying liquid nitrogen Cool down quenching；
6) stable crystal form is kept to naturally cool to room after the briquet after step 5) quenching being skipped decomposition temperature section Temperature obtains product tungsten wire array briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
Embodiment 5:
A kind of preparation process of negative thermal expansion material tungsten wire array, comprising the following steps:
1) ZrO is weighed respectively for 1:2.1 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, will mix It closes material and distilled water 1:2 in mass ratio is added to progress wet ball grinding 4.5h in ball mill, obtain mixture paste；
2) mixture paste is taken out, dries, drying temperature is 105 DEG C, and drying time 10h exists material after drying 2h is sintered under the conditions of 740 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar is sequentially entered in pushed bat kiln and is sintered, sintering temperature is 1190 DEG C, sintering time 2h, is burnt Fire door is opened after the completion of knot rapidly and releases saggar, when saggar is released pushed bat kiln, the intracorporal temperature of ejection plate kiln is not less than wolframic acid The decomposition temperature of zirconium；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device uses the mode for spraying liquid nitrogen Cool down quenching；
6) stable crystal form is kept to naturally cool to room after the briquet after step 5) quenching being skipped decomposition temperature section Temperature obtains product tungsten wire array briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
The ZrW that 1-5 of the embodiment of the present invention is prepared2O8Powder carries out XRD Quantitative Phase Analysis to detect ZrW2O8's Purity, the results are shown in Table 1:
Table 1:
Number ZrW2O8(%wt)
Embodiment 1 94.5
Embodiment 2 97.6
Embodiment 3 94.1
Embodiment 4 96.2
Embodiment 5 96.8
To sum up, the embodiment of the present invention has the following beneficial effects: ZrW made from 1-5 of the embodiment of the present invention2O8Purity all exists 94% or more, especially when the type of cooling is natural cooling, obtained ZrW2O8Purity it is higher and preparation process is simple, ring It protects pollution-free.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.

Claims (6)

1. a kind of preparation process of negative thermal expansion material tungsten wire array, which comprises the following steps:
1) ZrO is weighed respectively for 1:1.8-2.4 in molar ratio2Powder and WO3Powder mixes the two, obtains mixed material, will mix It closes material and distilled water is added in ball mill and carries out wet ball grinding, obtain mixture paste；
2) mixture paste is taken out, dries, material after drying is sintered 2h under the conditions of 600-800 DEG C；
3) will be cooling by the sintered material of step 2), grinding is pressed into briquet；
4) briquet merging saggar sequentially being entered in pushed bat kiln and is sintered, sintering temperature is 1150-1200 DEG C, sintering time 2h, Fire door is opened after the completion of sintering rapidly and releases saggar；
5) quenching device will be quickly put by the sintered saggar of step 4), quenching device is cooled down using the mode of spray liquid nitrogen Quenching；
6) it after the briquet after step 5) quenching being skipped decomposition temperature section, keeps crystal form to be cooled to room temperature, obtains product Tungsten wire array briquet；
7) obtained tungsten wire array briquet ball mill grinding is obtained into final product zirconium tungstate powder.
2. the preparation process of negative thermal expansion material tungsten wire array as described in claim 1, which is characterized in that mixture in step 1) Material and distilled water mass ratio are 1:1-2.5, and the wet ball grinding time is 3-6h.
3. the preparation process of negative thermal expansion material tungsten wire array as described in claim 1, which is characterized in that drying temperature in step 2) Degree is 90-110 DEG C, drying time 10-12h.
4. the preparation process of negative thermal expansion material tungsten wire array as described in claim 1, which is characterized in that sintering temperature in step 2) Degree is 680-740 DEG C, and sintering temperature is 1170-1190 DEG C in step 4).
5. the preparation process of negative thermal expansion material tungsten wire array as described in claim 1, which is characterized in that by saggar in step 4) When releasing pushed bat kiln, the intracorporal temperature of ejection plate kiln is not less than the decomposition temperature of tungsten wire array.
6. the preparation process of negative thermal expansion material tungsten wire array as described in claim 1, which is characterized in that using certainly in step 6) Right cold mode is but to room temperature.
CN201811544350.9A 2018-12-17 2018-12-17 A kind of preparation process of negative thermal expansion material tungsten wire array Pending CN109437898A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110128138A (en) * 2019-05-22 2019-08-16 无锡必创传感科技有限公司 The preparation method and fiber grating temperature compensator of ceramic substrate
CN111847515A (en) * 2020-06-30 2020-10-30 福建工程学院 Preparation method of zirconium tungstate
CN112299846A (en) * 2020-11-16 2021-02-02 郑州大学 Negative thermal expansion ceramic Ta2W2O11And solid phase sintering synthesis method thereof
CN112441618A (en) * 2020-12-14 2021-03-05 苏州锦艺新材料科技有限公司 Preparation method of zirconium tungstate powder
CN114031118A (en) * 2021-12-20 2022-02-11 哈尔滨工业大学 Preparation method of high-purity alpha-zirconium tungstate
CN114716247A (en) * 2022-03-21 2022-07-08 合肥精创科技有限公司 High-density zirconium tungstate solid solution ceramic and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王景红: "负热膨胀ZrW2O8粉体制备方法的对比研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *
谭澄宇等: "Cu-ZrW2O8复合镀层的制备", 《中南大学学报（自然科学版）》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110128138A (en) * 2019-05-22 2019-08-16 无锡必创传感科技有限公司 The preparation method and fiber grating temperature compensator of ceramic substrate
CN111847515A (en) * 2020-06-30 2020-10-30 福建工程学院 Preparation method of zirconium tungstate
CN111847515B (en) * 2020-06-30 2022-06-03 福建工程学院 Preparation method of zirconium tungstate
CN112299846A (en) * 2020-11-16 2021-02-02 郑州大学 Negative thermal expansion ceramic Ta2W2O11And solid phase sintering synthesis method thereof
CN112441618A (en) * 2020-12-14 2021-03-05 苏州锦艺新材料科技有限公司 Preparation method of zirconium tungstate powder
CN112441618B (en) * 2020-12-14 2022-01-21 苏州锦艺新材料科技股份有限公司 Preparation method of zirconium tungstate powder
CN114031118A (en) * 2021-12-20 2022-02-11 哈尔滨工业大学 Preparation method of high-purity alpha-zirconium tungstate
CN114716247A (en) * 2022-03-21 2022-07-08 合肥精创科技有限公司 High-density zirconium tungstate solid solution ceramic and preparation method thereof

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