CN109336585A - The method of porous ZnO ceramics is produced under a kind of low temperature - Google Patents
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Abstract
The method of porous ZnO ceramics is produced under a kind of low temperature disclosed by the invention, comprising the following steps: step 1 prepares Al-Zn single phase solid solution with Al ingot and Zn ingot；The Al-Zn single phase solid solution is placed in NaOH solution and corrodes by step 2, obtains porous Zn；The porous Zn is placed in drying in drying box by step 3；Step 4 aoxidizes the porous Zn after the step 3 is dry at low temperature to get ceramic to porous ZnO；Solve the problems, such as that sintering temperature present in current large scale ZnO Production of Ceramics is high, sintering time is long.
Description
Technical field
The invention belongs to ZnO ceramic production methods technical fields, and in particular to production porous ZnO ceramics under a kind of low temperature
Method.
Background technique
In the production process of current big size porous ZnO ceramics, usually using ZnO powder as raw material, process is various
Technique is processed into the porous ZnO precast body made of ZnO powder.Since porous ZnO precast body is piled up by ZnO powder,
Because the binding force between ZnO powder belongs to Van der Waals force, the binding force is weak, causes the bond strength between ZnO powder not high.
In order to enable the porous ZnO finally obtained has preferable mechanical property, it is necessary to be burnt to the precast body made of ZnO powder
Knot improves the binding force between powder so that a ZnO powder time realizes that atom bond is closed, so that precast body becomes tool
There are high-intensitive porous ZnO ceramics.Because ZnO belongs to ceramic material, to realize, atom bond is closed between ceramic powder, it is necessary to be given
Atom between powder interface provides enough energy, thus sintering temperature is usually very high, generally at 1100 DEG C or more, has
Point is even higher.High temperature is sintered that more stringent requirements are proposed to agglomerating plant for a long time, and it is high in this way at a temperature of it is long when
Between sintering will according at the energy a large amount of consumption.In addition, the specific surface of the ceramics after high temperature sintering is low, porous ZnO ceramics are answered
With having an adverse effect, (ZnO ceramics are made porous material and are just desirable to realize the acquisition of high-ratio surface, and high temperature is detrimental to high ratio
Surface ceramic is produced).Therefore it explores and realizes big size porous ZnO in low temperature (such as low as 300 DEG C or lower temperature)
The preparation of ceramics is influenced by the preparation on porous ceramics and using subversiveness is generated.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that porous ZnO ceramics are produced under low temperature, solve current large scale
The problem that sintering temperature present in ZnO Production of Ceramics is high, sintering time is long.
Technical solution used by the method for porous ZnO ceramics is produced under a kind of low temperature of the present invention, comprising the following steps:
Step 1 prepares Al-Zn single phase solid solution with Al ingot and Zn ingot:
The Al-Zn single phase solid solution is placed in NaOH solution and corrodes by step 2, obtains porous Zn；
The porous Zn is placed in drying in drying box by step 3；
Step 4 aoxidizes the porous Zn after the step 3 is dry at low temperature to get ceramic to porous ZnO.
The features of the present invention also characterized in that
Al ingot and Zn ingot are smelted into the Zn-Al alloy melt that Zn content is 30~80% by step 1.1；
Step 1.2, by the Zn-Al alloy melt, directly Al-Zn single phase solid solution is quenched into casting in the liquid state；
The purity of Al ingot and Zn ingot is not less than 99.9% in step 1.1.
Coolant liquid is water or salt water when casting is quenched in step 1.2, or is quickly cooled down using the method for single rolling or double rollings.
The concentration of NaOH solution is 0.1~5moL/L when corroding in step 2, in NaOH solution and Al-Zn single phase solid solution
The ratio between molal weight of Al is 1.2:1~5:1, and the corrosion temperature of NaOH solution is 0 DEG C~35 DEG C, and etching time is 10~20h.
The temperature of drying box is 100~120 DEG C in step 3, and drying time is 2~3h.
It is to aoxidize 2~4h, Huo Zhe at 300~550 DEG C in oxygen containing oxidizing atmosphere in step 4 when low-temperature oxidation
3~10h is aoxidized in the NaOH solution of low concentration at a temperature of 0~30 DEG C.
Oxygen containing oxidizing atmosphere is in air or pure oxygen, and the concentration of the NaOH solution of low concentration is 0.1~2mol/L.
The beneficial effects of the present invention are: the method for producing porous ZnO ceramics under a kind of low temperature of the invention, utilizes the present invention
The preparation method of offer, being able to achieve under lower temperature production has macroscopical large scale, very high specific surface area and high more of intensity
Hole ZnO ceramics, the production for solving big size porous ZnO at present have to pass through up to 1100~1300 DEG C of temperature long-time (greatly
In 2h) long-time heat preservation and caused by sintering temperature, sintering time be long, waste mass energy and the porous ZnO specific surface obtained
The problems such as product is low.
Specific embodiment
The present invention is described in detail With reference to embodiment.
The method of porous ZnO ceramics is produced under a kind of low temperature of the present invention, comprising the following steps:
Step 1 prepares Al-Zn single phase solid solution with Al ingot and Zn ingot, configures the specific steps of Al-Zn single phase solid solution
Are as follows:
Al ingot and Zn ingot are smelted into Zn content according to the requirement of Al, Zn alloy melting as 30~80% by step 1.1
Zn-Al alloy melt, wherein the purity of Al ingot and Zn ingot is not less than 99.9%；
Step 1.2, by Zn-Al alloy melt, directly Al-Zn single phase solid solution is quenched into casting in the liquid state, wherein casting is cold when quenching
But liquid is any one in water or salt water, or is quickly cooled down using the method for single rolling or double rollings；
Al-Zn single phase solid solution is placed in NaOH solution and corrodes by step 2, obtains porous Zn, wherein NaOH solution is dense
Degree is 0.1~5moL/L, and the ratio between Al ingot molal weight is 1.2:1~5:1, NaOH in NaOH solution and Al-Zn single phase solid solution
The corrosion temperature of solution is 0 DEG C~35 DEG C, and etching time is 10~20h；
Porous Zn is placed in drying box under the conditions of 100~120 DEG C dry 2~3h by step 3；
Step 4 aoxidizes the porous Zn after step 3 is dry at low temperature, is in oxygen containing oxidisability when low-temperature oxidation
Atmosphere aoxidizes 2~4h at 300~550 DEG C, or aoxidizes 3~10h at a temperature of 0~30 DEG C in the NaOH solution of low concentration,
Wherein oxygen containing oxidizing atmosphere is air or pure oxygen, and the concentration of the NaOH solution of low concentration is 0.1~2mol/L to get arriving
Porous ZnO ceramics.
Embodiment 1
Step 1, the Al ingot purity greater than 99.9% and Zn ingot are smelted into Zn content according to the requirement of Al, Zn alloy melting
The Zn-Al alloy melt that (mass percent) is 30%, then directly macroscopical large scale is quenched into casting to the alloy melt in the liquid state
Al-Zn single phase solid solution, casting is quenched cooling using NaCl solution, and single-phase Zn-Al single phase solid solution after cooling can be by each
The method of kind machining is processed into the blank of required size and shape；
Step 2 corrodes the large-sized Al-Zn solid solution of processing acquisition macroscopic view in NaOH solution, removes Al therein,
Just the porous Zn with large scale, very high specific surface area is obtained；Wherein the concentration of NaOH solution is 0.1moL/L, NaOH solution
It is 5:1 with the ratio between molal weight of Al in Al-Zn single phase solid solution, the corrosion temperature of corrosive liquid is 0 DEG C, etching time 20h；
Step 3, the porous Zn that corrosion is obtained dry 3h under the conditions of 100 DEG C in drying box, after just being dried
With large scale, the porous Zn of very high specific surface area；
Step 4 aoxidizes the porous Zn after drying at 300 DEG C in oxygen containing oxidizing atmosphere (in such as air or pure oxygen)
4h is oxidized to the large-sized porous ZnO of macroscopic view, just obtains final having large scale, very high specific surface area and intensity high
Porous ZnO ceramics.
Embodiment 2
Step 1, the Al ingot purity greater than 99.9% and Zn ingot are smelted into Zn content according to the requirement of Al, Zn alloy melting
The Zn-Al alloy melt that (mass percent) is 80%, then directly macroscopical large scale is quenched into casting to the alloy melt in the liquid state
Al-Zn single phase solid solution, casting is quenched cooling using NaCl solution；Needed for single-phase Zn-Al single phase solid solution after cooling is processed into
The blank of size and shape；
Step 2 corrodes the large-sized Al-Zn solid solution of processing acquisition macroscopic view in NaOH solution, removes Al therein,
Just the porous Zn with large scale, very high specific surface area is obtained；Wherein the concentration of NaOH solution is 0.1moL/L, NaOH solution
It is 1.2:1 with the ratio between molal weight of Al in Al-Zn single phase solid solution, the corrosion temperature of corrosive liquid is 20 DEG C, and etching time is
10h；
Step 3, the porous Zn that corrosion is obtained dry 2h under the conditions of 120 DEG C in drying box, after just being dried
With large scale, the porous Zn of very high specific surface area；
Porous Zn after drying is aoxidized 10h in 0 DEG C at a temperature of in the NaOH solution of 0.1mol/L by step 4, is oxidized to
The large-sized porous ZnO of macroscopic view just obtains final with large scale, very high specific surface area and the high porous ZnO pottery of intensity
Porcelain.
Embodiment 3
Step 1, the Al ingot purity greater than 99.9% and Zn ingot are smelted into Zn content according to the requirement of Al, Zn alloy melting
The Zn-Al alloy melt that (mass percent) is 50%, then directly macroscopical large scale is quenched into casting to the alloy melt in the liquid state
Al-Zn single phase solid solution, casting is quenched cooling using KCl solution, and single-phase Zn-Al single phase solid solution after cooling passes through machining
Method be processed into the blanks of required size and shape；
Step 2 corrodes the large-sized Al-Zn solid solution of processing acquisition macroscopic view in NaOH solution, removes Al therein,
Just the porous Zn with large scale, very high specific surface area is obtained；Wherein the concentration of NaOH solution is 1moL/L, NaOH solution with
The ratio between molal weight of Al is 2:1 in Al-Zn single phase solid solution, and the corrosion temperature of corrosive liquid is 35 DEG C, etching time 15h；
Step 3, the porous Zn that corrosion is obtained dry 2.5h under the conditions of 110 DEG C in drying box, after just being dried
Have large scale, the porous Zn of very high specific surface area；
Step 4 aoxidizes the porous Zn after drying at 550 DEG C in oxygen containing oxidizing atmosphere (in such as air or pure oxygen)
2h is oxidized to the large-sized porous ZnO of macroscopic view, just obtains final having large scale, very high specific surface area and intensity high
Porous ZnO ceramics.
Embodiment 4
Step 1, the Al ingot purity greater than 99.9% and Zn ingot are smelted into Zn content according to the requirement of Al, Zn alloy melting
The Zn-Al alloy melt that (mass percent) is 65%, then directly macroscopical large scale is quenched into casting to the alloy melt in the liquid state
Al-Zn single phase solid solution, casting is quenched cooling using NaCl solution；Single-phase Zn-Al single phase solid solution after cooling can be by each
The method of kind machining is processed into the blank of required size and shape；
Step 2 corrodes the large-sized Al-Zn solid solution of processing acquisition macroscopic view in NaOH solution, removes Al therein,
Just the porous Zn with large scale, very high specific surface area is obtained；Wherein the concentration of NaOH solution is 2moL/L, NaO solution with
The ratio between molal weight of Al is 2:1 in Al-Zn single phase solid solution, and the corrosion temperature of corrosive liquid is 20 DEG C, etching time 13h；
Step 3, the porous Zn that corrosion is obtained dry 2h under the conditions of 120 DEG C in drying box, after just being dried
With large scale, the porous Zn of very high specific surface area；
Porous Zn after drying is aoxidized 3h in 0 DEG C at a temperature of in the NaOH solution of 2mol/L by step 4, is oxidized to macro
Large-sized porous ZnO is seen, is just obtained final with large scale, very high specific surface area and the high porous ZnO ceramics of intensity.
Embodiment 5
Step 1, the Al ingot purity greater than 99.9% and Zn ingot are smelted into Zn content according to the requirement of Al, Zn alloy melting
The Zn-Al alloy melt that (mass percent) is 40%, then directly macroscopical large scale is quenched into casting to the alloy melt in the liquid state
Al-Zn single phase solid solution, casting is quenched cooling using NaCl solution, and single-phase Zn-Al single phase solid solution after cooling passes through various machines
The method of tool processing is processed into the blank of required size and shape；
Step 2 corrodes the large-sized Al-Zn solid solution of processing acquisition macroscopic view in NaOH solution, removes Al therein,
Just the porous Zn with large scale, very high specific surface area is obtained；Wherein the concentration of NaOH solution is 5moL/L, NaOH solution with
The ratio between molal weight of Al is 4:1 in Al-Zn single phase solid solution, and the corrosion temperature of corrosive liquid is 25 DEG C, etching time 12h；
Step 3, the porous Zn that corrosion is obtained dry 3h under the conditions of 100 DEG C in drying box, after just being dried
With large scale, the porous Zn of very high specific surface area；
Porous Zn after drying is aoxidized 3.5h at 450 DEG C in air by step 4, and it is large-sized porous to be oxidized to macroscopic view
ZnO is just obtained final with large scale, very high specific surface area and the high porous ZnO ceramics of intensity.
The porous ZnO ceramics of the method that porous ZnO ceramics are produced under a kind of low temperature of the invention, production have following spy
Sign:
Feature 1, may be implemented with this method macroscopical arbitrary shape and size big size porous ZnO ceramics production, should
The size and shape of the large-sized porous ZnO of macroscopic view replicate the Zn-Al single-phase alloy obtained after casting is quenched by machining completely
The shape and size of solid solution because Zn-Al alloy solid solution physical efficiency by mach method be worth any required shape with
Size, therefore this method just can produce the porous ZnO ceramics with any required shape and size；
Feature 2, the big size porous ZnO ceramics that can realize macroscopical arbitrary shape and size at low temperature with this method
Production can realize that macroscopic view is any required in oxidizing atmosphere (such as air or pure oxygen) at 300~550 DEG C at temperature
The production of the big size porous ZnO of shape and size；And in NaOH solution, it can realize that macroscopic view is appointed at a temperature of 0~30 DEG C
The production of the big size porous ZnO ceramics of shape and size needed for meaning；
Feature 3 has finely with this method macroscopical arbitrary shape produced and the big size porous ZnO ceramics of size
Nanostructure: the skeleton of porous ZnO is the nano-ZnO thin slice of nano-scale degree, thus the macroscopic view any required shape and ruler
Very little big size porous ZnO ceramics have very high specific surface area, can be up to 60m2/ g is even higher；
Feature 4 has well with this method macroscopical arbitrary shape produced and the big size porous ZnO ceramics of size
Mechanical property: its bending strength is up to 30MPa or more；Moreover, intensity will continue to mention with the reduction of porosity in porous ZnO
It rises.
By the above-mentioned means, the method for producing porous ZnO ceramics under a kind of low temperature of the present invention, it is more to solve current large scale
The production of hole ZnO ceramics has to pass through up to 1100~1300 DEG C of temperature and long-time heat preservation, and caused by sintering temperature it is high,
The problems such as sintering time length, low waste mass energy and the porous ZnO specific surface area of acquisition, the present invention provides one kind to be able to achieve
Macroscopic view is arbitrarily large-sized, has high surface area (up to 60m2/ g) and high-intensitive (bending strength is up to 30MPa) porous ZnO
The production method of ceramics.
Claims (8)
1. producing the method for porous ZnO ceramics under a kind of low temperature of the present invention, which comprises the following steps:
Step 1 prepares Al-Zn single phase solid solution with Al ingot and Zn ingot:
The Al-Zn single phase solid solution is placed in NaOH solution and corrodes by step 2, obtains porous Zn；
The porous Zn is placed in drying in drying box by step 3；
Step 4 aoxidizes the porous Zn after the step 3 is dry at low temperature to get ceramic to porous ZnO.
2. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 1, which is characterized in that the step 1
The specific steps of middle configuration Al-Zn single phase solid solution are as follows:
Al ingot and Zn ingot are smelted into the Zn-Al alloy melt that Zn content is 30~80% by step 1.1；
Step 1.2, by the Zn-Al alloy melt, directly Al-Zn single phase solid solution is quenched into casting in the liquid state.
3. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 2, which is characterized in that the step
The purity of Al ingot and Zn ingot is not less than 99.9% in 1.1.
4. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 2, which is characterized in that the step
Coolant liquid is any one in water or salt water when casting is quenched in 1.2, or is quickly cooled down using the method for single rolling or double rollings.
5. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 1, which is characterized in that the step 2
The concentration of NaOH solution is 0.1~5moL/L when middle corrosion, in NaOH solution and Al-Zn single phase solid solution the molal weight of Al it
Than being 0 DEG C~35 DEG C for the corrosion temperature of 1.2:1~5:1, NaOH solution, etching time is 10~20h.
6. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 1, which is characterized in that the step 3
The temperature of middle drying box is 100~120 DEG C, and drying time is 2~3h.
7. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 1, which is characterized in that the step 4
It is to aoxidize 2~4h at 300~550 DEG C in oxygen containing oxidizing atmosphere when middle low-temperature oxidation, or it is molten in the NaOH of low concentration
3~10h is aoxidized in liquid at a temperature of 0~30 DEG C.
8. producing the method for porous ZnO ceramics under a kind of low temperature according to claim 7, which is characterized in that described oxygen-containing
Oxidizing atmosphere be air or pure oxygen, the concentration of the NaOH solution of the low concentration is 0.1~2mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018565A (en) * | 2019-12-27 | 2020-04-17 | 苏州尼普环境科技有限公司 | Rod-shaped ZnO piezoelectric catalytic porous ceramic material, and method and application thereof |
| CN112877764A (en) * | 2021-01-11 | 2021-06-01 | 西安理工大学 | Method for preparing macroscopic-size porous ZnO by electrochemical corrosion |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602982A (en) * | 2012-03-14 | 2012-07-25 | 西安理工大学 | Method for preparing porous ZnO by means of combining dealloying method with ceramic coating |
| CN104528803A (en) * | 2014-12-24 | 2015-04-22 | 西安理工大学 | Preparation method of ZnO flaky porous nanometer material |
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2018
- 2018-11-29 CN CN201811447440.6A patent/CN109336585A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602982A (en) * | 2012-03-14 | 2012-07-25 | 西安理工大学 | Method for preparing porous ZnO by means of combining dealloying method with ceramic coating |
| CN104528803A (en) * | 2014-12-24 | 2015-04-22 | 西安理工大学 | Preparation method of ZnO flaky porous nanometer material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018565A (en) * | 2019-12-27 | 2020-04-17 | 苏州尼普环境科技有限公司 | Rod-shaped ZnO piezoelectric catalytic porous ceramic material, and method and application thereof |
| CN112877764A (en) * | 2021-01-11 | 2021-06-01 | 西安理工大学 | Method for preparing macroscopic-size porous ZnO by electrochemical corrosion |
| CN112877764B (en) * | 2021-01-11 | 2022-04-22 | 西安理工大学 | Method for preparing macroscopic-size porous ZnO by electrochemical corrosion |
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