CN105149607A - Preparation method of nano-porous titanium powder or nano-porous nickel powder - Google Patents
Preparation method of nano-porous titanium powder or nano-porous nickel powder Download PDFInfo
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- CN105149607A CN105149607A CN201510589628.4A CN201510589628A CN105149607A CN 105149607 A CN105149607 A CN 105149607A CN 201510589628 A CN201510589628 A CN 201510589628A CN 105149607 A CN105149607 A CN 105149607A
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Abstract
The invention discloses a preparation method of nano-porous titanium powder or nano-porous nickel powder, and relates to a preparation method of a nano-porous powder material, aiming at solving the problems that the existing preparation method of the nano-porous material is relatively complicated and the prepared porous material is relatively small in specific surface area and relatively poor in catalytic performance. The method comprises the following steps: 1, preparation of a precursor: putting Ti(x)Al(y) or Ni(x)Al(y) intermetallic compound powder into acetone, washing by utilizing ultrasonic oscillating, and then carrying out ultrasonic washing in absolute ethyl alcohol, thus obtaining precursor powder with cleaned surface; 2, dealloying: putting the precursor powder into a corrosive liquid to be subjected to chemical dealloying treatment; 3, subsequent treatment: taking out powder after dealloying, repeatedly washing with deionized water, then putting into absolute ethyl alcohol for ultrasonic washing, and putting wet powder into a vacuum drying oven for drying, thus obtaining the nano-porous titanium powder or nano-porous nickel powder. The method disclosed by the invention is used for preparing a nano-porous powdery material.
Description
Technical field
The present invention relates to a kind of preparation method of nanoporous powder body material.
Background technology
Nano-porous materials, since appearance, has had been a great concern because it has many excellent properties.Now prove by experiment nano-porous materials photocatalysis, chemical catalysis, electrode material, activation, sensing, etc. field have huge potential using value, these all give the credit to the pore passage structure of the very big specific area of nano-porous materials and its uniqueness had.And nano porous metal dusty material further increases its surface area due to the pore passage structure of its uniqueness, add and may produce hole confining effect, therefore have very wide application prospect at catalytic field.
Existing nano-porous materials preparation method is more complicated, and the porous material specific area of preparation is less, and catalytic performance is poor.
Summary of the invention
The present invention is that will to solve existing nano-porous materials preparation method more complicated, and the porous material specific area of preparation is less, and the problem that catalytic performance is poor, provides the preparation method of nanoporous titanium valve or nanoporous nickel powder.
The preparation method of nanoporous titanium valve of the present invention or nanoporous nickel powder, carries out according to the following steps:
One, presoma is prepared: by Ti
xal
yor Ni
xal
yintermetallic compound powder puts into acetone, and utilize sonic oscillation to clean 10 ~ 15min, ultrasonic cleaning 5 ~ 10min in absolute ethyl alcohol, obtains the precursor powder of surface cleaning subsequently;
Two, removal alloying: the precursor powder obtained in step one is placed in corrosive liquid, carry out chemical removal alloying process respectively, acid solution or the concentration of corrosive liquid used to be concentration be 0.1 ~ 10mol/L are the alkaline solution of 0.1 ~ 10mol/L, the temperature of removal alloying process is 15 ~ 95 DEG C, and the time of removal alloying process is 5 ~ 720min;
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse by deionized water, rinse 120 ~ 150s altogether, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10 ~ 15min, to remove other residual impurity attachment, the powder under moisture state is put into vacuum drying chamber, dry 5 ~ 8h, can obtain nanoporous titanium valve or nanoporous nickel powder.
The present invention utilizes Ti
xal
y, Ni
xal
yintermetallic compound powder, as presoma, prepares nanoporous titanium valve and nanoporous nickel powder by the method for removal alloying.Titanium valve and the nickel powder with nano-porous structure have very wide application prospect, nanoporous nickel has achieved through engineering approaches application as industrial hydrogenation catalyst, and the nickel powder with nano-porous structure is owing to having larger surface area, therefore catalytic effect is better.Except having excellent catalytic performance, nanoporous titanium valve can also at Surface Creation one deck TiO
2, therefore have huge application potential in photocatalysis field, the field such as sterilization, waste water control can be widely used in.
Principle of the present invention: removal alloying is also named selective corrosion, refer to that each element of component alloy or the potential difference respectively between phase differ larger, by chemistry or electrochemical action, relatively active alloying element is dissolved, and remaining inert element is by the diffusion of atom, from recombination, formed there is nanoscale three-dimensional, continuously, the loose structure of opening.For Ti-Al system alloy, can be determined by inquiry mark electrode potential handbook, the hydrogen mark electromotive force of Al is-2.300V, and in alkaline solution, be-0.882V by calculating the hydrogen mark electromotive force that can draw Ti, between visible Ti and Al two kinds of elements, there is larger electrode potential difference, meet the condition that removal alloying occurs, for Ni-Al system alloy, both standard electrode potential differences are 1.4V, therefore can obtain nanoporous titanium valve and nanoporous nickel powder by the method for chemical removal alloying process.Powder due to surface area larger, can contact fully with corrosive liquid, therefore removal alloying speed is faster.
Beneficial effect of the present invention:
1, compared with traditional noble metal, titanium and nickel all belong to more cheap metal, can effectively reduce costs.
2, compared with nanoporous block materials, nanoporous titanium valve and nickel powder have larger specific area, and therefore catalytic effect is better; Specific area reaches as high as 62m
2/ g, nanoporous powder is put into methyl orange solution and carries out catalysis degeneration experiment, degradation efficiency reaches 82%-89%.
3, preparation process of the present invention is simple, easily-controlled experimental conditions.
The present invention can obtain nanoporous titanium valve and nanoporous nickel powder.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: the preparation method of present embodiment nanoporous titanium valve or nanoporous nickel powder, carry out according to the following steps:
One, presoma is prepared: by Ti
xal
yor Ni
xal
yintermetallic compound powder puts into acetone, and utilize sonic oscillation to clean 10 ~ 15min, ultrasonic cleaning 5 ~ 10min in absolute ethyl alcohol, obtains the precursor powder of surface cleaning subsequently;
Two, removal alloying: the precursor powder obtained in step one is placed in corrosive liquid, carry out chemical removal alloying process respectively, acid solution or the concentration of corrosive liquid used to be concentration be 0.1 ~ 10mol/L are the alkaline solution of 0.1 ~ 10mol/L, the temperature of removal alloying process is 15 ~ 95 DEG C, and the time of removal alloying process is 5 ~ 720min;
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse by deionized water, rinse 120 ~ 150s altogether, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10 ~ 15min, to remove other residual impurity attachment, the powder under moisture state is put into vacuum drying chamber, dry 5 ~ 8h, can obtain nanoporous titanium valve or nanoporous nickel powder.
The object of the invention is to utilize the method for removal alloying to prepare the metal powder material with nanoscale porous, and study different alloying components, phase composition, Arrays Aluminum Films in Acid Solution and concentration, the conditions such as the temperature and time of removal alloying on the impact of the structure of final nanoporous titanium valve or nickel powder, thus improve the specific area of this bi-material further.The present invention is applicable to prepare the titanium valve and nickel powder with nanoscale porous.
Detailed description of the invention two: present embodiment and detailed description of the invention one are unlike Ti described in step one
xal
yintermetallic compound powder is Ti
3al, TiAl or TiAl
3.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two are unlike Ni described in step one
xal
yintermetallic compound powder is Ni
3al or NiAl.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three are unlike the acid solution of corrosive liquid to be concentration be 0.5 ~ 9mol/L in step 2.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to three are unlike the acid solution of corrosive liquid to be concentration be 1 ~ 7mol/L in step 2.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to three are unlike the acid solution of corrosive liquid to be concentration be 3 ~ 5mol/L in step 2.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are unlike the alkaline solution of corrosive liquid to be concentration be 0.5 ~ 9mol/L in step 2.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to six are unlike the alkaline solution of corrosive liquid to be concentration be 1 ~ 7mol/L in step 2.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to six are unlike the alkaline solution of corrosive liquid to be concentration be 3 ~ 5mol/L in step 2.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention one to nine unlike: acid solution described in step 2 is HCl, H
2sO
4or HNO
3.Other is identical with one of detailed description of the invention one to nine.
Detailed description of the invention 11: one of present embodiment and detailed description of the invention one to ten unlike: alkaline solution described in step 2 is NaOH or KOH.Other is identical with one of detailed description of the invention one to ten.
Detailed description of the invention 12: one of present embodiment and detailed description of the invention one to ten one unlike: the temperature of removal alloying process in step 2 is 25 ~ 85 DEG C.Other is identical with one of detailed description of the invention one to ten one.
Detailed description of the invention 13: one of present embodiment and detailed description of the invention one to ten one unlike: the temperature of removal alloying process in step 2 is 45 ~ 65 DEG C.Other is identical with one of detailed description of the invention one to ten one.
Detailed description of the invention 14: one of present embodiment and detailed description of the invention one to ten three unlike: the time of removal alloying process in step 2 is 20 ~ 60min.Other is identical with one of detailed description of the invention one to ten three.
Detailed description of the invention 15: one of present embodiment and detailed description of the invention one to ten three unlike: the time of removal alloying process in step 2 is 80 ~ 600min.Other is identical with one of detailed description of the invention one to ten three.
Detailed description of the invention 16: one of present embodiment and detailed description of the invention one to ten three unlike: the time of removal alloying process in step 2 is 200 ~ 400min.Other is identical with one of detailed description of the invention one to ten three.
Detailed description of the invention 17: one of present embodiment and detailed description of the invention one to ten six unlike: nanoporous titanium valve step 3 obtained is put into after the concentrated sulfuric acid stops 5 ~ 10s again and is taken out, and obtains surface and forms one deck TiO
2nanoporous titanium valve.Other is identical with one of detailed description of the invention one to ten six.
Adopt following verification experimental verification beneficial effect of the present invention:
Test one: this test prepares that the method for nanoporous titanium valve specifically completes according to the following steps:
One, presoma is prepared: by Ti
3al intermetallic compound powder puts into acetone, and utilize sonic oscillation to clean 10min, ultrasonic cleaning 8min in absolute ethyl alcohol, obtains the Ti of surface cleaning subsequently
3al precursor powder.
Two, removal alloying: by the Ti obtained in step one
3it is in the HCl solution of 1mol/L that Al precursor powder is placed on concentration, and carry out chemical removal alloying process, technological parameter is as follows: removal alloying temperature is 25 DEG C, and the time of removal alloying is 60min, in removal alloying process, be aided with sonic oscillation.
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse 120s by deionized water, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10min, to remove other residual impurity attachment, then the titanium valve under moisture state is put into vacuum drying chamber, after dry 5h, obtain nanoporous titanium valve.
The specific area of the nanoporous titanium valve of this test preparation is up to 62m
2/ g, puts into the nanoporous titanium valve of acquisition after the concentrated sulfuric acid stops 5s and takes out, can form one deck TiO at nano-porous surface
2, more improve photocatalysis efficiency.Then 0.025g nanoporous titanium valve is put into methyl orange solution and carry out catalysis degeneration experiment, test parameters is as follows: methyl orange concentration is 20mg/L, and dark surrounds medium ultraviolet light irradiation time is 280min, finds that its degradation efficiency reaches 85.68%.
Test two: this test prepares that the method for nanoporous titanium valve specifically completes according to the following steps:
One, prepare presoma: TiAl intermetallic compound powder is put into acetone, utilize sonic oscillation to clean 10min, subsequently ultrasonic cleaning 8min in absolute ethyl alcohol, obtain the TiAl precursor powder of surface cleaning.
Two, removal alloying: it is in the NaOH solution of 5mol/L that the TiAl precursor powder obtained in step one is placed on concentration, carry out chemical removal alloying process, technological parameter is as follows: removal alloying temperature is 25 DEG C, the time of removal alloying is 120min, in removal alloying process, be aided with sonic oscillation.
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse 120s by deionized water, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10min, to remove other residual impurity attachment, then the titanium valve under moisture state is put into vacuum drying chamber, after dry 5h, obtain nanoporous titanium valve.
The specific area of the nanoporous titanium valve of this test preparation is up to 60.3m
2/ g, puts into the nanoporous titanium valve of acquisition after the concentrated sulfuric acid stops 5s and takes out, can form one deck TiO at nano-porous surface
2, more improve photocatalysis efficiency.Then 0.025g nanoporous titanium valve is put into methyl orange solution and carry out catalysis degeneration experiment, test parameters is as follows: methyl orange concentration is 20mg/L, and dark surrounds medium ultraviolet light irradiation time is 280min, finds that its degradation efficiency reaches 86.14%.
Test three: this test prepares that the method for nanoporous titanium valve specifically completes according to the following steps:
One, presoma is prepared: by TiAl
3intermetallic compound powder puts into acetone, and utilize sonic oscillation to clean 10min, ultrasonic cleaning 8min in absolute ethyl alcohol, obtains the TiAl of surface cleaning subsequently
3precursor powder.
Two, removal alloying: by the TiAl obtained in step one
3it is in the HCl solution of 0.1mol/L that precursor powder is placed on concentration, and carry out chemical removal alloying process, technological parameter is as follows: removal alloying temperature is 25 DEG C, and the time of removal alloying is 20min, in removal alloying process, be aided with sonic oscillation.
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse 120s by deionized water, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10min, to remove other residual impurity attachment, then the titanium valve under moisture state is put into vacuum drying chamber, after dry 5h, obtain nanoporous titanium valve.
The specific area of the nanoporous titanium valve of this test preparation is up to 59.9m
2/ g, puts into the nanoporous titanium valve of acquisition after the concentrated sulfuric acid stops 5s and takes out, can form one deck TiO at nano-porous surface
2, more improve photocatalysis efficiency.Then 0.025g nanoporous titanium valve is put into methyl orange solution and carry out catalysis degeneration experiment, test parameters is as follows: methyl orange concentration is 20mg/L, and dark surrounds medium ultraviolet light irradiation time is 280min, finds that its degradation efficiency reaches 84.79%.
Test four: this test prepares that the method for nanoporous nickel powder specifically completes according to the following steps:
One, presoma is prepared: by Ni
3al intermetallic compound powder puts into acetone, and utilize sonic oscillation to clean 10min, ultrasonic cleaning 8min in absolute ethyl alcohol, obtains the Ni of surface cleaning subsequently
3al precursor powder.
Two, removal alloying: by the Ni obtained in step one
3it is in the NaOH solution of 5mol/L that Al precursor powder is placed on concentration, and carry out chemical removal alloying process, technological parameter is as follows: removal alloying temperature is 25 DEG C, and the time of removal alloying is 40min, in removal alloying process, be aided with sonic oscillation.
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse 120s by deionized water, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10min, to remove other residual impurity attachment, then the titanium valve under moisture state is put into vacuum drying chamber, after dry 5h, obtain nanoporous nickel powder.
The specific area of the nanoporous nickel powder of this test preparation is up to 60.7m
2/ g, puts into the nanoporous nickel powder of acquisition after the concentrated sulfuric acid stops 5s and takes out, can form one deck TiO at nano-porous surface
2, more improve photocatalysis efficiency.Then 0.025g nanoporous nickel powder is put into methyl orange solution and carry out catalysis degeneration experiment, test parameters is as follows: methyl orange concentration is 20mg/L, and dark surrounds medium ultraviolet light irradiation time is 280min, finds that its degradation efficiency reaches 83.11%.
Test five: this test prepares that the method for nanoporous nickel powder specifically completes according to the following steps:
One, prepare presoma: NiAl intermetallic compound powder is being put into acetone, utilize sonic oscillation to clean 10min, subsequently ultrasonic cleaning 8min in absolute ethyl alcohol, obtain the NiAl precursor powder of surface cleaning.
Two, removal alloying: it is that in the NaOH solution of 0.1mol/L, technological parameter is as follows that NiAl precursor powder step one obtained is placed on concentration: removal alloying temperature is 25 DEG C, the removal alloying time is 60min, in removal alloying process, be aided with sonic oscillation;
Three, subsequent treatment: the sample after removal alloying is taken out, first repeatedly rinse 120s by deionized water, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10min, to remove other residual impurity attachment, then the nickel powder under moisture state is put into vacuum drying chamber, after dry 5h, obtain nanoporous nickel powder.
The specific area of the nanoporous nickel powder of this test preparation is up to 58.9m
2/ g, puts into the nanoporous nickel powder of acquisition after the concentrated sulfuric acid stops 5s and takes out, can form one deck TiO at nano-porous surface
2, more improve photocatalysis efficiency.Then 0.025g nanoporous nickel powder is put into methyl orange solution and carry out catalysis degeneration experiment, test parameters is as follows: methyl orange concentration is 20mg/L, and dark surrounds medium ultraviolet light irradiation time is 280min, finds that its degradation efficiency reaches 85.45%.
Claims (10)
1. the preparation method of nanoporous titanium valve or nanoporous nickel powder, is characterized in that the method is carried out according to the following steps:
One, presoma is prepared: by Ti
xal
yor Ni
xal
yintermetallic compound powder puts into acetone, and utilize sonic oscillation to clean 10 ~ 15min, ultrasonic cleaning 5 ~ 10min in absolute ethyl alcohol, obtains the precursor powder of surface cleaning subsequently;
Two, removal alloying: the precursor powder obtained in step one is placed in corrosive liquid, carry out chemical removal alloying process respectively, acid solution or the concentration of corrosive liquid used to be concentration be 0.1 ~ 10mol/L are the alkaline solution of 0.1 ~ 10mol/L, the temperature of removal alloying process is 15 ~ 95 DEG C, and the time of removal alloying process is 5 ~ 720min;
Three, subsequent treatment: the powder after removal alloying is taken out, first repeatedly rinse by deionized water, rinse 120 ~ 150s altogether, and then put into absolute ethyl alcohol, utilize Ultrasonic Cleaning 10 ~ 15min, powder under moisture state is put into vacuum drying chamber, and dry 5 ~ 8h, can obtain nanoporous titanium valve or nanoporous nickel powder.
2. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that Ti described in step one
xal
yintermetallic compound powder is Ti
3al, TiAl or TiAl
3.
3. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that Ni described in step one
xal
yintermetallic compound powder is Ni
3al or NiAl.
4. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that corrosive liquid in step 2 to be concentration is the acid solution of 1 ~ 7mol/L.
5. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that corrosive liquid in step 2 to be concentration is the alkaline solution of 1 ~ 7mol/L.
6. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that acid solution described in step 2 is HCl, H
2sO
4or HNO
3.
7. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that alkaline solution described in step 2 is NaOH or KOH.
8. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that the temperature of removal alloying process in step 2 is 25 ~ 85 DEG C.
9. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that the time of removal alloying process in step 2 is 20 ~ 60min.
10. the preparation method of nanoporous titanium valve according to claim 1 or nanoporous nickel powder, is characterized in that nanoporous titanium valve step 3 obtained is put into after the concentrated sulfuric acid stops 5 ~ 10s again and takes out, obtain surface and form one deck TiO
2nanoporous titanium valve.
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CN109971985A (en) * | 2019-04-11 | 2019-07-05 | 南昌大学 | A kind of preparation method of POROUS TITANIUM |
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CN107680816A (en) * | 2017-09-29 | 2018-02-09 | 陕西理工大学 | Preparation methods of the porous Ti load hollow needle NiCo2S4 to electrode |
CN107680816B (en) * | 2017-09-29 | 2019-05-14 | 陕西理工大学 | Preparation method of the porous Ti load hollow needle NiCo2S4 to electrode |
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CN110482607A (en) * | 2019-07-30 | 2019-11-22 | 中南大学 | A kind of high grain boundary density MoO3Nanocrystalline and its preparation and the application in fragrant primary alconol catalysis oxidation |
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CN110284001A (en) * | 2019-08-06 | 2019-09-27 | 攀钢集团研究院有限公司 | The method that vanadium iron prepares vanadium metal |
CN111074330A (en) * | 2019-12-07 | 2020-04-28 | 西北有色金属研究院 | TiAl-series medical titanium alloy implant surface micropore preparation method |
CN111074330B (en) * | 2019-12-07 | 2021-04-02 | 西北有色金属研究院 | TiAl-series medical titanium alloy implant surface micropore preparation method |
CN111945028A (en) * | 2020-08-26 | 2020-11-17 | 中国矿业大学 | High-porosity micro/nano porous NiO/Ni material and preparation method and special equipment thereof |
CN111945028B (en) * | 2020-08-26 | 2021-09-03 | 中国矿业大学 | High-porosity micro/nano porous NiO/Ni material and preparation method and special equipment thereof |
CN113458393A (en) * | 2021-06-16 | 2021-10-01 | 中国科学院金属研究所 | Construction method of block nano porous metal |
CN113458393B (en) * | 2021-06-16 | 2022-09-13 | 中国科学院金属研究所 | Construction method of block nano porous metal |
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