CN104651815A - Method for preparing ZrB2-Cu composite powder - Google Patents
Method for preparing ZrB2-Cu composite powder Download PDFInfo
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- CN104651815A CN104651815A CN201410754464.1A CN201410754464A CN104651815A CN 104651815 A CN104651815 A CN 104651815A CN 201410754464 A CN201410754464 A CN 201410754464A CN 104651815 A CN104651815 A CN 104651815A
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- zrb
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- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 42
- 238000007747 plating Methods 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000007781 pre-processing Methods 0.000 claims abstract description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 8
- 230000002829 reductive effect Effects 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 101150003085 Pdcl gene Proteins 0.000 claims description 6
- 239000008139 complexing agent Substances 0.000 claims description 6
- 238000007772 electroless plating Methods 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 206010070834 Sensitisation Diseases 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 3
- 230000008313 sensitization Effects 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 239000000919 ceramic Substances 0.000 abstract description 6
- 229910007948 ZrB2 Inorganic materials 0.000 abstract description 5
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002905 metal composite material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 2
- 229910001111 Fine metal Inorganic materials 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 239000012798 spherical particle Substances 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
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- Powder Metallurgy (AREA)
- Chemically Coating (AREA)
Abstract
The invention provides a method for preparing ZrB2-Cu composite powder, belongs to the field of ceramic/metal composite material preparation and in particular relates to the method for preparing the ZrB2-Cu composite powder having a good internal metal-ceramic binding property. The method comprises two steps of ZrB2 preprocessing and chemical copper plating; the ZrB2 powder is chemically copper-plated by use of a chemical plating method, and then the Cu-coated ZrB2 powder can be prepared. The composite powder prepared by use of the method is good in dispersity; the copper coating is excellent in crystallinity without impurity phase; the surface of the coating is accumulated randomly by fine metal spherical particles; the coating is compact, uniform, flat and smooth, and has wide application prospect.
Description
Technical field
The invention belongs to ceramic/metal composite materials preparation field.
Background technology
ZrB
2-Cu matrix material is the immiscible ceramic/metal composite materials formed by the Cu of the ZrB2 of high-melting-point, high rigidity and high heat conduction, conductivity.This matrix material has the dual nature of pottery and metal, greatly can improve wear-resisting, the anti electric arc corrosion ability of material, is to have high conductivity, high-wear resistance, certain machinery and mechanical strength concurrently in the contact material of one.The domestic research to preparing zirconium diboride ceramics and copper composite material is very few at present, and the people such as Venkateswaran T adopt discharge plasma sintering (SPS) to make each to have the ZrB of higher hardness and fracture toughness property
2-6%Cu (massfraction) matrix material, adds due to Cu the electroconductibility significantly improving material.The people such as Norasetthekul S are 1700 DEG C of obtained ZrB of sintering under Ar atmosphere protection
2ceramic skeleton, then at 1200 DEG C, pressure-free impregnation Cu prepares ZrB
2-Cu matrix material is used as electric discharging machining electrode, compared to Cu, graphite and W-Cu electrode, and ZrB
2-Cu matrix material shows larger material removing rate and low electrode wear rate.But, due to ZrB
2poor with the wettability of Cu, two Entropy density deviation are difficult to evenly, and two-phase interface is in conjunction with weak, and the performance of matrix material is lower.
Summary of the invention
The object of this invention is to provide a kind of ZrB
2the ZrB that the inner two-phase of-Cu composite powder is combined
2the preparation method of-Cu composite powder.
The present invention is achieved by the following technical programs: one prepares ZrB
2the method of-Cu composite powder, comprises ZrB
2pre-treatment and electroless copper two step;
Described ZrB
2pre-treatment step is, by ZrB
2powder is immersed in dilute hydrochloric acid solution and cleans alligatoring 20 min, by washed with de-ionized water 3 times, then ZrB
2powder is immersed in SnCl2 solution sensitization 20 min, by washed with de-ionized water 3 times, finally by ZrB
2powder is immersed in PdCl
2activate 40min in solution, by washed with de-ionized water 3 times, preprocessing process all completes in magnetic stirring apparatus, and in its preprocessing process, concentration of hydrochloric acid is 100ml/L, SnCl
2+ HCl is 30g/L+25ml/L, PdCl
2+ HCl is 0.7g/L+30ml/L;
Described electroless copper step is, plating solution is by main salt CuS0
45H
20, reductive agent HCHO, complexing agent Na
2eDTA, stablizer 2,2 '-pyridine, pH adjusting agent NaOH formed, by pretreated for 15g ZrB
2powder puts into 200mL plating solution, magnetic force thermostatic mixer is adopted to carry out electroless plating experiment, the electroless copper in plating process with formaldehyde being reductive agent is very strong to PH dependency, and solution ph must reach more than 11, therefore, regulate plating solution pH value between 12 ~ 13, just there is enough reductive actions, select plating temperature at 30 ~ 70 DEG C, main salt concentration 5 ~ 15g/L, reductant concentration 12 ~ 28ml/L tests, complexing agent Na
2eDTA consumption is 30g/L, and its effect is and Cu
2+form title complex, reduce free Cu
2+concentration; Stablizer 2,2 '-dipyridyl consumption is at 0.05g/L, and its effect suppresses plating solution self-decomposition and is adsorbed on solid surface, and use washed with de-ionized water 3 times after electroless plating, then ethanol is washed 1 time and put into vacuum drying oven, and drying temperature 40 DEG C, time 6h, obtains ZrB
2-Cu composite powder.
Preferably, described electroless copper step China, main salt CuS0
45H
20 concentration is 10g/L, concentration of formaldehyde 20ml/L, and plating temperature is 50 DEG C
The present invention has following beneficial effect:
Adopt composite granule good dispersity prepared by the method for the invention, copper coating crystallinity is good, and without dephasign, coating surface is piled up at random by tiny metal ball particle and is formed, plated layer compact, even, flat smooth.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Specific embodiment: preparation process of the present invention comprises ZrB
2pre-treatment and electroless copper two step;
Described ZrB
2pre-treatment step is, by ZrB
2powder is immersed in dilute hydrochloric acid solution and cleans alligatoring 20 min, by washed with de-ionized water 3 times, then ZrB
2powder is immersed in SnCl2 solution sensitization 20 min, by washed with de-ionized water 3 times, finally by ZrB
2powder is immersed in PdCl
2activate 40min in solution, by washed with de-ionized water 3 times, preprocessing process all completes in magnetic stirring apparatus, and in its preprocessing process, concentration of hydrochloric acid is 100ml/L, SnCl
2+ HCl is 30g/L+25ml/L, PdCl
2+ HCl is 0.7g/L+30ml/L;
Described electroless copper step is, plating solution is by main salt CuS0
45H
20, reductive agent HCHO, complexing agent Na
2eDTA, stablizer 2,2 '-pyridine, pH adjusting agent NaOH formed, by pretreated for 15g ZrB
2powder puts into 200mL plating solution, magnetic force thermostatic mixer is adopted to carry out electroless plating experiment, the electroless copper in plating process with formaldehyde being reductive agent is very strong to PH dependency, and solution ph must reach more than 11, therefore, regulate plating solution pH value between 12 ~ 13, just there is enough reductive actions, select plating temperature at 30 ~ 70 DEG C, main salt concentration 5 ~ 15g/L, reductant concentration 12 ~ 28ml/L tests, complexing agent Na
2eDTA consumption is 30g/L, and its effect is and Cu
2+form title complex, reduce free Cu
2+concentration; Stablizer 2,2 '-dipyridyl consumption is at 0.05g/L, and its effect suppresses plating solution self-decomposition and is adsorbed on solid surface, and use washed with de-ionized water 3 times after electroless plating, then ethanol is washed 1 time and put into vacuum drying oven, and drying temperature 40 DEG C, time 6h, obtains ZrB
2-Cu composite powder
To the ZrB of preparation
2-Cu composite powder carries out thing phase and morphology analysis, draw composite granule good dispersity, copper coating crystallinity is good in dephasign, and coating surface is piled up at random by tiny metal ball particle and formed, plated layer compact, even, flat smooth, have the wide application prospect sent out.
Above content is the further description done the present invention in conjunction with concrete embodiment, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (2)
1. prepare ZrB for one kind
2the method of-Cu composite powder, is characterized in that: comprise ZrB
2pre-treatment and electroless copper two step;
Described ZrB
2pre-treatment step is, by ZrB
2powder is immersed in dilute hydrochloric acid solution and cleans alligatoring 20 min, by washed with de-ionized water 3 times, then ZrB
2powder is immersed in SnCl2 solution sensitization 20 min, by washed with de-ionized water 3 times, finally by ZrB
2powder is immersed in PdCl
2activate 40min in solution, by washed with de-ionized water 3 times, preprocessing process all completes in magnetic stirring apparatus, and in its preprocessing process, concentration of hydrochloric acid is 100ml/L, SnCl
2+ HCl is 30g/L+25ml/L, PdCl
2+ HCl is 0.7g/L+30ml/L;
Described electroless copper step is, plating solution is by main salt CuS0
45H
20, reductive agent HCHO, complexing agent Na
2eDTA, stablizer 2,2 '-pyridine, pH adjusting agent NaOH formed, by pretreated for 15g ZrB
2powder puts into 200mL plating solution, adopts magnetic force thermostatic mixer to carry out electroless plating experiment, regulates plating solution pH value between 12 ~ 13, and select plating temperature at 30 ~ 70 DEG C, main salt concentration 5 ~ 15g/L, reductant concentration 12 ~ 28ml/L tests, complexing agent Na
2eDTA consumption is 30g/L, stablizer 2, and 2 '-dipyridyl consumption is at 0.05g/L, and use washed with de-ionized water 3 times after electroless plating, then ethanol is washed 1 time and put into vacuum drying oven, and drying temperature 40 DEG C, time 6h, obtains ZrB
2-Cu composite powder.
2. prepare ZrB as claimed in claim 1
2the method of-Cu composite powder, is characterized in that: described electroless copper step China, main salt CuS0
45H
20 concentration is 10g/L, concentration of formaldehyde 20ml/L, and plating temperature is 50 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410754464.1A CN104651815A (en) | 2014-12-11 | 2014-12-11 | Method for preparing ZrB2-Cu composite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410754464.1A CN104651815A (en) | 2014-12-11 | 2014-12-11 | Method for preparing ZrB2-Cu composite powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104651815A true CN104651815A (en) | 2015-05-27 |
Family
ID=53243443
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410754464.1A Pending CN104651815A (en) | 2014-12-11 | 2014-12-11 | Method for preparing ZrB2-Cu composite powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104651815A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463450A (en) * | 2015-12-01 | 2016-04-06 | 仇颖超 | Method for manufacturing copper-based nano ceramic fiber composite material through laser cladding |
| CN108441728A (en) * | 2018-04-18 | 2018-08-24 | 明光市天淼新能源科技有限公司 | A kind of enhancing magnesium alloy materials |
| CN114606482A (en) * | 2022-03-15 | 2022-06-10 | 佛山科学技术学院 | Method for preparing Cu @ ZrC core-shell complex-phase particle material by chemical plating |
| CN115124350A (en) * | 2022-06-24 | 2022-09-30 | 林萍华 | A kind of preparation technology of ceramic composite material applied in high temperature environment |
-
2014
- 2014-12-11 CN CN201410754464.1A patent/CN104651815A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463450A (en) * | 2015-12-01 | 2016-04-06 | 仇颖超 | Method for manufacturing copper-based nano ceramic fiber composite material through laser cladding |
| CN108441728A (en) * | 2018-04-18 | 2018-08-24 | 明光市天淼新能源科技有限公司 | A kind of enhancing magnesium alloy materials |
| CN114606482A (en) * | 2022-03-15 | 2022-06-10 | 佛山科学技术学院 | Method for preparing Cu @ ZrC core-shell complex-phase particle material by chemical plating |
| CN115124350A (en) * | 2022-06-24 | 2022-09-30 | 林萍华 | A kind of preparation technology of ceramic composite material applied in high temperature environment |
| CN115124350B (en) * | 2022-06-24 | 2024-03-08 | 林萍华 | Preparation process of ceramic composite material applied to high-temperature environment |
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Legal Events
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150527 |