CN116750763A - Surface treatment process for etching diamond based on hydrogen-free metal powder - Google Patents

Surface treatment process for etching diamond based on hydrogen-free metal powder Download PDF

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Publication number
CN116750763A
CN116750763A CN202310618643.1A CN202310618643A CN116750763A CN 116750763 A CN116750763 A CN 116750763A CN 202310618643 A CN202310618643 A CN 202310618643A CN 116750763 A CN116750763 A CN 116750763A
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Prior art keywords
diamond
etching
powder
metal powder
hydrogen
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CN202310618643.1A
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吴建
刘小东
纪勇
程何敏
魏江洪
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Huada Superabrasive Tool Technology Co ltd
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Huada Superabrasive Tool Technology Co ltd
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Priority to CN202310618643.1A priority Critical patent/CN116750763A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/25Diamond
    • C01B32/28After-treatment, e.g. purification, irradiation, separation or recovery

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The application relates to the technical field of diamond surface treatment, in particular to a surface treatment process for etching diamond based on hydrogen-free metal powder. According to the surface treatment process for etching the diamond based on the hydrogen-free metal powder, the diamond, the metal powder etchant, the additive and the dispersing agent are added into a three-dimensional mixer to be uniformly mixed; then placing the uniformly mixed mixture into a muffle furnace for etching heat treatment; finally, taking out the diamond after the treatment is finished, sieving the diamond, metal mixed powder, the additive and the dispersing agent by using a sieve to obtain the diamond with rough surface, and the production process is simple, does not need to carry out post-treatment on the diamond, and effectively improves the production efficiency; the use of the additive enhances the etching effect, greatly reduces the production cost, and effectively improves the holding force of the diamond tool on the diamond; meanwhile, the method can be used for single mass production and has wide market application prospect.

Description

Surface treatment process for etching diamond based on hydrogen-free metal powder
Technical Field
The application relates to the technical field of diamond surface treatment, in particular to a surface treatment process for etching diamond based on hydrogen-free metal powder.
Background
Since the advent of diamond, the material has many advantages such as extremely high mechanical hardness, excellent wear resistance and heat conduction and insulation properties, and low thermal expansion coefficient, and has been widely used in the fields of cutting tools, drilling detection tools, optical window materials, electrode materials, biosensors, quantum information computation and image processing, aerospace, and the like. The diamond has small size and excellent chemical stability, so that the diamond is extremely difficult to generate chemical reaction with other substances, the diamond is mechanically inlaid with materials such as other metals, resin, ceramics and the like with weak binding force in the actual production process of the diamond tool, the diamond is easy to fall off in the use process, the service life of the tool is reduced, the cost of the tool is increased, the efficiency and the accuracy of the diamond tool are reduced, and the diamond tool has poor application effect in the fine fields such as aerospace, semiconductors and the like.
The novel etching process can improve the surface roughness of the diamond, greatly improve the binding force of the diamond with metal, resin and ceramic, and effectively improve the efficiency, service life and precision of the diamond tool.
At present, two main processes for diamond etching exist in China:
1) Mixing diamond with NaNO3 or KNO3 and other salts to carry out high-temperature heat treatment, etching the surface of the diamond, cleaning and drying for a plurality of times after the treatment, and taking a lot of time in the cleaning and drying process in the post-treatment process, so that the production efficiency is low.
2) The diamond and the metal powder are put into a tube furnace for etching under the hydrogen atmosphere, so that the production cost is high, the number of the diamond etched at a time is too small, and the diamond is protected under the hydrogen atmosphere in the treatment process, so that the cost is high, and the large-scale production is not facilitated.
Disclosure of Invention
The application aims to at least solve one of the technical problems in the prior art, and provides a surface treatment process based on hydrogen-free metal powder etching diamond, which has strong universality, low production cost and high production efficiency and can be used for single mass production.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows: a surface treatment process for etching diamond based on a hydrogen free metal powder comprising the steps of:
s1, adding diamond, a metal powder etchant, an additive and a dispersing agent into a three-dimensional mixer, and uniformly mixing;
s2, placing the mixture uniformly mixed in the step S1 into a muffle furnace for etching heat treatment;
and S3, taking out the diamond after the treatment in the step S2 is finished, and sieving the diamond and metal mixed powder, the additive and the dispersing agent by using a sieve to obtain the diamond with rough surface.
Further, the addition amount of the metal powder etchant is 8-9%, and the addition amount of the diamond is 87-88%; the additive is added in an amount of 2-3% and the dispersant is added in an amount of 1-2%.
Further, the metal powder etchant includes one or more of FAM1022 prealloyed powder, iron powder, cobalt powder.
Further, the mixture ratio of FAM1022 prealloy powder, iron powder and cobalt powder in the metal powder etchant is as follows: the ratio of the FAM1022 prealloyed powder is 40% -70%, the iron powder is 20% -40%, the cobalt powder is 7% -15%, and the ratio of the metal powder etchant is selected according to the grain size of diamond.
Further, the FAM1022 prealloyed powder comprises the following raw materials in percentage by weight, namely, 81-83% of Fe and 17-19% of Ni; wherein the particle size of the FAM1022 prealloy powder is 800-1200 meshes, the particle size of the iron powder is 400-800 meshes, and the particle size of the cobalt powder is 2400-2600 meshes.
Further, the additive comprises one or more of lactic acid, disodium EDTA, naCl, NH4Cl and KCl.
Further, the mixture ratio of lactic acid, EDTA disodium, naCl, NH4Cl and KCl in the additive is as follows: 5% -11% of lactic acid, 2% of EDTA disodium, 42% -45% of NaCl, 42% -45% of NH4Cl and 3% of KCl.
Further, the dispersing agent is white corundum sand with the particle size of 180 meshes.
Further, the diamond particle sizes were 25/30, 30/35, 35/40, 40/45, 45/50, 50/60, 70/80.
Further, the etching temperature in the etching heat treatment is 820-850 ℃, and the etching temperature is selected according to the grain size of the diamond.
The application has the beneficial effects that: as can be seen from the above description of the present application, compared with the prior art, the surface treatment process based on the etching diamond of the hydrogen-free metal powder has the advantages of simple production process, no need of post-treatment of diamond, and effectively improved production efficiency; the use of the additive enhances the etching effect, greatly reduces the production cost, and effectively improves the holding force of the diamond tool on the diamond; meanwhile, the method can be used for single mass production and has wide market application prospect.
Drawings
FIG. 1 is a flow chart of a surface treatment process for etching diamond based on a hydrogen free metal powder in a preferred embodiment of the application;
FIG. 2 a is a graph showing the roughness of the (111) plane of diamond in example 1; b and c are enlarged roughness figures of the diamond (100) crystal planes in example 1;
FIGS. 3 a and b are enlarged views of the roughness of the diamond crystal planes in example 2;
fig. 4 a and b are enlarged views of the roughness of the diamond crystal planes in example 3.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the application.
Referring to fig. 1, a surface treatment process for etching diamond based on a hydrogen-free metal powder according to a preferred embodiment of the present application comprises the steps of:
s1, adding diamond, a metal powder etchant, an additive and a dispersing agent into a three-dimensional mixer, and uniformly mixing;
wherein the addition amount of the metal powder etchant is 8-9%, and the addition amount of the diamond is 87-88%; the addition amount of the additive is 2-3%, and the addition amount of the dispersing agent is 1-2%;
the metal powder etchant comprises one or more of FAM1022 prealloyed powder, iron powder and cobalt powder; in the embodiment, the mixture ratio of the FAM1022 prealloyed powder, the iron powder and the cobalt powder in the metal powder etchant is as follows: 40% -70% of FAM1022 prealloyed powder, 20% -40% of iron powder and 7% -15% of cobalt powder, and the proportion of the metal powder etchant is selected according to the grain diameter of diamond;
as the preferable FAM1022 prealloyed powder, the FAM1022 prealloyed powder comprises the following raw materials, by weight, 81% -83% of Fe and 17% -19% of Ni; wherein, the particle size of the FAM1022 prealloy powder is 800-1200 meshes, the particle size of the iron powder is 400-800 meshes, the particle size of the cobalt powder is 2400-2600 meshes, and the powder is produced by adopting an atomization method so as to ensure that the particle size of the metal powder is uniform;
the additive comprises one or more of lactic acid, EDTA disodium, naCl, NH4Cl and KCl; in the embodiment, the mixture ratio of lactic acid, EDTA disodium, naCl, NH4Cl and KCl in the additive is as follows: 5% -11% of lactic acid, 2% of EDTA disodium, 42% -45% of NaCl, 42% -45% of NH4Cl and 3% of KCl;
the dispersing agent is white corundum sand with the particle size of 180 meshes;
the grain size of the diamond is 25/30, 30/35, 35/40, 40/45, 45/50, 50/60, 70/80;
s2, placing the mixture uniformly mixed in the step S1 into a muffle furnace for etching heat treatment;
wherein the etching temperature in the etching heat treatment is 820-850 ℃, and the etching temperature is selected according to the grain diameter of diamond
And S3, taking out the diamond after the treatment in the step S2 is finished, and sieving the diamond and metal mixed powder, the additive and the dispersing agent by using a sieve to obtain the diamond with rough surface.
The following is a description of specific examples:
example 1
30/35 diamond hydrogen-free atmosphere metal powder etching treatment
S101, preparation of metal mixed powder
280g of FAM1022 prealloy powder, 80g of 600-mesh iron powder and 40g of 2500-mesh cobalt powder are taken and fully mixed in a three-dimensional mixer for 40 minutes, so that different powders are uniformly mixed together.
S102, preparation of additive
13.2g of lactic acid, 2.4g of EDTA disodium, 50.4g of NaCl, 50.4g of NH4Cl and 3.6g of KCl were weighed, and the mixture was stirred.
S103, mixing diamond, metal mixed powder, additive and dispersing agent
4000g of 30/35 diamond, 400g of metal mixed powder, 120g of chemical additive agent and 40g of 180-mesh white corundum sand are weighed and placed into a three-dimensional mixer to be mixed for 1.5 hours.
S104, heat treatment of diamond
Putting the mixed diamond into a muffle furnace, wherein the temperature of the muffle furnace is set as follows: the heating time from 120 ℃ to 630 ℃ is 120 minutes, the heating time from 630 ℃ to 820 ℃ is 60 minutes, the heat preservation temperature is 820 ℃, the heat preservation time is 10 minutes, and the cooling time is set to be automatically cooled. The diamond was etched according to this procedure.
And taking out the diamond after the automatic cooling is finished, and sieving the diamond and metal mixed powder, the chemical additive agent and the corundum sand by using a sieve to obtain the diamond with rough surface.
The obtained diamond with rough surface was placed under a 300-fold microscope and a 500-fold microscope, respectively, and the results are shown in fig. 2 a, b and c. As can be seen from FIG. 2, the (111) crystal face of the diamond which is more difficult to etch by adopting the process 30/35 also has deeper etching pits.
Example 2
45/50 diamond hydrogen-free atmosphere metal powder etching treatment
S101, preparation of metal mixed powder
200g of FAM1022 prealloy powder, 160g of 600-mesh iron powder and 40g of 2500-mesh cobalt powder are taken and fully mixed in a three-dimensional mixer for 40 minutes, so that different powders are uniformly mixed together.
S102, preparation of additive
9.6g of lactic acid, 2.4g of EDTA disodium, 51.84g of NaCl, 51.84g of NH4Cl and 3.6g of KCl were weighed, and the mixture was stirred.
S103, mixing diamond, metal mixed powder, additive and dispersing agent
4000g of 45/50 diamond, 400g of metal mixed powder, 120g of chemical additive agent and 40g of 180-mesh white corundum sand are weighed and placed into a three-dimensional mixer to be mixed for 1.5 hours.
S104, heat treatment of diamond
Putting the mixed diamond into a muffle furnace, wherein the temperature of the muffle furnace is set as follows: the heating time from 120 ℃ to 630 ℃ is 120 minutes, the heating time from 630 ℃ to 830 ℃ is 65 minutes, the heat preservation temperature is 830 ℃, the heat preservation time is 10 minutes, and the cooling time is set to be automatically cooled. The diamond was etched according to this procedure.
And taking out the diamond after the automatic cooling is finished, and sieving the diamond and metal mixed powder, the chemical additive agent and the corundum sand by using a sieve to obtain the diamond with rough surface.
The surface roughened diamond obtained was placed under a 1000-fold microscope, and the results are shown in fig. 3 a and b. It can be seen from FIG. 3 that the 45/50 diamond crystal face also has deeper etching pits by this process.
Example 3
70/80 diamond hydrogen-free atmosphere metal powder etching treatment
S101, preparation of metal mixed powder
180g of FAM1022 prealloy powder, 160g of 600-mesh iron powder and 60g of 2500-mesh cobalt powder are taken and fully mixed in a three-dimensional mixer for 40 minutes, so that different powders are uniformly mixed together.
S102, preparation of additive
6g of lactic acid, 2.4g of EDTA disodium, 54g of NaCl, 54. 54gNH4Cl and 3.6g of KCl were weighed, and the mixture was stirred.
S103, mixing diamond, metal mixed powder, additive and dispersing agent
4000g of 30/35 diamond, 400g of metal mixed powder, 120g of chemical additive agent and 40g of 180-mesh white corundum sand are weighed and placed into a three-dimensional mixer to be mixed for 1.5 hours.
S104, heat treatment of diamond
Putting the mixed diamond into a muffle furnace, wherein the temperature of the muffle furnace is set as follows: the temperature rise time from 120 ℃ to 630 ℃ is 120 minutes, the temperature rise time from 630 ℃ to 850 ℃ is 70 minutes, the heat preservation temperature is 850 ℃, the heat preservation time is 10 minutes, and the temperature reduction time is set to be automatic temperature reduction. The diamond was etched according to this procedure.
And taking out the diamond after the automatic cooling is finished, and sieving the diamond and metal mixed powder, the chemical additive agent and the corundum sand by using a sieve to obtain the diamond with rough surface.
The obtained diamond with rough surface was placed under 500-fold microscope and 1500-fold microscope, respectively, and the results are shown in fig. 4 a and b. As can be seen from FIG. 4, the diamond crystal planes using this process 70/80 also have deeper etch pits.
The application has simple production process, does not need post-treatment of diamond, and effectively improves the production efficiency; the use of the additive enhances the etching effect, greatly reduces the production cost, and effectively improves the holding force of the diamond tool on the diamond; meanwhile, the method can be used for single mass production and has wide market application prospect.
The above additional technical features can be freely combined and superimposed by a person skilled in the art without conflict.
It will be understood that the application has been described in terms of several embodiments, and that various changes and equivalents may be made to these features and embodiments by those skilled in the art without departing from the spirit and scope of the application. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the application without departing from the essential scope thereof. Therefore, it is intended that the application not be limited to the particular embodiment disclosed, but that the application will include all embodiments falling within the scope of the appended claims.

Claims (10)

1. A surface treatment process for etching diamond based on a hydrogen-free metal powder, comprising the steps of:
s1, adding diamond, a metal powder etchant, an additive and a dispersing agent into a three-dimensional mixer, and uniformly mixing;
s2, placing the mixture uniformly mixed in the step S1 into a muffle furnace for etching heat treatment;
and S3, taking out the diamond after the treatment in the step S2 is finished, and sieving the diamond and metal mixed powder, the additive and the dispersing agent by using a sieve to obtain the diamond with rough surface.
2. A surface treatment process for etching diamond based on hydrogen free metal powder as claimed in claim 1, wherein: the addition amount of the metal powder etchant is 8-9%, and the addition amount of the diamond is 87-88%; the additive is added in an amount of 2-3% and the dispersant is added in an amount of 1-2%.
3. A surface treatment process for etching diamond based on a hydrogen-free metal powder according to claim 1 or 2, characterized in that: the metal powder etchant comprises one or more of FAM1022 prealloyed powder, iron powder and cobalt powder.
4. A surface treatment process for etching diamond based on a hydrogen free metal powder according to claim 3, wherein: the metal powder etchant comprises the following components in percentage by weight: the ratio of the FAM1022 prealloyed powder is 40% -70%, the iron powder is 20% -40%, the cobalt powder is 7% -15%, and the ratio of the metal powder etchant is selected according to the grain size of diamond.
5. A surface treatment process for etching diamond based on a hydrogen free metal powder according to claim 3, wherein: the FAM1022 prealloyed powder comprises the following raw materials in percentage by weight, namely, 81-83% of Fe and 17-19% of Ni; wherein the particle size of the FAM1022 prealloy powder is 800-1200 meshes, the particle size of the iron powder is 400-800 meshes, and the particle size of the cobalt powder is 2400-2600 meshes.
6. A surface treatment process for etching diamond based on a hydrogen-free metal powder according to claim 1 or 2, characterized in that: the additive comprises one or more of lactic acid, disodium EDTA, naCl, NH4Cl and KCl.
7. A surface treatment process for etching diamond based on hydrogen free metal powder as claimed in claim 6, wherein: the mixture ratio of lactic acid, EDTA disodium, naCl, NH4Cl and KCl in the additive is as follows: 5% -11% of lactic acid, 2% of EDTA disodium, 42% -45% of NaCl, 42% -45% of NH4Cl and 3% of KCl.
8. A surface treatment process for etching diamond based on a hydrogen-free metal powder according to claim 1 or 2, characterized in that: the dispersing agent is white corundum sand with the particle size of 180 meshes.
9. A surface treatment process for etching diamond based on a hydrogen-free metal powder according to claim 1 or 2, characterized in that: the particle size of the diamond is 25/30, 30/35, 35/40, 40/45, 45/50, 50/60, 70/80.
10. A surface treatment process for etching diamond based on hydrogen free metal powder as claimed in claim 1, wherein: the etching temperature in the etching heat treatment is 820-850 ℃, and the etching temperature is selected according to the grain size of the diamond.
CN202310618643.1A 2023-05-30 2023-05-30 Surface treatment process for etching diamond based on hydrogen-free metal powder Pending CN116750763A (en)

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