CN115851069A - PCD compact metallographic protective agent and preparation method and application thereof - Google Patents
PCD compact metallographic protective agent and preparation method and application thereof Download PDFInfo
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- CN115851069A CN115851069A CN202211455974.XA CN202211455974A CN115851069A CN 115851069 A CN115851069 A CN 115851069A CN 202211455974 A CN202211455974 A CN 202211455974A CN 115851069 A CN115851069 A CN 115851069A
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Abstract
The invention provides a PCD compact metallographic protective agent, which mainly comprises the following raw materials in percentage by mass: 5-20% of phenolic resin, 3-5% of hydrophobic base film forming agent, 0.5-1% of surfactant, 0.1-0.5% of polydimethylsiloxane and the balance of solvent. The invention also provides a preparation method of the PCD compact metallographic phase. The invention also provides a method for protecting the metallographic phase of the PCD compact, which comprises the following steps: forming a protective layer, and uniformly coating the PCD composite sheet metallographical protective agent on the surface of a material layer of the PCD composite sheet to form a metallographical protective film; ultrasonic flaw detection treatment and protective layer removal. Above-mentioned compound piece metallography protective agent simple manufacture of PCD can form the hydrophobic protection film of one deck on compound piece surface of PCD, and the protection compound piece metallography is not destroyed, and this protection film can not influence ultrasonic inspection's testing result.
Description
Technical Field
The invention relates to the technical field of polycrystalline diamond compact surface processing, in particular to a PCD compact metallographic protective agent, a preparation method and an application protection method thereof.
Background
The PCD compact is a novel superhard composite material formed by sintering diamond particles and a hard alloy matrix at high temperature and high pressure. It has high hardness, wear resistance, small friction coefficient, high heat conductivity, low heat expansion coefficient and the strength and toughness of hard alloy, is an ideal material for making superhard cutter and is widely used in important fields of aerospace, automobile, energy source, geological petroleum exploration, war industry, precision manufacture and the like. In order to improve the machining precision and surface quality of the machined workpiece, the PCD surface for making the cutter is generally required to be machined to a mirror surface effect.
Ultrasonic flaw detection is a main detection method for detecting internal defects of a PCD composite sheet, a coupling agent required for detection is water without bubbles, dust and impurities, but when the PCD composite sheet with a good mirror effect and a good metallographic phase is contacted with water, the metallographic phase of the PCD composite sheet can be damaged, and because water has certain Co leaching capacity, the defect of a cobalt-free area appears on the surface within a certain depth range, and in a certain thickness range, gaps are formed among diamond grains due to Co deficiency, so that the binding force among the diamond grains is weakened, and a diamond cutter in the state has adverse effects on the processing precision and the surface quality of a processed workpiece.
Disclosure of Invention
In view of the above, the present invention provides a PCD compact metallographic protective agent, a preparation method and an application thereof, so as to protect the metallographic surface from being damaged and not to affect the ultrasonic flaw detection result.
Specifically, the invention provides a PCD compact metallographic protective agent which mainly comprises the following raw materials in percentage by mass: 5-20% of phenolic resin, 3-5% of hydrophobic group film-forming agent, 0.5-1% of surfactant, 0.1-0.5% of polydimethylsiloxane and the balance of solvent.
Based on the above, the hydrophobic base film-forming agent is barium dinonyl naphthalene sulfonate, barium petroleum sulfonate, aluminum stearate and other materials capable of forming a directional adsorption hydrophobic protective film on the surface of the PCD.
The PCD compact metallographic phase protective agent comprises the following raw materials in percentage by mass: 8-15% of phenolic resin, 3-5% of barium dinonyl naphthalene sulfonate, 0.5-0.8% of surfactant, 0.1-0.3% of polydimethylsiloxane and the balance of solvent.
Based on the above, the surfactant is fatty alcohol-polyoxyethylene ether, sorbitan fatty acid ester or a mixture of the fatty alcohol-polyoxyethylene ether and the sorbitan fatty acid ester, and mainly plays a role in emulsification, so that the PCD compact metallographic phase protective agent can form a stable system.
Based on the above, the solvent is one or more of ethanol, acetone and ethyl acetate, and is mainly used for dissolving other components in the PCD compact metallographic protective agent to promote the PCD compact metallographic protective agent to form a stable system.
The invention also provides a preparation method of the PCD compact metallographic phase, which comprises the following steps: dissolving phenolic resin in the solvent, adding the hydrophobic group film-forming agent, the surfactant and the polydimethylsiloxane, and stirring for 0.5-1 h.
The invention also provides a method for protecting the metallographic phase of the PCD compact, which comprises the following steps:
forming a protective layer, and uniformly coating the PCD composite sheet metallographical protective agent on the surface of a material layer of the PCD composite sheet to form a metallographical protective film;
ultrasonic flaw detection treatment, namely placing the PCD composite sheet with the metallographic protective film in a coupling agent for ultrasonic flaw detection treatment;
and removing the protective layer and removing the metallographic protective film on the PCD composite sheet subjected to ultrasonic flaw detection treatment.
Based on the above, the step of forming the protective layer includes: and uniformly coating the PCD composite sheet metallographical protective agent on the surface of a material layer of the PCD composite sheet, and standing for 2-3 min to form the metallographical protective film.
Based on the above, the ultrasonic flaw detection processing includes: firstly, placing a water coupling agent in ultrasonic equipment, then placing the PCD composite sheet formed with the metallographic protective film in water for ultrasonic flaw detection, and taking out the composite sheet after flaw detection.
Based on the above, the step of removing the protection layer includes: the cleaning agent is dipped in the non-woven fabric firstly, and then the non-woven fabric dipped with the cleaning agent is used for wiping the metallographic protection film on the PCD composite sheet subjected to ultrasonic flaw detection treatment, wherein the cleaning agent is ethanol, acetone, ethyl acetate or any combination thereof. The cleaning agent is preferably ethanol, because ethanol is safer for workers.
In the formation process of the PCD composite sheet metallographic protection film, the main function of the hydrophobic base film forming agent is to form a directional adsorption protection film on the surface of the PCD composite sheet material layer, the directional adsorption protection film plays a role in shielding the surface of the PCD composite sheet material layer, the directional adsorption protection film is composed of hydrophobic bases, the directional adsorption protection film belongs to a low-energy surface, and a water medium serving as a coupling agent can form a large contact angle on the directional adsorption protection film and is not easy to permeate, so that the contact between the water medium and the surface of the PCD composite sheet material layer is prevented. However, when the content of the hydrophobic film forming agent is relatively small, a phenomenon that a film is difficult to form on the surface of the PCD composite sheet material occurs.
The phenolic resin used as the binder can improve the wetting film-forming speed of the hydrophobic film-forming agent, so that the oriented adsorption protective film has certain bonding strength and adhesive force. However, when the content of the phenolic resin is relatively small or even absent, the film forming speed of the hydrophobic film forming agent is relatively slow, and the formed protective film has low adhesion and is easily damaged.
The polydimethylsiloxane is used as a defoaming agent, has extremely low surface tension and is easy to spread, the continuity of the directional adsorption protective film is enhanced, and the PCD composite sheet material layer is effectively protected. However, when the content of polydimethylsiloxane is relatively low, bubbles existing in the metallographic protective agent of the PCD compact in the coating process cannot be effectively eliminated, and once the bubbles are broken, the surface of the PCD composite sheet material layer cannot be effectively protected.
Therefore, the components in the PCD compact metallographic protective agent provided by the invention are matched with each other and have synergistic effect, so that the PCD compact metallographic protective agent formed by compounding can be stably stored, and if the content of each component exceeds the range defined by the invention, the condition of layering or precipitation can occur, a stable system cannot be formed, and the PCD compact metallographic protective agent is difficult to maintain for a long time.
Therefore, the PCD composite sheet metallography protective agent provided by the invention can form a layer of hydrophobic protective film on the surface of the PCD composite sheet in the using process, the PCD composite sheet metallography is protected from being damaged, and the protective film does not influence the detection result of ultrasonic flaw detection. In addition, the preparation method of the PCD compact metallographic phase protective agent is simple and easy to operate. The method for protecting the metallographic phase of the PCD compact provided by the invention is simple and effective and is easy to realize.
Drawings
FIG. 1 is a 500-fold magnified metallographic image of a comparative reference sample provided in example 1 of the present invention.
FIG. 2 is a photograph of a gold phase at 500 times magnification of a sample from an experimental group provided in example 1 of the present invention.
Fig. 3 is a diagram showing the ultrasonic flaw detection results of a PCD compact of an experimental group in which a protective layer was formed in the method for protecting the metallographic phase of the PCD compact according to example 1 of the present invention.
Fig. 4 is a graph showing the ultrasonic testing results of the experimental group of samples obtained by the method for protecting the metallographic phase of the PCD compact provided in example 1 of the present invention.
Fig. 5 is a gold phase diagram of a PCD compact treated by the method for protecting the gold phase of the PCD compact provided by example 4 of the present invention, at a magnification of 500 times.
Fig. 6 is a gold phase diagram, at 500 times magnification, of a PCD compact treated by a method for protecting the gold phase of the PCD compact provided in example 5 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
Example 1
The metallographic pictures of the PCD compact used in the present example were measured by a three-dimensional microscope VHX-5000.
The embodiment of the invention provides a PCD compact metallographic protective agent, which comprises the following components in percentage by mass: 11% of phenolic resin, 4% of barium dinonylnaphthalene sulfonate, 84.3% of ethanol, 0.5% of fatty alcohol-polyoxyethylene ether AEO-4 and 0.2% of polydimethylsiloxane.
The preparation method of the PCD compact metallographic protective agent comprises the following steps: weighing a certain amount of components according to the component proportion improved in the embodiment, firstly placing phenolic resin in a glass container, adding ethanol, placing the glass container in a rotor, placing the glass container on a magnetic stirrer, stirring until the phenolic resin is completely dissolved, then sequentially adding barium dinonylnaphthalene sulfonate, fatty alcohol-polyoxyethylene ether AEO-4 and polydimethylsiloxane, and stirring for 0.5-1 h to obtain the PCD metallographic protective agent; the components in the PCD compact metallographic protective agent are uniformly dispersed to form a stable system, and the phenomenon of layering or precipitation does not occur.
The embodiment also provides a method for protecting the metallographic phase of the PCD compact, which comprises the following steps of taking 10 PCD compacts, uniformly coating 2 mL of PCD metallographic protective agent provided by the embodiment on the surfaces of 5 PCD compacts, standing for 2 min to form a protective layer on the material bed surface of the corresponding PCD compact as an experimental group; the other 5 tablets were not coated with protective agent as a control reference; then putting the PCD composite sheets of all the experimental groups and the comparison reference groups into ultrasonic equipment with water as a coupling agent for ultrasonic flaw detection, and taking out all the PCD composite sheets after the flaw detection is finished; wiping the PCD compact with the protective layer by using non-woven fabric dipped with ethanol, removing the protective layer on the surface of the material layer, and drying to obtain an experimental group sample; the PCD compact of the comparative reference group, which was taken out after the completion of the dry testing, was used as a comparative reference group sample.
And respectively detecting metallographic pictures of the experimental group sample and the comparative reference group sample by using a three-dimensional microscope VHX-5000. Wherein, fig. 1 is a metallographic picture of a comparative reference group sample, and fig. 2 is a metallographic picture of an experimental group sample. As can be seen from fig. 1 and 2: the metallographic structure in fig. 2 is obviously smaller than that in fig. 1, and the metallographic structures in fig. 2 are distributed more uniformly, so that the protective agent and the protective method for the PCD compact provided by the embodiment of the invention can effectively protect the surface of the material layer of the PCD compact, and the protective effect is obvious.
The test results of the PCD compact of the test group in which the protective layer was formed are shown in fig. 3; the same ultrasonic testing treatment was performed on a test group sample belonging to the same PCD compact as the test result shown in fig. 3, and the results are shown in fig. 4. As can be seen from fig. 3 and 4: the flaw detection results in the two figures are basically consistent, so that the protective film formed by the metallographic protective agent of the PCD composite sheet provided by the embodiment of the invention in the using process does not influence the ultrasonic flaw detection result of the PCD composite sheet.
The reason why the metallographic protective agent for the PCD compact provided by the embodiment can effectively protect the surface of the material layer of the PCD compact is mainly that: in the process of forming a protective layer on the surface of the material layer of the PCD composite sheet, barium dinonyl naphthalene sulfonate can form a directional adsorption protective film on the surface of the material layer of the PCD composite sheet, and the directional adsorption protective film plays a role in shielding the surface of the material layer of the PCD composite sheet; the directional adsorption protective film is composed of a hydrophobic group, belongs to a low-energy surface, and an aqueous medium serving as a coupling agent forms a large contact angle on the directional adsorption protective film and is not easy to permeate, so that the contact between the aqueous medium and the surface of the PCD composite sheet material layer is prevented. The phenolic resin used as a binder can improve the wetting speed of barium dinonyl naphthalene sulfonate, so that the directional adsorption protective film has certain bonding strength and adhesive force; polydimethylsiloxane is taken as a defoaming agent, the surface tension is extremely low, the spreading is easy, and the continuity of the directional adsorption protective film is enhanced, so that a PCD composite sheet material layer is effectively protected, and the surface of the PCD composite sheet material layer cannot be effectively protected if bubbles exist in the PCD composite sheet metallographical protective agent in the coating process and are destroyed.
Example 2
The embodiment of the invention provides a PCD compact metallographic protective agent, which comprises the following components in percentage by mass: 11.3% of phenolic resin, 3% of barium dinonylnaphthalene sulfonate, 84.9% of acetone, 0.5% of fatty alcohol-polyoxyethylene ether AEO-3 and 0.3% of polydimethylsiloxane.
In the embodiment, the PCD compact metallographic protective agent is prepared by the same method as the first embodiment, and all components in the PCD compact metallographic protective agent are uniformly dispersed to form a stable system, so that the phenomenon of layering or precipitation is avoided, and the long-term maintenance is facilitated.
In this embodiment, a method for protecting the metallographic phase of a PCD compact, which is substantially the same as the experimental group provided in the first embodiment, is adopted, and the main difference is that: the PCD compact metallographic protective agent adopted in the embodiment is the PCD compact metallographic protective agent provided by the embodiment. The metallographic phase diagram of the PCD compact treated by the method for protecting the metallographic phase of the PCD compact provided by the embodiment is closer to that of fig. 2, and is not provided any more.
Example 3
The embodiment of the invention provides a PCD compact metallographic protective agent, which comprises the following components in percentage by mass: 14.8% of phenolic resin, 4.9% of barium dinonylnaphthalene sulfonate, 79.6% of ethyl acetate, 0.3% of sorbitan fatty acid ester Span-20, 0.3% of polyoxyethylene sorbitan fatty acid ester Tween-21, and 0.1% of polydimethylsiloxane.
In the embodiment, the PCD compact metallographic protective agent is prepared by the same method as the first embodiment, and all components in the PCD compact metallographic protective agent are uniformly dispersed to form a stable system, so that the phenomenon of layering or precipitation is avoided, and the long-term maintenance is facilitated.
In this embodiment, a method for protecting the metallographic phase of a PCD compact, which is substantially the same as the experimental group provided in the first embodiment, is adopted, and the main difference is that: the PCD compact metallographic protective agent adopted in the embodiment is the PCD compact metallographic protective agent provided by the embodiment. The metallographic phase diagram of the PCD compact treated by the method for protecting the metallographic phase of the PCD compact provided by the embodiment is closer to that of fig. 2, and is not provided any more.
Example 4
The embodiment of the invention provides a PCD compact metallographic protective agent, which comprises the following components in percentage by mass: 8% of phenolic resin, 3% of barium petroleum sulfonate, 87.5% of ethanol, 1% of Tween-20 and 0.5% of polydimethylsiloxane.
In the embodiment, the PCD compact metallographic protective agent is prepared by the same method as the first embodiment, and all components in the PCD compact metallographic protective agent are uniformly dispersed to form a stable dispersion system, so that the phenomenon of layering or precipitation does not occur.
In this embodiment, a method for protecting the metallographic phase of a PCD compact, which is substantially the same as the experimental group provided in the first embodiment, is adopted, and the main difference is that: the PCD compact metallographic protective agent adopted in the embodiment is the PCD compact metallographic protective agent provided by the embodiment. A metallographic graph of the PCD compact treated by the method for protecting the metallographic phase of the PCD compact provided in this example is shown in fig. 5.
Example 5
The embodiment of the invention provides a PCD compact metallographic protective agent, which comprises the following components in percentage by mass: 20% of phenolic resin, 3% of aluminum stearate, 75.9% of ethyl acetate, 0.7% of Tween-20 and 0.4% of polydimethylsiloxane.
In the embodiment, the metallographic protective agent of the PCD compact is prepared by the same method as in the first embodiment, and each component in the metallographic protective agent of the PCD compact is uniformly dispersed to form a stable dispersion system, so that the phenomenon of layering or precipitation does not occur.
In this embodiment, a method for protecting the metallographic phase of a PCD compact, which is substantially the same as the experimental group provided in the first embodiment, is adopted, and the main difference is that: the PCD compact metallographic protective agent adopted in the embodiment is the PCD compact metallographic protective agent provided by the embodiment. A metallographic graph of the PCD compact treated by the method for protecting the metallographic phase of the PCD compact provided in this example is shown in fig. 6.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (10)
1. A PCD composite sheet metallographic phase protective agent mainly comprises the following raw materials in percentage by mass: 5-20% of phenolic resin, 3-5% of hydrophobic base film forming agent, 0.5-1% of surfactant, 0.1-0.5% of polydimethylsiloxane and the balance of solvent.
2. The PCD compact metallography protective agent of claim 1, wherein the hydrophobic base film forming agent is barium dinonylnaphthalene sulfonate, barium petroleum sulfonate or aluminum stearate.
3. The PCD compact metallographic protective agent of claim 2, which consists of the following raw materials in percentage by mass: 8-15% of phenolic resin, 3-5% of barium dinonyl naphthalene sulfonate, 0.5-0.8% of surfactant, 0.1-0.3% of polydimethylsiloxane and the balance of solvent.
4. A PCD compact metallographical protective agent according to claim 1, 2 or 3, characterised in that the surfactant is fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester or a mixture of both.
5. The PCD compact metallographical protective agent according to claim 4, wherein the solvent is one or more of ethanol, acetone and ethyl acetate.
6. A method of making a PCD compact metallographic phase according to any one of claims 1 to 5, comprising: dissolving phenolic resin in the solvent, adding the hydrophobic group film-forming agent, the surfactant and the polydimethylsiloxane, and stirring for 0.5-1 h.
7. A method for protecting a PCD compact metallographic phase comprises the following steps:
forming a protective layer, and uniformly coating the PCD compact metallographic protective agent of any one of claims 1 to 5 on the surface of a material layer of the PCD compact to form a metallographic protective film;
ultrasonic flaw detection treatment, namely placing the PCD composite sheet with the metallographic protective film in a coupling agent for ultrasonic flaw detection treatment;
and removing the protective layer and the metallographic protective film on the PCD composite sheet after ultrasonic flaw detection treatment.
8. The protection method according to claim 7, wherein the step of forming a protection layer includes: and uniformly coating the PCD composite sheet metallographical protective agent on the surface of the material layer of the PCD composite sheet, and standing for 2-3 min to form the metallographical protective film.
9. The protection method according to claim 7 or 8, characterized in that the step of ultrasonic flaw detection processing includes: firstly, placing a water coupling agent in ultrasonic equipment, then placing the PCD composite sheet formed with the metallographic protective film in water for ultrasonic flaw detection, and taking out the composite sheet after flaw detection.
10. The protection method according to claim 9, wherein the step of removing the protection layer comprises: the cleaning agent is dipped in the non-woven fabric firstly, and then the non-woven fabric dipped with the cleaning agent is used for wiping the metallographic protection film on the PCD composite sheet subjected to ultrasonic flaw detection treatment, wherein the cleaning agent is ethanol, acetone, ethyl acetate or any combination thereof.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103305317A (en) * | 2012-03-09 | 2013-09-18 | 中国石油天然气股份有限公司 | Metal antirust compound containing oil-soluble polyaniline and application thereof |
| CN104450045A (en) * | 2014-11-10 | 2015-03-25 | 安徽威萨重工机械有限公司 | Anti-corrosive grease type rustproof oil and preparation method thereof |
| CN104845701A (en) * | 2014-02-14 | 2015-08-19 | 吉坤日矿日石能源株式会社 | Rust-proof oil composition |
| CN111253815A (en) * | 2020-02-17 | 2020-06-09 | 丫肯(上海)新材料科技有限公司 | Antirust agent and preparation method thereof |
| CN113845809A (en) * | 2021-10-10 | 2021-12-28 | 山立欣业新材料(广东)有限公司 | Cleaning-free antirust material capable of being stripped or cleaned by heating as well as preparation and application thereof |
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- 2022-11-21 CN CN202211455974.XA patent/CN115851069A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305317A (en) * | 2012-03-09 | 2013-09-18 | 中国石油天然气股份有限公司 | Metal antirust compound containing oil-soluble polyaniline and application thereof |
| CN104845701A (en) * | 2014-02-14 | 2015-08-19 | 吉坤日矿日石能源株式会社 | Rust-proof oil composition |
| CN104450045A (en) * | 2014-11-10 | 2015-03-25 | 安徽威萨重工机械有限公司 | Anti-corrosive grease type rustproof oil and preparation method thereof |
| CN111253815A (en) * | 2020-02-17 | 2020-06-09 | 丫肯(上海)新材料科技有限公司 | Antirust agent and preparation method thereof |
| CN113845809A (en) * | 2021-10-10 | 2021-12-28 | 山立欣业新材料(广东)有限公司 | Cleaning-free antirust material capable of being stripped or cleaned by heating as well as preparation and application thereof |
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