Manufacturing method of gallium nitride laser

During the preparation process of gallium nitride laser, vacuum annealing and real-time stress monitoring technology are used to solve the problem of structural deterioration and stress concentration in the annealing and pre-oxidation process, and the high toughness and low stress state of the material are achieved, and the stability and reliability of the product are improved.

CN119627611APending Publication Date: 2025-03-14何舜宇
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Patent Information

Application Number
CN202411650911.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-19
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

During the annealing and preoxidation process, existing gallium nitride lasers are prone to deterioration of the material's crystal structure and stress concentration, increasing brittleness, and it is difficult to effectively monitor and control stress.

Method used

Annealing is carried out using a vacuum annealing furnace, setting the temperature to 750℃, and annealing time is 75 minutes to reduce thermal stress and crystal structure degradation; during the entire annealing and sintering process, temperature and stress changes are monitored in real time, and data is recorded and analyzed through strain gauge and temperature monitoring equipment, and processing conditions are dynamically adjusted.

Benefits of technology

Effectively improve the toughness of the material, reduce thermal stress, avoid structural deterioration and stress concentration, ensure that the stress of the gallium nitride laser is lower during the preparation process, and improve the stability and reliability of the product.

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Abstract

The invention relates to the technical field of lasers, and discloses a manufacturing method of a gallium nitride laser, which comprises the following steps: step 1, preparing and cleaning; step 2, annealing treatment; step 3, real-time monitoring; step 4, pre-oxidation treatment; step 5, assembling; and step 6, sintering. In the second step, the vacuum environment of-103 Pa is adopted for annealing, so that the influence of oxidation and other gases is reduced, the thermal stress is reduced, the degradation of a crystal structure is prevented, the temperature is set to be 750 DEG C, the annealing time is 75 minutes, the toughness of the material can be effectively improved, meanwhile, the crystal structure of the material is prevented from being damaged due to too high temperature, and the service life of the material is prolonged. And by adopting staged heating, the structural deterioration caused by too high temperature or non-uniform heating is avoided, and the beneficial effect that the annealing and pre-oxidation temperature for preparing the gallium nitride laser is proper and does not cause the structural deterioration is achieved.
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Description

Technical Field

[0001] The present invention relates to the technical field of lasers, and in particular to a method for manufacturing a gallium nitride laser. Background Art

[0002] With the continuous development of the optical field, laser devices are also developing in the direction of miniaturization and high power, and the heat dissipation requirements for the package tube shell are also greatly improved. Especially for laser devices, a large amount of heat is generated when they are working. The greater the power, the more obvious the thermal effect. Gallium nitride laser is a semiconductor laser, also known as a laser diode.

[0003] Prior art CN 117175346 A is a gallium nitride laser and its processing technology. The heat dissipation structure of the laser produced by the processing technology can efficiently and quickly dissipate heat from the electronic components, and the internal heat dissipation component in the heat dissipation structure can also fix the electronic components, while the external heat dissipation component can wrap the electronic components, which not only plays a role in heat dissipation but also provides excellent protection effect.

[0004] Although annealing and pre-oxidation help improve the grain boundary structure, excessive heat treatment caused by the annealing temperature of 850°C and the pre-oxidation of 500-550°C will lead to the degradation of the material's crystal structure. At the same time, the difference in thermal expansion coefficients between Kovar alloy and glass materials will also cause stress concentration at the joint and increase brittleness. This requires real-time stress monitoring to avoid brittle cracking of the laser due to excessive stress. Summary of the invention

[0005] Technical issues solved:

[0006] In view of the shortcomings of the prior art, the present invention provides a method for manufacturing a gallium nitride laser, which has the advantages of suitable annealing and pre-oxidation temperature for preparing the gallium nitride laser without causing structural degradation, and real-time monitoring of various data in the gallium nitride laser preparation process to reduce stress, thereby solving the problems of the above-mentioned technologies. Technical solution:

[0007] To achieve the above object, the present invention provides the following technical solution: a method for manufacturing a gallium nitride laser, comprising the following steps:

[0008] Step 1, preparation and cleaning: reserve a hole for installing the insulator on the base, install the PIN pin and the insulator in the hole, and ensure a firm bond through high-temperature sintering, plate gold on the surface of the substrate to form a gold-plated layer, weld the gallium nitride chip on the substrate, perform metal patterning on the surface of the substrate to replace the current and electrical signal transmission of the gold wire, add a glass blank at the joint between the tube shell and the heat dissipation window, seal and fix them through high-temperature sintering, fix the tube shell on the base, put it in an ultrasonic cleaner, use 13.5mol / L acetone to clean it for 10-15 minutes, and then use 97% alcohol to clean it for 10-15 minutes until there is no impurity on the surface;

[0009] Step 2: Annealing: Place the cleaned PIN pins and tube shell into a high-purity graphite container and place it in a vacuum annealing furnace in a vacuum environment with the temperature set to 750°C to reduce the generation of thermal stress and the degradation of the crystal structure, and shorten the annealing time to 60-90 minutes to improve the toughness of the material;

[0010] Step 3: Real-time monitoring: During the entire annealing and sintering process, record the temperature change every minute, use strain gauges to monitor the changes in the internal stress of the material, transmit the temperature and stress monitoring data to the control center in real time, and use data analysis tools to monitor abnormal conditions during the process;

[0011] Step 4: Pre-oxidation treatment: Place the annealed sintered part into a tube furnace, introduce dry nitrogen at a flow rate of 3.5L / min, heat the PIN pins to 400-450°C, keep for 15-20 minutes, heat the base and tube shell to 500-550°C, keep for 20-25 minutes, to form a dense oxide layer and enhance the anti-oxidation performance;

[0012] Step 5: Assembling: Assembling the pre-oxidized sintered parts through a graphite jig;

[0013] Step 6, sintering: put the assembled parts into a tubular furnace, introduce nitrogen and hydrogen mixed gas, the ratio of nitrogen to hydrogen is 3.5:0.3, the flow rate is 5L / min, the initial heating is 80-85 minutes, heating from room temperature to 750-800℃; the secondary heating is 25-30 minutes, rising to 900-950℃; keeping warm for 25-30 minutes, then cooling to 500-550℃, 55-60 minutes, and then keeping warm for 60-65 minutes; finally, cooling to room temperature.

[0014] Preferably, the vacuum environment in the vacuum annealing furnace in step 2 is -103 Pa, and the annealing time in step 2 is 75 minutes.

[0015] Preferably, the temperature change record expression in step 3 is:

[0016]

[0017] Where: T(t) is the temperature at time t;

[0018] k T is the temperature variation coefficient, which reflects the sensitivity of the material to temperature changes;

[0019] T0 is the initial temperature;

[0020] R T (t') is the temperature change rate function, which describes the temperature change rate during the heating process. Preferably, the stress change monitoring expression in step 3 is:

[0021]

[0022] Where: σ(t) is the stress at time t;

[0023] k σ is the stress variation coefficient, which reflects the material’s sensitivity to stress changes;

[0024] Δσ(t) is the stress change due to external factors: load change;

[0025] σ0 is the initial stress;

[0026] R σ (t′) is the stress change rate function, which describes the change of stress at different time points;

[0027] dt′ is the integral of the time variable t′.

[0028] Preferably, the stress-temperature relationship expression in step 3 is:

[0029] σ(t)=E·(∈(t)+α·(T(t)-T0))

[0030] Where: E is Young's modulus, which represents the stiffness of the material;

[0031] α is the coefficient of thermal expansion, which describes the volume change of the material due to temperature change;

[0032] T0 is the initial temperature.

[0033] Preferably, the abnormal situation monitoring expression in step 3 is:

[0034]

[0035] Where: T 设定 is the set target temperature;

[0036] ∈ T is the allowable deviation of temperature.

[0037] Preferably, the expression for detecting data transmission in step 3 is:

[0038] D(t)=f(T(t),σ(t))

[0039] Where: D(t) is the monitoring data at time t.

[0040] Preferably, the real-time data update expression in step 3 is:

[0041] D 实时 (t) = D 实时 (t-1)+ΔD(t)

[0042] Where: D 实时 (t) is the real-time monitoring data at time t;

[0043] ΔD(t) is the change in temperature and stress at time t.

[0044] Preferably, the gas flow rate expression in step 6 is:

[0045] Q=5L / min

[0046] Where: Q is the gas flow rate;

[0047] The expression of the initial heating process is:

[0048] t1=80 to 85min,T1=750 to 800℃

[0049] Where: t1 is the initial heating time;

[0050] T1 is the initial heating temperature.

[0051] Preferably, the secondary heating process in step 6 is expressed as

[0052] t2=25 to 30min,T2=900 to 950℃

[0053] Where: t2 is the initial heating time;

[0054] T2 is the initial heating temperature.

[0055] Compared with the prior art, the present invention provides a method for manufacturing a gallium nitride laser, which has the following beneficial effects:

[0056] 1. In the present invention, in step 2, a vacuum environment of -103Pa is used for annealing, which helps to reduce the influence of oxidation and other gases, reduce thermal stress, and prevent degradation of the crystal structure. The temperature is set to 750°C and the annealing time is 75 minutes, which can effectively improve the toughness of the material and prevent the crystal structure of the material from being damaged due to excessive temperature. Staged heating is adopted to control the heating rate to reduce the influence of thermal shock on the material and ensure uniform release of internal stress of the material. A dense oxide layer is formed by heating the PIN pin to 400-450°C and the base and the tube shell to 500-550°C. This oxide layer not only enhances the antioxidant performance, but also provides additional protection to prevent the material from being damaged during subsequent processing. The state of the material is recorded in real time through strain gauges and temperature monitoring, so that abnormal conditions in the processing process can be discovered and adjusted in time to avoid structural degradation caused by excessive temperature or uneven heating, thereby achieving the beneficial effect of preparing gallium nitride lasers with appropriate annealing and pre-oxidation temperatures without causing structural degradation.

[0057] 2. The present invention records the temperature change regularly once per minute in step three, so as to timely grasp the dynamic change of temperature and prevent stress accumulation caused by excessive temperature fluctuations. The strain gauge is used to monitor the change of internal stress of the material, and the stress state can be fed back in real time, so as to facilitate timely adjustment of processing parameters when abnormalities occur to avoid excessive stress. The real-time data is transmitted to the control center, and the abnormal situation is monitored by data analysis tools, so that potential problems can be identified at an early stage, and corresponding adjustments can be made to reduce unnecessary stress accumulation. The stress change monitoring expression σ(t) is used, combined with the stress change coefficient of the material, so that the stress state of the material during annealing and sintering can be more accurately predicted and controlled. Through the real-time monitoring data, the heating rate, holding time and other processing conditions can be dynamically adjusted to ensure that the material is always in a safe temperature range during the processing process, reduce thermal stress, and achieve the beneficial effect of real-time monitoring of various data in the gallium nitride laser preparation process to reduce its stress. BRIEF DESCRIPTION OF THE DRAWINGS

[0058] Figure 1 It is a schematic diagram of the steps of the present invention; DETAILED DESCRIPTION

[0059] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0060] See also Figure 1, a method for manufacturing a gallium nitride laser, comprising the following steps:

[0061] Step 1, preparation and cleaning: reserve a hole for installing the insulator on the base, install the PIN pin and the insulator in the hole, and ensure a firm bond through high-temperature sintering, plate gold on the surface of the substrate to form a gold-plated layer, weld the gallium nitride chip on the substrate, perform metal patterning on the surface of the substrate to replace the current and electrical signal transmission of the gold wire, add a glass blank at the joint between the tube shell and the heat dissipation window, seal and fix them through high-temperature sintering, fix the tube shell on the base, put it in an ultrasonic cleaner, use 13.5mol / L acetone to clean it for 10-15 minutes, and then use 97% alcohol to clean it for 10-15 minutes until there is no impurity on the surface;

[0062] Step 2: Place the cleaned PIN pins and tube shell into a high-purity graphite container and place it in a vacuum annealing furnace in a vacuum environment with the temperature set to 750°C to reduce the generation of thermal stress, reduce the degradation of the crystal structure, and shorten the annealing time to 60-90 minutes to improve the toughness of the material;

[0063] Step 3: Real-time monitoring: During the entire annealing and sintering process, record the temperature change every minute, use strain gauges to monitor the changes in the internal stress of the material, transmit the temperature and stress monitoring data to the control center in real time, and use data analysis tools to monitor abnormal conditions during the process;

[0064] Step 4: Pre-oxidation treatment: Place the annealed sintered part into a tube furnace, introduce dry nitrogen at a flow rate of 3.5L / min, heat the PIN pins to 400-450°C, keep for 15-20 minutes, heat the base and tube shell to 500-550°C, keep for 20-25 minutes, to form a dense oxide layer and enhance the anti-oxidation performance;

[0065] Step 5: Assembling: Assembling the pre-oxidized sintered parts through a graphite jig;

[0066] Step 6, sintering: put the assembled parts into a tubular furnace, introduce nitrogen and hydrogen mixed gas, the ratio of nitrogen to hydrogen is 3.5:0.3, the flow rate is 5L / min, the initial heating is 80-85 minutes, heating from room temperature to 750-800℃; the secondary heating is 25-30 minutes, rising to 900-950℃; keeping warm for 25-30 minutes, then cooling to 500-550℃, 55-60 minutes, and then keeping warm for 60-65 minutes; finally, cooling to room temperature.

[0067] In step 2, annealing is performed in a vacuum environment of -103 Pa, which helps to reduce the effects of oxidation and other gases, reduce thermal stress, and prevent degradation of the crystal structure.

[0068] Setting the temperature to 750°C and the annealing time to 75 minutes can effectively improve the toughness of the material while preventing excessive temperature from causing damage to the crystal structure of the material.

[0069] In step six, staged heating (primary and secondary heating) is adopted. By controlling the heating rate, the impact of thermal shock on the material can be reduced and the internal stress of the material can be ensured to be released evenly.

[0070] In step 4, a dense oxide layer is formed by heating the PIN pin to 400-450°C and the base and tube shell to 500-550°C. This oxide layer not only enhances the anti-oxidation performance, but also provides additional protection to prevent the material from being damaged during subsequent processing.

[0071] In step three, the state of the material is recorded in real time through strain gauges and temperature monitoring, which can promptly detect and adjust abnormal conditions during the processing process to avoid structural degradation caused by excessive temperature or uneven heating.

[0072] Specifically, the vacuum environment in the vacuum annealing furnace in step 2 is -103 Pa, and the annealing time in step 2 is 75 minutes.

[0073] Specifically, the temperature change record expression in step 3 is:

[0074]

[0075] Where: T(t) is the temperature at time t;

[0076] k T is the temperature variation coefficient, which reflects the sensitivity of the material to temperature changes;

[0077] T0 is the initial temperature;

[0078] R T (t′) is the temperature change rate function, which describes the rate of temperature change during the heating process.

[0079] Specifically, the stress change monitoring expression in step 3 is:

[0080]

[0081] Where: σ(t) is the stress at time t;

[0082] k σ is the stress variation coefficient, which reflects the material’s sensitivity to stress changes;

[0083] Δσ(t) is the stress change due to external factors: load change;

[0084] σ0 is the initial stress;

[0085] R σ (t′) is the stress change rate function, which describes the change of stress at different time points;

[0086] dt′ is the integral of the time variable t′.

[0087] Specifically, the stress-temperature relationship expression in step 3 is:

[0088] σ(t)=E·(∈(t)+α·(T(t)-T0))

[0089] Where: E is Young's modulus, which represents the stiffness of the material;

[0090] α is the coefficient of thermal expansion, which describes the volume change of the material due to temperature change;

[0091] T0 is the initial temperature.

[0092] Specifically, the abnormal situation monitoring expression in step 3 is:

[0093]

[0094] Where: T 设定 is the set target temperature;

[0095] ∈ T is the allowable deviation of temperature.

[0096] Specifically, the expression for detecting data transmission in step 3 is:

[0097] D(t)=f(T(t),σ(t))

[0098] Where: D(t) is the monitoring data at time t.

[0099] Specifically, the real-time data update expression in step 3 is:

[0100] D 实时 (t) = D 实时 (t-1)+ΔD(t)

[0101] Where: D 实时 (t) is the real-time monitoring data at time t;

[0102] ΔD(t) is the change in temperature and stress at time t.

[0103] By using the stress change monitoring expression σ(t) combined with the material's stress change coefficient, the stress state of the material during annealing and sintering can be more accurately predicted and controlled.

[0104] Through real-time monitoring data, the heating rate, holding time and other processing conditions can be dynamically adjusted to ensure that the material is always within a safe temperature range during the processing process, reducing thermal stress

[0105] Specifically, the gas flow expression in step 6 is:

[0106] Q=5L / min

[0107] Where: Q is the gas flow rate;

[0108] The expression of the initial heating process is:

[0109] t1=80 to 85min,T1=750 to 800℃

[0110] Where: t1 is the initial heating time;

[0111] T1 is the initial heating temperature.

[0112] Specifically, the expression of the secondary heating process in step 6 is:

[0113] t2=25 to 30min,T2=900 to 950℃

[0114] Where: t2 is the initial heating time;

[0115] T2 is the initial heating temperature.

[0116] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations may be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for manufacturing a gallium nitride laser, characterized in that: The following steps are involved: Step 1, preparation and cleaning: reserve a hole for installing the insulator on the base, install the PIN pin and the insulator in the hole, and ensure a firm bond through high-temperature sintering, plate gold on the surface of the substrate to form a gold-plated layer, weld the gallium nitride chip on the substrate, perform metal patterning on the surface of the substrate to replace the current and electrical signal transmission of the gold wire, add a glass blank at the joint between the tube shell and the heat dissipation window, seal and fix them through high-temperature sintering, fix the tube shell on the base, put it in an ultrasonic cleaner, use 13.5mol / L acetone to clean it for 10-15 minutes, and then use 97% alcohol to clean it for 10-15 minutes until there is no impurity on the surface; Step 2: Annealing: Place the cleaned PIN pins and tube shell into a high-purity graphite container and place it in a vacuum annealing furnace in a vacuum environment with the temperature set to 750°C to reduce the generation of thermal stress and the degradation of the crystal structure, and shorten the annealing time to 60-90 minutes to improve the toughness of the material; Step 3: Real-time monitoring: During the entire annealing and sintering process, record the temperature change every minute, use strain gauges to monitor the changes in the internal stress of the material, transmit the temperature and stress monitoring data to the control center in real time, and use data analysis tools to monitor abnormal conditions during the process; Step 4: Pre-oxidation treatment: Place the annealed sintered part into a tube furnace, introduce dry nitrogen at a flow rate of 3.5L / min, heat the PIN pins to 400-450°C, keep for 15-20 minutes, heat the base and tube shell to 500-550°C, keep for 20-25 minutes, to form a dense oxide layer and enhance the anti-oxidation performance; Step 5: Assembling: Assembling the pre-oxidized sintered parts through a graphite jig; Step 6, sintering: put the assembled parts into a tubular furnace, pass nitrogen and hydrogen mixed gas, the ratio of nitrogen to hydrogen is 3.5:0.3, the flow rate is 5L / min, the initial heating is 80-85 minutes, heating from room temperature to 750-800°C; the secondary heating is 25-30 minutes, rising to 900-950°C; keep warm for 25-30 minutes, then cool down to 500-550°C, 55-60 minutes, and keep warm for 60-65 minutes; finally, cool down to room temperature.

2. The method for manufacturing a gallium nitride laser according to claim 1, characterized in that: The vacuum environment in the vacuum annealing furnace in step 2 is -103 Pa, and the annealing time in step 2 is 75 minutes.

3. The method for manufacturing a gallium nitride laser according to claim 1, characterized in that: The temperature change record expression in step 3 is: Where: T(t) is the temperature at time t; k T is the temperature variation coefficient, which reflects the sensitivity of the material to temperature changes; T0 is the initial temperature; R T (t') is the temperature change rate function, which describes the rate of temperature change during the heating process.

4. The method for manufacturing a gallium nitride laser according to claim 3, characterized in that: The stress change monitoring expression in step 3 is: Where: σ(t) is the stress at time t; k σ is the stress variation coefficient, which reflects the sensitivity of the material to stress changes; Δσ(t) is the stress change due to external factors: load change; σ0 is the initial stress; R σ (t') is the stress change rate function, which describes the change of stress at different time points; dt' is the integral of the time variable t'.

5. The method for manufacturing a gallium nitride laser according to claim 4, characterized in that: The stress-temperature relationship expression in step 3 is: σ(t)=E·(∈(T)+α·(T(t)-T0)) Where: E is Young's modulus, which represents the stiffness of the material; α is the coefficient of thermal expansion, which describes the volume change of the material due to temperature change; T0 is the initial temperature.

6. The method for manufacturing a gallium nitride laser according to claim 5, characterized in that: The abnormal situation monitoring expression in step 3 is: Where: T 设定 is the set target temperature; ∈ T is the allowable deviation of temperature.

7. The method for manufacturing a gallium nitride laser according to claim 6, characterized in that: The expression for detecting data transmission in step 3 is: D(t)=f(T(t),σ(t)) Where: D(t) is the monitoring data at time t.

8. The method for manufacturing a gallium nitride laser according to claim 7, characterized in that: The real-time data update expression in step 3 is: D 实时 (t)=D 实时 (t-1)+ΔD(t) Where: D 实时 (t) is the real-time monitoring data at time t; ΔD(t) is the change in temperature and stress at time t.

9. The method for manufacturing a gallium nitride laser according to claim 8, characterized in that: The gas flow rate expression in step 6 is: Q=5L / min Where: Q is the gas flow rate; The expression of the initial heating process is: t1=80to 85min,T1=750to 800°C Where: t1 is the initial heating time; T1 is the initial heating temperature.

10. The method for manufacturing a gallium nitride laser according to claim 9, characterized in that: The secondary heating process in step 6 is expressed as t2 = 25 to 30 min, T2 = 900 to 950 ° C Where: t2 is the initial heating time; T2 is the initial heating temperature.

Citation Information

Patent Citations

  • Gallium nitride laser and processing technology thereof

    CN117175346A